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US4119746A Expired / Lapsed US ⏱️ 0.0 years remaining

Cross-linking resin saturant and method

Assignee: WR Grace and Co
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Filing: 1977-06-14
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Granted: 1978-10-10
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Expires: 1997-06-14
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Abstract

Abstract Porous, fibrous materials such as non-woven polyester or polypropylene web materials, cotton web, paper and other materials are saturated with a storage stable one-package latex composition. The latex composition is modified with a temperature sensitive cross-linking agent and neutralizing agents. The latex composition is tailored such that a fibrous material may be impregnated and dried at controlled temperature whereby a thermoplastic resin saturant web intermediate stock material having thermoset properties is produced. The cross-linking system in the latex composition is later activated in a specific manufacturing process at heat forming and molding temperatures to obtain a specifically shaped manufacture of desired rigidity and flexibility.

Inventors

  • 👤 Merrill Bleyle

Bibliographic Details

Application Number —
Jurisdiction US
Data Source google_patents
Last Synchronized 2026-10-23 09:32
CPC Classifications
C; C08; C08F; C08F246/00; D; D04; D04H; D04H1/00; D04H1/40; D04H1/58; D04H1/587; D04H1/64; Y; Y10; Y10T; Y10T442/00; Y10T442/20; Y10T442/2139

Claims Analysis

Total Claims: 14
Claim 1
Independent Claim 191 words
The method of preparing a resin impregnated non-woven web having thermoplastic characteristics at temperatures below 190° F. and thermoset characteristics at temperatures above 190° F. comprising: (a) preparing a cross-linking latex composition by (1) charging a reaction vessel with a small amount of a seed latex polymer along with an initiator in an aqueous phase to provide nucleating sites for polymerization, (2) adding, substantially continuously, monomers and emulsifiers at a controlled rate, said monomer consisting essentially of about 59 parts by weight styrene, about 41 parts by weight ethylacrylate, and 2 parts by weight N-methylolacrylamide, the addition taking place at about 150° F. over a 41/2 hour period, (3) post cooking the latex composition up to about three additional hours to reduce the free monomers content of the latex composition, (4) adjusting the latex composition after polymerization is completed from as manufactured state to a pH value between 6.0 and 8.0 with a neutralizing agent; (b) saturating a non-woven web with the adjusted latex composition; (c) drying the saturated web at a temperature below about 190° F. whereby an impregnated thermoplastic non-woven web having thermoset properties above 190° F. is produced.
Claim 2
Independent Claim 191 words
The method of preparing a resin impregnated non-woven web having thermoplastic characteristics at temperatures below 190° F. and thermoset characteristics at temperatures above 190° F. comprising: (a) preparing a cross-linking latex composition by (1) charging a reaction vessel with a small amount of a seed latex polymer along with an initiator in an aqueous phase to provide nucleating sites for polymerization, (2) adding, substantially continuously, monomers and emulsifiers at a controlled rate, said monomer consisting essentially of about 59 parts by weight styrene, about 41 parts by weight ethylacrylate, and 2 parts by weight N-methylolacrylamide, the addition taking place at about 150° F. over a 41/2 hour period, (3) post cooking the latex composition up to about three additional hours to reduce the free monomers content of the latex composition, (4) adjusting the latex composition after polymerization is completed from as manufactured state to a pH value between 6.0 and 8.0 with a neutralizing agent; (b) saturating a non-woven web with the adjusted latex composition; (c) drying the saturated web at a temperature below about 190° F. whereby an impregnated thermoplastic non-woven web having thermoset properties above 190° F. is produced.
Claim 3
Dependent Claim 24 words
The method of claim 1 wherein the neutralizing agent is selected from ammonium hydroxide, sodium hydroxide, potassium hydroxide, morpholine, methylamine, dimethylamine and mixtures thereof.
Claim 4
Independent Claim 156 words
A method of preparing a resin impregnated non-woven fibrous web having thermoplastic characteristics at temperatures below 190° F. and thermoset characteristics at temperatures above about 190° F. comprising: (a) providing a storage stable one-package polymerized latex composition consisting essentially of the polymerization reaction product of (1) from about 40 to about 70 parts by weight of a first monomer selected from styrene, vinylidene chloride, methylmethacrylate, butylmethacrylate and mixtures thereof, (2) from about 30 to about 60 parts by weight of a second monomer selected from methylacrylate, ethylacrylate and butylacrylate, proplyacrylate, 2-ethylhexylacrylate, mixtures thereof, and, (3) from about 0.5 to about 6.0 parts by weight of N-methylolacrylamide; said composition having been treated with a neutralizing agent after completion of polymerization reaction to prevent cross-linking below temperatures of 190° F.; (b) applying said neutralized composition to a non-woven fibrous web to impregnate the web, and (c) drying the impregnated non-woven fibrous web at a temperature below 190° F.
Claim 5
Independent Claim 156 words
A method of preparing a resin impregnated non-woven fibrous web having thermoplastic characteristics at temperatures below 190° F. and thermoset characteristics at temperatures above about 190° F. comprising: (a) providing a storage stable one-package polymerized latex composition consisting essentially of the polymerization reaction product of (1) from about 40 to about 70 parts by weight of a first monomer selected from styrene, vinylidene chloride, methylmethacrylate, butylmethacrylate and mixtures thereof, (2) from about 30 to about 60 parts by weight of a second monomer selected from methylacrylate, ethylacrylate and butylacrylate, proplyacrylate, 2-ethylhexylacrylate, mixtures thereof, and, (3) from about 0.5 to about 6.0 parts by weight of N-methylolacrylamide; said composition having been treated with a neutralizing agent after completion of polymerization reaction to prevent cross-linking below temperatures of 190° F.; (b) applying said neutralized composition to a non-woven fibrous web to impregnate the web, and (c) drying the impregnated non-woven fibrous web at a temperature below 190° F.
Claim 6
Dependent Claim 24 words
The method of claim 3 wherein the neutralizing agent is selected from ammonium hydroxide, sodium hydroxide, potassium hydroxide, morpholine, methylamine, dimethylamine and mixtures thereof.
Claim 7
Dependent Claim 35 words
The process of claim 4 wherein the first monomer is 59 parts by weight and is styrene, the second monomer is 41 parts by weight and is ethylacrylate, and N-methylolacrylamide is 2 parts by weight.
Claim 8
Dependent Claim 163 words
A process for forming a thermoplastic heat stable stock material for later cross-linking by saturating a non-woven web with a cross-linking resin saturant having cross-linking reaction activation temperature above 190° F. comprising the steps of: (a) preparing a polymerized resin composition consisting essentially the polymerization reaction product of: (1) from about 40 to about 70% by weight of a first monomer selected from styrene, vinylidene chloride, methylmethacrylate, butylmethacrylate and mixtures thereof, (2) from about 30 to about 60% by weight of a second monomer selected from methylacrylate, ethylacrylate, butylacrylate, propylacrylate, 2-ethylhexylacrylate, and mixtures thereof, and, (3) from about 0.5 to about 6.0% by weight of N-methylolacrylamide; said composition having been treated with a neutralizing agent upon completion of polymerization reaction to prevent cross-linking below 190° F.; (b) saturating a non-woven web with the resin from step (a); (c) drying the resin saturated web at a temperature below the cross-linking temperature of the resin whereby a thermoplastic stock material having thermoset properties is produced.
Claim 9
Dependent Claim 163 words
A process for forming a thermoplastic heat stable stock material for later cross-linking by saturating a non-woven web with a cross-linking resin saturant having cross-linking reaction activation temperature above 190° F. comprising the steps of: (a) preparing a polymerized resin composition consisting essentially the polymerization reaction product of: (1) from about 40 to about 70% by weight of a first monomer selected from styrene, vinylidene chloride, methylmethacrylate, butylmethacrylate and mixtures thereof, (2) from about 30 to about 60% by weight of a second monomer selected from methylacrylate, ethylacrylate, butylacrylate, propylacrylate, 2-ethylhexylacrylate, and mixtures thereof, and, (3) from about 0.5 to about 6.0% by weight of N-methylolacrylamide; said composition having been treated with a neutralizing agent upon completion of polymerization reaction to prevent cross-linking below 190° F.; (b) saturating a non-woven web with the resin from step (a); (c) drying the resin saturated web at a temperature below the cross-linking temperature of the resin whereby a thermoplastic stock material having thermoset properties is produced.
Claim 10
Dependent Claim 26 words
The process of claim 6 wherein the first monomer is 59% and is styrene, the second monomer is 41% and is ethylacrylate, and N-methylolacrylamide is 2%.
Claim 11
Dependent Claim 24 words
The process of claim 7 wherein the neutralizing agent is selected from ammonium hydroxide, morpholine, potassium hydroxide, sodium hydroxide, methylamine, dimethylamine and mixtures thereof.
Claim 12
Dependent Claim 144 words
A process for treating a non-woven web which comprises: (a) contacting said web with a thermosetting latex saturant composition having thermoplastic characteristics at temperatures below about 190° F. when dried on a non-woven fibrous material consisting essentially of a polymerization reaction product of: (1) 40 to 70 parts by weight of a first monomer selected from styrene, vinylidene chloride, methylmethacrylate, butylmethacrylate and mixtures thereof, (2) 30 to 60 parts by weight of a second monomer selected from methylacrylate, ethylacrylate, butylacrylate, propylacrylate, 2-ethylhexylacrylate and mixtures thereof, and (3) 0.5 to 6 parts by weight of N-methylolacrylamide, said product buffered to a pH range of from about 6.0 to about 8.0 with a neutralizing agent after completion of polymerization reaction; to impregnate said web with said composition, and (b) drying the impregnated web at temperatures below about 190° F. whereby the impregnated web has thermoplastic characteristics.
Claim 13
Dependent Claim 144 words
A process for treating a non-woven web which comprises: (a) contacting said web with a thermosetting latex saturant composition having thermoplastic characteristics at temperatures below about 190° F. when dried on a non-woven fibrous material consisting essentially of a polymerization reaction product of: (1) 40 to 70 parts by weight of a first monomer selected from styrene, vinylidene chloride, methylmethacrylate, butylmethacrylate and mixtures thereof, (2) 30 to 60 parts by weight of a second monomer selected from methylacrylate, ethylacrylate, butylacrylate, propylacrylate, 2-ethylhexylacrylate and mixtures thereof, and (3) 0.5 to 6 parts by weight of N-methylolacrylamide, said product buffered to a pH range of from about 6.0 to about 8.0 with a neutralizing agent after completion of polymerization reaction; to impregnate said web with said composition, and (b) drying the impregnated web at temperatures below about 190° F. whereby the impregnated web has thermoplastic characteristics.
Claim 14
Dependent Claim 30 words
The process of claim 9 including the additional step of thermally cross-linking the impregnated web by heating to a temperature above 190° F. to thermoset said composition on said web.

USPTO Annuity & Maintenance Windows

Annuity Stage Window Opens Payment Deadline Surcharge Period Until Estimated Fee Status
3.5 Years (Year 4) 1981-10-09 1982-04-10 1982-10-10 $2000.00 Window Closed / Lapsed
7.5 Years (Year 8) 1985-10-09 1986-04-10 1986-10-10 $3760.00 Window Closed / Lapsed
11.5 Years (Year 12) 1989-10-09 1990-04-10 1990-10-10 $7700.00 Window Closed / Lapsed

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