US5741542A — Process of making thermal free-radical cure adhes…

Claim 1

Independent Claim 71 words

A process for making an adhesive comprising allowing a carrier web coated with a thermally, free-radically polymerizable mixture, comprising at least one thermally, free-radically polymerizable monomer and at least one thermal initiator in a catalytically effective amount to remain in contact with a thermal buffer having a heat transfer coefficient of at least 25 W/(m 2 .K) for a time sufficient to effect conversion of the coated mixture to an adhesive.

Claim 2

Dependent Claim 71 words

A process for making an adhesive comprising allowing a carrier web coated with a thermally, free-radically polymerizable mixture, comprising at least one thermally, free-radically polymerizable monomer and at least one thermal initiator in a catalytically effective amount to remain in contact with a thermal buffer having a heat transfer coefficient of at least 25 W/(m 2 .K) for a time sufficient to effect conversion of the coated mixture to an adhesive.

Claim 3

Dependent Claim 77 words

A process for thermal polymerization of a free-radically polymerizable adhesive composition comprising maintaining a carrier web coated with the free-radically polymerizable adhesive composition, comprising at least one thermally, free-radically polymerizable monomer and at least one thermal initiator in a catalytically effective amount at a temperature between ±20° C. of thermal buffer temperature by contacting the coated carrier web with the thermal buffer, the thermal buffer having a heat transfer coefficient of at least 25 W/(m 2 .K).

Claim 4

Dependent Claim 77 words

A process for thermal polymerization of a free-radically polymerizable adhesive composition comprising maintaining a carrier web coated with the free-radically polymerizable adhesive composition, comprising at least one thermally, free-radically polymerizable monomer and at least one thermal initiator in a catalytically effective amount at a temperature between ±20° C. of thermal buffer temperature by contacting the coated carrier web with the thermal buffer, the thermal buffer having a heat transfer coefficient of at least 25 W/(m 2 .K).

Claim 5

Dependent Claim 15 words

The process according to claim 1 or claim 2 wherein the thermal buffer is water.

Claim 6

Dependent Claim 56 words

The process according to claim 1 or claim 2 wherein the thermal buffer is selected from the group consisting of propylene glycol, a mixture of water and propylene glycol, a perfluorinated hydrocarbon fluid, a buffered acidic mixture of inorganic salts in water, a buffered acidic mixture of organic salts in water, condensing steam, helium and hydrogen.

Claim 7

Dependent Claim 34 words

The process according to claim 1 or claim 2 wherein the thermally, free radically polymerizable mixture comprises at least one ester of acrylic acid and an alcohol having from 1 to 14 carbon atoms.

Claim 8

Dependent Claim 52 words

The process according to claim 1 or 2 wherein the thermally free-radically polymerizable mixture comprises at least one acrylic acid ester selected from the group consisting of methyl acrylate, ethyl acrylate, n-butyl acrylate, t-butyl acrylate, hexyl acrylate, isooctyl acrylate, 2-ethylhexyl acrylate, isononyl acrylate, isobornyl acrylate, phenoxyethyl acrylate, decyl acrylate and dodecyl acrylate.

Claim 9

Dependent Claim 21 words

The process according to claim 1 or claim 2 wherein the heat transfer coefficient is at least 100 W/(m 2 .K).

Claim 10

Dependent Claim 21 words

The process according to claim 1 or claim 2 wherein the heat transfer coefficient is at least 500 W/(m 2 .K).

Claim 11

Dependent Claim 147 words

A process for making a pressure sensitive adhesive comprising the steps of: (1) coating onto at least one major surface of a carrier web a substantially solvent-free thermally polymerizable mixture, wherein (a) the polymerizable mixture comprises at least one free-radically polymerizable monomer, and at least one thermal initiator in a catalytically effective amount, and (b) the viscosity of the polymerizable mixture is suitable for coating the carrier web; (2) contacting the coated carrier web with a thermal buffer having a heat transfer coefficient of at least 25 W/(m 2 .K), wherein the thermal buffer is maintained at a temperature, sufficient to initiate thermal polymerization of the polymerizable mixture; (3) allowing the coated carrier web to remain in contact with the thermal buffer for a time sufficient to effect conversion of the polymerizable mixture to an adhesive; and (4) removing the coated carrier web from the thermal buffer.

Claim 12

Dependent Claim 147 words

A process for making a pressure sensitive adhesive comprising the steps of: (1) coating onto at least one major surface of a carrier web a substantially solvent-free thermally polymerizable mixture, wherein (a) the polymerizable mixture comprises at least one free-radically polymerizable monomer, and at least one thermal initiator in a catalytically effective amount, and (b) the viscosity of the polymerizable mixture is suitable for coating the carrier web; (2) contacting the coated carrier web with a thermal buffer having a heat transfer coefficient of at least 25 W/(m 2 .K), wherein the thermal buffer is maintained at a temperature, sufficient to initiate thermal polymerization of the polymerizable mixture; (3) allowing the coated carrier web to remain in contact with the thermal buffer for a time sufficient to effect conversion of the polymerizable mixture to an adhesive; and (4) removing the coated carrier web from the thermal buffer.

Claim 13

Dependent Claim 26 words

The process according to claim 9, further comprising the step of excluding oxygen from contact with the thermally polymerizable mixture during step (2) and step (3).

Claim 14

Dependent Claim 31 words

The process according to claim 9, wherein the thermally free radically polymerizable mixture comprises at least one ester of acrylic acid and an alcohol having from 1 to 14 carbon atoms.

Claim 15

Dependent Claim 50 words

The process according to claim 9 wherein the thermally free-radically polymerizable mixture comprises at least one acrylic acid ester selected from the group consisting of methyl acrylate, ethyl acrylate, n-butyl acrylate, t-butyl acrylate, hexyl acrylate, isooctyl acrylate, 2-ethylhexyl acrylate, isononyl acrylate, isobornyl acrylate, phenoxyethyl acrylate, decyl acrylate and dodecyl acrylate.

Claim 16

Dependent Claim 17 words

The process according to claim 9, further including at least one copolymerizable comonomer in the polymerizable mixture.

Claim 17

Dependent Claim 130 words

A process for making a pressure sensitive adhesive comprising the steps of: (1) preparing at least one mixture comprising at least one thermal free-radically polymerizable monomer and at least one component of a thermal initiator; (2) adjusting the viscosity of the mixture to a value suitable for coating; (3) degassing the mixture; (4) coating the degassed mixture onto a least one substrate; (5) contacting the coated substrate with a thermal buffer having a heat transfer coefficient of at least 25 W/(m 2 .K), wherein the thermal buffer is heated to a temperature sufficient to initiate thermal polymerization; (6) allowing the coated substrate to remain in contact with the thermal buffer for a time sufficient to effect conversion of the mixture; and (7) removing the coated substrate from the thermal buffer.

Claim 18

Dependent Claim 130 words

A process for making a pressure sensitive adhesive comprising the steps of: (1) preparing at least one mixture comprising at least one thermal free-radically polymerizable monomer and at least one component of a thermal initiator; (2) adjusting the viscosity of the mixture to a value suitable for coating; (3) degassing the mixture; (4) coating the degassed mixture onto a least one substrate; (5) contacting the coated substrate with a thermal buffer having a heat transfer coefficient of at least 25 W/(m 2 .K), wherein the thermal buffer is heated to a temperature sufficient to initiate thermal polymerization; (6) allowing the coated substrate to remain in contact with the thermal buffer for a time sufficient to effect conversion of the mixture; and (7) removing the coated substrate from the thermal buffer.

Claim 19

Dependent Claim 134 words

A process for making a pressure sensitive adhesive comprising the steps of: (1) preparing at least one mixture comprising at least one thermal free-radically polymerizable monomer; (2) adjusting the viscosity of the mixture to a value suitable for coating; (3) admixing at least one component of a thermal initiator with the mixture; (4) degassing the mixture; (5) coating the degassed mixture onto a least one substrate; (6) contacting the coated substrate with a thermal buffer having a heat transfer coefficient of at least 25 W/(m 2 .K), wherein the thermal buffer is heated to a temperature sufficient to initiate thermal polymerization; (7) allowing the coated substrate to remain in contact with the thermal buffer for a time sufficient to effect conversion of the mixture; and (8) removing the coated substrate fom the thermal buffer.

Claim 20

Dependent Claim 134 words

A process for making a pressure sensitive adhesive comprising the steps of: (1) preparing at least one mixture comprising at least one thermal free-radically polymerizable monomer; (2) adjusting the viscosity of the mixture to a value suitable for coating; (3) admixing at least one component of a thermal initiator with the mixture; (4) degassing the mixture; (5) coating the degassed mixture onto a least one substrate; (6) contacting the coated substrate with a thermal buffer having a heat transfer coefficient of at least 25 W/(m 2 .K), wherein the thermal buffer is heated to a temperature sufficient to initiate thermal polymerization; (7) allowing the coated substrate to remain in contact with the thermal buffer for a time sufficient to effect conversion of the mixture; and (8) removing the coated substrate fom the thermal buffer.

Claim 21

Dependent Claim 132 words

A process for making a pressure sensitive adhesive comprising the steps of: (1) preparing at least one mixture comprising at least one thermal free-radically polymerizable monomer and at least one component of a thermal initiator; (2) adjusting the viscosity of the mixture to a value suitable for coating; (3) degassing the mixture; (4) coating the degassed mixture between a first and second substrate to form a sandwich; (5) contacting the sandwich with a thermal buffer having a heat transfer coefficient of at least 25 W/(m 2 .K), wherein the thermal buffer is heated to a temperature sufficient to initiate thermal polymerization; (6) allowing the sandwich to remain in contact with the thermal buffer for a time sufficient to effect conversion of the mixture; and (7) removing the sandwich from the thermal buffer.

Claim 22

Dependent Claim 132 words

A process for making a pressure sensitive adhesive comprising the steps of: (1) preparing at least one mixture comprising at least one thermal free-radically polymerizable monomer and at least one component of a thermal initiator; (2) adjusting the viscosity of the mixture to a value suitable for coating; (3) degassing the mixture; (4) coating the degassed mixture between a first and second substrate to form a sandwich; (5) contacting the sandwich with a thermal buffer having a heat transfer coefficient of at least 25 W/(m 2 .K), wherein the thermal buffer is heated to a temperature sufficient to initiate thermal polymerization; (6) allowing the sandwich to remain in contact with the thermal buffer for a time sufficient to effect conversion of the mixture; and (7) removing the sandwich from the thermal buffer.

Claim 23

Dependent Claim 136 words

A process for making a pressure sensitive adhesive comprising the steps of: (1) preparing at least one mixture comprising at least one thermal free-radically polymerizable monomer; (2) adjusting the viscosity of the mixture to a value suitable for coating; (3) admixing at least one component of a thermal initiator with the mixture; (4) degassing the mixture; (5) coating the degassed mixture between a first and second substrate to form a sandwich; (6) contacting the sandwich with a thermal buffer having a heat transfer coefficient of at least 25 W/(m 2 .K), wherein the thermal buffer is heated to a temperature sufficient to initiate thermal polymerization; (7) allowing the sandwich to remain in contact with the thermal buffer for a time sufficient to effect conversion of the mixture; and (8) removing the sandwich from the thermal buffer.

Claim 24

Dependent Claim 136 words

A process for making a pressure sensitive adhesive comprising the steps of: (1) preparing at least one mixture comprising at least one thermal free-radically polymerizable monomer; (2) adjusting the viscosity of the mixture to a value suitable for coating; (3) admixing at least one component of a thermal initiator with the mixture; (4) degassing the mixture; (5) coating the degassed mixture between a first and second substrate to form a sandwich; (6) contacting the sandwich with a thermal buffer having a heat transfer coefficient of at least 25 W/(m 2 .K), wherein the thermal buffer is heated to a temperature sufficient to initiate thermal polymerization; (7) allowing the sandwich to remain in contact with the thermal buffer for a time sufficient to effect conversion of the mixture; and (8) removing the sandwich from the thermal buffer.

Claim 25

Dependent Claim 178 words

A process for making a pressure sensitive adhesive comprising the steps of: (1) preparing at least one mixture comprising at least one thermal free-radically polymerizable monomer and at least one component of a thermal initiator; (2) adjusting the viscosity of the mixture to a value suitable for coating; (3) degassing the mixture; (4) preparing a stacked article comprising the steps: (a) coating the degassed mixture between a first and second substrate to form layers of a sandwich; (b) repeating step (a), wherein the degassed mixture is coated between the second substrate and a sequentially adjacent substrate; and (c) continuing to repeat step (a) while adding additional substrates; (5) contacting the stacked article with a thermal buffer having a heat transfer coefficient of at least 25 W/(m 2 .K), wherein the thermal buffer is heated to a temperature, sufficient to initiate thermal polymerization; (6) allowing the stacked article to remain in contact with the thermal buffer for a time sufficient to effect conversion of the mixture of each layer; and (7) removing the stacked article from the thermal buffer.

Claim 26

Dependent Claim 178 words

A process for making a pressure sensitive adhesive comprising the steps of: (1) preparing at least one mixture comprising at least one thermal free-radically polymerizable monomer and at least one component of a thermal initiator; (2) adjusting the viscosity of the mixture to a value suitable for coating; (3) degassing the mixture; (4) preparing a stacked article comprising the steps: (a) coating the degassed mixture between a first and second substrate to form layers of a sandwich; (b) repeating step (a), wherein the degassed mixture is coated between the second substrate and a sequentially adjacent substrate; and (c) continuing to repeat step (a) while adding additional substrates; (5) contacting the stacked article with a thermal buffer having a heat transfer coefficient of at least 25 W/(m 2 .K), wherein the thermal buffer is heated to a temperature, sufficient to initiate thermal polymerization; (6) allowing the stacked article to remain in contact with the thermal buffer for a time sufficient to effect conversion of the mixture of each layer; and (7) removing the stacked article from the thermal buffer.

Claim 27

Dependent Claim 33 words

The process according to claim 18 further including a final layer of the degassed mixture coated onto the topmost substrate prior to contacting the stacked article with the thermal buffer in step 5.

Claim 28

Dependent Claim 182 words

A process for making a pressure sensitive adhesive comprising the steps of: (1) preparing at least one mixture comprising at least one thermal free-radically polymerizable monomer; (2) adjusting the viscosity of the mixture to a value suitable for coating; (3) admixing at least one component of a thermal initiator into the mixture; (4) degassing the mixture; (5) preparing a stacked article comprising the steps: (a) coating the degassed mixture between a first and second substrate to form layers of a sandwich; (b) repeating step (a), wherein the degassed mixture is coated between the second substrate and a sequentially adjacent substrate; and (c) continuing to repeat step (a) while adding additional substrates; (6) contacting the stacked article with a thermal buffer having a heat transfer coefficient of at least 25 W/(m 2 .K), wherein the thermal buffer is heated to a temperature, sufficient to initiate thermal polymerization; (7) allowing the stacked article to remain in contact with the thermal buffer for a time sufficient to effect conversion of the mixture of each layer; and (8) removing the stacked article from the thermal buffer.

Claim 29

Dependent Claim 182 words

A process for making a pressure sensitive adhesive comprising the steps of: (1) preparing at least one mixture comprising at least one thermal free-radically polymerizable monomer; (2) adjusting the viscosity of the mixture to a value suitable for coating; (3) admixing at least one component of a thermal initiator into the mixture; (4) degassing the mixture; (5) preparing a stacked article comprising the steps: (a) coating the degassed mixture between a first and second substrate to form layers of a sandwich; (b) repeating step (a), wherein the degassed mixture is coated between the second substrate and a sequentially adjacent substrate; and (c) continuing to repeat step (a) while adding additional substrates; (6) contacting the stacked article with a thermal buffer having a heat transfer coefficient of at least 25 W/(m 2 .K), wherein the thermal buffer is heated to a temperature, sufficient to initiate thermal polymerization; (7) allowing the stacked article to remain in contact with the thermal buffer for a time sufficient to effect conversion of the mixture of each layer; and (8) removing the stacked article from the thermal buffer.

Claim 30

Dependent Claim 33 words

The process according to claim 20 further including a final layer of the degassed mixture coated onto the topmost substrate prior to contacting the stacked article with the thermal buffer in step 6.

Claim 31

Dependent Claim 23 words

The process according to any of claims 9, 14, 15, 16, 17, 18, or 20 wherein at least one coated layer is multi-layered.

Claim 32

Dependent Claim 217 words

A process for thermal polymerization of free-radically polymerizable composition comprising the step of maintaining the temperature between values T min , and T max by thermal contact of the polymerizable composition with a heat exchange medium characterized by a minimum heat transfer coefficient h min wherein: T max =E a /(R In(A/k dmax )) or the boiling point of the thermal transfer medium, whichever is greater, T min =E a /(R In(A/k dmin )), k dmax ={k p M!/X n k t 1/2 } 2 / I!, k dmin =k t (R pmin /k p M!) 2 / I!, h min =DR pmax H p /(T max-T buf ), R pmax ={k p M!/k t 1/2 } 2 /X n , E a is a thermal initiator activation energy, R is the gas constant, A is the initiator prefactor, k t is the monomer termination rate constant, k p is the monomer propagation rate constant, R pmin is the minimum desired rate of polymerization, M! is the monomer concentration, I! is the initiator concentration, T buf is the temperature of the thermal buffer, X n is the desired average number of monomers per polymer chain, D is the thickness over which the temperature difference T max -T buf exists, and H p is the heat of polymerization.

Claim 33

Dependent Claim 217 words

A process for thermal polymerization of free-radically polymerizable composition comprising the step of maintaining the temperature between values T min , and T max by thermal contact of the polymerizable composition with a heat exchange medium characterized by a minimum heat transfer coefficient h min wherein: T max =E a /(R In(A/k dmax )) or the boiling point of the thermal transfer medium, whichever is greater, T min =E a /(R In(A/k dmin )), k dmax ={k p M!/X n k t 1/2 } 2 / I!, k dmin =k t (R pmin /k p M!) 2 / I!, h min =DR pmax H p /(T max-T buf ), R pmax ={k p M!/k t 1/2 } 2 /X n , E a is a thermal initiator activation energy, R is the gas constant, A is the initiator prefactor, k t is the monomer termination rate constant, k p is the monomer propagation rate constant, R pmin is the minimum desired rate of polymerization, M! is the monomer concentration, I! is the initiator concentration, T buf is the temperature of the thermal buffer, X n is the desired average number of monomers per polymer chain, D is the thickness over which the temperature difference T max -T buf exists, and H p is the heat of polymerization.

Claim 34

Dependent Claim 211 words

A process for thermal polymerization of free-radically polymerizable composition comprising the step of maintaining the temperature between values T min and T max by thermal contact of the polymerizable composition with a heat exchange medium characterized by a minimum heat transfer coefficient h min wherein: T max =E a /(R In(A/k dmax )) or the boiling point of the thermal transfer medium, whichever is greater, T min =E a /(R In(A/k dmin )), k dmax ={R pmax k t 1/2 /k p M!} 2 / I!, k dmin =k t (R pmin /k p M!) 2 / I!, h min =DR pmax H p /(T max -T buf ), R pmax is the maximum desired rate of polymerization, R pmin is the minimum desired rate of polymerization, E a is a thermal initiator activation energy, R is the gas constant, A is the initiator prefactor, k t is the monomer termination rate constant, k p is the monomer propagation rate constant, R pmin is the minimum desired rate of polymerization, M! is the monomer concentration, I! is the initiator concentration, T buf is the temperature of the thermal buffer, D is the thickness over which the temperature difference T max -T buf exists, and H p is the heat of polymerization.

Claim 35

Dependent Claim 211 words

A process for thermal polymerization of free-radically polymerizable composition comprising the step of maintaining the temperature between values T min and T max by thermal contact of the polymerizable composition with a heat exchange medium characterized by a minimum heat transfer coefficient h min wherein: T max =E a /(R In(A/k dmax )) or the boiling point of the thermal transfer medium, whichever is greater, T min =E a /(R In(A/k dmin )), k dmax ={R pmax k t 1/2 /k p M!} 2 / I!, k dmin =k t (R pmin /k p M!) 2 / I!, h min =DR pmax H p /(T max -T buf ), R pmax is the maximum desired rate of polymerization, R pmin is the minimum desired rate of polymerization, E a is a thermal initiator activation energy, R is the gas constant, A is the initiator prefactor, k t is the monomer termination rate constant, k p is the monomer propagation rate constant, R pmin is the minimum desired rate of polymerization, M! is the monomer concentration, I! is the initiator concentration, T buf is the temperature of the thermal buffer, D is the thickness over which the temperature difference T max -T buf exists, and H p is the heat of polymerization.

Annuity Stage	Window Opens	Payment Deadline	Surcharge Period Until	Estimated Fee	Status
3.5 Years (Year 4)	2001-04-20	2001-10-20	2002-04-21	$2000.00	Window Closed / Lapsed
7.5 Years (Year 8)	2005-04-20	2005-10-20	2006-04-21	$3760.00	Window Closed / Lapsed
11.5 Years (Year 12)	2009-04-20	2009-10-20	2010-04-21	$7700.00	Window Closed / Lapsed

Process of making thermal free-radical cure adhesives

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