Complaint - Berry v. Intertape

UNITED STATES DISTRICT COURT
SOUTHERN DISTRICT OF INDIANA
EVANSVILLE DIVISION
BERRY PLASTICS CORPORATION,
Plaintiff,
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INTERTAPE POLYMER CORPORATION,
Defendant.
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JURY TRIAL DEMANDED
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COMPLAINT FOR DECLARATORY JUDGMENT
Plaintiff Berry Plastics Corporation, by and through its attorneys, for its Complaint
against Defendant, alleges as follows:
1. This is an action for declaratory judgment pursuant to 28 U.S.C. § 2201 that
Defendant's U.S. Patent No. 7,476,416 is invalid and unenforceable under the patent laws of the
United States, Title 35, United States Code.
PARTIES
2. Plaintiff, Berry Plastics Corporation is a corporation organized and existing under
the laws of the State of Delaware, having its principal place of business at 101 Oakley Street,
Evansville, Indiana 47710. Except where otherwise noted, Berry Plastics Corporation is referred
to herein as "Berry Plastics."
3. Defendant, Intertape Polymer Corporation is a corporation organized and existing
under the laws of the State of Delaware, having its principal place of business at 3647 Cortez
Road West, Bradenton, Florida 34210. Except where otherwise noted, Intertape Polymer
Case 3:10-cv-00076-RLY-WGH Document 1 Filed 05/13/10 Page 1 of 10
Corporation is referred to herein as "Intertape."
JURISDICTION AND VENUE
4. This is an action for a declaratory judgment pursuant to 28 U.S.C. § 2201, for the
purpose of determining a case of actual controversy between the parties, as hereinafter more
fully appears. Jurisdiction is proper pursuant to 28 U.S.C. §§ 1331, 1338(a), and 2201. Venue is
proper in this district pursuant to 28 U.S.C. § 1391.
BACKGROUND
5. Intertape is the listed assignee of U.S. Pat. No. 7,476,416 (the '''416 patent"),
issued January 13,2009.
6. Intertape is engaged in the business of manufacturing, distributing, and selling a
variety of tapes including adhesive tapes.
7. Berry Plastics is engaged in the business of manufacturing and selling a variety
of products including plastic packaging, thermoformed products, flexible films, tapes (including
adhesive tapes) and coatings and directly competes with Intertape.
8. Intertape, through its attorneys, sent a notice letter dated November 12, 2009
(hereinafter "the Letter") to Berry Plastics asserting ownership of U.S. Pat. No. 7,476,416 and
related published U.S. patent application Nos. US20070196572, US20070173622,
US20080058483, and US20090048407. A copy of the Letter is attached hereto as Exhibit A. The
Letter required Berry Plastics to take actions to avoid infringing Intertape's patent rights. The
Letter also requested a visit by Intertape to Berry Plastics' plant prior to commercial production
to ensure Intertape's patent rights are not violated. The '416 patent claims, inter alia, a process
for preparing an adhesive including a step whereby primary raw materials are mixed in a
compounding section of a planetary roller extruder with at least one spindle that is a double
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transversal mixing spindle with a plurality of back-cut helical flights.
9. Berry Plastics has taken substantial steps in meaningful preparation for the
manufacture and sale of adhesive tapes including substantial capital investment at one of its
manufacturing plants for commercial production and sale of adhesive tapes.
10. Berry Plastics has purchased from Entex Rust & Mitschke GmbH (hereinafter
"Entex") a planetary roller extruder having a double transversal mixing spindle with back cut
helical flights for the purpose of manufacturing and selling adhesive for tapes.
11. The planetary roller extruder that Berry Plastics purchased from Entex has been
installed in Berry Plastics' Franklin, Kentucky facility and is currently capable of producing
adhesive for tapes.
12. Since at least May 3, 2010, Berry Plastics has been using the planetary roller
extruder purchased from Entex to test and make adhesive for tapes.
13. Berry Plastics intends to be manufacturing and offering for sale tapes made with
adhesive using the planetary roller extruder purchased from Entex by June 1,2010.
14. By letter to Intertape's counsel dated January 22,2010, Berry Plastics requested a
covenant not to sue from Intertape with respect to any use of the Entex planetary roller extruder
and any product made using that machinery. True and correct copies of that letter and the
requested covenant not to sue are attached as Exhibits B and C. Intertape has advised through its
counsel that it will not provide the requested covenant not to sue. Its counsel responded to
Exhibits Band C with a letter dated March 4, 2010 stating that they "believe strongly that our
client's patent is both valid and enforceable" and stating Intertape was "willing to resolve this
matter by licensing Berry's production of duct tape under the '416 patent." A true and correct
copy of that letter is attached as Exhibit D.
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COUNT 1- UNENFORCEABILITY
15. Plaintiff Berry Plastics incorporates each of the preceding paragraphs 1-14 as if
fully set forth herein.
16. Entex was an exhibitor at the National Plastics Expo, June 2003, Chicago, IL.
(hereinafter "the Expo 2003").
17. Entex displayed extruder equipment and distributed brochures describing
planetary extruders with double transversal mixing spindles with back cut helical flights at the
Expo 2003. The brochures indicated that the planetary extruder having double transversal mixing
spindles with back cut helical flights could be used to extrude rubber, a non-thermoplastic
material to form an adhesive.
18. Two employees of Intertape, Mr. David Kovach and Mr. Thomas Lombardo, both
named inventors on the' 416 patent, were present at the Expo 2003.
19. Mr. Kovach and Mr. Thomas Lombardo visited Entex's exhibitor booth, where
brochures describing the planetary extruder having double transversal mixing spindles with back
cut helical flights were provided to them. A true and correct copy of the Entex brochure is
attached hereto as Exhibit E.
20. The process of using the planetary extruder to extrude non-thermoplastic
materials to form adhesive was explained to Mr. Kovach and Mr. Lombardo by Entex personnel
at the Expo 2003.
21. On November 24, 2003, Intertape, through its counsel Mark P. Levy at Thomson
Hine LLP, filed a provisional patent application titled "Process for preparing adhesive using
planetary extruder" that was assigned U.S. Ser. No. 60/524,505 (herein after "the Provisional
Application"). A true and correct copy of the Provisional Application is attached hereto as
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Exhibit F.
22. Figure 1 of the Provisional Application is identical to the image of the double
transversal mixing spindle with back cut helical flights of the Entex brochure that was provided
to Mr. Kovach and Mr. Lombardo ofIntertape by Entex at the Expo 2003.
23. The Provisional Application lists John Kinch Tynan, Jr., Richard Walter St.
Coeur, David Michael Kovach, and Thomas Lombardo as inventors.
24. Intertape and one or more of the listed inventors John Kinch Tynan, Jr., Richard
Walter St. Coeur, David Michael Kovach, and Thomas Lombardo, had knowledge of the Entex
brochure that was publicly displayed at the Expo 2003 during the preparation and filing of the
provisional application that included Figure 1.
25. On November 24, 2004, Intertape filed a non-provisional application titled
"Process for preparing adhesive using planetary extruder." The non-provisional application was
assigned U.S. Ser. No. 10/997,827 (hereinafter "the '827 application"). The '827 application
claimed priority to the Provisional Application.
26. The '827 application lists John Kinch Tynan, Jr., Richard Walter St. Coeur, David
Michael Kovach, and Thomas Lombardo as inventors.
27. On April 14, 2005 applicants filed executed declarations from the listed inventors
acknowledging their duty to disclose information that is material to patentability and their
knowledge of the priority benefit of the provisional application.
28. One or more of the listed inventors John Kinch Tynan, Jr., Richard Walter St.
Coeur, David Michael Kovach, and Thomas Lombardo and/or their counsel had knowledge of
Figure 1 of the Provisional Application, which is identical to the image of the double transversal
mixing spindle with back cut helical flights of the Entex brochure provided to inventors Mr.
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David Kovach and Mr. Tom Lombardo by Entex at the Expo 2003.
29. Intertape prosecuted the '827 application before the United States Patent &
Trademark Office ("USPTO") and the '827 application issued as the '416 patent.
30. Intertape filed five separate Information Disclosure Statements on August 22,
2005; September 16, 2005; January 13, 2006; May 9, 2007; and October 4, 2007 during the
prosecution of the' 827 application.
31. Entex's public presentation of the planetary extruder for use with non-
thermoplastic materials and the Entex brochure provided to Intertape at the Expo 2003 were
material to the patentability of one or more claims of the '416 patent, because they teach and/or
render obvious the claimed invention relating to the use of a planetary extruder having double
transversal mixing spindles with back cut helical flights to process non-thermoplastic material to
form an adhesive, and the examiner would have relied on this information to reject the presently
patented claims.
32. The listed inventors of the '827 application and/or the prosecuting counsel did not
disclose the material information regarding Entex's public presentation of the extruder for use
with non-thermoplastic material to form an adhesive and the Entex brochure provided at the
Expo 2003 in any of the Information Disclosure Statements filed by Intertape, and did not
apprise the examiner of the material information for determining patentability of the then
pending claims.
33. The '416 patent specification states that double transversal spindles are
commercially available from Entex. Col. 4, lines 50-2 of the '416 patent. The listed inventors
John Kinch Tynan, Jr., Richard Walter St. Coeur, David Michael Kovach, and Thomas
Lombardo and/or the counsel of record had knowledge of the statement with respect to Entex in
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the specification of the '416 patent, but failed to disclose the information in an information
disclosure statement to the examiner.
34. The listed inventors of the '416 patent and/or the prosecuting counsel
intentionally withheld material information regarding Entex's public presentation of the
planetary extruder for use with non-thermoplastic materials to form an adhesive and the Entex
brochure at the Expo 2003, which were prior to the earliest claimed priority date of the '416
patent.
35. The applicants committed inequitable conduct before the USPTO during the
prosecution of the' 416 patent by intentionally failing to disclose material information regarding
Expo 2003 to the USPTO and the information provided by Entex relating to processing of non­
thermoplastic material with the intent to mislead the USPTO.
36. Prior to the filing date of the priority Provisional Application of November 24,
2003, Entex recommended to Intertape the use of a planetary extruder having double transversal
mixing spindles with back cut helical flights for processing non-thermoplastic materials to form
an adhesive. Entex also provided Intertape with documents illustrating the planetary extruder
having double transversal mixing spindles with back cut helical flights and provided photographs
of the same. Intertape was aware that the claimed invention of the '416 patent was originally
provided by Entex to Intertape prior to the filing date of the Provisional Application.
37. Intertape intentionally failed to disclose to the USPTO the material information
that Entex provided to Intertape regarding the claimed use of a planetary extruder having double
transversal mixing spindles with back cut helical flights for processing a non-thermoplastic
material into an adhesive with the intent to mislead the USPTO.
38. The '416 patent is unenforceable because Intertape committed inequitable
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conduct to obtain the '416 patent by intentionally failing to disclose material information that
showed that Intertape did not invent the claimed invention of the '416 patent and that Entex
provided the claimed invention to Intertape.
39. The '416 patent and any subsequent related applications are unenforceable
because Intertape committed inequitable conduct by listing Intertape personnel as inventors who
are not the actual inventors and excluded Entex personnel as inventors with deceptive intent to
obtain the' 416 patent.
40. Berry Plastics will be substantially and irreparably damaged if Defendant
Intertape is permitted to assert patent rights based on the unenforceable' 416 patent or any of its
subsequent related patent applications and thereby prevent Berry Plastics from manufacturing
and selling in the immediate future adhesive for tapes using the Entex planetary roller extruder
now installed in its Franklin, Kentucky plant.
COUNT II - PATENT INVALIDITY
41. Berry Plastics incorporates each of the preceding paragraphs 1-40 as if fully set
forth herein.
42. The United States Patent No. 7,476,416 ("the '416 patent"), entitled "Process for
preparing adhesive using planetary extruder" lists 2 independent claims and 32 dependent
claims. A true and correct copy of the' 416 patent is attached hereto as Exhibit G.
43. One or more claims of the' 416 patent are invalid for failing to satisfy the written
description and/or definiteness and/or enablement and/or best mode requirements of 35 U.S.C. §
112.
44. One or more claims of the' 416 patent are invalid as being anticipated under 35
U.S.C. § 102.
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45. One or more claims of the '416 patent are invalid under 35 U.S.C. § 102(±)
because applicants themselves did not invent the subject matter sought to be patented and
derived the invention from Entex.
46. One or more claims of the ' 416 patent are invalid as being invalid under 35
U.S.C. § 101.
47. One or more claims of the '416 patent are invalid under 35 U.S.c. § 256 because
the applicants, with deceptive intent, omitted inventors, and named persons who are not
inventors.
48. One or more claims of the '416 patent are invalid for being obvious under 35
U.S.c. § 103.
49. Berry Plastics will be substantially and irreparably damaged if Defendant
Intertape is permitted to enforce the '416 patent or any of its subsequent related patent
applications and thereby prevent Berry Plastics from manufacturing and selling in the immediate
future adhesive for tapes using the planetary roller extruder now installed in its Franklin,
Kentucky plant.
PRAYER FOR RELIEF
WHEREFORE, Plaintiff requests the following relief individually, cumulatively and/or
alternatively:
(a) A judgment ordering that the' 416 patent and any of its subsequent related
patent applications are unenforceable due to inequitable conduct at the patent office;
(b) A judgment that one or more of Entex personnel are the sole inventors of
the' 416 patent;
(c) A judgment that one or more of Entex personnel are co-inventors of the
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Case 3:10-cv-00076-RLY-WGH Document 1 Filed 05/13/10 Page 9 of 10
'416 patent;
(d) A judgment that the' 416 patent is invalid under 35 U.S.C §§101, 102, 103
and/or 112;
(e) A declaration that Berry Plastics may use the planetary roller extruder in
its Franklin, Kentucky plant free and clear of the '416 patent and any of its subsequent related
patent applications;
(f) A declaration that this is an exceptional case and an award of attorneys'
fees pursuant to 35 U.S.C. § 285;
(g) An award of Plaintiff's costs and expenses in this action; and
(h) Such further and other relief as this Court may deem just and proper.
Respectfully submitted,
Dated: { V 1 ~ 1 ( ~ Lot o
James D.r.fuhnson,
RUDoLPH, FI
221 N. W. Fifth treet
Attorney #11984-49
, PORTER & JOHNSON, LLP
P.O. Box 1507
Evansville, Indiana 47708
Telephone: (812) 422-9444
Facsimile: (812) 421-7459
E-Mail: [email protected]
Daniel P. Albers
Jonathan P. Froemel
Mark 1. Nahnsen
BARNES & THORNBURG LLP
One North Wacker Dr., Suite 4400
Chicago, Illinois 60606
Telephone: (312) 357-1313
Facsimile: (312) 759-5646
Attorneys for PlaintiffBerry Plastics Corporation
CHDSO] 599062v]
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EXHIBIT A
Case 3:10-cv-00076-RLY-WGH Document 1-1 Filed 05/13/10 Page 1 of 3
TO:317 231 7433
NOV-16-2009 09: 36 FRO!"!:
COLUMBUS NEW VOR.K
ArLANTA CINCINNATI
DAYTON WASH INGTON. D.C.
CLEVIl.ANI)
November 12, 2009
VI;\. FEDERAL EXPRESS
Mr. Tom Salmon
Berry Plastics Corporation and Subsidiaries
Tapes and Coatings Division Headquarters
25 Forge Parkway
Franklin, MA 02038-313 5
RE: U.S. Patent No. 7,476,4] 6/lntertape Polymer Group
PROCESS FOR PREPARING ADHESIVEUSING PLANETARY EXTRUDER
Our Ref.: 411738-00001
Dear Mr. Salmon:
We represent Intertape Polymer Group. Our client is the owner ofthe following U.S. patent and
published patent applications in the United States:
Patent No./Reference
Inventor(s)
U.S. Patent No. 7,476,416 John K. Tynan, Jr., et al.
U.S. 2007/0196572 John K. Tynan, Jr., et al,
U.S. 2007/0173622 John K. Tynan, Jr., et al,
U.S. 2008/0058483 Mark D. Barbieri, et al.
U.S. 2009/0048407 Mark D. Barbieri, et al.
Our client recently read a press release dated September 30, 2009 in which Berry Plastics announced that
it is making capital improvements, in the amount of $20 Million. to its facility in Franklin, Kentucky,
Intertape is aware that Berry manufactures a number of tape products at its Franklin facility, including
duct tape.
The purpose ofthis letter is to place Berry Plastics Corporation On notice of the foregoing patent and
published applications so that Berry Plastics can take steps to avoid infringing them. Intertape will
revisit this matter with Berry periodically in the future, particularly as Intertape's pending applications
issue. Additionally, before Berry's new facilities begin commercial production, Intertape will need
assur-ances that Berry's processes do not infringe. At that time, Intertape will also want to make
arrangements for its counsel, and possibly an independent coating engineer, to visit the Franklin facility
to verify that lntertape's patented technology is not being used,
Mark.Lovy@ThompwnHim:.com Phone 937.44Hi949 Fax 937.443.6637
sjb 593300.1
THOMPSON HINl; LiP
IofWw. Tbompsonf-line.com
A1i'OI\NEYSAT LAw P.O, Box 8801
Phone 93'.443.6600
Dayton, Ohio 45401-&801
fM:937.443.6635
Case 3:10-cv-00076-RLY-WGH Document 1-1 Filed 05/13/10 Page 2 of 3
NOV-16-2009 09:36 FROM:
TD:317 231 7433
THOMPSO __N:.:.- _
-m
NE
-
Mr. Tom Salmon
November 12,2009
Page 2
We appreciate your cooperation in this regard. We can assure you that Intertape intends to vigorously
enforce its rights in its current and future patents.
Case 3:10-cv-00076-RLY-WGH Document 1-1 Filed 05/13/10 Page 3 of 3
EXHIBIT B
Case 3:10-cv-00076-RLY-WGH Document 1-2 Filed 05/13/10 Page 1 of 4
BARNES &TIIORNBURG lLP
Suite4400
One North Wacker Drive
Chicago, IL60606·2833 U.S.A.
(312)357·13L3
Fax(312) 759·5646
Daniel p..Albers
(312) 214·8311
www.bdaw.com
[email protected]
BY EMAIL AND CERTIFIED U.S. MAIL
RETURN RECEIPT REQUESTED
January 22, 2010
Mark. P. Levy
Thompson Hine LLP
2000 Courthouse· Plaza, N.E.
lOW. Second Street
Dayton, Ohio 45402
Re: U.S. Pat. No. 7,476,416/ Intertape Polymer Group
Our Case No.: 5723-210327
DearMr. Levy:
We represent Berry Plastics Corporation ("Berry Plastics") in its intellectual property
matters. All future correspondence in this matter should be directed to my attention. We received
a copy of your letter to Berry Plastics dated November 12,2009 alleging infringement ofD.S.
Pat. No. 7,476,416 (the '416 patent) and published U.S. applications US20070196572,
US20070173622, U820080058483, and US20090048407 (the Intertape Intellectual Property).
In investigating the matters raised in your letter, we understand that Intertape employees,
including Mr. David Kovach and Mr. Thomas Lombardo, attended the National Plastics Expo in
June 2003 (hereinafter "Expo") in Chicago, where Entex Rust & Mitschke GmbH (hereinafter
"Entex") was an exhibitor. At the Expo, Entex gave a presentation on a planetary extruder
having double transversal mixing spindles with back cut helical flights (the ''Noppenspindel'') for
use with non-thermoplastic materials to form adhesive and distributed brochures to Intertape
describing the same at the Expo. The brochures indicate that such equipment is used with rubber,
a non-thermoplastic materiaL
In addition, Mr. Kovach and Mr. Lombardo from Intertape visited Entex's exhibitor
booth, where brochures describing the Noppenspindel was displayed. We also understand that
Mr. Kovach and Mr. Lombardo were lectured by Entex regarding the use of the planetary
extruder with the Noppenspindel for use with non-thermoplastic materials to form adhesive.
Intertape had knowledge of Entex's public presentation on the planetary extruder using the
Noppenspindel for non-thermoplastic materials. This is the same method that Intertape now
claims it invented as claimed. in the '416 patent. Despite having knowledge of the public display
Indiana
\VashiJljCl(m. D.C.
Case 3:10-cv-00076-RLY-WGH Document 1-2 Filed 05/13/10 Page 2 of 4
MarkP. Levy
Page 2
and other information provided by Entex in June 2003, Intertape filed a provisional application
within five months, in November 2003, using a photocopy of an image of the Noppenspindel
provided by Entex and shown in their brochure, as Figure 1 in the provisional application.
Intertape also filed and prosecuted the corresponding non-provisional application (U.S. Ser. No.
10/997,827) that resulted in the '416 patent. Even though Intertape had knowledge ofEntex's
prior invention, none of the information disclosure statements filed contained any reference to
the 2003 Expo or Entex's public demonstration or publication prior to the filing date of the
provisional application.
In addition, Intertape argued against the alleged non-obviousness of the claimed methods
by stating that a skilled artisan would not consider adding a double transversal planetary spindle
to a planetary extruder for processing non-thermoplastic materials. Yet, the Entex brochure, the
public presentation, and information provided to Mr. Kovack and Mr. Lombardo showed that
non-thermoplastic material (e.g., rubber) was being used with planetary extruders having double
transversal mixing spindles with back cut helical flights by Entex. Despite having knowledge of
the Entex Noppenspindel at the 2003 Expo and brochures describing the same, these false
statements regarding non-obviousness were made by Intertape through its counsel to the USPTO.
Intertape failed to disclose to the USPTa material information regarding Entex's public
presentation of the planetary extruder having the Noppenspindel and the brochures describing the
same that occurred prior to the filing date of the provisional application. Intertape also made
false statements regarding non-obviousness before the USPTa to obtain the '416 patent. The
failure to disclose the material information regarding patentability to the USPTO and false
statements made regarding prior art render the' 416 patent and all of its related applications
invalid and unenforceable. Despite having this knowledge, Intertape now makes frivolous
allegations of infringement that in turn, have needlessly increased the commercial production
and litigation costs for Berry Plastics to defend its right to manufacture.
Prior to the filing of Intertape's provisional application, Entex provided documents to
Intertape and first suggested the use of a planetary extruder having Entex's Noppenspindel for
rubber. Entex also processed Intertape material in its planetary extruders equipped with the
Noppenspindels. Despite this, Intertape excluded Entex personnel, from the '416 patent and
instead named its own employees as inventors. We presume you have seen Entex's letter of
December 28,2009 to Intertape. A copy is also attached. None of this material information
regarding inventorship was disclosed to the USPTO during the prosecution of the '416 patent or
its related subsequent patent applications.
Given the conduct of Intertape, Berry Plastics has filed and we enclose a declaratory
judgment complaint to invalidate and render unenforceable the '416 patent. Please understand
that Berry Plastics will aggressively move for reimbursement ofits litigation expenses, including
attorney's fees, and costs to defend against Intertape's baseless allegations. We have not yet
served the complaint on Intertape, but we will do so unless we can bring this matter to an
expeditious resolution.
In order to resolve this matter, we demand that Intertape agree to a covenant not to sue
Berry Plastics and its customers based on the '416 patent and any related applications or future
BARNES&1HORNBURG llP
Case 3:10-cv-00076-RLY-WGH Document 1-2 Filed 05/13/10 Page 3 of 4
MarkP. Levy
Page 3
related applications, for the use of any machinery Berry Plastics acquires from Entex relating to
extrusion of non-thermoplastic material and any product resulting from the use ofsuch
machinery. A proposed covenant not to sue is enclosed. IfIntertape agrees to such covenant,
Berry Plastics will dismiss its complaint without prejudice. Please advise us within the next two
weeks, before February 5th with respect to Intertape's response regarding the covenant not to
sue.
Very truly yours,
BARNES & THORNBURG LLP
~ -
~ ; ( l b e r
Cc: Jeff Thompson, Esq.
CHDSOI 580640"I
BARNES&1HORNBURG UP
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EXHIBIT C
Case 3:10-cv-00076-RLY-WGH Document 1-3 Filed 05/13/10 Page 1 of 5
COVENANT NOT TO SUE
This Covenant Not to Sue ("Agreement") is made and effective as of the L-) day of
____,2010, by and between Intertape Polymer Corporation (hereinafter "INTERTAPE"),
a corporation organized and existing under the laws ofthe State of Delaware, having its principal
place ofbusiness at 3647 Cortez Road West, Bradenton, Florida 34210, and Berry Plastics
Corporation (hereinafter "BERRY PLASTICS"), a corporation organized and existing under the
laws of the State of Delaware, having its principal place of business at 101 Oakley Street,
Evansville, Indiana 47710.
Whereas INTERTAPE is the listed assignee of issued U.S. Pat. No. 7,476,416 and has
ownership interests in published U.S. applications US20070196572, US20070173622,
US20080058483, and US20090048407 (collectively, hereinafter referred to as "the Intertape
Intellectual Property"); and
Whereas BERRY PLASTICS is planning to manufacture, sell, distribute, and offer to sell
a variety of tapes including adhesive tapes having an adhesive processed by a planetary extruder
having double transversal mixing spindles with back cut helical flights with machinery
purchased from Entex Rust & Mitschke GmbH (hereinafter "Entex");
Whereas INTERTAPE has sent a letter to BERRY PLASTICS putting them on notice of
their rights in the Intertape Intellectual Property including U.S. Pat. No. 7,476,416;
Whereas BERRY PLASTICS has filed a declaratory judgment action (Civil Action Case
No. lO-cv-OOO 14) in the District Court, Southern District ofIndiana (hereinafter "DJ Action") to
inter alia, invalidate and render unenforceable U.S. Pat. No. 7,476,416; and
Case 3:10-cv-00076-RLY-WGH Document 1-3 Filed 05/13/10 Page 2 of 5
Whereas, the parties desire to settle and resolve all controversies and claims relating to
The Intertape Intellectual Property and the DJ Action lawsuit to avoid the burden and expense of
further litigation;
IN CONSIDERATION OF the mutual covenants contained herein, the parties stipulate
and agree as follows:
1. This Agreement is entered into solely for the purpose of avoiding the burden and
expense of further litigation and neither it nor any negotiations leading up to it is intended to be,
or shall be construed as, an admission of fact or liability by either INTERTAPE or BERRY
PLASTICS.
2. INTERTAPE covenants not to sue BERRY PLASTICS or any of its parents,
subsidiaries, affiliates, any of the foregoing's respective past, present or future officers, directors,
shareholders, employees, agents, attorneys, direct or indirect importers, suppliers, manufacturers,
distributors, customers, users or any other parties for the importation, export, manufacture, use,
sale, or offer for sale by BERRY PLASTICS or its subsidiaries or affiliates ofEntex planetary
extruders having double transversal mixing spindles with back cut helical flights and products
manufactured using the same or a substantially similar process or equipment, including but not
limited to any manufacture using machines or know-how provided by Entex for infringement or
on any other theory including direct or indirect infringement, inducement or contribution, under
the Intertape Intellectual Property or any other basis.
3. INTERTAPE also hereby grants BERRY PLASTICS a permanent, fully paid-up,
irrevocable, non-terminable, non-exclusive, worldwide license under the Intertape Intellectual
Property, as well as any patents or patent applications claiming priority therefrom, together with
any divisionals, continuations, continuations-in-part, reissues, reexaminations and foreign
2
Case 3:10-cv-00076-RLY-WGH Document 1-3 Filed 05/13/10 Page 3 of 5
equivalents thereof, to make, have made, import, export, use, sell, and offer for sale. BERRY
PLASTICS' rights hereunder shall be transferable by operation oflaw or in connection with the
sale of any relevant portion of its business or substantially all of the assets of such portion of its
business.
4. BERRY PLASTICS agrees to voluntarily dismiss the DJ Action without prejudice
within ten (l0) business days of the effective date of this Agreement.
5. This Agreement shall benefit and be binding upon the parties, successors and their
respective assigns. INTERTAPE acknowledges and agrees that this covenant not to sue is
extended on behalf of (and extends to) any and all of its affiliates, subsidiaries, and parents and
runs with the title of the Intertape Intellectual Property for any activity, inducement, contribution,
or infringement, direct or indirect, under the Intertape Intellectual Property.
6. This Agreement, including its validity and interpretation, shall be governed by
Indiana Law, and the parties agree that the sole venue for enforcement of this Agreement shall be
the United States District Court for the Southern District of Indiana.
7. This Agreement supersedes and abrogates all former verbal or written agreements
between the parties hereto related to the subject matter hereof, and is the only agreement in
existence between the parties and is not subject to change except by mutual agreement, in writing,
signed by all parties.
8. The parties warrant and represent that each has been represented by counsel of
their choice in connection with the review, approval and execution of this Agreement; that each
has shown this Agreement to its respective attorney who has explained it and advised it that it is
a legally binding contract; that each has read and understood this Agreement; and that each
intends to be bound by each provision of this Agreement.
3
Case 3:10-cv-00076-RLY-WGH Document 1-3 Filed 05/13/10 Page 4 of 5
-------------
-------------
-------------
9. The parties declare and represent that no promise, inducement or agreement
which is not specifically provided in this Agreement has been made by any party to this
Agreement; that this Agreement contains the entire agreement among the parties; and that the
terms of this Agreement cannot be modified except in writing signed by all of the parties.
10. This Agreement maybe executed in counterparts each of which shall constitute an
original.
In witness thereof, the undersigned have executed this Agreement.
Intertape Polymer Corporation
By: _
Date
Name: _
Title:
Berry Plastics Corporation
By:
Date
Name:
Title:
CHDSOl580857vl
4
Case 3:10-cv-00076-RLY-WGH Document 1-3 Filed 05/13/10 Page 5 of 5
EXHIBIT D
Case 3:10-cv-00076-RLY-WGH Document 1-4 Filed 05/13/10 Page 1 of 2
ATLANTA CINCINNATI COLUMBUS NEW YORK
BRUSSElS CLEVELAND DAYTON WASHINGTON. D.C.
THOMPSON
-HINE-----------­
Stephen J. Butler
(513) 352-6587
[email protected]
March 4,2010
Daniel P. Albers, Esq.
Barnes & Thornburg LLP
Suite 4400
One North Wacker Drive
Chicago, Illinois 60606-2833
Re: Berry Plastics Corporation v. Intertape Polymer Corporation
Gentlemen:
We appreciate your cooperation in giving us time review the allegations of Berry
Plastic's complaint with our client. Based on that review, we have concluded that your claims
have no merit.
We have thoroughly investigated the what seems to be the linchpin of your case,
which is the supposed interaction between representatives of Entex and Intertape Polymer
Corporation at the Chicago trade show in June, 2003. We do not know the source of your beliefs
about what happened at that show, but you have the facts wrong. Furthermore, the Entex
document that you attached as an exhibit to the complaint does not teach the invention claimed in
Intertape's '416 patent. We continue to believe strongly that our client's patent is both valid and
enforceable. Our analysis is based in part on Hess v, Advanced Cardiovascular Systems, Inc.,
106 F.3d 976, as well as the heavy burden of proof that your client must meet to prevail.
Nevertheless, Intertape would be willing to resolve this matter by licensing
Berry's production of duct tape under the '416 patent. If Berry is interested in a resolution of this
nature, we would be happy to prepare a draft agreement for your review. If not, we will accept
service on the complaint on behalf of our client.
Stephen J. Butler
SJB/SEB
#76478I-vI
THOMPSON HINE LLP 312 Walnut Street www.ThompsonHine.com
ATTORNEYS AT LAW 14th Floor Phone 513.352.6700
Cincinnati, Ohio 45202-4089 Fax 513.241.4771
Case 3:10-cv-00076-RLY-WGH Document 1-4 Filed 05/13/10 Page 2 of 2
EXHIBIT E
Case 3:10-cv-00076-RLY-WGH Document 1-5 Filed 05/13/10 Page 1 of 19
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Case 3:10-cv-00076-RLY-WGH Document 1-5 Filed 05/13/10 Page 2 of 19
Case 3:10-cv-00076-RLY-WGH Document 1-5 Filed 05/13/10 Page 3 of 19
ENIEX
Speech D1K '03 Seite 1
Bochum, January 2003
Rubber - The Tailor-Made Material
Compounding of Elastomer Masses in a Planetary Roller Extruder
Ladies and Gentlemen,
I would like to thank you very much in the name of ENTEX for giving me the
opportunity to present to you the construction and mode of action of the planetary
roller extruder.
First of all I want to introduce the ENTEX company. ENTEX has been founded in
1986 and has today 88 employees. The name ENTEX stands for "ENTwicklung
EXtrusion" = development extrusion. Right from the beginning, we at ENTEX
identified ourselves with this name which is proved by more than 30 patents and
patented designs.
Our main product is the planetary roller extruder. More than 40 years ago Mr.
Wittrock of Messrs. Chemische Werke Hills AG has invented the planetary roller
extruder. Since that time this system is an integral part, especially regarding the
compounding of PVC, which - as we all know - is a thermal sensitive material so
that already here the characteristic of this system is demonstrated. There is no
other system existing which allows not nearly such an excellent temperature
control in the compounding process.
Besides the well-known types of plastics such as thermoplast (PVC, PP. PE,
TPU), duroplast, powder coatings, which are at present processed by means of a
planetary roller extruder, ENTEX has made a leap in an effective and economical
method of compounding elastomer masses.
Elastomers are cross-linked (vulcanized) polymer materials, being glassy hard at
very low temperature and showing a rubber-elastic behaviour at room
temperature. At higher temperatures, as well, no viscous flow properties can be
observed, so that today elastomers will be used in numerous fields of application.
Due to their special properties, as for example damping characteristics, media and
ageing resistance as well as their thermal stability, elastomers are used more and
more as insulating material, insulations, adhesives and much more in the
automotive industry, by cable makers and in many other industrial ranges.
In the past caoutchouc masses were produced almost exclusively on
discontinuously operating internal mixers. The course of the charge drive made
and makes - even at most complex process control - large fluctuations in the
quality of the material unavoidable.
The small cooling area and the relatively large volume of the chamber of the
internal mixer only allow a slight effect on the temperature control, which results in
a relatively long mixing period or alternately formulating compromises are made in
this area.
Case 3:10-cv-00076-RLY-WGH Document 1-5 Filed 05/13/10 Page 4 of 19
ENIEX
Speech DIK '03 Seite 2
This disadvantage regarding the temperature control and formulation does not
exist in the case of the planetary roller extruder.
Moreover, the discontinuous mixing process incurs high energy and economic
costs and must be regarded, due to the system, as requiring intensive time and
capital. In order to achieve a better process with regard to a continuously good
quality in mixing it is better to use a planetary roller extruder in view of process
technique and economy.
But at first some words concerning the construction of the planetary roller extruder:
The planetary roller extruder is a mixing heat exchanger with dynamic discharging
effect. The planetary roller part is the constructive and dominating zone with
regard to the process technique. The planetary roller part is constructed similar to
a planetary gear (Fig. 1). The drive is carried out via the central spindle which, in
turn, distributes the torque to the planets. These roll off in the 45
0
helical toothed
cylinder.
Fig. 1: Sectional draWing of a cylinder assembly
Due to the helical gearing of the planetary system a continuous rolling out of the
material is built up at simultaneous discharge in direction outlet of the roller part.
This guarantees the best self-cleaning effect of all compounding extruders. When
using an open stop ring practically the whole material - except few material
residues - will be rolled out of the roller part so that e.g. very economic changes
in colour resp. formulations can be achieved.
Case 3:10-cv-00076-RLY-WGH Document 1-5 Filed 05/13/10 Page 5 of 19
Speech DIK '03 Seite 3
Construction sizes:
The size of the extruder (Fig.
2) is destined by the
diametrical pitch of the toothed
liner.
ENTEX fabricates planetary
roller extruders from 50 mm ­
TP-WE 50 - up to 500 mm ­
TP-WE 500 - with a spindle
equipment of 6 - 24 spindles.
Fjg. 2: Model of a WE 400
Characteristics:
Due to the extremely thin wall thickness (Fig. 3) of the cylinder assembly and the
central spindle an excellent controlling of the temperatures of the contact surface
area is given. By the introduction of the pressure water heating and an improved
construction of the cooling channels which allow a product-near temperature
control thus influencing decisively the heat transmission, this system has found an
increasing acceptance.
Fig. 3: Roller model with "old" and "new" thermodynamic
There is no other compounding system existing which allows not nearly such an
excellent temperature control in the compounding process.
Case 3:10-cv-00076-RLY-WGH Document 1-5 Filed 05/13/10 Page 6 of 19
Speech DIK '03 Seite 4
It will be more simple to explain this in comparison with other systems, co-kneader
or twin screw {Fig. 5}.
Fig. 4:
The contact surface area
exchanges in comparable short
time is in the case of the
planetary roller extruder approx. 5
times larger than in the case of
the systems we have compared.
When you have a look at the co-kneader and the twin screw you will recognize
that these systems are systems of internal friction and that for the plasticizing they
have to be filled.
Screw fllte
Heating/Cooling
Kneading segment
Kneading housing
cooling passages
Heating elements
chamber
Fig. 5: Comparison of different compounding systems
Case 3:10-cv-00076-RLY-WGH Document 1-5 Filed 05/13/10 Page 7 of 19
EN'EX
Speech DIK '03 Seite 5
The essential advantage of the planetary system is a perpetual rolling-out of the
material to thin layers. We know that the materials to be processed, e.g. ASS,
PVC, TPU or elastomers, are bad heat conductors so that an exact temperature
control, also at different construction sizes, will only be possible when the
portioned material is rolled-out between the blanks and the individual planets.
To give you an impression of the contact surface area of a planetary roller extruder
we will look at the standard size of an extruder for calender feeding, i.e. TP-WE
250/2000-M2 (Fig. 6). On one rotation of the central spindle this extruder contacts
an area of more than 12 m
2
,
Fig. 6: Planetary roller extruder TP-WE250/2000·M2
i.e. at 50 r.p.m. an area of 600 m
2
. This corresponds nearly to twice the size of a
tennis court (Fig. 8).

fH'I<:l1l!' [rn'l
e 1f.,O
0100
.
[rrunl
Fig. 7: Contact surface area exchange of different construction sizes
Case 3:10-cv-00076-RLY-WGH Document 1-5 Filed 05/13/10 Page 8 of 19
ENJEX
Speech DIK '03 Seite 6
Fig. 8: Contact surface area of a TP-WE 250/2000-M2 at 50 r.p.m.
Planetwalzen­
Einschnecken­ Doppelschnecken­
Extruder
Extruder Extruder
Planetary F.:oller Smc!e- ScrEW T." .. vm-Sr rsvv
Extruder
Extruoer
kWrl/kg
i
0,09
/
0,08
0,07
0,06
0,05
0,04
0,03
0,02
0,01
°
Qmech JQlfch
Vergleich der Energiebll21nz verschledener AufbereitungsSY5teme (bel mutter ern Eurchsetz)
Fig. 9: Energy balance of different compounding systems in comparison
Fig. 9 shows the energy balance of different compounding systems. You will see
that the planetary roller extruder - at less drive power - offers due to its surface an
essentially larger heat exchange than the two other systems. The bottom part
shows the supplied motor energy, the upper part the heating capacity to be
possibly supplied. the outside part represents the radiation energy released by the
machine surface.
Moreover, due to the modular construction, the temperature profile and thus the
melt temperature can be controlled in a wide range, more details will follow later.
Case 3:10-cv-00076-RLY-WGH Document 1-5 Filed 05/13/10 Page 9 of 19
EN'EX
Speech DIK '03 Seite 7
Until now, the compounding in the caoutchouc industry takes place - contrary to
the planetary roller extruder - by batch-wise discontinuous mixing in the internal
mixer (Fig. 10), if necessary in several mixing stages.
cyllnder.--·..·..
Fig. 10: Drawing of a
standard internal mixer
feeding
reeding punch
blade
c001lng zcone
----­ slide door
housing
intermediate
:.- .. stage
, /'
stopper rod
ground floor
1011111111
"The rruxmq in a planetary roller extruder, however, is a continuous one step
process".
Tangential GK-N-rotor geometries
Fig. 11: Function modes in the internal mixer
Intermeshing GK-E- rotor geometries
The gelation process in the internal mixer is executed in a closed chamber (Fig.
11) in which two opposed rotors, equipped with kneading elements, are running.
Case 3:10-cv-00076-RLY-WGH Document 1-5 Filed 05/13/10 Page 10 of 19
ENJEX
Speech DIK '03 Seite 8
The real plasticizing parts are the kneading blades (Fig. 12). Here you have to
make a distinction between two different arrangements: the tangential (left) and
the intermeshing (right) rotors.
Fig. 12: Different kneading geometries of the kneading blades
For heating and cooling purposes respectively the chamber is a double-walled
execution. The rotors are cooled as well. The feed opening normally is operated
by means of a cooled, pressure air operated punch and the outlet opening is
closed by means of a cooled drop door.
In the case of the conventional tangential rotors the outer rotor diameter
corresponds approx. to the distance of the axles which means that the blades are
not intermeshing and therefore can be operated with different speed (= friction).
In the case of intermeshing rotors both kneading blades must run with the same
speed. By this principle the material will be in fact (due to the higher supplied
shear energy) quicker plasticized, unfortunately, however, the thermal charge will
be higher. Remedy can be achieved by lowering of the filling grade by which,
however, the throughput is decreased as well.
This makes clear the great difference between the discontinuous processing on an
internal mixer and the continuous processing in a planetary roller extruder.
The planetary roller extruder of the construction size 250 (TP-WE 250) has per
each cylinder assembly a max. filling volume of 9,5 I (at full planet equipment) with
a heating/cooling area of more than 20.000 em", From one litre material results
therefore a static contact surface area of 2.100 ern", a value to which no internal
mixer will come up. A comparable internal mixer reaches - depending on the filling
level - 1/10 up to 1/8 of this value. We have already got to know which dimensions
the contact surface area of the planetary roller extruder can achieve during
operation (Fig. 8 - tennis court).
Moreover you will see that the wall thickness (Fig. 13) between heating-cooling
medium and material to be processed is essentially thinner and therefore more
economical in the case of a planetary roller extruder. But there is no other
possibility as the internal mixer requires - due to its high power for the kneading
process - of course a strength which such a thin wall thickness does not allow.
Case 3:10-cv-00076-RLY-WGH Document 1-5 Filed 05/13/10 Page 11 of 19
ENJEX
Speech DIK '03 Seite 9
Fig. 13: Cooling of the kneading
blades of an internal mixer
Also with regard to the power it becomes clear that the planetary roller extruder
needs a clearly smaller amount of energy required, the already above mentioned
TP-WE 250 requires "only" a 350 kW drive. The variations of different specific
drives, e.g. 0,05 - 0,3 kW/kg for elastomers at a constant outlet enthalpy (losses in
temperature) of the material, can only be realized with a planetary roller extruder.
Moreover, the required mechanical energy is brought in into the material in a
controlled way and damages caused by overheating are not possible as - due to
the function mode of the planetary roller extruder - this will we withdrawn from the
material immediately.
1st Step - The Raw Materials
A further essential difference between internal mixer and the planetary roller
extruder is the feeding.
The caoutchouc balls used in the internal mixer are still today weighed out
manually and all further ingredients are adapted accordingly. The possible sources
of error in this procedure might be known.
In the planetary roller extruder exclusively caoutchouc pellets (Fig. 14) are used.
This is necessary in order to guarantee an optimal feeding of the aggregate and to
make a constant feeding possible in general.
Fig. 14: Pellets of comminuted caoutchouc balls for continuous feeding of the extruder
Case 3:10-cv-00076-RLY-WGH Document 1-5 Filed 05/13/10 Page 12 of 19
ENIEX
Speech DIK '03 Seite 10
The essential difference to the internal mixer is that the planetary roller extruder
can be fed only with pellets. Therefore, the caoutchouc balls must be comminuted
and pelletized at first.
In both cases the pelletized raw materials can be stored in silos or tanks and can
be supplied to the compounding machines via pneumatic conveyor equipment or
optionally in barrels or bags.
2nd Step - Weighing
In the case of the internal mixer the weighing of the formulation components is
done automatically, normally, however, manually.
the feeding of the planetary roller extruder takes place by means of the continuous
dosing with gravimetric dosing units. By means of the gravimetric dosing a
computer controlled material feeding is possible. This means that also during
running production process optimizing can occur, errors in dosing can be avoided
and therefore a constant high material quality can be maintained.
3rd Step - Mixing Process
As explained already above, in the case of the internal mixer the mixing process is
a discontinuous process consisting of feeding - mixing - emptying and, should the
occasion arise, the mixing takes place even in several mixing stages.
In the case of the planetary roller extruder the mixing process is a continuous,
single stage process.
4th Step - After-Treatment
After the mixing in the internal mixer, further treatment is carried out in the rolling
mill. The mixture is rolled out as a sheet, which is then cooled and coated with
parting agents. Then the sheet is dried and laid down before it is supplied to a
calender or extruder for further processing.
When using a planetary roller extruder you can give up these intermediate steps.
The compounded material will be e.g. further processed directly by means of a
gear pump or via a flat film die.
The following table (table 1) presents an economical comparison of internal mixer
and planetary roller extruder with regard to manpower requirement, investment
requirement and quality.
Case 3:10-cv-00076-RLY-WGH Document 1-5 Filed 05/13/10 Page 13 of 19
ENiEX
Speech DIK '03 Seite 11
Internal Mixer in Comparison with Planetary Roller Extruder
state-of-the-art state-of-the-art
internal mixer planetary roller
extruder
manpower pelletizing
required weighing
persons (estimated)
mixing
after-treatment
investment pelletizing X
required weighing X XX
x 500.000€ each
mixing XX X
(estimated)
after-treatment XX X
quality formulation ++ ++
change
self-cleaning ++
dosing ++ ++
mixture quality ++ +++
comparable
aggregates with a
throughput of
approx. 1.200 kg/h
table 1:
comparison of
investment in first
reconciliation as
per customers'
information
The above comparison can only present an approximate order of magnitude. A
specific cost accounting can, of course, only be made by the user himself, after a
customer-specific concept of a production line has been developed. On principle
we are convinced - also due to the resonance of our customers - that not only the
cost situation says something for the planetary roller extruder but above all the
continuous high quality of the compounded material. We would be pleased to
demonstrate you in our Technical Centre the qualities which can be achieved with
your material.
In the following exemplary process diagram (Fig. 15) a planetary roller extruder
for example can be fed with up to seven solid components (e.g. caoutchouc,
resins, additives etc.) simultaneously, parallel and in every requested dosing.
Furthermore, this is also still possible for two liquid components (e.g. softener).
Thus, at the touch of a button, the formulation can be changed at any time or the
throughput can be adapted - without down-times, without conversion works and
thus without set-up costs.
Fig. 15: Schematic concept of a production line for the continuous compounding of elastomers
Case 3:10-cv-00076-RLY-WGH Document 1-5 Filed 05/13/10 Page 14 of 19
Speech DIK '03 Selle 12
Development:
Now I want to familiarize you with some steps of development of the
planetary roller extruder during the past years.
A pioneering progress has been the production of the heatable cylinder by means
of the spark erosion process.
Fig. 16a: Spark erosion machine Fig. 16b: Inside view with roller cylinder
The pictures (Fig. 16a-d) show the function and mode of action of the spark
erosion technology. By this technology an electrode consisting of graphite is
produced on an involute milling machine. Then this will be eroded, practically 1 : 1,
in a hardened steel cylinder. The erosion process guarantees an optimal
development of the involute with all necessary profile displacements, i.e. every
clearance modifies inevitably the involute curve.
Fig. 16d: Electrode and electro-carbon
Fig. 16c: Electrode at diving
machined cylinder assembly
Case 3:10-cv-00076-RLY-WGH Document 1-5 Filed 05/13/10 Page 15 of 19
ENiEX
Speech DIK '03 Seite 13
The advantage of this erosion process is that you can practically erode in very
steel, notwithstanding the hardness.
The electro-carbon machining - invented by ENTEX - makes it possible to
produce liners of a length of 1.500 mm in one piece. No other process offers this
possibility. Due to the tool conditions and the necessary forces, such a length
without warpage will be possible neither by whirling, nor by grinding, nor by
drawing.
Today the grinding is restricted to approx. 500 mm, so that the liners should be
coupled or welded respectively.
In case liners must be coupled or welded you have to calculate with a heat
warpage. In order to avoid this heat warpage, wall thicknesses which are possible
with the erosion technique, cannot be achieved. Therefore, you will not get the
heat transfer possibilities for these extruders as per the whirling or grinding
process, which you can achieve with an eroded roller part. This means a reduction
of the process window.
The erosion technique has been a milestone in the development of the planetary
system and the outcome was to fabricate the planetary roller extruder in modular
construction.
Fig. 17: Presentation of the "modular construction" of the planetary roller extruder
At this kind of construction several cylinder assemblies (modules) are flanged to
each other (Fig. 17). Whereas the central spindle is covering the whole processing
length, every module can be equipped with a different number of planetary
spindles. The single cylinder sections are connected to each other via intermediate
stop rings. The planetary spindles are running against these stop rings.
By means of the equipment of the planetary spindles and the variation of the stop
ring diameter the dwell time of the melt and the pressure build-up can be varied.
Case 3:10-cv-00076-RLY-WGH Document 1-5 Filed 05/13/10 Page 16 of 19
Speech DIK '03 Sette 14
Process affects
______________________E: ... I E: ><
-'-­
200
150
planetav
__ ---,- .__--__;_-------4-s'--plndles
I I i
7 PSP 6 PSP 5 PSP
uecenuence..Q!.ttle.m.elt.preSS.Ule._.spe.Clllc.ener.I:l{.. .. ,p.lJ]di.e.L..
rs
Fig. 18 Dependence of the pressure build-up of the planetary roller extruder on the number of
planetary spindles
Fig. 18 shows the dependence of the specific power, melt temperature and
melt pressure on the number of planetary spindles. It becomes clear that with
for
inte
example
rmediate
7
sto
planetary spindles the pressure
p ring is essentially higher.
build-up in front of the
_______.._.
Process affects
E: ><
luph
200
190
'juG ..j
..
170 HO-- :
:mo-i
planetary
'-­ -'--__--,--__--, ,­ --4,,5.;....'Pln
JjleS
I I I
7 PSP 6 PSP 5 PSP
Pr.oc.e.5.s.. atf.e.ctS.DJ.S1DP..flI.1Q..d.larneter.a.ndnumber,.or.'p.lanetaclspmcllt:5.
rs
Fig. 19 shows the process effect of stop ring diameter and number of planetary spindles
The new modular system allows the variation of the process length and thus a
gentle compounding of materials which are difficult to disperse or homogenize, as
for example recycled materials, adhesives, caoutchoucs, etc.
The difference in quality between the known extruders and the planetary roller
extruders in modular construction is more than grave.
Case 3:10-cv-00076-RLY-WGH Document 1-5 Filed 05/13/10 Page 17 of 19
ENIE:X
Speech DIK '03 Seite 15
Fig. 20: Variations of planetary spindles, special design
We see further developments in Fig. 20 and Fig. 21. On the one hand the (for
special applications) varied tooth geometry of the planetary spindles becomes
visible, on the other hand the construction of the separable dispersion ring is
perceptible. This is used mainly when processing liquids and very low viscous
materials.
Fig. 21: Central spindle (left) and separated dispersion ring (right)
Glimpsing ahead with regard to the possibilities of the roller mixer system I want to
present you some types of extruder (Fig. 22 - 25):
Fig. 22: Reaction roller mixer with 4 modules
Fig. 23: Planetary roller extruder,
vertical construction
Case 3:10-cv-00076-RLY-WGH Document 1-5 Filed 05/13/10 Page 18 of 19
ENIEX
Speech DIK '03 Seite 16
These are used in the: chemical reaction technology, compounding of adhesive
masses and aircraft industry and made us to one of the leading producers within a
few years.
Fig. 24: Chemical roller mixer C-WM 400/3000-M3
Fig. 25: Planetary roller extruder
TP-WE 250 with twin stuffing
device
In future, the demand for high efficient compounding extruders like the planetary
roller extruder will increase due to new developed formulations.
EN EX
Rust & Mitschke GmbH
Heinrichstr. 67
44805 Bochum
Tel.: +49 (0)234 - 891 22-0
Fax: +49 (0)234 - 891 22-99
e-mail:
www.Entex-Bochum.de
Case 3:10-cv-00076-RLY-WGH Document 1-5 Filed 05/13/10 Page 19 of 19
EXHIBIT F
Case 3:10-cv-00076-RLY-WGH Document 1-6 Filed 05/13/10 Page 1 of 12
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Richard Waller St. Coeur Marysville, Michigan
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Case 3:10-cv-00076-RLY-WGH Document 1-6 Filed 05/13/10 Page 4 of 12
Attorney Docket No. 411738-021-P
PROCESS FOR PREPARING ADHESIVE USING PLANETARY EXTRUDER
The present invention relates to a continuous, low-temperature process for the
mastication and compounding of non-thermoplastic elastomers with tackifying resins and
with or without any combination of the following; thermoplastic elastomers, extenders,
plasticizers and oils, activators, anti-degradents, crosslinking agents, colorants, solvents,
and foaming agents, and subsequent application to a web-form material via slot-die.
The general purpose of the invention is to provide a method for producing a self
adhesive composition by mastication of non-thermoplastic elastomers in a planetary
roller extruder (PRE). In one embodiment mastication is achieved to produce a low
viscosity adhesive that can be applied using a slot die through the use of 'back-cut"
planetary spindles, in combination with full-flight planetary spindles.
Back-cut planetary spindles are spindles having openings in the flights that permit
material to pass between the wall of the barrel and the screw and slow the rate with which
material passes through the PRE. One example of a back-cut spindle is a so called
porcupine spindle. Another example is shown in Fig 1 hereto. PRE's having back-cut
spindles are commercially available from Rust-Mitschke-Entex. By adjusting the number
of full flight and open or back-cut spindles, the rate with which material passes through
the PRE and hence the amount of mastication that is done on the material is controlled. A
PRE with all full flight spindles does less masticating than a PRE with spindles in which a
portion of the flights is open or back-cut. Conventional PRE's contain at least 3 and can
contain up to 20 spindles, depending on the diameter of the cylinder and process design.
- 1 ­
Case 3:10-cv-00076-RLY-WGH Document 1-6 Filed 05/13/10 Page 5 of 12
Attorney Docket No. 411738-021-P
In one embodiment of the invention, a PRE having a 70mm diameter cylinder having 6
spindles is used. Another factor that affects the amount of mastication is the internal
diameter of the stop ring. By narrowing the gap between the stop ring or dosing ring and
the spindle, more mastication can be performed. In one embodiment of the invention
solid components, e.g. thermoplastic elastomers, tackifying resins, extenders, activators,
crosslinkers, and colorants, in addition to liquid components, are fed into the
compounding sections of the PRE. Additionally, and perhaps most importantly, one
embodiment of the invention involves the feeding of solvent into the compounding
sections of the PRE via dosing rings. Another embodiment of the invention involves
coating the self-adhesive composition on a web-form material, where the coating of the
web-form material is carried out using a slot-die applicator unit. One slot die unit that is
used in one embodiment includes a spindle that trails the die lip. One example of such a
die is commercially available from SIMPLAS
Simply stated, the disadvantage of the methods taught in the Beiersdorf patents
are: 1) Beiersdorf does not teach the effective, efficient, and controlled mastication of
non-thermoplastic elastomers, e.g. natural rubber, particularly through the use of "back­
cut" planetary spindles, in combination with full-flight planetary spindles, 2) the Beiersdorf
process is restricted to the addition of liquid components to the compounding section - it
does not teach the feeding of solid components, e.g. thermoplastic elastomers, resins,
extenders, activators, anti-degradents, crosslinkers, colorants and foaming agents into
the compounding section of the PRE, 3) the Beiersdorf process does not teach the
compounding of adhesives with solvents, and 4) the Beiersdorf process does not teach
- 2 ­
Case 3:10-cv-00076-RLY-WGH Document 1-6 Filed 05/13/10 Page 6 of 12
Attorney Docket No. 411738-021-P
adhesive coating methods other than a multi-roll applicator unit. These disadvantages
combine to limit the flexibility in designing the performance properties of the finished
adhesive, and the production of pressure-sensitive tape with that adhesive.
Modified PRE - The improved process is accomplished via a modified PRE.
Specifically, the modified PRE includes a feeding section and subsequent compounding
sections. The feeding section includes a single-screw barrel section with a throat into
which solid or liquid raw materials, e.g. elastomers, resins, extenders, activators,
antidegradents, and crosslinking agents, etc, can be introduced. The single screw then
conveys these raw materials into the first compounding section. In one embodiment a
PRE having four compounding sections, i.e., four planetary roller barrel sections
separated by stop or dosing rings. Each planetary compounding section consists of a 45°
helical toothed cylinder, a 45° helical toothed main spindle and three or more (for
example up to X) 45° helical toothed planetary spindles. The maximum number of
planetary spindles is a function of the diameter of the cylinder. The planetary spindles
can exhibit many different tooth geometries, e.g. full helical flights (Planetspindel), back­
cut helical flights (Noppenspindel), or zoned helical flights (Igelspindel), etc. The number
of planetary spindles chosen and their geometries (e.g., open vs. full flight) can be
manipulated in such a way as to influence the dynamic discharging effect of each
compounding cylinder and the discharging differential between cylinders. Liquid
materials, e.g. liquid elastomers, molten resins, oils, solvents, etc., can be introduced into
the compounding sections via injection nozzles through the dosing ring assemblies.
Additionally, the gap between the dosing ring and the main spindle can be changed to
- 3 ­
Case 3:10-cv-00076-RLY-WGH Document 1-6 Filed 05/13/10 Page 7 of 12
Attorney Docket No. 411738-021-P
vary the dynamic discharging effect of each compounding cylinder and the discharging
differential between the compounding sections. Moreover, each compounding section
can be modified with twin-screw dosing units. The twin screw dosing units are typically
positioned perpendicular to the axis of the compounding sections and are typically located
near the beginning of the compounding sections directly adjacent to the dosing rings.
The twin-screw dosing units can be employed to introduce solid components, e.g.
thermoplastic elastomers, resins, extenders, activators, anti-degradents, crosslinkers,
etc., to the compounding sections.
Raw Materials: Typical non-thermoplastic elastomers employed in this process
include natural rubber, synthetic polyisoprene, styrene butadiene rubber, butyl rubber and
polyisobutylene rubber, and any combination thereof. Typical thermoplastic elastomers
employed in this process are block copolymers, e.g. SIS, SBS, SEBS, and SEPS, and
any combination thereof. Typical resins include hydrocarbon resins, partially or fully
hydrogenated wood, gum, or tall oil rosins, esterified wood, gum or tall oil rosins, alpha
and beta pinene resins, and polyterpene resins. The resins can be introduced in both
solid and molten form. Typical extenders include clays, calcium carbonate, talc, and
aluminum hydrates. Typical activators include zinc oxide and magnesium oxide. Typical
antidegradents include antioxidants (AO), ultraviolet absorbers (UVA), and ultraviolet
stabilizers (UVS). Typical crosslinking agents include isocyanates, elemental sulfur,
sulfur donors, primary and secondary accelerators and phenolformaldehyde resins.
Typical colorants are titanium dioxide and other various metal pigments. Typical liquid
elastomers are low molecular weight natural rubber and low molecular weight synthetic
- 4 ­
Case 3:10-cv-00076-RLY-WGH Document 1-6 Filed 05/13/10 Page 8 of 12
Attorney Docket No. 411738-021-P
polyiosoprene and polybutene rubbers. Typical oils can be paraffinic, isoparaffinic,
napthenic, aromatic, or polyaromatic. Typical solvents are non-polar aromatics and
aliphatics such as toluene, hexane, heptane, and blends thereof. Examples of foaming
agents include Cellogen foaming agents and gases
Simply stated, the advantages of the new invention/method include; 1) purposeful,
effective, and efficient mastication of non-thermoplastic elastomers, 2) the introduction of
various solid raw materials into the compounding sections, 3) the introduction of solvent
into the compounding sections, and 4) the use of slot-die coating technology.
The purposeful mastication of non-thermoplastic elastomers is accomplished as
the elastomers are forced with the single-screw from the feeding section between the
dosing ring and the main spindles into the compounding sections, where it is intensively
mixed and subsequently masticated. The degree of mastication is further enhanced
through the use of back-cut, or Noppenspindel, planetary spindles. Mastication of the
non-thermoplastic elastomer translates into more efficient compounding of the elastomer
with other solid and liquid materials, yields the potential for a greater ratio of tack to
adhesion in the finished adhesive and yields a finished adhesive with lower viscosity that
is not limited to being coated via a multiple roll applicator unit (calender). This provides
an opportunity to employ more-prevalent, or existing coating equipment, as opposed to
purchasing a multiple-roll coating unit.
The introduction of various solid raw materials into the compounding sections has
several advantages. First, all solid materials do not have to be introduced all at once in
the feeding section of the PRE, i.e. they can be dosed in one or more of the compounding
- 5 ­
Case 3:10-cv-00076-RLY-WGH Document 1-6 Filed 05/13/10 Page 9 of 12
Attorney Docket No. 411738-021-P
sections. ~ r h i s gives the elastomer more time to be masticated prior to the addition of
solid raw materials and increases the mixing efficiency of the PRE up to 25%. Second,
solid resin, as opposed to molten resin can be introduced into the compounding sections.
The solid resin has a viscosity that more closely resembles the elastomer, when
compared to molten resin. As a consequence, the addition of solid(as contrasted with
liquid) resin further enhances mixing efficiency, whereas molten resin tends to act as a
lubricant and retards mixing efficiency. Additionally, the solid resin has a specific heat
which affords it the ability to act as a heat sink, l.e. take heat away from the process,
thereby minimizing the temperature of the melt during the compounding process.
Conversely, molten resin increases the temperature of the melt in the compounding
process.
The introduction of solvent into the compounding sections has several advantages.
First, small amounts (e.g., typically 10 to 20% by weight but amounts up to 50% could
feasibly be used) of solvent, introduced to the adhesive through several dosing rings,
enhances mixing efficiency, i.e. maintains homogeneity, while significantly lowering the
viscosity of the finished adhesive. The solvent is readily absorbed by the adhesive
composition and the incorporation of solvent lowers the resultant homogenous adhesive's
viscosity to the point that its application to a web-form material is not restricted to a multi­
roll applicator unit (calender). Rather, the lower-viscosity adhesive can now be applied to
web-form material via slot-die, roll-aver-roll, knife-aver-roll, or any number of traditional
adhesive application techniques. The subsequent liberation of the solvent from the
adhesive that has been applied to the web-form material affords the ability to effect
- 6 ­
Case 3:10-cv-00076-RLY-WGH Document 1-6 Filed 05/13/10 Page 10 of 12
318914
Attorney Docket No. 411738-021-P
numerous surface geometry profiles, i.e. degrees of foaming, in the adhesive film.
Subsequently, the performance properties of the adhesive film can be further
manipulated, i.e. in addition to degree of elastomer mastication and formulation.
The use of a slot-die for coating adhesives to web-form material has particular
advantages over a multi roll applicator unit (calenderer). Web-form adhesive coating
speeds, when employing multi roll applicator units (calendars), are typically limited to 300
meters per minute. However, the use of slot-die coating technology, particularly when
employed in conjunction with lower-viscosity, high-solids adhesives, e.g. 80-90%, as
opposed to higher-viscosity, 100% solids adhesives, is of particular interest, as
application speeds easily approach 900 meters per minute or more.
- 7 ­
Case 3:10-cv-00076-RLY-WGH Document 1-6 Filed 05/13/10 Page 11 of 12
FIG. 1
Case 3:10-cv-00076-RLY-WGH Document 1-6 Filed 05/13/10 Page 12 of 12
EXHIBIT G
Case 3:10-cv-00076-RLY-WGH Document 1-7 Filed 05/13/10 Page 1 of 17
11111111111111111111111111111111 1I1I111111111111111111111111111111111111111
US007476416B2
(12) United States Patent (10) Patent No.: US 7,476,416 B2
Tynan, Jr. et at (45) Date of Patent: Jan. 13,2009
(54) PROCESS FOR PREPARING ADHESlVE
USING PLANETARY EXTRUDER
(75)
Inventors: John Kinch Tynan, Jr., Port Huron, MI
(US); Richard Walter St. Coeur,
Marysville, Ml (US); David Michael
Kovach, Marysville, Ml (US); Thomas
Lombardo, Bradenton. Fl. (US)
(7:') Assignee: Intertape Polymer Corp.. Bradenton,
FL (US)
( " ) Notice: Subject to any disclaimer. the term of this
patent is extended or adjusted under 35
U.S.C. l54(b) by 7R3 days.
(2\ ) Appl. No.: 10/997,827
(22) Filed: Nov. 24, 2004
(65) Prior Publication Data
US AI Aug. 4, 2005
Related U.S. Application Data
«()()) Provisional application No. 60/524,505, filed on Nov.
24.2003.
(51) Int. Cl.
B05D 5/10 (2006.01)
(52) U.S. Cl. 427/207.1; 427/177; 427/420;
427/42R.0I
(58) Ficld of Classification Search 427/177,
427/207.1,420,42[\,42[\01: 264/21123
See application file for complete search history.
(56) References Cited
U.S. PATFNT nOC1IMFNTS
3,645,980 A 2/ 1972 cl al.
28
3,914,484 A IOII975 Creegan et al.
3,941,535 A 311976 Street
4,404,324 A 911983 Fock et al.
4,RR9,430 A 12!19R9 Mueller
(Continued)
FOREIGN PATENT DOCUMENTS
CA 69R518 It/t964
(Continued)
OTHER PUBLICATIONS
"Planetary Extruder," by Lanhang Machinery Co., Ltd., on web page
allproducts.com (date of first publication unknown). Applicants
admit the status of this publication as prior 3It for the limited purpose
of examination of this application. but otherwise reserve the right to
challenge the statns of this publication as prior an.
(Continued)
Primary Examiner-Kirsten C Jolley
(74) Attorney, Agent. or Firm-Thompson Him: 1.1 l'
(57) ABSTRACT
A process for preparing a pressure sensitive adhesive using a
modified planetary roller extruder is described. The process
in accordance with one aspect ofthe invention includes intro­
ducing primary raw materials including a non-thermoplastic
elastomer into a feeding section of the modified planetary
roller extruder, conveying the raw materials from the feeding
section to a compounding section of the modified planetary
roller extruder, continuously mixing the primary raw materi­
als in the compounding section to produce a homogeneous
adhesive composition. The adhesive composition may be
applied to a web-form material. TIle compounding section of
the modified planetary roller extruder includes a main spindle
surrounded by and intermeshed with a plurality of planetary
spindles at least one of which is a double transversal mixing
spindle having a plurality of back-cut helical flights.
34 Claims, 5 Drawing Sheets
32
Case 3:10-cv-00076-RLY-WGH Document 1-7 Filed 05/13/10 Page 2 of 17
US 7,476,416 82
Page 2
u.s. PArENT DOCUMENTS 2003/0032691 AI 2/2003 Bolte et at
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5,162,457 A 11/1992 Hansel el al.
2005/0165164 AI 7/2005 Moeller et al.
5,19R,0ti4 A 111991 Tani et al.
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Hawrylko
DE 1954214 5/1971
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DE 3908415 9/1990
5,'i50,175 A R1l996 Bredahl et al
DE 19653790 6/1998
5,605,720 A 211997 Allen et al,
lP 3017176 1/1991
5,760,135 A 6/1998 Korpman et al.
lP 11-080690 3/1999
5,776,998 A 711998 Southwick et al.
lP 11-216764 10/1999
'i,849,145 A 12/1998 Tornctti
WO (WII17'i 'i/1994
'i,858,1 so A 1/1999 Yarusso er al.
WO 99/42276 8/1999
5,910,542 A 611999 SI Clair et aI.
WO 2004/037941 5/2004
6,I50JJl7 A I Jl2000 Burmeister et al.
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OTHER PUBLlCAT10NS
6.251.517 HI 61200 I Sashihara d al.
6j06,447 1>1 1/2001 Hirsch er al.
Angier, OJ, et al., "Mastication ofRubber. VI. Viscosity andMolecu­
6,527.8')9 ill 3
/2003
Dietz ct al. lar Weight Relationships for Natural Rubber after Cold Mastication,"
7
/2004
6,759,122 Il2 Spies et al. Journal ofPolymer Science, vol, XXV, pp. 129-138 (l9'i7).
6,780,271 B 1 8
/2004
Burmeister et al. Rauwendaal. C .. "The Multisercw Extruder with More Than Two
6,799,881 B2 10' 2004 r ischer Screws." Polymer Extrusion, Hanser Publishers, pp. 11-12 t 1986)
6,822,048 B1 1Jl2004 Burmeister el al.
Author Anonymous, "Adhesive compounding process for production
6,881,796 B2 4/2005 Yamaguchi et al. of prcssur42 sensitive tapes." published [It www.researchdisclosure.
2001'0039302 Al 11/2001 Wustling ct al. com (Oct. 3 L 2003).
Case 3:10-cv-00076-RLY-WGH Document 1-7 Filed 05/13/10 Page 3 of 17
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Case 3:10-cv-00076-RLY-WGH Document 1-7 Filed 05/13/10 Page 4 of 17
u.s. Patent Jan. 13,2009 Sheet 2 of 5 US 7,476,416 B2
32
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FIG.3
Case 3:10-cv-00076-RLY-WGH Document 1-7 Filed 05/13/10 Page 5 of 17
U.S. Patent Jan. 13,2009 Sheet 3 of 5 US 7,476,416 B2
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Case 3:10-cv-00076-RLY-WGH Document 1-7 Filed 05/13/10 Page 6 of 17
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Case 3:10-cv-00076-RLY-WGH Document 1-7 Filed 05/13/10 Page 7 of 17
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Case 3:10-cv-00076-RLY-WGH Document 1-7 Filed 05/13/10 Page 8 of 17
US 7,476,416 B2
1
PROCESS FOR PREPARING ADHESIVE
USING PLANETARY EXTRUDER
REFERENCE TO RELATED APPLlCATION
This application claims the benefit of U.S. Provisional
Application No. 60/524.505, filed Nov. 24, 2003.
1'1i.'LD 01; riu: INVIiNTlON
111C present invention relates to a continuous, low-tem­
perature process for the mastication and compounding of
non-thermoplasuc elastomers with tackitying resins and may
include one or more of the following: thermoplastic elas­
tomers. extenders, plasticizers and oils, activators, anti-de­
gradents, crosslinking agents, colorants, solvents, and foam­
ing agents. In oue aspcct of the invention, the adhesive may be
applied directly to a web-form material.
The general purpose of the invention is to provide a method
for producing a self adhesive composition by mastication of
non-thermoplastic elastomers in a planetary roller extruder
(PRE). In one embodiment mastication is achieved through
the use of double transversal or "back-cut" planetary
spindles, in combination with full-flight planetary spindles 10
produce an adhesive that can he applied to a web-form mate­
rial using a slot die.
HACKliROUND OF THE INVENTION
Pressure sensitive adhesive compositions are blends ofsev­
era! raw materials including elastomers, resins, plasticizers
and other additives such as antioxidants, fillers, pigments, etc.
Since these ingredients must be blended in the proper ratio to
obtain the adhesive having the desired properties, the raw
materials arc typically blended with a mechanical mixer
II nder controlled conditions as part ofa balch-wise process to
obtain a thoroughly mixed product having the appropriate
relative amounts of the raw materials.
Planetary roll extruders have been known and have typi­
cally been used in processing ofthermoplastics such as PVC,
for example, where they were used primarily to supply the
downstream units such as, for example, calendars or roll
mills. Planetary roll extruders have typically been used to
process heat-sensitive compounds with a minimum of dcgra­
dation because thin layers of compound can be exposed to
large surface areas thereby resulting in effective heat
exchange, mixing and temperature control, Planetary roll
extruders are available in various designs and sizes. The
diameters of the roll cylinders, depending on the desired
throughput, arc typically between 70 nun and 500 HUU.
Planetary roll extruders generally have a filling section and
a compounding section. The filling section typically includes
a conveying screw to which certain raw materials are fed
continuously. The conveying screw then passes the material
to the compounding section. The compounding section
includes a driven main spindle and a number of planetary
spindles which rotate around the main spindle within a roll
cylinder with internal helical gearing. The rotary speed ofthe
main spindle and hence the rotarioual speed of the planetary
spindles can be varied and is one parameter to be controlled
during the compounding process. The materials me circulated
between the wain and planetary spindles, or bel ween the
planetary spindles and the helical gearing of the roll section,
so that under the materials are dispersed to form a homoge­
neous composition.
The number of planetary spindles rotating in each roll
cylinder can be varied and thus adapted to the requirements of
2
the process. TIle number of spindles influences the free vol­
ume within the planetary mil extruder, the residence time of
the material in the process, and also determines the surface
area for heat and material exchange. By way ofthe dispersive
" energy introduced, the number of planetary spindles has an
influence on the result of compounding. Given a constant
diameter of roll cylinder, a larger number of spindles permit
better homogenization and dispersion or, respectively, a
greater product throughput.
iu
The maximum number of planetary spindles iustallable
between the main spindle and the roll cyl indcr depends on the
diameter of the roll cylinder and on the diameter of the plan­
crary spindles used. When using relatively large roll diarn­
\ 5 ctcrs, as required fur obtaining production-scale throughputs,
and/or relatively small diameters for the planetary spindles,
the roll cylinders can be equipped with a relatively large
number of planetary spindles. With a roll diameter PI' D=70
nun, typically up to seven planetary spindles arc used,
en whereas with a roll diameter of D=200 rum ten, tor example,
and a roll diameter of D ~ 4 0 0 mrn 24 for example, plunctury
spindles can be used. However. these examples arc in no way
limiting to those skilled in the art. I'or example, ifthe diameter
ofthe main spindle is smaller relative to a lnrgcr main spindle,
2:' the 11111nber ofplanetary spindles can be increased.
3(1
35
411
45
5«
"
6<1
Ii'
SUMMARY OF TIlL' INVENTION
The present invention is directed to a process lor preparing
an adhesive using a modified planetary roller extruder. The
process in accordance with one aspect of the invention
includes introducing primary raw materials including a nou­
thermoplastic elastomer into a feeding section of the modified
planetary roller extruder, conveying the raw materials from
the reeding section to a compounding sectiou olthc modified
planetary roller extruder.mixing the primary raw materials in
the compounding section, producing a homogeneous adhe­
sive composition and applying the adhesive composition to a
web- form material. The compounding section of the modified
planetary roller extruder includes a main spindle surrounded
by and intermeshed with a plurality of planetary spindles at
least one of which is a double transversal mixing spindle
having a plurality of back-cut helical flights.
In accordance with another aspect of the invention. the
modified planetary roller extruder is used to produce an adhe­
sive composition. TIle process in accordance with this aspect
of the invention includes continuously metering into a plan­
etary roller extruder primary raw materia Is of an adhesive
composition comprising a non-thermoplastic elastomer and a
tackifyiug resin, continuously mixing the raw male rials in a
compounding section of the planetary roller extruder to Ionu
a homogeneous adhesive composition wherein the com­
pounding section includes a main spindle surrounded by and
intcrmcshcd with a plurality ol'planctary spindles wherein at
least one of the planetary spindles is a double transversal
mixing spindle having a plurality of back-cut helical flights,
and continuously discharging the homogeneous adhesive
composition from the extruder. In accordance with certain
embodiments, the self-adhesive composition may be applied
10 a web-formed material using an applicator unit such as a
slot-die applicator unit and subsequently crosslinked.
In accordance with another aspect of the invention. the
elastomer is masticated such that M" is reduced to less than
1.000,000 as measured by (We. In other aspects of the inven­
tion, the elastomer may be masticated to cause 11 reduction in
Case 3:10-cv-00076-RLY-WGH Document 1-7 Filed 05/13/10 Page 9 of 17
US 7,476,416 82
3
M; of more than about 50%, more particularly more than
about 80%, relative to tile original M", tor the elastomer.
BRIEF DESCRIPTION OF THE DRAWINGS
An exemplary embodiment of the invention is explained in
more detail below with reference to the drawings in which:
FI(;. I is a longitudinal sectional view ofa planetary roller
extruder in accordance with one aspect of the present inven­
tion:
FIG. 2 is an enlarged view of an exemplary double trans­
versal mixing spindle;
FIG. 3 is a cross-sectional view of a dosing ring from the
planetary roller extruder in FIG. I;
PIG. 4 is cross-sectional view of a slot die coater;
FlO. 5 is a longitudinal sectional view ofa planetary roller
extruder and slot die coater in accordance with one aspect of
the present invention: and
FlO. 6 is a cross-sectional view of the planetary roller
extruder in FIG. 1 along line 6-6.
DETAILED DESCRIPTION OF THE INVPNTION
.\11 documents cited are, in relevant part. incorporated
herein by reference: the citation of any document is not to be
construed as an admission that it is prior art with respect to the
present invention.
Turning now to the drawings, and referring initially to FIG.
1, n planetary roller extruder in accordance with one embodi­
ment of the present invention is illustrated and generally
designated by the reference 10. It will be appreciated that the
planetary roller extruder system 10 is illustrated in diagram­
matic form in order to explain its operation in easily under­
staudablc manner. However, in actual practice. tile shape and
size of the system 10 might be substantially different from
that illustrated and yet still be within the scope of the claims
set forth herein.
TIle planetary roller extruder system 10 includes a feeding
section 12 and a compounding section 14. 111eprimary adhc­
sive raw materials are added into the feed throat 16 and
metered onto the conveying screw 18 ofthe tilling section 12.
As used herein. the term "primary raw materials" refers to
those materials of the adhesive formulntion added into the
feed section 12 of the planetary roller extruder 10. Primary
raw materials may include, but are not limited to. elastomers.
resins, extenders, activators. anti-dcgradcnts. and crosslink­
ing agents. 111e screw 18 conveys the primary raw materials
into the compounding section 14. The compounding section
14. as illustrated in FIG. 1, includes four planetary roller
barrel sections 20a. 20h. 20, and 20d separated by dosing
rings 22a, 22b and 22,. Each roller barrel section 20 includes
a 45" helical toothed cylinder 24. a 45° helical toothed main
spindle 26 and a plurality of 45° helical toothed planetary
spindles 2N. 30. The helical gearing can have any suitable
angle. for example. an angle of 10 to 60°, more particularly
somewhat greater than 20° may be useful. In accordance with
the certain aspects of the present invention. at least one or the
roller barrel sections 20 includes a double transversal plan­
etary spindle 28. The present invention is not limited to the
usc of donble transversal planetary spindles. Other spindle
configurations that provide the desired levels of mixing can
also be used.
The maximum number of planetary spindles 2N. 30 is a
function ofthe diameter of'thc main spindle 26 and the helical
toothed cylinder 24. The planetary spindles 28, 30 can exhibit
many different tooth geometries. e.g .. ful I helical flights
(Planetspiudel) 30. double transversal helical flights (also
III
I"
ell
e5
311
.1"
411
4"
511
"
611
0"
4
known as back-cut spindles or Noppenspindel) 28, or zoned
helical flights (Igclspindcl), etc. TIle number of planetary
spindles chosen and their geometries (e.g., open vs. full
flight) can be manipulated in such a way as to influence the
dynamic discharging effect of each roller barrel section 20
and the discharging differential between sections. Addition­
any. the gap between the dosing ring 22 and the main spindle
26 can be changed to vary the dynamic discharging effect or
each barrel section 20 and the discharging differential
between the barrel sections 20.
A standard planetary spindle 30 is represented by a cylin­
der in which g.woves or flights have been cut at 45° angles to
the spindle ax is, the same angle as the main spindle flights.
The planetary spindles ride in the main spindle flights and this
design yields identical surface speeds or the planetary
spindles 28, 30 and the main spindle 26. There is a gap
between the main and planetary spindles which is tilled with
process material and the net result is that ncar zero-shear
distributive and dispersive mixing can occur between the
main spindle 26. the planetary spindles 28. 30, and the barrel
wall 24.
Another net result ol the 45° angle cut into the planetary
and main spindles is a positive pressure. a forwarding motion
imparted on the process material. A variation which yields
less pressure, more slippage, less forwarding motion. longer
residence time and hence greater mixing is the usc of or
double transversal spindles 28 (also known as noppen­
spindles or back-cut spindles).
I>oublc transversal planetary spindles 28 arc spindles hav­
ing openings in the flights that penni! material to pass
between the wall of the barrel 24 and the main spindle 26 and
slow the rate with which material pnsses through the plan­
etary roller extruder system 10. One example of a double
transvcrsnlspindle 28 is a so-called porcupine spindle. A par­
ticulnr cxumplc ola double transversal spindle 2N is shown in
detail in lK]. 2. back cut openings 32 increase residence time
and improve mixing. The design of a double transversal
spindle 28 is a variation of the standard planetary spindle,
with the addition of channels cut into the 45" angled flights.
The angle of these back cut channels can range from about
45-135° relative to the spindle nights. more particularly from
about 75-105°, and in accordance with certain aspects of the
invention the back cut channels may be at an angle of about
90°, The number and depth of these channels may also be
varied and can be de1ined in more simplistic terms by the
following: l(total channel area cut into the spindle flights/total
area of spindle flights)x 100%]. This value may range Irom
about 10-90%. more particularly from about 40-60%, and in
certain embodiments ofthe invention the value may be about
50%. Planetary roller extruders having double transversal­
spindles 28 arc commercially available from Rust-Mitschke­
Entex. By adjusting the number of fnll llight 30 and open or
double trausversalspiudlcs 28. the rate with which material
passes through the planetary roller extruder and hence the
amount of mastication that is done on the material can be
controlled.
Conventional plnnetury roller extruders contain M least 3
and can contain up to 24 spindles depending on the din meter
of the cylinder and process design. Of course. one of skin in
the art would realize that a greater number of planetary
spindles could be nsed depending on the specific dimensions
and construction of the extruder, In one embodiment of the
invention, a planetary roller extruder 10 having a 70 nun
diameter cylinder having 6 spindles 2N. 30 is used. In accor­
dance with certain aspects ofthe invention. the double trans­
versal spindles 28 account for more than 20%. more particu­
larly more than 50%. of the number of planetary spindles 2N.
Case 3:10-cv-00076-RLY-WGH Document 1-7 Filed 05/13/10 Page 10 of 17
US 7,476,416 B2
5
30 in the planetary roller extruder 10. FIG. 6 shows a cross­
section for a planetary extruder in accordance with a particu­
lar embodiment of the invention that includes four (4) double
transversal planetary spindles 28 and two (2) full flight
spindles 30.
The rotation of the main spindle 26 causes the planetary
spindles 28, 30 to be set in rotational movement, as a resnlt of
the helical gearing ofthe main spindle 26 interacting with the
helical gearing of the planetary spindles 28, 30.
The planetary spindles 28, 30 also mesh with the internal
gearing ofthe cylinder section 24. "111e helical gearing of the
main spindle 26. the planetary spindles 28, 30 and the cylin­
der section 24 conveys the raw materials to be compounded in
the direction of the d ischarge orifice 34.
11lCterm "secondary raw materials" as used herein refers
to raw materials or solvents introduced into the compounding
section 14 or the plunetary roller extruder 10. Secondary
liquid materials. such 'IS liquid elastomers, molten resins,
oils. solvents, etc., can be introduced into the compounding
section 14 via injection nozzles (not shown) through the
dosing ring 22 assemblies. As shown in FIG. 3. the dosing
rings 22 include radially extending bores 23 that allow lor
metered addition ofliquids to the compounding section 14.1u
accordance with one embodiment of the invention. the pro­
cess involves the feeding of solvent into the compounding
section 14 of the planetary roller extruder 10 via the dosing
rings 22.
Secondary solid raw materials can be added to the com­
pounding section 14 through a side feeder 36 or twin screw
dosing units 38. '111e twin screw dosing units 38 are typically
positioned perpendicular to the axis of the compounding sec­
tion 14 and arc typically located near the beginning of the
com pounding section directly adjacent to the dosing ring 220.
The twin screw dosing units 38 cau be employed to introduce
solid components such as thermoplastic elastomers. resins,
extenders, activators. anti-degradents. crosslinkers, etc .. to
the individual roller barrel sections 20.
Another embodiment of the invention involves coating the
self-adhesive composition on a web- form material, where the
coating of the web-form material may be carried out using
any of a variety of coating, techniques including" but not
limit cd to, slot-die coating. roll-over-roll coating, reverse roll
and knife-over-roll coating. In accordance with certain
embodiments of the present invention, the adhesive compo­
sition is applied to the web-form material using a slot-die
applicator unit. Particularly useful methods for applying the
adhesive composition to the web-form material include slot­
die coating using a rotating lip die or a fixed lip contact die.
One particular slot die unit that can be used is a rotating lip die
having a spindle that trails the die lip. One example of such a
die is commercially available from SIMPLAS and is shown in
FI(r. 4. Rotating lip die 40 includes an inlet 42 for receiving
the adhesive composition from the extruder 10. As shown in
FIG. 5, the adhesive composition is continuously conveyed
from the extruder 10 to the rotating lip die applicator 40 to be
applied to a web-form material through slot 44. '111e rotating
lip die applicator 40 further includes a rotating spindle 46 at
the trailing edge ofthe die lip that improves coating properties
of the applied adhesive. Adjustable bolts 48 on the rotating lip
die applicator 40 enable the operator to easily adjust the lip
opening and control the adhesive coating thickness.
In accordance with another aspect ofthe present invention,
the self-adhesive composition may be crosslinked. More spe­
cifically the coated adhesive composition may be crosslinked
with the aid of electron beams or IN rays by means of
ionizing radiation. such as electron beams. for example, so
that the resultant self-adhesive tape becomes shear-resistant
111
15
:11
:5
311
35
40
45
50
"
60
I>.i
6
and temperature-stable. UV rays as well can be used for
crosslinking, in which case appropriate UV promoters, for
example such as Ebecryl140 from OC8, must be added to the
selt-adhesive composition. Chemical and/or thermally
induced crosslinking may also be used.
The non-thermoplastic elastomer may be chosen from the
group of the natural rubbers or of the synthetic rubbers or of
any desired blend of'natural rubbers and/or synthetic rubbers,
it being possible to choose the natural rubber or rubbers in
principle from all available grades, such as, for example,
crepe, RSS. ADS, TSR, SIR 10. SIR 5L or CV grades.
depending on the required purity and viscosity level, and it
being possible to choose the synthetic rubber or rubbers from
the group of the randomly copolymerized styrene-butadiene
rubbers (SBR), butadiene rubbers (BR). synthetic polyiso­
prenes (lR). butyl rubbers (IJR), polyisobutylene rubber,
halogenated butyl rubbers (Xl lk). acrylate rubbers (ACM).
ethylene vinyl acetate copolymers (EVA) and polyurethanes,
and/or blends thereof.
Thermoplastic elastomers with a weight fraction of Irom 1
to 100% by weight, based on the total non-thermoplastic
elastomer content. can be added to the non-thermoplastic
elastomers. As representatives, mention may be made <It this
point in particular ofthe highly compatible styrene-isoprene­
styrene (SIS), styrene-butadiene-styrene (SBS), styrene iso­
prene butadiene styrene (SmS) grades as well as SFflS, and
SEPS, and any combination thereof.
Tackifier resins which can be used arc, without exception,
all tackifier resins that can function as tackifiers in the formu­
lation. 'lackifier resins may be present in the adhesive corn­
position at from 40% to 200% weight fraction based on elas­
tomer. Representatives that may be mentioned include the
rosins, their disproportionated. hydrogenated, polymerized
and esterified derivatives and salts. the aliphatic and aromatic
hydrocarbon resins, terpene resins und terpene-phenolic res­
ins. Typical resins include partially or fully hydrogenated
wood, gum, or tall oil rosins. esterified wood, gum or tall oil
rosins, alpha and beta pinene resins, and polyterpene resins.
More specifically, resins useful herein include C5 hydrocar­
bon resins, C9 hydrocarbon resins and mixtures thereof Con­
ruarouc indcuc and alpha-methyl styrene resins call also be
used. The resins can be introduced in both solid and molten
form. Any desired combinations of these and other resins can
be used ill order to adjust the properties of the resultant
adhesive composition in accordance with what is desired.
Reference may be made expressly to the depiction ofthe state
of knowledge in "Handbook of Pressure Sensitive Adhesive
Technology" by Donatus Satas (van Nostrand, 1989).
Typical extenders include clays, calcium carbonate, talc,
and aluminum hydrates. Typical activators include zinc
oxide, zinc chloride, magnesium chloride and magnesium
oxide. Typical anti-degradcnts include antioxidants (AO),
ultraviolet absorbers (UVA), and ultraviolet stabilizers
(lNS). Typical opacifiers and colorants include. but are not
limited to, titanium dioxide and other various metal pigments
known to those skilled in the art.
Typical solvents are non-polar aromatics and aliphatic>
such as acetone, toluene, hexane, heptane, and blends thereof.
When a highly foamed adhesive is desired. the solvent con­
tent of the adhesive may be increased. This aspect of the
disclosure overcomes the problems typically encountered
with typical hot melt adhesives that experience problems
caused by the higher densities and smooth. non-extensible
surfaces of extruded adhesives which result in a low ratio of
tack to adhesion in the finished adhesive. Solvents, when
present ill the formulation, may be used in any amounts lip to
about 70"10, more particularly up to about 50%, by weight of
Case 3:10-cv-00076-RLY-WGH Document 1-7 Filed 05/13/10 Page 11 of 17
US 7,476,416 B2
7
the adhesive composition. Typical liquid elastomers are low
molecular weight natural rubber and low molecular weight
synthetic polyiosoprene and polybutene rubbers. Typical oils
can be paraffinic, isoparalfinic, naptheuic, aromatic, or pol­
yaromatic. Examples of foaming agents include Cellogen
foaming agents and gases.
Plasticizers which can be used are all plasticizing sub­
stances known from adhesive tape technology. Examples of
useful plasticizers include. but arc not limited to, the paraf­
finic and naphtheuic oils. (functionalized) oligomers such as
oligobutadiencs and oligoisoprenes, liquid nitrile rubbers,
liquid terpene resins, animal and vegetable oils and fats,
phthalates. and functionalized acrylates.
Simply stated. some advantages ofcertain embodiments of
the new invention/method include: I) purposeful. effective,
and efficient mastication of non-thermoplastic elastomers, 2)
the introduction of various solid raw materials into the com­
pounding section, 3) the introduction ofsolvent into the com­
pounding section, and 4) the use of slot-die coating technol­
ogy to achieve an adhesive coated web-form material with a
unique balance of converged panel adhesion and quick stick
properties.
The purposeful mastication of non-thermoplastic elas­
tomers is accomplished as the elastomers arc forced with the
single-screw from the feeding section between the dosing
ring and the main spindles into the compounding section,
where it is intensively mixed and subsequently masticated.
Tile degree of mastication is further enhanced through the use
of double transversa! planetary spindles. Another Iactor that
affects the amount of mastication is the internal diameter of
the stop ring. By narrowing the gap between the stop ring or
dosing ring and the spindle, more mastication can be per­
formed. Mastication of the non-thermoplastic elastomer
translates into more efficient compounding of the elastomer
with other solid and liquid materials. yields the potential for a
greater ratio of tack to adhesion in the finished adhesive and
yields a finished adhesive with lower viscosity that is not
limited to being coated via a multiple roll applicator unit
(calendar). This provides an opportunity to employ more­
prevalent. or existing coating equipment. as opposed to pur­
chasing a rnuhiple-ro ll coating unit.
ln accordance with one aspect nf the invention, the clas­
tomer is masticated such that M", is reduced to less than
I ,000.000 as measured by GPc. In other aspects ofthe inven­
tion. the elastomer may be masticated to cause a reduction in
M". of more than about 50%, more particularly more than
about gO%, relative to the initial M". for the elastomer. The
initial molecular weight refers to the molecular weight of the
non-thermoplastic elastomer as it is being introduced into the
planetary roller extruder. As such. the initial molecular
weight may already have been reduced [IS a result of prepro­
cessing of the elastomer as compared to the molecular weight
for the unprocessed elastomer. Therefore, the reduction in
molecular weight referred to herein is based 011 the reduction
in molecular weight obtained by processing on the planetary
roller extruder. The reduction in molecular weight as
described herein is calculated by l-ormuln I:
IJI
111e introduction of various solid raw materials into the
compounding sections has several advantages. First, all solid
materials do not have to be introduced all at once in the
feeding section of the planetary roller extruder. i.e.. they can
be dosed ill one or more of the roller barrel sections of the
compounding section. This gives the elastomer more time to
be masticated prior to the addition of solid raw materials and
increases the mixing efficiency of the planetary roller
8
extruder, Second, solid resin, as opposed to molten resin can
be introduced into the compounding section. The solid resin
bas a viscosity that more closely resembles the elastomer,
when compared to molten resin. As a consequence. the addi­
tion ofsolid (as contrasted with liquid) resin further enhances
mixing efficiency. whereas molten resin tends to act as a
lubricant and retards mixing efficiency. Additionally, the
solid resin has a specific heat which affords it the ability to act
as a heat sink. i.c, take heat away from the process, thereby
III minimizing the temperature of the melt during the com­
pounding process. Conversely, molten resin increases the
temperature of the melt in the compounding process.
The introduction of solvent into the compounding sections
has several advantages. First. small amounts (e.g .. typically
I" 10 to 20% by weight but amounts up to 50% could lcasibly be
nscd) of solvent. introduced to the adhesive through several
dosing rings, enhances mixing efficiency, i.e. maintains
homogeneity, while significantly lowering the viscosity ofthc
finished adhesive. 111e solvent is readily absorbed by the
211 adhesive composition and the incorporation oI'solvent lowers
the resultant homogeneous adhesive's viscosity to the point
that its application to a wcb-Iorm matcrial is not restricted to
a multi-roll applicator unit (calendar). Rather. the lower-vis­
cosity adhesive can now be applied to web-form material via
25 slot-die. reverse roll, roll-over-roll, knife-over-roll, or any
number oftraditional adhesive application techniques includ­
ing the use of multi-roll applicators. The subsequent libera­
tion of the soJvent from the adhesive that has been applied to
the web-form material affords the ability to affect numerous
31l adhesive surface geometry profiles, i.e. degrees of foaming,
in the adhesive film. Subsequently. the performance proper­
ties of tile adhesive film can be further manipulated, i.e. in
addition to degree of elastomer mastication and formulation.
The use of a slot-die for coating adhesives to web-form
3" mutcrial bas particular advantages over a mull i mll applicator
unit (calendar). Web-form adhesive coating speeds. when
employing multi roll applicator units (calendars). are typi­
cally limited to 300 meters per minute. However. the use of
slot-die coating technology, particularly when employed in
40 conjunction with lower-viscosity. high-solids adhesives, e.g.
80-90%. as opposed to higher-viscosity. 100% solids adhe­
sives. is of particular interest, as application speeds easily
approach 500 meters per minute or more.
The process of the invention permits the production of
45 high-performance self-adhesive compositions and, espe­
cially in conjunction with a downstream coating and
crosslinking unit, permits the production of high-perter­
mance scl l-udhcsivc tapes accompanied by particular cost
advantages.
51) In the first process step, a composition comprising the
elastomers and the known adjuvants required Ior the produc­
tion of self-adhesive compositions. such as extenders, anti­
oxidants, activators. colorants, ageing inhibitors. plasticizers
and tackifier resins, is produced in a planetary roll extruder,
55 the composition having a final temperature of less than 150
0
C., typically less than 130° C. and, more particularly. between
about 25° C. and 100° C. The overall residence time ofthe
composition in the planetary roll extruder wiJl typically not
exceed about three minutes.
60 In accordance with certain aspects of the invention, the
adhesive formulation from the extruder is applied to a web­
Iorm material. This can be done in a particularly effective and
advantageous manner using a slot-die applicator unit. espe­
cially using a rotating lip slot-die applicator unit similar to
1i5 that shown in fIcr. 4.
In accordance with another aspect of the present invention,
the self-adhesive composition may be crosslinked using eJec­
Case 3:10-cv-00076-RLY-WGH Document 1-7 Filed 05/13/10 Page 12 of 17
US 7,476,416 B2
9
tron beams or UV rays to provide a self-adhesive tape having
the desired properties. For further improved performance, Of
in the ease of Electron Beam (EBC)-sensitive carriers,
crosslinking can also be carried out by means of'heat-activat­
able crosslinkers under the effect of temperature. The heating
of the pressure-sensitive adhesive composition that is
required for this purpose can be done with the aid of the
known techniques. especially with the aid of high-tempera­
ture duels, or else with the aid of infrared lumps. or by means
of high-frequency magnetic alternating fields, examples
being l lf waves. UIIP waves or microwaves.
Crosslinking of the pressure-sensitive adhesive composi­
tion can be carried out. furthermore. by means of a combina­
tion of ionizing radiation and hcat-activatablc chemical
crosslinkers. The result may be a highly shear-resistant pres­
sure-sensitive self-adhesive composition. FoB curing sets the
adhesive so that it can be converted while having a residual
latent hcat-activatable curing agent available for end use
application.
For the purpose of heat-induced and/or chemical crosslink­
ing. it is possible in the process of the invention 10 use all
known heat-nctivatnble and/or chemical crosslinkers, such as
accelerated sulphur or sulphur donor systems, isocyanate sys­
terns. reactive melamine resins. Iormaldchydc resins and (op­
tionally halogenated) phenol-formaldehyde resins and/or
reactive phenolic resins or diisocyanate crosslinking systems
with the corresponding activators, cpoxidizcd polyester res­
ins and acrylate resins, and combinations thereof
The crosslinkers are preferably activated at temperatures
above 500 c.. in particular at temperatures from 100
0
c. to
J60
0
C. and, in accordance with certain embodiments. at
temperatures [rom 110
0
c.to 140
0
C. The thermal excitation
ofthe crosslinkers Crill also be effected by 111eanS ofIR rays or
high-energy alternating fields. Some crosslinkers may remain
in the composition after curing and, therefore. be available Ior
activation during the end use application.
Further embraced by the concept of the invention is a
sci f-adhcsrvc tape produced with the aid of the pressure­
sensitive adhesive composition by applying the self-adhesive
composition to at least one side of a material in web form.
Depending on the intended use of the adhesive tape. suita blc
web-form carrier materials for the self-adhesive composi­
lions processed and produced in accordance with the inven­
tion are all known carriers, with or without appropriate
chemical or physical surface pretreatment olthc coating side,
and anti-adhesive physical treatment or coating ofthe reverse
side. Mention may be made, lor example. of creped and
non-crcpcd papers, pulycthylenc, polypropylene and mono-
or hiaxially oriented polypropylene films. polyester, PVC and
other films, foam materials in web form, made from polyeth­
ylene and polyurethane, for example. wovcns, knits and non­
wovens.Finally, the web-form material can be a material with
an antiadhesivc coal ing on both sides. such as release papers
or release films.
111ethickness ofthe self-adhesive composition on the web­
form material can be between I 0 urn and 2000 11m. preferably
between 15 urn and 150 Finally. the self-adhesive com­
position can be applied in a thickness offrom 800 to 1200
11m on a release paper. An adhesive-composition layer ofthis
kind, especially after crosslinking, can be used diversely as a
backing-less double-sided self-adhesive tape.
TIle following examples illustrate aspects of the invention,
without intending to be limiting thereof.It will be appreciated
that other modifications of the present invention, within the
10
skill of those in the art, can be undertaken without departing
from the spirit and scope of this invention.
IU
J 5
2CJ

PRE having three barrel cylinders. represented by 100 phr
JU natural rubber, 130 phr C5 resin, 2 phr Ti02. and 2 phr
antioxidant. The rubber used in this adhesive was SIR Sf,
ground to an average particle size un; nun with talc used as an
anti-agglomerating agent. TIle C5 resin was added in flake
Ionu and Antioxidant was introduced a powder. The adhe­
sive raw materials were all added into the feed throat of 11 70
.1.5
40
45
511
55
60
65
EXAMPLES
Example 1
Ground Ground
Natural Rubber
Rnbhcr Adhesive
Rubber (Kg/hr) 17.1
Resin (Kg/hr) 22.2
TiO} + antioxidant (Kg/hr) 1).7
Speed (rpm) 71)
Adhcsive temp. between h:IITeI 72 l'.
cylinder 1&2
Adhesive temp, between barrel N/A 52' C.
L:ylindcI2&3
Adhesive outlet temperature 86' C.
Extruder Residence Time (5) 1)0
Adhesive homogeneity lvo gets
Mw(GPL'j 4,136,1 lU
Percent Drop in Mw
Mw(fhfH) 1,724JIUO (,9 l.IllJ(1
Percent Drop in Mw 1.)°'0
A standard carton sealing adhesive was produced with the
nun PRE. TIle raw materials were subsequently compounded
into an adhesive after being mixed in three 400 rnm barrel
sections each containing 2 normal and 4 double transversal
mixing spindles rotating at 70 rpm. The finished adhesive wa s
determined to be completely homogeneous (gel free). Subse­
quent molecular weight analysis of the adhesive was CO!l1­
pleted via gel permeation chromatography (GPe) and ther­
mal field flow analysis (Th1'F1'). The molecular weight
ana lysis indicated that the natural rubber had been reduced in
molecular weight by approximately 80%.
Example 2
Ground
Rnhhet
Adhesive
Rubber (Kg/hr)
Resin (Kg/hr)
Ti0
2
• antioxidant (Kg/Iu') n.?
Solveu! {toluene I 12.()
Screw Speerl (rpm)
u'
Adhesive temp, between burrel cylinder 62' C
Adhesive temp, between h:UTCI cylinder 2&3 57" C.
Adhesive outlet tempernrurc -l2" C.
Extruder Residence TilTH.. ' (s I YU
Adhesive homogeneity )',.0 gels
A standard carton sealing adhesive was produced with the
PRI\ having three barrel cylinders. represented by 100 phr
natural rubber, 130 phr C5 resin. 2 phr TiO}, and 2 phr
antioxidant. The rubber used in this adhesive was SIR 51.,
Case 3:10-cv-00076-RLY-WGH Document 1-7 Filed 05/13/10 Page 13 of 17
us 7,476,416 B2
11 12
ground to an average particle sizeof8 nun with talc used as an
anti-agglomerating agent. The C5 resin was added in flake
form and antioxidant was introduced as a powder. The adhe­
sive row materials were all added into the feed throat of a 70
nun PRE. The raw materials were subsequently compounded
into an adhesive after being mixed in the first ofthree 400 nun
barrel sections each containing 2nonnal and 4 double trans­
versal mixing spindles rotating at 65 rpm. The entire cornplc­
rncnt ofsolvent was added viu an injcction valve inserted into
a dosing ring. The finished adhesive was determined to be 111
completely solvated and homogeneous (gel free).
Example 3
15
-continued
Pelletized
Rubber
Adhesive
Screw Speed (rpm) 144
Adhesive temp. between barrel cylinder 1&2 64" C,
Adhesive temp, between barrel cylinder 2&3 2')" C.
Adhesive outlet temperature c.
Extruder Residence Time (1') 120
Adhesive homogeneity No gels
A standard masking tape adhesive was produced with the
I'RF having three bnrrcl cylinders. represented by 100 phr
natural rubber. lIS phr C5 resin. 50 phr kaolin clay. 5 phr
7nO. 2.5 phr Ti02. and 2 phr antioxidant. 111e rubber used ill
this adhesive was SIR 51" pre-masticated and blended with 2
phr antioxidant in a Banbury and subsequently processed in
an underwater pelletizer to yield 8 111m pellets with talc used
[IS an anti-agglomerating agent. 11lCC5 resin was added iu
flake form. and the ZnO and Ti02 were introduced ;IS plW'­
ders. Ihe adhesive raw materials were all added into the
fccdthroat of a 70 nun PRE. The raw materials were subsc­
qucutly compounded into an adhesive after being mixed in
the firs: of three 400 nun barrel sections each containing 2
normal and 4 double transversal mixing spindles rotating at
144 rpm. The solvent was added via injection valves inserted
into dosing rings. with 5 kg/hr added into the dosing ring
located between barrels I&2 and 35 kg/hr being added into
the dosing ring located between barrels 2&3. The finished
adhesive was determined to be completely solvated and
homogeneous (gel tree).
Example 5
Ground
Rubber
Adhesive
Rubber and Antioxidant (Kg/hr) t4.76
Resin - Fccdthroar (Kg-hn R.!)!)
Resin - SIJefeedcr (Kg-hr l
l-il'cr. 7110, Ti02 (Kg/hr) g.12
Solvent - Toluene ':;"3 tKg/llfJ 11.1)
Solvent - Tolucuc . 3i -l tKg/hr) 19.0
Screw Speed (rpm) 141
Adhesive temp, between barrel cylinder 1&2 110 C
Adhesive temp, between barrel cylinder 2&3 61\ r.
Adhesive temp, between barrel cylinder 3&4 33" C.
Adhesive outlet temperature II r C.
Extruder Residence Time (5) 73
Adhesive homogeneity No gels
A standard masking tape adhesive was produced with the
PRF having fOUT barrel cylinders, represented by 100 phr
natural III bber, 115 phr C5 resin. 50 phr kaolin clay. 5 phr
InO, 2.5 phr Ti02. and 2 phr antioxidant. The rubber used in
this adhesive was SIR 10, ground to an average particle size of
8nlln with talc used as au anti-agglomerating agent. A portion
of the C5 resin was added in flake fonn into the feedthroat of
a 70 mm PRE, along with the ZnO and Ti02 powders. The
raw materials were subsequently mixed in the first offour 400
mm barrel sections each containing 2 normal and 4 double
transversal mixing spindles rotating at 141 rpm. The remain­
ing flake resin was added via a side feeder located immedi­
ately upstream from the first dosing ring and subsequently
mixed ill the second barrel section. Solvent was added via
Pelletized
Naluml
Rubber
Rubber and Antioxidant l Kg.hr)
Resin (Kghn
fJlkr, 7110. Ti02 (Kglllr)
Screw Speed (rpm)
temp. between barrel
cylinder
Adhesive ternp , between barrel
cylinder
Adhesive outlet temperature
Extruder Resideuce'! ime (s)
Adhesive homogeuctly
Mw (f,PCj
Percent Drop in Mw
Mw IThFFF)
Percent Drop in .\1\\
!'i/A
KIA
!'i/A
l'iA
KiA
KiA
KIA
1.n2Ci,(i71
666.1)1»)
Pelletized
Rubber
.. \dhesive
cO
14.1)8
15.88
7.93
7ll
50'· c.
c5
5Y' C.
76' C.

No gels
4SY)79
]11
52.J
o
·o
sro.ooo
51.5%
A standard masking tape adhesive was produced with the J5
PRE having three barrel cylinders. represented by 100 phr
natural rubber. lIS phr C5 resin, 50 phr kaolin clay, 5 phr
ZnO. 2.5 phr Ti02, and 2 phr antioxidant. The rubber used in
this adhesive was SIR 5L, pre-masticated and blended with 2
phr antioxidant in a Banbury and subsequently processed in 411
an underwater pelletizer to yield 8 nun pellets with talc used
au anti-agglomcrauug agent. The C5 resin was added in
flake form. and the 7nO and Ti02 were intrndueed as pow­
ders. The adhesive raw materials were all added into the
Iccdrhroat or a 70 nun PRE. The raw materials were subse- 45
quently compounded into an adhesive after being mixed in
three 400 mIII barrel sections each containing 2 normal and 4
double transversal mixing spindles rotating at 70 rpm. 111e
finished adhesive W[lS determined to be completely hornoge­
ncous (gel free). Subsequent molecular weight analysis ofthe 51)
adhesive was completed via gel penn eat ion chromatography
(GPC) and thermal field 110w analysis (ThFFF). The molecu­
lar weight analysis indicated that the natural rubber had been
reduced in mulecular weight by approximately 50%.
i5
Example 4
60
yer.erized
Rubber
Adhesive
Rubber and Antioxidant (Kg/hr) 14.08
Resin (Kg/hr) 15.88
hiler, ZnO, TiO=' (Kg/lIn 7.93
6."
Solvent - Tol1l011e (KWhr) 4().(J
Case 3:10-cv-00076-RLY-WGH Document 1-7 Filed 05/13/10 Page 14 of 17
US 7,476,416 B2
13
injection valves inserted into dosing rings, with II kg/hr
added into the dosing. ring located between barrels 2&3 and
29 kg/hr being added into the dosing ring located between
barrels 3&4. The finished adhesive was determined to be
completely homogeneous and solvated (gel free).
Having described various aspects and embodiments olthe
invention aud several ndvantages thereof, it will be recog­
nized by those of ordinary skills that the invention is suscep­
tible to various modifications. substitutions and revisions
within the spirit and scope of the appended claims.
What is claimed is:
I. A process for preparing an adhesive, the process com­
prising the steps of:
a.) introducing primary raw materials comprising a non­
thermoplastic elastomer into a feeding section of il plan­
crary roller extruder:
b.) conveying the primary raw materials from the feeding
section to a compounding section of the planetary roller
extruder;
c.) mixing the primary raw materials in the compounding
section, wherein the compounding section comprises a
main spindle surrounded by and intermcshed with a
plurality olplanetary spindles wherein at least oue ofthe
planetary spindles is a double transversal mixing spindle
comprising il plurality of back-cut helical flights;
d.] producing a homogeneous adhesive composition: and
e.) applying the adhesive composition to a web-form mate­
rial.
2.lhe process ofclaim l wherein the compounding section
comprises from 3 to 24 planetary spindles.
3. The process ofclaim l wherein the compounding section
further comprises planetary spindles having Ii.IlI helical
flights.
4. The process of claim 3 wherein the double transversal
mixing spindles account for more than 20 percent ofthe total
number of planetary spindles in the compounding section.
5. The process ofclaim4 wherein the compounding section
comprises twice as many double transversal spindles as
spindles having full helical flights.
6. The process of claim 1 further comprising adding sec­
ondary raw materials to the compounding section.
7. The process of claim 6 wherein the secondary raw mate­
rials comprise solid raw materials selected from the group
consisting of thermoplastic elastomers, tackifying resins,
extenders. activators. crosslinkers, colorants. and mixtures
thereof.
8. 111eprocess of claim 6 wherein the secondary raw mate­
rials comprise liquid raw materials selected from the group
consisting of liquid elastomers, molten resins, oils, solvents
and mixtures thereof.
9. The process of claim 8 wherein the solvent is selected
lrom the group consisting or acetone, toluene, hexane, hep­
tane. and mixtures thereof
10. The process of claim I wherein the compounding sec­
tion comprises a plurality of roller barrel sections.
II. The process of claim 10 wherein each barrel section
comprises a double transversal spindle.
12. The process of claim 1 wherein the primary raw mate­
rials comprise natural rubber and tackifying resin.
13. The process ofclaim 11 wherein the primary raw mate­
rials further comprise an activator selected from the group
consisting of zinc oxide.magnesium oxide and combinations
14
14. The process of claim 1 wherein the elastomer is mas­
ticatcd such that M
w
is reduced to less than 1,000,000 as
measured by (iPe.
15. "TIle process or claim 1 wherein the non-thermoplastic
5 elastomer is selected from the group consisting of natural
rubber, synthetic polyisoprene, styrene butadiene rubber.
butyl rubber, polyisobutylenc rubber. and combinations
thereof.
16. The process ofclaim 1 wherein the step ofapplying the
10 adhesive composition to a web-form material comprises a
coating process selected from the group consisting of slot-die
coating, reverse roll. roll-over-roll coating and knife-over-roll
coaling.
17. The process of claim 16 wherein the coating process
15 comprises slot-die coating using a rotating lip die or a fixed lip
contact die.
l8. The process olclairn I further comprising:
f.) crosslinking the adhesive composition.
19. The process of claim 18 wherein step f comprises
211 crosslinking the adhesive composition using a process
selected from the group consisting of EB crosslinking, VV'
crosslinking, thermal and/or chemical crosslinking and corn­
binarions thereof.
20. The process of claim 1 wherein the non-thermoplastic
:25 elastomer has all initial molecular weight (Mldmlriall) bclor
processing and a final molecular weight (Mw(lin"ll) after pro­
cessing and said non-thermoplastic elastomer cxibits a %
reuctiou in M",ofmore than about 50% as caculated in accor­
dance with Formular I:
311
(II.
21 . A process for producing an adhesive composition com­
prising:
a.) continuously metering into a planetary roller extruder
35 primary raw materials of an adhesive composition com­
prising a non-thennoplastic elastomer and a tackilying
resin;
b.) continuously mixing the primary raw materials in a
compounding section of the planetary roller extruder to
4(1
form a homogeneous adhesive composition wherein the
compounding section comprises a main spindle sur­
rounded by and intermeshed with a plurality ofplanetary
spindles wherein at least one of the planetary spindles is
a double transversal mixing spindle comprising a plu­
45 rality of back-cut helical flights: and
c.) continuously discharging the homogeneous adhesive
composition from the extruder.
22. The process ofclaim21 wherein the non-thermoplastic
'0 elastomer is selected from the group consisting of natural
rubber. synthetic polyisoprcnc, styrene butadiene rubber.
butyl rubber, polyisobutylcne rubber, and combinations
thereof
23. The process ofclaim 22 wherein the uon-therinoplustic
" elastomer comprises pre-masticated natural rubber.
24. The process of claim 2l wherein the compounding
sections comprises a plurality of roller barrel sections.
25. The process of claim 24 wherein each roller barrel
section comprises at least one double transversal mixing
611
spindle.
26. TIle process of claim 21 further comprising adding
solvent to the raw materials in the compounding section.
27. '111e process of claim 21 further comprising:
d.) applying the adhesive composition to a web-form mate­
thereofand an extender selected from the group consisting of Ii' rial.
clays. calcium carbonate. talc, aluminum hydrates and C0111­ 28. '111e process of claim 27 wherein the adhesive compo­
biuations thereof. sition is applied to the web-form material using a coating
Case 3:10-cv-00076-RLY-WGH Document 1-7 Filed 05/13/10 Page 15 of 17
US 7,476,416 B2
15 16
process selected from the group consisting ofslot-die coating,
reverse roll, roll-aver-roll coating and knife-aver-roll coating,
29. The process ofcia im 27 wherein the web- form material
selected from the group consisting of paper, polyethylene,
polypropylene, polyester. polyvinylchloride and combina­
tions thereof
30. The process of claim 29 further comprising crosslini­
king the adhesive couipositiou.
31. The process of claim 21 further comprising adding
secondary raw materials to the compounding section.
32. The process of claim 31 wherein the secondary raw
materials comprise solid materials.
33. The process ofclaim 32 wherein the solid materials are
selected tram the group consisting of thermoplastic elas­
tomers, resins, extenders. activators, anti-dcgradcnts,
crosslinkers and mixtures thereof.
34.lhe process of claim 32 wherein the compounding
section further comprises a twin screw dosing unit and the
solid materials are added to the compounding section via the
10 twin screw dosing unit.
* * * * *
Case 3:10-cv-00076-RLY-WGH Document 1-7 Filed 05/13/10 Page 16 of 17
UNITED STATES PATENT AND TRADEMARK OFFICE
CERTIFICATE OF CORRECTION
PATENT NO. : 7,476,416 B2 Page 1 of 1
A?PLICAnON NO. : 10/997827
DATED : January 13, 2009
It'-IYENTOR(S) : JOIUl Kinch Tynan, Jr. et al.
It is certified that error appears in the above-identified patent and that said Letters Patent is
hereby corrected as shown below:
Claims:
Claim 20, Col. 14, Line 25
"befor" should read "before"
Claim 20, Col. 14, Line 29
"Formular" should read "Formula"
Signed and Sealed this
Fifth Day of May, 2009
JOH:'I DOLL
Acting Director oft/If: United States Palen! and Trademark 0.llicl'
Case 3:10-cv-00076-RLY-WGH Document 1-7 Filed 05/13/10 Page 17 of 17