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# OAR Box 

# 1413 Prepped by Ollie Stewart



## Document

Number: 

# 52 ) 11-1-5 2

Docket Number: 

# A-94-5 2

Printed 7/9/2008 3:11:22 PM

Sheet 52 of 114P. 2 A 1/A UU U Ufltt/ t* w A * / U U 

# lll l Unite d State s Paten t(i9

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# lllllll l l 

# »ui„ 1 U 

# „ «,_,, , n US003260006 A H 7 ^"" * 

## Paten tNumber : 5,260,00 6 JJ^J-5 2 Dat e o f Patent : Not . 9,199 3

(54 ] METHO D AN D APPARATU S FO R CONTINUOU S CASTIN G O F POLYMERIZABL E THERMOSETTIN G MATERIA L [75 ] Inventors : Herber tI . Sefccr , PDtesville ; len d S .

Uagar , Randalhtown ; Richar d R . Badtr , Jr , Annapolis , d l o f Md . [73 ) ' Assignee ; Nsrama r Corporation , Odenton , Md . [21 ] Appl-N o J 799,74 0 [22 ] Filed : Nov . 22,199 1

Rdste d US . Appllcstfo n Dat a [63 ] CMuianula a o f

Ser . No . 468.921 . Jan . 23 . 1990* . »Un doned . [51 ] [52 ]

[58 ]

(56 ] Int . CU - 

# us . a ».B29 C 35/1 0 264/2*264/148 ; 264/216 ; 264/236 ; 264/347 ; 264/BS ; 264/166 ;

425/174.4 ; 425/174. 8 * 425/22 4 Fiel d o f Searc h J 264/22.25,26 . IS , 264/331.18 , 148 , 166.216 , 236 , 347 ; 425/224 , 174.4.174, 8 R Reference s Che d U.S . PATEN T DOCUMENT S 2.136.422 2J79.24 S 2,603.14 1 2*663.90 8 &049.76 1 3*091.81 1 M8U4 6 1521.13 1 2J29J2 S 3-mj.a 3^00.49 0 3.801.40 7 3.821.33 7 11/193 8 Field s

C/194 S Muikat . 7/195 2 Seifiiet

f e l sl > . - 12/195 3 Maieratl . . 8/196 2 Ytfcobflt . 6/196 3 Hieken . 1/197 0 Daisies . 9/19X ) Duggin s . 9/197 0 Duggta* . 7/197 1 Meri u 8/197 1 BMngsleyctaf. . 4/197 4 Qoldswonhyct d 6/197 4 BoncUrkeid . . 264/331.1 8

—264/34 7

264/23 6 3,172.19

7 3,894.81 6 3.90(416 8 3,923,94 1 3571.17 1 

## x»njun •4^0136 1 4/HI*4 2 4.133.86 1 4,18604 4 4.221.253 4,298.41 3 4.314.03 6 4.42SJ8 7 4,626,11 7 4.710.SJ 3 4439.12 5 3/197 5

7/197 5 9/197 5 12/197 5 1/197 6 10/197 6 1/197 7 4/197 7 1/197 9 1/198 0 9/198 0 11/198 1 2/198 2 9/198 3 1/198 4 12/198 6 12/198 7 .6/198 9 Katocti l 264/16 6 Kato . Hanus a . Waver . Othtaueia L Kato eta l . MkMu c e t»

U Kkaeia L . Kaio . Bradle y etal . Seibeilin g • Tcare . Throne ai d Hank . He m etal . . Murakam i c i a L — M a 264/34 7

-.264/21 6

.

_264/21 6 FOREIG N PATEN T DOCUMENT S 00368) 9 9/198 1 Europea n Pat . Off . . 0246806 11/198 7 Europea n Pfe b Off . . 3943266 6/198 6 Fed . lUp-eTOeriMn y . 149143 7 7/196 7 Franc

a . 149770 2 9/196 7 Fianc e . 499916 3 9/197 4 Japan . 53-14036 2 12/197 4 Japa

n . Primary Examiner-- Jeffery Thurlo w Attorney, Agnt, orfirm—loots, Day , Reavi s ftRogu e 

### [« ] ABSTRAC T A metho d an d apparatu s fo r continuou s canin g o f poty mernabl e thermosettin g material s oompria m mirin g di e material s wid i controlle d amount s o f tw o e r mor e cata lys tgroup s an d pauin g sai d mixtur e throug h tw o o r mor e serie s o f

heatin g sages . Th e initiall y gelle d mi v tur e whie h ha s no tye tundergon e excessiv e shrinkag e i s mechanicall y isolate d from th e ungdle d mixture .

1 9 Claims , 4 Drawin g Sheet sP. 3



# U.S . Paten

t Nov , 9,199 3 Sheet1 o f 4 

# 5,260,006

RESI N FILLE R 

# 4

PIGMENT S 

# I MONOMERS , MODIFIERS , ETC

.

COMPOUN D MATRI X CATALYSTS SYSTE M 1 

### ^ - U MIXE R I COMPOUNDIN G SECTIO N

CAS T UQUI D MATRI X ONT O A MOVIN G CARRIE R WE B AN D ESTABUS H LEVE L SURFACE

. 

# i l CASTIN G SECTIO N HEAT CELLE D SHEERS ) T O

HIGHE R TEMPERAlllRE . 

# I (HOL D A T A SECOND 7 

### SOAKIN d TEMPERATUR E THA T I S CLOSE ! ' T P TH E PEA KTEMPERATUR E ATTAINE D FRO M TH E AUTOGENI C REACTIO N UNDE R ADIABATI C CONDITIONS

.

HEA T MATRI X T O A GELLIN G TEMPERATURE . 

# I

HOL D MATRI X A T A FIRS T .SOAKIN G TEMPERATUR E EQUA L TO TH E GELLIN G TEMPERATUR E 1 

### UNTI L TH E MATRI X I S GELLE D BU T NO T LON G ENOUG H FD R IT S DENSIT Y T O CHANG E SIGNIFICANTL Y v CELLIN G f SECTIO N CUR E SECTIO N



# » J

PEE L CARRIE R WE B FRO M BOTTO M O F GELLE D MATRI X SHEE T BEFORE SHRINKAG E

BEGINS

. COO L SHEET(S ) UNTI L WEL L BELO W CLAS S TRANSITIO N TEMPERATUR E (fe m WHIL E

II M FLAT . HOLDIN G TH E



### COO L

PHYSICALL Y ISOLAT E DOWNSTREA M CELLE D MATRI X SHEE T FRO M UPSTREAM

. .ISOLATIO N SECTIO N [COO L SHEET S T O ROO M

TEMPERATURE .

COOLIN G SECTIO N 

# Ffe. 1

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# U.S . Patent Nov . 9,199 3 P-4 - 

## Shee t2 o f 4 

# 5,260,00 6



# v 5P J i D M DI-U i TI U TAIO M ^A1_C ^ • 1-i.tL-OU

• IJwi U • UXJOIlU^U t 'ITAL\JI *J U 

# U.S . Paten

t Nov

. 9,199 3 Shee

t3 o f 4 5,260,00 6

TEMPERATUR E O F MOVIN G BEL T O R MOL D SURFAC E

/ VTEMPERATUR E O F

' ^ TH E MATRI X

VISCOSITY RELATIV E LON G PERIO D O F RAPI D SETTUN G O F FILLE R O R PARTICLE S



### —I N MATRI

X — SETTUN G VELOCIT Y

TIM E 

### (O RDISTANC E ALON G BELT ) 

# h DURATIO N

- OF—• ] RADIATIO N TEMPERATUR E O F MATRI X 

# l

VISCOSIT Y

RAPI D SETTUN G PERIO D O F FILLE R O R PARTICLE S (MUC H SHORTE R PERIO D WIT H RADI O FREQUENC Y

HEATING ) 

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# 4

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TEMPERATUR E RIS C DU E T O EXOTHERMI C REACTIO N

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# 1 RRS T SOAKIN G

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## 5,260,00 6 1 2 matri x i s war m enoug h i o "luc k oIT* th e polymerizado n METHO D AN D APFARATXJ S FO RCONTINUOU S reaction whic h the n sustains itsel f

b y it s ow n hea

to f CASTING O F POLYMERIZABL E reactio

n u d actuall

y i s coole d b y dissipatin g hea l bac k THERMOSETTIN

G MATERIA

L t

o tha i environment

. Thi s proces s continue s unti l sub * i stantiall

y al l o f th e unsamrate

d bond s o f

th e resin an

d Th b application i

a a continuatio

n o f application Ser . monome r component

s nr e consume d and th e resin i s N a 07/468,921 , filed Jan . 23,1990 , no w abandoned . cued . The .mel d I s then opene d nite r codin g an d n 

# .ACKORO U 

# K D 

# OFTME D 1 

# V EOT 

# , O N 

# •X - 

# «^'E3:52tt?2 I . Rei d o f

th e Invention 1 0 thermodynami

c an d many othe r aspects ofthi s conven Th e presentinventio n relate s t o » ne w metho d in d tona l approach, apparatu s fo r continuously eastin

g certai n thick , shee tSue

h a batc h proces s has significanc e shortcomings , material s sometime s used a i surfac e overly , bu

twhic h I ti s slo w an

d inefficientrequirin g n grea tdea l o f mate * als o ean b e used , withoutunderlay, suc h a s for a stand - ria

l handlin g equipmentI tpresent

s significan

tpruibalon e restauran

ttable top . Mor

e particularly , th e pies - I

S len s wit

h controlling th e matrUmriformitym th e mold , en tinventio n relates t o a ne w metho d an d apparatu

s fo r particularl

y where decorativ e partide s ar e nse d i n th e continuousl y castin g polynurictbcrinosettin g materials matrix. Fo r example , flow patterns an d convectio n whie h shrin

k durin g polymerization . cunenuinthemstrixcinresaltinnonunifonidtyofd> e I L Descriptio n o f

Ui e Prior Ar

tdecorative pattern. I n addition , aue h a batc h proces s Thermosettin g polymeric material s suc h as thermo - 2

0 ca n presen tcuring problem

s i f th e matri x i s no theale d settin g rains ar

v commonl

y use d a s surfac

e coverin g uniforml

y and , thai , doe s no tpolymeriz e atth e same materials . Sheets o f

thes e material

s ar e ote d a s decora * sat

e throughou

tth e mold cavity . Th e resul tca n b e tiv e finishin g material

s i n ne w boOdm

g constructio n an

d localize d shrinkin

g whic h ma

y caus e crack s o r tears i n remodelin g fo r aud i applications a s bathroo m vanit y th e final core

d materia l tops , kitche n counte r tops , furnitur e components , res - 2

5 Severa

l prior attempt

s hav e been made t o develo p a tauran ttables , wal l panelin

g an d othe r uses . Th e sheets continuous castin g techniqu e e a a n alternative t o th e ee n b e nud e o f

plai n soli d colo n o r can b e patterne d t o batc

h process fo

r thermosetting "f'Trif 1 * whic h shrin

k hav e tb e appearanc

e o f marble , granit

e o r othe r patterns upo n curing . U.S . Pat . N a 3,60049 0 issued t o BQlings o r texture ! decoratio n and ofte n ar e loade d wh h decora - le y eta l for example, teache s tha ti f th e stmctur e core s liv e particle s t o provide thes e characteristics . Th e rain 3 0 unevenly , s s busil y th e case , ocrtni n area s ofth e mas

s compositio n typtcsDy include s minera l fillers such a s wil l harde n an d shrin k unevenly , distortin g th e east calcium carbonat

e o r aluminu

m trihydrate. I ti s pre - produc tT o avoi d th e proble m o f wrinklin g o r tearin g felted tha tth e patter

n i n thes e material

s b e uniforml

y a n th e snrfhe

e o f th e matri x durin g shrinking , Biffings * distribute d an d tha tth e fins) produc

tb e flat , smoot h le y teaches th e us

e of a thi n film and lubrican

tt o penn b and fre e o f

warpage . bend s o r wrinkles . I ti s als o pre - 3

5 belto f tb e conveyor . Specifically , Billingsley teache s a -ferre d tha tn flatsurfac

e b e obtaine

d wit h tb e minimu

m proces s whereb

y tb e matri

x rests m s laye r of a A m o f sanding o r machining . • which shrink s durin g bestin g a tth e same rat e n s th e Th e compositio n ofthes e material s typicall y ca n b e a curin g matrix

. BOtingsle

y teache s th e us e o f

oi l o r a singl e thermosetting resi

n o r a mixtur

e e f resin s suc h a s simila

r liqui d lubrican tbetwee n th e film laye r aa d d w unsaturate

d polyesters an

d acryli c resi

n precursors . 4 0 conveyo r beh . I n thi s approach , th e film shrink s wit h Such resin s requir

e a caulys tand/o r promoter system th e matri x an d th e thi n film doe s no tban g u p o n th e t o initiat e th e proces s o f

free radica

l polymerization , conveyo r belt s as i tshrinks . Typica l resin s ar

e characterize

d b y havin

g a significan

tAnother cononuoos castin g approac h ca a b e fonn

d i n exothermi c reaction during polymerizatio n an d a sub - US . Pit . N a 3.9M.098 issue d i o Kat o e ta l Kat o stantia l increas e o f

densit y durin g tha tprocess . Thus , n 4

5 teache s a dua

l bd tsyste

m whic h use s th e forc e o f a typical mixtur

e o f 65 % filler an

d 35 % resi

n (a "matrix" ) confined spac e t o control th e tendencie s ofth e matri x t o shrink s durin g th e polymerizatio n process s o tha

tth e distor

torsee r Itsel

f apar tdurin g th e polymerixadon cure d soli d compositio n ha s a densit y abou t5-7 % process . Tb e matri x b passe d through a confine d spac e highe r tha

n th e liquid matrix. Thi s shrinkag e present s define

d b y uppe r an d lowe r belts whic h force th e mstrix processin g problem

s relate d t o th e presen

tinventio n S

O t o maintai

n a fiatrectangula

r cros s sectio n despite di e which ' ar e discussed bdow . presenc e o f interns ! force s broughtabou tb y localize d A variet y o f prio r method s hav e bee n use d t o achiev e curing whic h woul d otherwis e caus e th e matri x t o pull syntheti c sheetmaterial

s havin g a decorativ

e pattern , apart

, war p o r bend . On e metho d involve s a batc h process , h i thi s process . Fro m th e foregoing I

tca n b e see n tha

tth e prio r ar

t th e matri x i s prepare

d b y mixin

g ib e thermosettin

g 5 5 continuou

s canin g processe s involv e expensiv e an d resins wh h tb e filler an

d th e desire

d decorative panicle s complicate d arrangement

s l o contro l ib e curing o f tb e o r colorin g material

s an d a standar

d quantit y o f cats - thermosettin

g material. Prior a n castin g method s als o lyst . Th a amoun

to f catalys ttypicall

y recommende

d i n pos e quaUt

y problems . I n conventional be h castin g th e prio r ar

ti s on e half

t o tw o percen

tbase d o n th e equipmen

tth e liqui d mstri x ofte n i s heated b y tb e eon Hqui d resin fraction. Thi s matri x I s the n poured o r 6

0 duction o f

hea tthroug h thebdt s whic h ar

e endose d i s pumpe d int o a larg

e casting mol

d an d seale d in the a

n environmen

to f heate d fluid o r gas . Wit

h ooaven mold . Th e mol d i s then subjecte d t o sufficien

theatt o tioaa

l conductive heating , i f

th e mol d o r bel tsurface i s begi n decompositio n o f

th e catalyst

, which initiate s to o hot, i twill cause initiation of a rapid aooeleruhng polymerisatio n o f

the rcsin . Becaus

e th e polymerizatio

n reactio

n befor e curin g l a complete . Thi s can caus e loca l i s a n exothermi c process , th e reactio n contribute

s t o th e 6 5 boiling , o

r a tleast, irregula

r cur e wi m shrinkag

e hea to f th e system leadin

g t o furthe r catalys tdecompo - stresses , cracking, ripple , craz e layers , etc . I f th e heating sltio n and a

n increase

d rat e o f polymerization . Tiii s i s done o n a single supportin g bel t(withou ta to p belt) , follow s tb e convectiv e hea tenvironmen

tapplie d t o the tb e botto

m o f th e mstri x laye r can polymeriz e before 

# (0P. 8



### 5,260,00 6 3 4 th e top , causin g sever e warp , concav e upward . Also . an d withouttransmittin g stresse s t o th e softe r ge l excessiv e temperature difference s betwee n th e matri x forme d durin g th e initial gellin g i n th e firatzone . Ac resul ti n objections ] appearanc e o f mottlin g o r streaks . cordin g t o th e invention , substantiall y adiabati c corin g Thus , th e us e o f

convectio n hea l an d typica l bd l SI'S - oondition a preferably ar c supplied I n Ih e secon d zone , tern s wil l resul ti n th e nee d t o limitth e rat e o f heating , S Th e presen tinventio n ba s th e benefi to f providin g a n resultin g i n a lon g heatin g tim e whic h the n require s a efficientuncomplicate d metho d o f continuou s castin g highe r matri

x viscosity , an d longe r equipmen ti n th e Ou tavoid s th e creatio n o f inten d stresses . I tha s th e cas e o f continuou s casting . Problem s aris e becaus e wh h benefi tofprovidin g a mean s t o isolate th e curin g matri x th e longe r heatin g time , th e viscosit y o f Ih e matri x i s from destructiv e internal an d extema l force s whic h reduce d fo r a longe r perio d o f tim e befor e I

trapidl y 1 0 toa d t o produc e distortion . I tab o ha s th e Vrnif h et dimb s jus tprio r t o gelling . Till s i s illustrate d i n FIO . 1 . producin g a cure d homogeneou s matri x wit h unifor m Tb e lowe r viscosit y fo r a n extende d tim e permit s lh e propertie s an d appearance . I tab o h u th e benefi to f minera l filler t o settl e an d als o *n y dens e panicle s use d providin g individua l sheet s whic h shrink uniforml y to decorativ e effec tma y s* ^ resultin g i n a non - throughou tth e shee tmateria l thu s avoidin g warpage , homogenou s shee tbot b m physica l properties , and i n 1 5 wjvfaess , o r odie r sign s o f irregular ihrinkag e durin g appearance a

ta cu tedge . c m eve n thoug h n o externall y applied pressur e bpro SUMMAR Y O F TH E INVENTIO N -Had. Additiona l advantage s an d benefit s wil l b e ap - ..-., . paren tt o thoa e skille d i a th e a n upo n readin g thi s dh > I ti s a n objecto f

th e presen tinventio n t o provid e a n closure , efficien taa d simpl e metho d for continuou s castin g o f 20 tbenaosettin g material s whic h shrin k upo n curing . I ti s BRIE F DESCRIPTIO N O F TH E DRAWING S a n objec tt o provid e a metho d ^ e 

### }^ eK 

### ***J" FIO . 1 i s a schemati c flo w fflustrstioa whic h depict s problem s o f

particl e settlemen tan d surfac e distortio n tk - 

### _-~~ « „ M 

### «-«««. . * . „-, , —Z^J—. • Jr\tZ durin g th e corin g process . I

tu « objec

tt o provid e a SLEThSSK.^^ ^ t o on e embodimen

l o f th e metho d whic h will preven

tth e creatio n o f interna l 1 5 "TO . 2 fa a diagiamatl

c sid e devationa

l vie w o f oo e stresse s (an d th e associate d problem s o f warn , cur l an d i « Mi^TMTM**** . H»«ITHMH I W W 

### w

t« n whlcbwfilavoythetendeneyorthesbrinkingmatii x J^^?ff^^l^£^t?2jJ ^ t o detac h itsdf du e t o shrinkag

e from th e Squi d matri x ^J? 1 

### * * o f



### t " % . * * *J5fiL*fa* ? attteenrryeadofthe^m ? ^ w 

### matri x prio r s o the gellin

g m a ccnvendona

l heatin g Addmona l Objects , advantage

s an d nove l feamre s o f "»•?,,TS^^n^SSSL^S , th e inventio n wU l b e se tfortht o pa n ia th e descriptio

n .r^"'**^3^i^ , 

### T^^z!^. * whic h follows, «, d i n pa

n wfllbecom e appaie

u t o **?**»** "I* - 1 

### £* £ ft"* ? f ^Ti thos e skille d i a th e a n upo n examinatio n ofth e follow . £* • «*••••»* ; P 0ttW e b 

### » * • «»P">Y« I ***** « * in g o r ma y b e learne d b y practic e o f th e invention . Tb e J

$ "epresa tinvenfitm . objec u an d advantage s ofth e inventio n ma y b e reahzr i , "? • » • • ff* ****** • » « abo 

### » a 

### * n < 

### j f » • an d attained b y mean s o f

th e instrumentalitie s an d com * healin g sequenc e accordin g t o th e presentinvention , bination s particularl y pointe d on ti n th e appende d DETAILE D DESCRIPTIO N O F TH E PRESEN T d 

### ^ W 

### * J 

### . . -. , , , ^ u . A m. . INVENTIO N T o achiev e th e foregoin g an d othe r object s and i

n 4 0 . ^ . accordanc e wh h th e purpos e o f tb e presen tinvention , **• * P*© 6

### ** * »*? • «th e presentinventio n ar e sebe th e inventio n provide s a metho d an d apparatu s for con - markall y illustrate d i n F1Q . tA a ahow a i n FIO . 1 , t o tinuons castin g of a polymerizabl c thermosettin g mate* hegin , •" " m 

### • ,,is 

### , i , 

### W*** """ f • •mixtur e o f resin , rial whic h shrink

s upo n curing . Accordin g 1 0 th e pres - fiDer

### *** opdo*mt f inononiera , modifiers o r othe r tngre ^ en tinvention , th e thermosettin g compositio n I s mixe d 4 5 dbnts . Th e matrix i s the n prepare d for castin g wit h th e usin g a controlle d amoun to f a firstcatalys thavin g a addWo n o f pigmentsan d catalysts . Th e decorativ e shee t limite d activatio n temperatur e an d a secon d catdys tnateria l ma y b e mad e o f an y thermosettin g materia l hsvw g a sufllcitnil y highe r activatio n temperature . Th e *«*• « th e desire d propertie s o f bee tresistance , colo r matri x fa then deposite d i n a control M amounto n a stability , clarity , domica l an d stai n resistance , aa d singl e laye r we b whic h i s travelin g o n a conveyo r o r S O othe r physica l propertie s snitab k fo r eas y mtchinsbilii y eve r a fixed supportplate . Th e matrix , whic h i s fas a an d fabricatio n hs th e polymerize d (bra . Hi e presen t liqui d state , i s allowe d t o trave l b r enoug h t o allo w th e inventio n i s particularl y we U suite d l o material s whic h to p surftc e an

d edge s 10 becom e leve l and smooth , shrin k upo n curing . Suc h thermosettin g material s ar e Accordin g l o lh e presen tinvention , th e matrix i s ibe a discusse d i a greate r detai l below . heate d fata firstzon e t o a temperature lha tinitiate s 5 5 A oatdys tsyste m typicall y consistin g o f tw o o r mor s decompositio n ofth e catalys thavin g tb e limite d active - catalys tgroup s i tused . Th e catalys tgroup s ar o selecte d tio n temperature . I tha tbee n found i n accordanc e wh h suc h thaton e catalys tgrou p ha s a limite d activatio n th e presentinventio n Iha

l th e mstrix es n b e mad e t o temperature aa d th e remainin g catdyt tgroup(s ) hav e a partianypdymerii e t o a rubber y g d quickl y i n th e firat-sufficientl y highe r activatio n tenipcistitfc . Typically , zon e withou texcessiv e shrinkage . Th e gelle d matri x fa 60 eac h o f

thes e group s oomp:rfse

s onl y a singl e catalys tbu t then mechanicall y isolate d from th e Uquid matri x nea r ca n b e mad e o f

tw o o r mor e catalys tl a a group . I tfa th e entry end . Th e gelle d an d isolate d matri x i s then critica l for performanc e tha

ttb e difference i n tempera heate d i a a secon d zon e t o a highe r temperature tha ttur e betwee n ih e lowe r activatio n teaperatur e caulys t initiate s decompositio n o f

th e secon d caulyst , whic h grou p an d th e nex thighe r activatio n temperatur e cata ba s a sufficiently hig h activatio n temperatur e Accord * 6 5 lys tgrou p mus tb e s i leas t1 0 degree s fthrenhett. Th e in g t o th e presen

tinvention , i tha s bee n foun d tha tth e preferre

d diflerenc e i s a l leas t3 0 degree s and . i n th e isolate d gelle d matri

x ca n freel y shrink i n th e secon d preferre d embodiment , Ib e differenc e i s a tleas t5 0 de zon e withou tcausin g wrinkle s o n th e botto m surface greet . 

# nP. 9 

## 5,260,00 6 5 6 Th e activatio n temperatur e o f th e firstcatdys tgroup whic h tak e plac e later in th e process . A s explained should b e i n th e rang

e o f 10 0 t o 220 degree s F . Th e belo w i n greate r detdl , this i tdon e i n tw o step s i n th e activatio n temperatur

e ofth e nex

thigher catdys tgroup preferre d embodiment

. Firs tth e carrie

r we b i s pede d ahoul d b e i n th e rang

e o f approximatel

y U O t o 28 0 from th e botto m ofth e gelle d matrix . Next , th e gelle d degree s F . Th e preferre

d rang e for thi s secon d group i s 5 mstri x n physkdl y isolate

d fro m tb e upstrea

m matrix. IS O t o 2B0 degree s F . Thi s ma y b e done b y a variet

y ofmethod s suc

h as pinc h A variatio n o n thi s metho

d use s s singl e temperatur

e rollers or , in th e preferre d embodiment

, b y cuttin g th e activatio n of a portio n ofth e catalys t(th e firstcatdys tcontinuous gdle d shee tint o predetermined length s group) , havin g another portio n o f th e catalys t(th e using a travelin g saw . secon d catdys tgroup) , t o activat e a ta suffideatl y I

O Th e isolated gdle d matri x fa the o heate d t o a secon d highe r temperature . Fo r purpose s o f thi s discussion , an

y temperature. Th e secon d temperatur e i s sufficientt o such metho d whic h involve s caulys tactivatio n a ttw o aeti ^ aMt tmar e o f tb e remaining eatalyst

tgroup s o r mor e differen tstaged temperature

s wil l b e included sodthei^imtktcanacoeleraiodpol'ymeritaiionraac withi n tb e definitio n o f

th e caulys tsyste

m o f th e pres - tioo which reaction generate s hea tto th e preferre d *cn tinvention . I S embodiment

, th e matri x b then hel d a ta secon d soakin g I l fa abocritk d tha

tth e amoun

to f th e catdys thav . temperatur e approximatel

y equ d t o th e pea

k tempera in g th e lowe r activatio n temperatur e b e limited such ture obtaine d fiom Ib e heato f

thi s secon d reactio n th u th e lowe r tempenture catdys tgroup wi n brin g unde

r adiabati c conditions . Th e matri

x ia hel d a tthi s abou ta proper amoun

to f parti d polymerizatio

n ofth e temperatur

e a tleas tunti l th e shrinkage fa substantially matrix . Th e minimu

m amoun to f lh e lowe r temperatur

e 3 0 complete . I n th e preferre d embodiment, i tfa hd d a tthi s catdys tgrou p selecte d i s th e amoun tsufficien tt o caus e temperatur

e unti l th e desire

d polymerisatio n fa oom th e matri x t o polymeris e t o a rubber y g d befor

e i tha s ptete . reached th e poin ti n tiie proces s where th e matri x i s Findly , th e sheet s are hd d fiatand coole d unt O wd l mechanically isolate d fro

m th e les s polymerized matrix. bdo w th e glas s transitio n temperatur

e o f th e matri

x A s o n uppe

r limit , th e amoun

tofth e lowe r temperatur

e 2 5 materid . I

n coolin g a relativel y thic k shee to f plasti c caulys tgroup shoul d b e hel d belo w th e amoun t.whic h composition , unequa l shrinkag

e stres s "ma

y occu r woul d caus e excessiv e Shrinkag e o f th e matri x befor e i tthroug

h th e cross-section du e t o th e fac tthatih e surfoc e has leache d th e poin tin th e proces s where th e matri x i s o f th e shee tmus tcoo l befor

e th e center . I f

th e coolin g mechanically isolate d fro

m th e les s polymerize

d matrix. i s slightl y asymmetrica l from on e race t o th e other , th e ExcettivesluulugefathataiioumwliicKinthecaseo f 3 0 shee tcas twar p o r cur i durin g coofing . whic h warp o r th e give n matrix , causes th e matri x t o form surfac

e cur l ca n b e permanen

tThus , during th e coolin g phas e wrinkles , resided stresses , war p or.l n extreme cases , t o iti s preferre d t o hol d th e sheet

s fla tunti l wd l bdo w th e tea r itsel f apartThus , th e quantit

y ofth e lowe r temper- glas s transitio n temperature

, atur e catdys tgrou p preferabl y i s n o mor

e lha n lha tTh e preferre

d method o f

beatin g i s b y a radi o fro whic h fa Jus

trequired t o brin

g abou ta rubber

y g d 3 5 quene y field. B y thi s method * th e Squid matri x ca n b e under th e selecte d firsthearin g condition s A s explaine

d heate d very rapidly withoutloca l teaperatur e varia more full y bdow , i tha s been foun

d tha tth e matri

x ma y tion! tha

tcaus e objection* ) flow pattens . Aha, pro b e paniaD y polymerize d t o the poin to f creating a soli d vfde

d ho tspo u du

e t o Interferenc

e node s a n eUml

rubber y materia l suitable fo r furthe

r processing i n ac - nated . ih e uppe r temperatur

e limitdurin g gdlin g ea

n b e cordance with th e inventio n befor e a n excessiv e amoun

t4 0 raise d withou tidtiatin g •K^P**- * prematur e autogeni c o f shrinkag e occurs . Th e amoun

tofth e lowe r tempera

- reaction. Thus , a shu n heatin g section * les s restriction s tur e caulys tgroup , expresse

d a s percen

tsctiv e o f cau - o n matri

x viscosity , negligibl e settlin g o f filler, and lys tbase d o a th e liqui d approximsldy 0X101 0 sn d 0.02 exedien thealin g conlrol dynamic

s ar tobtained , percen tgive s a convention d matri x compositio n an

d Os o embodimen

te f s n apparatu

s accordin g t o th e ove n parameters . Th e preferre d rang e i s betwee n sp - 4

5 presen tinventio n i s shown i n FIO . 2 . Tb e castin g appa proximatd

y Q0O1 3 an d OSH. Thi s fa discusse

d in greate

r ratusofFI0.2ma y b e divide d int o tw o genera l section s detai l below . for purpose s o f dlscusrion , Th e firstia a aectic o i n whic h Retunung ; toFIG . I , th e liqui d mstri x with th e adde

d tiie mstri

x I s cas tan d initially gdle d Th e secon d i s a catdys tsystem i s dispense d in controlled smoun u onto sectio n i n whic h th e matri

x to full y polymerize d an d a movin g carrie

r we b aa d moved a sufficien

tdistance t o 5

0 cooled . Thes e section

s ar e divide d b y a mean

s whic h establis h a lev d surfac e I n th e nex tste p o f tb e proces s serve s to isolat e th e transmissio

n o f mechsiuca l stresse s deplete d i n FIGS . 1 an

d 5 , th e matri

x i s quickl y poly - resulting from tutri x shrinkag e from th e gellin g stag e merite d t o th e pointwher

e i tcreate s a soli d rubber

y gd . o f

th e process . l n ue'preferre d embodiment , thi s i s accomplished b y Viewe d fro m lef tt o right, tb e presen

tinventio n pro heatin g th e nutri a b y radi

o frequenc y energy t o a first5

5 vide s a n unwin d roll 2 which carries s we b 4 upon tempenture (tb e gellin g temperature ) an d holdin g th e which th e matri x i s cas tI n oo e embodimen tthi s we b matri x ata aoakin

g temperatur

e equ d t o tha

i tempera- oonsU u o f

a release coated roDoTpsper, bu ti tcouJ d b e tore fo r a -predetermine

d lengt h o f time. Th e firsttem - an y manne r o f travdin g surfac

e such a s a properly peratur e fas temperatur

e sufficien tt o activat

e th e lowe r treated conveye r bd tT o tb e rightofth e roll 2 ther e fa activation tempentur e caulys tgrou p bu tao thig h 6 0 provided a conveye r platfor m 6 whic h run

s th e entire enoug h t o activate tb e second catalys tgroup . Th e ma

- lengt h of th e firstsectio n o f

th e apparatus . Th a coo tri x i s hel d a

tthi s temperatbr

e unti l th e matri

x ha s be - veyo r platfor m 6 . provide s a surfac e aeroa a whic h we b 4 com a a rubber

y soli d bu tha s no tye tha

d a n excessiv e fa pulle d I

n th e antin g process . Th e conveyo r platfor m change i n i u density . Activatio n temperatur e i s th e 4 i n o f a sequenc e o f

fla tsap temperetur

e a twhic h th e catdys trapidl y decomposes 6

5 por tsurface s mad e o f shee tmet d o r othe r materi d in resin an

d initiate s a polymerizatio n reaction. suitabl e t o ihe environment . Th e portio n o f

th e surfoc

e Next , th e matri

x i s manipulate

d t o isolat e th e gellin g i n th e radio frequency cavitie s describe d belo w nam sectio n fro

m th e transmissio

n o f shrinkag e stresse s idl y mut

tb e nud e of

a radio wav e transparen

tmateri d^ P.1 0 

# " .^myy^Myyriyrrrr^; .'., " r 

# 101-60*1040*'»toi ov 3,260,006 7 8 suc h a s plat

e glass , polypropylene , glas s reinforce d tion snd withoutcausin g shrinkag e tha tca n caus e th e silico n resi

n an d others . carrie r web t o ripple o rwrinkl e befor e i tis peele d of

f b y A tth e entranc

e en d o f tb e conveyo r platform , ther e rolls 20,2 2 an

d 24 . i s provide d a

n apparatu

s fo r foldin g sharpl

y uprigh tthe We

b 4 then advance s throug

h exi tinterferenc

e chok e edge s o f th e pape r we b 4 l o for

m vertical edge s o f

a 5 1 6 an

d throug h isotherma

l soakin g chambe r I f whic h i s predetermine

d height . Thi s cause s we b 4 t o tak e the maintaine

d atth e sam

e firsttemperatur

e throughoutit s form o f a continuou s pan . I

twQ I b e obviou s t o thos e length . In thi s manner, th e combinatio n o f starting resin, skille d i n th e s n tha

tothe r means coul d b e used t o catdyst , firs theatin g temperatur

e an d rate o f advanc e provid e appropriat

e edge s t o th e we h t o reui n th e ma - ofth e we b ca

n b e adjuste

d ro provide a firm rubber y g d trix . Doumatrea

m ofth e foldin g apparatus there i s pro * 1 0 exiting th a soakin g chambe r I f whic h g d ha s no tye t vide d a eaatin

g hea d g fo r th e liqui d matrix. Down * undergon e excessiv e shrinkage , strea m from th e castin g head tther e fa provide d a con - Th e geUe d matri x shee t4 2 carrie

d o n th e we b 4 vemioa d radi

o wav e interference chok e 2 0 whic h pre - emerge

s from soakin g chamber I I int o tb e bobdo a vent tth e radi

o frequency energ y from leaking ou tInt o section . There , th e we b 4 fa peele d from th e botto m o f th e room . Th e interference chok e 1 0 i s attache d t o a 1 5 tb e matri

x sheet42 . The n trsvdin g saw 2 4 whos e ma firstheatin g cavity 12 . A s mentione d above , i n tb e re - chine dircction d velocit y fa carefull y aynchronisad gio n ofth e heating cavity 1 2 th e conveyo r platfor m 6 fa whh th e we b 4 velocity , make s a transverse co tthroug h constructe d o f

a radi o wav e transparen tplate . Th e th e matri x 42 . Tbf a separation b y cuttin g i s a preferre d heatin g cavit

y 1 3 i s appropriaid y blankata d wit h mar tmetho

d o f physicall y isolatin g tha dalicat- a aa d deform* - ga s throug

h inlet1 4 t o avoi d th e possibilit y o f igniting 2

0 able portions o f

th e gelle d matri

x from shrinkage flammable gase s du e t o th e potenti d electrical arcing . stresse s produce d i n th e downstrea

m curin g step . Tiios e T o th e ex h aid s o f th e heatin g cavit y ther

e i s pro - skille

d in th e srtwil l recognize tha tothe r method s o f vide d s n exh interferenc

e chok e 16 . Adjacen tt o th e exitprovidin g physic d isolatio n ar

e ab o possible. ' interference chok e 1 6 ther e fa provide d a firstbother - In thi s embodiment, th e individu d gdle d sheet s 4 4 m d soakin g chambe

r 14 . Th b b constructe d suc h tha t2 5 ar e redeposlte

d o n th e movin g we b 4 . Th e we b 4 , no w di e temperatur

e o f Ih e environmentsurroundin g th e loosd y supporting flu gdle d duet t44 , advance s int o matri x i s unifor

m o n al l sides , includin g th e bottom th e second heating, cavit y 32 . Her e th e gdle d shee t4 4 fa whic h has s beating due l belo w th e conveyo r platfor m heate

d t o s secon d temperatur e tha i activate s th e re 4 . mamlngcatdy ^ Th b initiat m a reaedoa ofth e partially Jus tbeyon d th e exi ten d o f th e firstfaothermd soak*

- 3 0 pdymaize d rcsi n which , a s describe d below . I s carrie d in g chambe

r 14 . a aerie

s o f non-driven roller s 20,2 2 an d outapproximaidy adiabstically . Th e polymerizatio n 2 4 fa provided beneat

h th e pisiform < I

n a configuration cause s th e temperatur

e o f th e gelle d mstri

x 4 4 t o rapidl y whic h draw s th e we b 4 awa y from th e gelle d matrix. In increas e t o a peakvdue . Thi s pea k valu e depend s o n th e th e regio n where th e matri x sn d we b are separated , degree o f polymerizatio n whe n lh e reaction begins , th e ther e b provide

d a travelin g saw

* 26 . 3

5 concentratio

n o f resi n m th e matri

x an d th e hea l capac Downstrea

m o f di e travelin g sa w 26, ther e i s pro - h y ofth e matrix, vide d a secon d sectio n o f conveyo r platfor

m 24 . Ju n Th e rapidl y curin g matri

x 44 , afte r exitin g chok e 34 , beyon d th e secon d sectio n o f conveyo r platfor

m 24 , enter

s th e soaking chamber M l Th b chambe r S I fa main ther e fa provided a secon d radi o wav e interferenc e tame d a tapproximaid y th e sam

e temperatur

e a s tli e chok e 2 0 adjacen

ta secon d heatin g chamber 32 . Agdn . s o expecte d pea k temperatur

e o f th e exothermi c curin g th e heatin g dumbe r 2 2 i s appropriately blankete d wh h / reaction i n orde r t o provid e s n adiabati c reactio n envi iner tga s throug

h inle t34 . A tth e exi taide ofth e secon d \ ronmentTha tis , sinc e th e surroundin g ga s an d sup beatin g chambe

r il there fa provide d a

n exi l interfer

e portin

g member s i n th e chambe r 2 1 ar

e hd d t o th e sam e enc e chok e 36 . Adjacen

tt o lh e exi l Interferenc

e chok e temperatur

e as th e expecte d pea

k o f th e curin g matri

x 24 , a secon d soakin g chamber 2 4 b provided . Down - 4 5 shee t44 , th e matri

x effectivd y fa i n therma l isolatio n strea m o f th e secon d soakin g chambe r 34 , ther e fa a from it tenvironmet M durin g ihbsoaltingand.pdym ^ coolin g section . ~ zitfo n process . Th b provides E a unifor

m tereperarur

e In th e preferre

d embodiment

, operatio n o f

th e appa - profil e te s D directions , unifor

m cross-sections ! shrink rate s o f th e presen

tinventio n proceed s a s follows . A age an d mhtlmiiatio n o f

warps , wavines s aad unbal rdeas e coate d pape

r sheet4 i s pulle d from tb e roll 2 an d 5 0 ance d stresses . threade d throug

h th e entir

e lengt h o f ih e equipmen

tHn e Th e presen

tinventio n relies, in part , upo n eertsi n t o th e motorized rewin

d rol l 40 . A s th e we b 4 advances , -relationship s fatth a shrinkage an

d polymarizstio a prop jus tprior t o tb e entrance t o ih e eastin g section , ib e erties o f thermosetting resi n materials an d thd r cats edge s ofth e we b 4 ar

e folde d Sharpl

y uprigh tt o for m a lyt u systems dbcovered'i o b e advantageou s i n th e con movin g troug

h wit b vertic d edges . 3 5 tinueus casting o f

thermosettin g materials . Various ms A liquid matri

x 4 2 s s describe d abov e b pumpe d a ta teria

h were use

d i n th e work reported sn d tha msteria b constantflow rat

e throug h th e castin g hea

d I onto the ofth e presen tinventio n ar

e characterised a s follows bu t movin g web 4 . Th e relationship amon g th e matri x flow ar

e no tmean tt o b e limite d b y th e folbwit ^ deacriptien . rate , th e we b velodt y an

d tb e we b widt h csublbhe s th e Thos e skilled i a th e ar twil l recognise tb e variou s sverag e thickness o f

th e liqui d mstri x 42 . Th e we b 4 C O classe s c f thermosetting materid s whic h ea n b e use d i n advance s a sufficien

tlengt h t o allo w tb e liquid matri x accordance-wit

h th e presen tinvention . *42toflowtoalevdsurfkee.Theweb4thenentersth e ^ ^ ,

_. firstheating cavit

y 1 2 throug h th e interference chok e Polyeste r Kes u 10 . I n tha theatin g cavit y 12 , th e liqui d matri

x b heate d A a unsaturate

d polyeste r easting resin fa prepare d b y t o a firsttemperature selecte d t o activate Ih e lowe r ( 5 a condensatio

n reaction o f

dihydri c dcoho l sn d dibari e temperatur

e caulys tgrou

p an d caus e polymerization t o adds . Th e viscou s reaction product s ar e the n dissolve d a g d stat e withou tcausing prematur

e initiation o f

the i n viny l o r acryli c monomer

s auc h as styrene , viny l othe r caulys tgroup(s ) o r a strongl y exothermi c rcac - toluen e o r methyl methacrylat e (MMA) . Tb a resins 

# 9PJJ

_ 

### S.260,00 6 9 1 0 use d containe d abou t30% styren

e monomer

, abou t50% t

o 65% , th e lowe r ratio , o f course, brin

g th e mos t 0-15 % MM

A monome

r an d hav e a viscosit y o f abou tdifficd

trebtiv e t o hea to f reaction. The lower pre

50 0 t o ZO0 0 cp a t2 0 degree s C . ferre d rati o o f AT H b approximatel

y th e minimu m These resin

s typicall y contai n a smal l amoun to f in - concentratio

n tha tstil l provide s goo d fire-hazard char

hibhor , suc h as hydroquiaon

e t o preven tprematur e 5 actcristic

s suitabl e fo r buildin g applications, bu

tlowe r gellin g durin g storage. The

y als o typicall y contai n and - ratios coul

d b e we d irfireresbunce b o r n o concern, or oxidant s an d U V absorber

s t o hel p contro ] agin g an d if othe r mean s ar e use d t o provid e fire resistance. U V degradatio

n ofth e cure

d part s whic h caus e yellow teg, embrittlemen

tan d othe r physica l deterioration

. "HI-POIN

T 90 " (Wlte

o Chemica l Co. ) Th e spedfic resin

s used , ar e purchase d from commer

- 1 0 Methy l ethy l keton e peroxid e (MEKP ) fa a catdys t ci d resi n supplier s an d thei r exac tcompositio

n fa pro- typicaO

y nse d m initiat e fre e radicdreaetio

M in polyes prieur y t o tbesupplier. However

, tiiose foun

d patticu - te r resins. Whe

n i tb use d ston e i n the resin, i tbegin

s t o Isrl y wd l suite

d t o b e adapte

d fo r us e i n ihe presen

tdecompos

e s ts fairl y hig h temperatur

e abov e 200 * P . inventio n hav e the followin

g characteristics : (1 ) The

y Whe n •$*& n^ h • w*m\} **«$** efmrttl mvfll\r

,mt 

### t ca n b e polymerize

d t d a thermosettin

g sut e b y a free 1

5 or octoate . however

, MEK P resets s tlowe r tempers ssdic d reaction ndtiate

d b y catdysts ; sn

d (? ) Th e den - rum . Thus, polyeste

r resi n containin

g abou t1-2 * o f all y o f th e cure d red n fa substsntidl

y highe r tha n the MEKP

, sn d shou tOuCH % coppe r msphihenat

e ha tbee n Squi d resin. le , th

e red n shrink s durin g curing . Ao - found t

o g d i n shou t30-6 0 minute s a t80* EF , aa d i n cordin g t o publishe

d an d measure d densities , fh e an - abou

tonl y 5 minute s a t150 * F . I tfa auppSe d a a a 50 % filled resi n typicall y ca n shrin k u p t o abou t15 % durin g 2 0 activ e mixtur e dbsdve d i n dimethy l phthalate . polymerizatio

n o f polyeste r sn d u p t o abou t20 % i n th e cas e o f unfille d scryH c resin. Th e mixture s o f resin sa d "USP-245 " (Witc o Chante d Co. ) fifler me d (abou t35 % resi n sn d 65% minera

l filler) 2^dimethyW, 3 b b (2-etbyl-bexanoy

l penn y hextypicall y increas e in densit y abou t3-8 % from th

a liqui d ene ) b a liqui d catdys ttha tdecompose

s rapidl y in pOlymatri x t o th e find cure. Thus , if

th e shrinkag e occur s 2 5 este r rest e mahou t180 * F . I tbeupphe d a s s*0 « activ

e faotropteauy, LC , the sam e amoun tin eac h direction

, a mixture

, volum e shrinkag e o f 7 % woul d b e rautr d b y linea r shrinkag e o f 244% . Lower filfcr rate

s wi U hav e corre- "PERCADO X 16 " (AKZ

O Chemical

s Inc. ) spond ^ highe

r shrinkage

. ..... . DH^Jmiyl-cydohexylHierox y dkarbonat

e fa a I n the ess e o f

a mineral-fille

d reti n matri x i n whic h 3 0 po^e , „ « dj^ ^ h 

### „,„, * ^awne, , .n d dee0 

### m . th e filler ha s a substantia

l hea tcapacity , muc h o f th e p^ * ^j y fa th

e mi n s tabou

t110 * P . I tha s bee n freemagy chang

e dunngpolymerizatio

n result s m a n f ^ to fftaoee 

### , ^ „„ , ^ ^ ^^g , „ 1Jn 

### . R 

### facmsed temperatur

e tf th e filler a s wdl a s th e win . an

d thu s S u b e use

d a s e n alternativ

e t o tb e oembins - * * w , 

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### ^ . , d 

### ^ ^ t e 

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### ^ " : m 

### donofME»andcobdtnuphibenate.ltissuppHedss v^^Idbecu^lemsressonabfysbortperio d 3 5 m 

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h th e find cur e i s conducte

d i n a n osen . b 

### , ^^^ lo w 

### .enqwwwe catdyst . tiaHy thermall

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twithou tth e inter - r 

### n d hea to f reactio n causin g enoug h temperatur

e ris e t o "TRIGONO

X C (AKZ

O Chemical

s Ine. ) csurethermd degradatio

n o f th e pdymer . t^tyliwroddcbenzt^ba^uldthatdecooinose s Aluminu m Trihydnie (ATH

) rapidl

y fo polyeste

r a i abou t250'F . I tfo supplie d a s a n

. . . —_- . . ..-„ . . . . „ , .• ' 100 % activ e ingredien

tI n th e presen tinvention , th b fa ArumhumTrih^ntctATWbsnatu^yoccunto g t

### preferre d h $ tempcretur

e eitdy* . minera l derive d from processin

g o f bauxit e or e use d I n •» - —»

—# th e manufactur

e o f aluminu m meta l It s molecula r for - EXAMPLE S ^fa^0j3bl3HA^fatepure.refteedsute . 4 5 ^pee u o f

th e presen tinventio n ar e diown b y the findv"^? ^5ftT£!!3SKl S « I folIowteTex-npl m for purpou

s o f illustration

. Thes e |fa« y groun

d form,j^TH hasb^^Wd y use d a s a ^^^ an

d embodimentsar

e no tmean tWlim H th e filler fa plastic

s l o improv

e fire resistance

. I tb mos tfc,v«,Uon fa an

y way . Thos e skiDa d I n sh e ar twil l rec1 ^ : 

### ^X^^^^^Si ^ " ^^withlntiieHdrit^scopeoftheteveotion . tite viscosit

y o f th e resin - AT

H msut o Tha tis , a s th e EXAMPL E 1 AT H particl e st a faMred»ced JtsJiighei.surfac e are a ^ A 

### ^ ^ mlxWr e h 

### „,, , ^ ^ resdis i n incresse d viscosit y o f th e matrix , makin g i t let s suitabl e in th e presen tinvention . A tabov e abou t5 5 20-50,00 0 cp , i tbecome

s ver y difficul tt o process , pum p aa d pou r the -matrix

. Wit h a desire d mixtur e o f 65 % ATH , 35 % redn . thi

s vbeoslt y rang e occur * wit h AT H particl e sin e o f abou t10-2 0 micron

s dependin g o n th e processin g condition

s an d th e particula r bran d o f ATH . 6 0 Th e hig h practica l lim b o f particl e aze woul d b e determine d b y it s settlin g rat e an d thu s b dependen

to n th e concentratio

n i n th e resi n an d tb e g d tim e o f th e matrix . Fo r 65 % ATH . 35*%

" redn mixtures

, i ti s preferabl

e i n Th e resin , th e MM A monome r conuinlng th e coba

h th e presen tinventio n tha tparticl e siz e no texcee d shou t6 5 promote r an d th a AT H ar e mixe d unde r vacuu m t o 3 0 microns . obtai n a unifor m mixtur e o f abou t6-12,000 cp . free e f Th e preferre d filler ratio

s ar e fro m abou t40 % t o si r bubbles . Th e fasttw o catalyst s ar e adde d an d sdrre d abou t15% , sn d th e mor e preferre d rati o i s fro m abou tunti l uniforml y dispersed . A silico n resin-coated pape

r UMiiurut d poiycjic r mi n Cobal t aaphdicMi t PIMBM W <U « aaive ) MahyiMdMcfybitartavM r AT H pewte r Moby ! ethy l ktioi t |nwild e caitly a (SM I Kth* ) -USM45 " auJy a O M active ) 30 4 *awt

k O. I put s 4 4 re m 61 0 pu o 14 1 put. OJ S part s



# 10Tfcnw^/^t ^ 7~, W?W ^

*JI_. - ' i u » 

## UT7^7777I^73II 7

. ,-ir35'T' , 

## l 0 

## :2 3 : , ; 

## - 19199410234:327/5 0 5,260,00 6 1 1 1 2 i s folde d int o th e shap e o f

s tra y abou t8 " x8" x I " high , surfac e badly wrinkled , a

s b th e carrie

r pape r when iti s wit h th e comer s tape

d togethe r an

d wit h th e release peele

d fro m th e cure d plasti c sheet . I

ti s observed tbs t surface inside th e pan. Th e paper tra y i s placed i

n a the resin b shrun

k wit h th e mstri

x still adhere

d 1 0 th e polypropylen e pa

n of a siz e tha tprovide s suppor

tt o the crie r we 

### b , resultin g i n a badl y wrinkle d bottom sur upfolde d edge s o f

th e pspe r tray . Th e mstri x b poure d 5 face . I ti s obseive d thatth e ftabhe d shee ttha temerge d . int o ih e pape

r tra y t o for m s bye r abou

tI" duck . Th e fl 

### o m th e end o f th e secon d heating zon e i tbadl y matrixiRile d trey sn d suppor

tpa n are the n placed m a warpe

d an d conldn s crscl u an

d lean , mostl

y oriente d WO^microwaveoven . • . . • . i a themschin e direction . Th e ove n i s energized fo r a lon g enoug h tim e s o tha t th e matri x temperatur

e rb « afte r severa l intnute s t o IS O i o EXAMPL E 4 abou t5 minute , th e temnvatiir c ef th e cdla d matri

x Exampl

e J i s repeate d excep ttha

tih e microwav e exc«d,250-F,c.uscdbythe«oihcrmicreactlcn.Th e ^S^SiX l ^S£?^ S ££!?2i5?? I matri x i s dlowe d t o cure far 3 5 minute s an d the n re- v 

### ^^j'J^ A 

### ^1^^^Tf!± c 

### ^ b 

### t move d fro m thepspertray . I tuobscrvi d tha tthecwe d J

J abou t150 degree s F. I ti s observed th u th e materi d parti s smalle r tha

n th e origin d siz e e f

tb e tray . Th e emer 

### » i n 

### « •*•• * e firstcavit y fa slightly sof tt o tb e botto m surface o f

th e cure d matri

x an d th e botto

m «ow*butsoli d enoug h t o handle . A s th e pape r i s peele d l^pe r surface o f

th e pape r tn y ar

e bot h severd y wrin - from th e botto m ofth e rubber

y matri x sheet , i tfa ob kle d du e t o shrinkag

e o f th e matri x whil e adhering t o served t o b e relstivdy smoot h an d fre e o f wrinkles . Jus t tb e paper . 2 0 afte r

### * * W *

* P ee 

### * te d fron 

### * * gdle d matri x sheet , ' the shee tb cross-ca tb y th e travelin g MW , sa d flie re E X AMPL E 2 suhmgsectfonitredepositedonthemovfagpaper.l t ExperimentI b repeated excep tthatth e microwav e the n travd s throug

h th e secon d heating cavity , th e ove n i s turne

d offa ta tim e whe n th e matri x temperatur

e curin g ove n sn d throug h s coolin g zone . I n th e secon d reache s abou

t140-IS O degree s F . Afte r abou t7 minute s 2 5 heatin g cavity , th e plasti c shee ti s heate d t o abou t25 0 i ti s foun d tha

tth e matri x fa gelle d sufficientl y t o b e degrees F . handle d sn d ca n b e pulled from th e paper . I ti s immedi - Th e finished coole d plasti c shee ti s observed t o hav e ately'returne d rothe paper , place d back i n th e ove n an d a smoot

h bottom surface . I tdso b ds o observe d t o hav e heate d t o abov e 12 0 degree s F t o complete -th e cute , a series o f

lengthwis e parell d peak

s an d valley s o n th e agaf a b abou t3 5 mmutes . Thi s cured , shrunke n par ti s 3 0 uppe r surface , witb d m peak

s a s snuc h a s abou t6O>7 0 remove d from tb e trey . I tfa found t o hav e a smoot h tnif a highe r tha

n th e troughs . Abo . lh e finished shee tfa botto m surface , fre e o f

wrinkles . Th e paper tra

y ds o fa subsuotiall y curled fa dtecross-mschfa e direction , indi free o f wrinkles . Littl e o r n o machining o r sanding b cstin g lhatth e sheetdevelope d stresse s durin g curing . required t o provid e a flit, smoot h surface - Th e cress«achln e directio n apadn g o f th e ridgea fa EXAMPL E 3 ** obsen«dto*coiitipoi»dtoTiot^oti"inilieflriiheat - * * u~. u . 1 1

_« . J «. « frf ctv 

### Hy » *Wd » locall y hea tth e liquid matri x t o a A . A liqui d mairixmlxtur e fa prepare d a s follows: te^tnr e abov e Ig O degree s F , ile a iboug h th e aveng e temperatur

e i s onl y about15

0 degree s F . Thes e localized temperature

s are observe d t o b e abov e tb e rapi d decompositio n poin to f

tb e higher temperatur

e caulys t EXAMPLE S Th e abov e mixtur

e fa mixe d a thig h shear under vac - Meu l paneb hinge d atthei r lo p ar e hung abou

t2 " nu m unti l a unifor m mixtur e b obtdne d fre e o f

a b bub - 5 

### awa

y from each vertica

l wal l ofth e microwave cavit y ble s an d ha s a viscosit

y o f abou t10,00 0 cp . Th e mixtur

e an d parell d t o each correspondin g wall . Mean s are fa pumpe d a ta stead y rate o f 22^#/rdnut e ut o a con - provide d t o swin g th e bottom.o f

esc h pan d bac

k sn d tfouou s mixe r t o whic h I

s introduce d ai7l#/minuteo f forth m an are abou

t4 " long . Whe

n th e panel s sr s fa a caulys tmixture : motion , th e radio wav e node s caused b y multipl e fatera d reflections sr e cause d m mov e fats random pattern . •yggf -.- - Th e formulation an d running conditions o f Exampl e -LUPERSO L 

### w nj * 4 ar e repeated , cmc

a with th e pand s stil l an

d onc o wit b -TJSMSS " 

### u.t*9 th e paneb moving , fo eac h case , across-machin e direc g tion temperatur

e profil e ofth e gelle d matri

x n recorde d Th b provide s a concentratio n o f caulys ti n th e resin «* * «"* « *** * • *?*&••? * P e 

### T - - 

### *•* * fractio n o f th e matri x o f abou t2.1% . Th b mixtur

e fo afte r eeoltog , sr e exsnuiie d for th e ridges described fa eas tfro m a do tont o a movin g paper web , as described Exampl e 4 . abov e fa connectio n wit

h HO . 2 , wh h folded edge s 3 2 Wt tth e panels no tmoving ; ih e crou-meekin e dire e bi . apar tan d movin g a

t2. 0 ft/minute. Th b resul u fa a 60 tion temperatur e profil e I s observe d t o hav e peak

s and liqui d laye r havin g a

n averag e thicknes s o f

about0-50 *a*aejf

a wh h a n amplitude o f

abou t7 0 degree s F . Tb e inches . cure d sheet s contai n sever e ridge s abou

tth e sam e a s fa Th e energ y outpu

to f th e firstmicrowav e heating Exampl e 4 . Whe n th e pane b are caused t o reciprocate cavit y fo se ta

tabou t3 2 KW . Th e matri

x temperatur

e a ta * m e o f abou t15-2 0 times/minute, (h e amplitud e o f exceed s 11 0 degree s F a

tth e end o f

th e firstheating 6

5 the temperatur

e profile i s abou

t1 5 degrees F , an

d th e cavity— a temperatur

e whic h exceed s tb e activatio n severit y o f the ridges fa th e cure

d sheet s b sharpl y temperatur

e ofth e "USP-245 * catdys tTh e hardene d diminished. However , th e thee u stil l hav e substantia ) shee temerge s fro

m th e firstcavity wit

h th e bottom cur

l in th e cres s machine direction . 

# / I UwaturMr

d pelytSlf r Nt b Cobal t maphtbenii r promote

r AT H pcrdt r JS. S 

### a s JUL. n sP.1 3 ^i_ i > i u i - w o i i v inii_M i oni_i_ o I ~lii"c»V J 

### i3iaaiiu^4:»20/:» u



### 1 3 EXAMPL E 6 

## 5,260,00 6

A matri x b prepare

d usin g tbe formulatio

n of Exam pl e 2 , bu twit h a caulys tmixtur

e a s follows : 209 b TERCADOX-16 - S 1 % "TRIGANOX-C * 89 % Styren e Whe n th b catdys tmixtur

e b adde d e ta rat e o f 0.263 % "PERCADOX " fraction o n th e resi n fractio n o f th e Squid matrix , th e low-temperatur e caulys t"PERCA - 1

0 DOX-16 " pmvide a a g d lim e o f abou t3 0 minute

s a t 130degree s F , 7- 1 minute s at15 0 degree s Fund ibou i 2- 3 minutes a

t170 degree s F . Th e TRIGANOX-C ' b a highe r temperatur

e catelys l ths tdoe s no trapidl y de compos e unti

l abou t25 0 degree s F . 1 5 Whe n tb e matri

x formula o f

Exampl e 3 i s castusin

g th b caulys tsystem , the . followin g da u b obtained . Tcarpcntw * Hitin g Bra ratio M 0 degree * P . • . •rave cavfc

y *" ' fesotham tempera-ar

e rit e a tca d 6 0 degrees F . o f «MUS | ov a Uatwritrinkafca f

pile d nitri x OT 9 Ju ( prio r t o peeEn s of

f pipe r carte r en d ih e avr . . Th e finbhed shee tfa observe d t o b e smoot h o o th e bottom . Furthe r experimen u ar e conducted t o observe th e change s ta shrinkage an

d th e resulting product

. Th e 3 0 concentration o f

th e "PERCADOX-16 " fa varie d i n atepta s show n i n th e followin g uble : 

### 1 4 EXAMPL E 7 I n th tpreviou

s examples , th e ambien

ttemperatur

e o f th e secon d cavit

y i s se tsuc h tha tit ttemperatur

e i s equ d t o th e temperatur

e o f th e sheeta

s itemerge s from tb e secon d heatin

g cavity . Fo r example , i

f th e energ y out pu tofth e second heatin

g cavity , plu s th e hea

l o f reac tion ofth e polymerizatio

n initiate d fa th e secon d cavity , cause s th e curing sheett o pee k a t250 * F , th e g n tem peratur e aad th e wal b o f

th e secon d cavii y sr o se tat 250 * F . Widi lid s eoadition , aa d using th e g d zon e condition s e f

Exampl e 6, tb e cured shee ti s essentiall y flatand free o f

significan tstresses sfte r coding . I n exampl e 7 , th e bottom bas e plat

e o f th e cure , ove n i s raise d abou t50 * above th e pea

k adiabati c tempentur e o f th e shee tb th b condition , th e cure d shee tha s a pronounce

d cur l towar d th e upwar

d fisee. Next , th e bottom base plat

e o f th e cur e ove n fa lowere d abou tSV bdo w th e pea

k adiabati c temperature . I n th b condition , th e cured sheetb u a pronounced cur ttowar d th e bot tom face . Th e foregoing description of a prefene d embodimen t alternat e embodimeat

tsn d example

s o f th e inventio n hav e bee n presente

d fo r purpose

s e f illustratio n an

d description . Tb e description b no tbunde d t o b e ex haustive o r t o limitth e inventio n t o th e precis e form disclosed . Obvlosdy , man y modifications and varia tions ar e possibl e in ligh to f

tb e abov e teaching . Th e embodimem

s an d example s presented abov e wer e chose n an d describe d i n orde r t o bes

texplai n tli e princi ple s o f th e inventio

n an d i u practic d applicatio n t o thereb y enable other

s skille d fa th e an t o be i utiliz e th e

TERCAD0X.14-.O . BASE D ONUQLtDltESt N FRACTIO N O P MATRI X PERCEN T ACTIV E OXYGE N O F CATALYS T BASE D O N UQUI D KBSM

FHACTJO

N O F MATM X SHRINKAG E 9 LINEA R DIMENSION . JUS T MUORTOTHESA V 0ELTEMF.T . cus s ai m aus t ottt t ao» « OO M OO M aos z aaos i moot ! MO M OttOS I 0.002 0 UD1 ? W» » unt o as s ats o e « 03 0 OL O O J Ot O Oi l M I K

I N ra i n i n m i » 11 0 11 9

A s th e "PERCADOX-16 " i s reduced, i tb necessar

y t o mcreas e th e energ y outpu

to f th e firstheatin

g cavit y t o * ° ensur e tha tth e matri

x gel a befor

e emergin g from th e soaking oven . Th e following dat a i s obtaine

d usin g abou t0i04 % o n th e redn ; 5 5 Tcapcraiw c eabln i radio wav e cwfc y Eulbci a tenpeiMW c rise a t en d o f toaUa g ovc a Shee r ahrialiag

e o f gdle d auul i Jus tprior 1 0 pesSo s of

f r carrie r 17 0 degree s P . 12 0 degree s F . 0 * 

### C

O

Th e matri x emergin g from the g d oven ha s a rubber y consistenc y an d ver y lilll e surfac

e ripple. Itb observe

d tha tth e rubber

y gelle d matri

x i s free o f

significan t6 5 shrinkag e an d toug h enough t o be pede d fro m th e carryin g we b sn d cu tint o piece s befor e furthe r curin g an d shrinkage. Inventio n in variou

s embodiment

s and wh h variou s modification

s a s ar e suited t o th e particula

r us e contem plated . Wha tfa claime d fa L. * A method o f

continuous castin g o f

a polymerizabl e materi d whic

h shrink s upon curing , comprisin g th e step s of : '(a ) mixing sai

d materi d wit

h a firs tcatalys tgrou p having a tower activation temperatur e sa d a sec ond catdys tgrou

p having a higher activatio n tem peratur e t o form a mixture ; (b ) depositing s tleas ton e liqui d laye r o f sd d mixtur

e oa aa entr y en d o f a n termined nee d t o provide a movin g laye r o f said mixture ; (c ) heatin g sai d moving mixtur

e fa a firatregion t o a firsttemperature a

tleastequ d t o ui d lowe r activa tio n temperatur

e whereb y sd d movin g mixtur e partblly polymerize

a t o a firstnoa-Jiqui

d stat e

. withou texcessive shrinkage ; (d ) providing condition s fb r sd d movin g laye r o f

sd d mixtur e t o increas

e i n temperature i n a secon d 

# ttr f? : VJA*'*#**?>-ti%, 10100. 1 U^-J- i • it4010V



## IB 5,260,006 1 6 regio n l o a secon d temperatur e abov e sai

d higher activatio n temperatur

e whereb y shrinkag

e occur s substantiall

y uniforml

y i n al l direction s in sd d mix ture ; an d (e ) Manipulatin

g said laye r o f

mid mixtur

e t o preven

t dirinkag e parall d t o sai d we b movemen

tfrom transmissio

n t o th e portion o f

sai d mixtur

e resting e n sai d we b fa th e vicinit y o f sai d firstregion , thereb y preventin g sai

d shrinkag

e fro m damagin

g sai d materia

L 2 . Tb e metho d accordin g t o clai m 1 furthe r compris in g th e ste p o f

detachin g mid non-liquid mixtur e from sai d we b afte

r said ste p o f

heatin g said mixtur

e t o a first temperature . 2 . Th e metho d accordin g t o chi m 1 wherein ad d ste p o r providin g temperatur

e increas e condition s comprise s th e step s o f

heatin g t o a secon d temperatur e above said highe r activatio n temperatur e an d holdin g sai

d mixtur e a tapproximatel

y sai d temperature unti l shrinkag e b substantiall

y complete . 4 . Th e method accordin g t o dsh n 2 wherein ssi d step o r providin g temperatur

e increas e condition s comprise s th e sup s o f

bestin g t o s secon d temperatur e above sd d highe r activatio n temperatur e sn d holdin g sai

d mixtur e atapproximatel

y sd d temperamr

e unti l shrinkag

e i s substantiall

y complete . 5 . Th e metho d accordin g t o claim s 1 , 2 , 2 o r 4 wherei n sai

d highe r activatio n temperatur e fa a i leas t1 0 degree s fahrenhei

tgreate r tha

n sd d lowe r activation temperature . « . Th e metho d accordin g t o claim s L 2 , 3 o r 4 wherei n sd d ste p o f

providin g temperatur

e increas e condition s comprise s th e step s o f heatin g t o a second temperatur

e sbov e ssi d highe r activatio n temperamr e 3 3 an d holdin g said mixtur

e al approximatel

y ssi d second temperatur

e a tleastunti l shrinkag

e o f sai d materid fa substantiall

y complete . 7 . Th e metho d accordin g t o dai m 4 wherei n sd d secon d temperatur

e i s approximatel

y th e pea k tempera - 4 0 tur e generate d unde r adiabati c condition s b y th e poly merizatio n reactio n durin g sai

d secon d heating . 2 . Th e methed accordin g t o dai m 4 wherei n th e quantit y o f sai d firstcatdys tgrou

p b a n amoun tsuffiden tt o polymeriz e said materi d t o a g d befor e h ba s 4 5 reache d th e locatio n o f

sd d shrinkag

e transmissio

n pre ventio n ste p bu

tle u tha n th e amoun

twhic h wif

i pro duc e excessiv e shrinkag

e befor e sd d location . 1 0



### 1 5

2 0



### 2 5

3 0 11 . Th e metho d accordin g t o clai m S wherei n sai

d second catolysl group ha

s a n activatio n temperatur

e in th e rang e o f approximaid y 11 0 t o 28 0 degree s F . 12 . Th e metho

d accordin g t o claim 1 wherein sai d heatin g b applie

d subsuntidl y uniforml

y throughou

t rh e cross-sectio n o f

ui d mixtur

e whereb y a substan tially unifor

m temperature gradien

tI s mdnuine d fa sai

d mixture . 13 . Th e mediod accordin g t o efai m 1 2 wherei n said heatin g comprises irradfatin

g sai d mixtur

e wit h radi o frequency energy . 14 . Tb e method sccordin g t o dsi m 1 2 wherei n sai d radio fluenc y energy fa projecte d fa a unifor m patter n whereb y energy concentration s ar e substantiall y dis persed . 15 . Th e methe d aocordin g t o dai m 5 wherei n sai d firstcaulys tgroup an

d said secon d catalys tgroup com petit e sam

e caulys ttyp e an

d said firstcaulys tgrou p furthe r include s a promoter . 16 . A n apparatu

s fo r oontfauous castin g of a polymer izahl e materi d whic h shrink s upon curing , comprising : (a ) a mixer suitable t o combine ssi d materi d wi A a firstcatdys tgroup havin g a lowe r activatio n temperatur e an d a secon d catdys tgrou p havin g a highe r activatio n temperature ; (b ) a casting hea

d adapte d t o deposi tatleastoa e liquid laye r o f

said mixtur

e o n aa entr

y en d o f a n ope n we b movin g s ta 'predetermine d nee d t o provid e a movin g laye r o f sd d mixture ; (c ) a heater suitable t o bea tlai d movin g mixtur

e t o a finttemperatur

e a tleas tequ d t o said lowe r activa tio n temperatur

e whereb y sai d movin g mixtur e polymerize s t o a fintnon-liquid Sttt e withou tex cessiv e shrinkage ; (d ) a dumbe r adapte

d t o increas e th e temperatur e o f said movin g mixtur

e t o s secon d tempentur e s t leastequ d t o sd d highe r sctivstio a temperatur e whereb y shrinkag

e occur s substantiall

y uniforml

y i n al l direction s ta sai d mixture ; an d (e ) s mechanica

l isolato r adapte

d t o substantiall

y preven tshrinkag e parall d 1 0 said we b movemen t from transmissio

n t o th e mixtur

e restin g o n th e we b i n th e vicinit

y o f said firstheater , thereb y prevent in g ssi d shrinkag

e from damagin

g sd d materid . 17 . A n apparatu

s accordin g t o dai m I C further com prisin g mean s for detachin g ad d nonJiaul d mixtur e from ui d we b afte

r sd d heating o f

sai d mixture . is . A n spparatu

s sccordin g t o claim 1 4 wherei n said heater comprise

s a mean s for irradiatin

g sai d mixtur

e f . Th e method accordin g t o dai m I wherein sd d first catdys tgroup comprises , a s a percen tactiv e oxyge

n o f 5 0 wit h radi o frequency energy , catdyst . abou

t0.0010*9 4 t o abou t0.02 % .o f

th e liqui d IP . A n apparatu

s accordin g t o dai m I twherei n said resin fractio

n o f ui d materia

L radi o frequency energy b projected ta a unifor m patter n 10 . Tb e metho d accordin g t o clai m S wherei n sai d whereb y energy concentrations ar e substantiall

y dis firstcaulys tgrou p ha

s a n activation temperature fa th e persed . rang e o f approximatel

y IO O t o 22 0 degree s fahrenhdt5 5 • • • • •

6 5 

# iyOO V I OI-U J I I U IftlUV I OALC i • i-i4-o<J • iO-40 _ _ P.1 5 LOi 00*1V40* • n-ttLI vJ U



### 5,183,60 0 1 3 

### 1 4 (b ) heatin g sai d mixtur e substantially uniforml y (c ) inean s fo r bolatm g shrinkag e force s thatoccu r in throughou ti u cros s sectio n b y radio frequenc y u 

### * "Jj - 

### * rwiher^wnstrea m **»«* * beatin g v . . energ y downturn TM o f

raid depositin g step a tleas t^ J for'SdnuS Sd'S£ » thereafte r fa t o a temperatur

e sufficien tt o mitut e polymeriza - 5 

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