US4701480A — Stable, aqueous dispersions of polyurethane-ureas

Claim 1

Independent Claim 146 words

A process for the preparation of an aqueous polyurethane-urea dispersion with improved hydrolytic stability which comprises (a) forming an aqueous polyurethane-urea dispersion containing (i) about 5 to 120 milliequivalents per 100 grams of polyurethane-urea of chemically incorporated anionic groups wherein at least about 50% of said anionic groups are carboxylic acid groups neutralized with volatile organic bases and (ii) up to about 10% by weight, based on the weight of said polyurethane-urea, of lateral and/or terminal hydrophilic chains containing ethylene oxide units and (b) converting the volatile organic base-neutralized carboxylic acid groups to non-volatile cation-neutralized carboxylate groups by adding an alkali metal salt of an organic or inorganic acid having a pKa greater than 0 to the aqueous polyurethane-urea dispersion of (a) in an amount sufficient to displace at least a portion of said volatile organic bases as the neutralizing agent for said carboxylic acid groups.

Claim 2

Dependent Claim 146 words

A process for the preparation of an aqueous polyurethane-urea dispersion with improved hydrolytic stability which comprises (a) forming an aqueous polyurethane-urea dispersion containing (i) about 5 to 120 milliequivalents per 100 grams of polyurethane-urea of chemically incorporated anionic groups wherein at least about 50% of said anionic groups are carboxylic acid groups neutralized with volatile organic bases and (ii) up to about 10% by weight, based on the weight of said polyurethane-urea, of lateral and/or terminal hydrophilic chains containing ethylene oxide units and (b) converting the volatile organic base-neutralized carboxylic acid groups to non-volatile cation-neutralized carboxylate groups by adding an alkali metal salt of an organic or inorganic acid having a pKa greater than 0 to the aqueous polyurethane-urea dispersion of (a) in an amount sufficient to displace at least a portion of said volatile organic bases as the neutralizing agent for said carboxylic acid groups.

Claim 3

Dependent Claim 19 words

The process of claim 1 which comprises removing at least a portion of the volatile organic bases by distillation.

Claim 4

Dependent Claim 17 words

The process of claim 1 wherein said organic or inorganic acids have a pKa greater than 5.

Claim 5

Dependent Claim 24 words

The process of claim 1 wherein said alkali metal salt comprises a member selected from the group consisting of sodium carbonate and sodium bicarbonate.

Claim 6

Dependent Claim 23 words

The process of claim 1 wherein at least about 80% of said anionic groups are carboxylic acid groups neutralized with volatile organic bases.

Claim 7

Dependent Claim 13 words

The process of claim 1 wherein said volatile organic bases are tertiary amines.

Claim 8

Dependent Claim 131 words

A process for the preparation of an aqueous polyurethane-urea dispersion with improved hydrolytic stability which comprises (a) forming an aqueous polyurethane-urea dispersion containing (i) about 10 to 120 milliequivalents, per 100 grams of polyurethane urea of chemically incorporated anionic groups wherein at least about 80% of said anionic groups are carboxylic acid groups neutralized with volatile tertiary amines and (ii) up to about 10% by weight, based on the weight of said polyurethane-urea of lateral and/or terminal hydrophilic chains containing ethylene oxide units, (b) converting the volatile tertiary amine-neutralized carboxylic acid groups to non-volatile cation-neutralized carboxylate groups by adding an alkali metal salt of an organic or inorganic acid having a pKa greater than 5 to the aqueous polyurethane-urea dispersion of (a) and (c) removing the volatile tertiary amines by distillation.

Claim 9

Dependent Claim 131 words

A process for the preparation of an aqueous polyurethane-urea dispersion with improved hydrolytic stability which comprises (a) forming an aqueous polyurethane-urea dispersion containing (i) about 10 to 120 milliequivalents, per 100 grams of polyurethane urea of chemically incorporated anionic groups wherein at least about 80% of said anionic groups are carboxylic acid groups neutralized with volatile tertiary amines and (ii) up to about 10% by weight, based on the weight of said polyurethane-urea of lateral and/or terminal hydrophilic chains containing ethylene oxide units, (b) converting the volatile tertiary amine-neutralized carboxylic acid groups to non-volatile cation-neutralized carboxylate groups by adding an alkali metal salt of an organic or inorganic acid having a pKa greater than 5 to the aqueous polyurethane-urea dispersion of (a) and (c) removing the volatile tertiary amines by distillation.

Claim 10

Dependent Claim 183 words

A process for the preparation of an aqueous polyurethane-urea dispersion with improved hydrolytic stability which comprises (a) forming an aqueously dispersed isocyanate-terminated prepolymer containing (i) about 10 to 120 milliequivalents, per 100 grams of polyurethane-urea of chemically incorporated anionic groups wherein at least about 80% of said anionic groups are carboxylic acid groups neutralized with volatile tertiary amines and (ii) up to about 10% by weight, based on the weight of said polyurethane-urea, of lateral and/or terminal hydrophilic chains containing ethylene oxide units, (b) converting the volatile tertiary amine-neutralized carboxylate groups to non-volatile cation-neutralized carboxylate groups by adding an alkali metal salt of an organic or inorganic acid having a pKa greater than 0 to the aqueous medium used for dispersing said isocyanate-terminated prepolymer either before or after dispersing the prepolymer therein, in an amount sufficient to displace at least a portion of the volatile tertiary amines as the neutralizing agent for said carboxylic acid groups, (c) chain extending said isocyanate-terminated prepolymer to form said aqueous polyurethane-urea dispersion and (d) removing the volatile teritary amines by distillation either before and/or after step (c).

Claim 11

Dependent Claim 183 words

A process for the preparation of an aqueous polyurethane-urea dispersion with improved hydrolytic stability which comprises (a) forming an aqueously dispersed isocyanate-terminated prepolymer containing (i) about 10 to 120 milliequivalents, per 100 grams of polyurethane-urea of chemically incorporated anionic groups wherein at least about 80% of said anionic groups are carboxylic acid groups neutralized with volatile tertiary amines and (ii) up to about 10% by weight, based on the weight of said polyurethane-urea, of lateral and/or terminal hydrophilic chains containing ethylene oxide units, (b) converting the volatile tertiary amine-neutralized carboxylate groups to non-volatile cation-neutralized carboxylate groups by adding an alkali metal salt of an organic or inorganic acid having a pKa greater than 0 to the aqueous medium used for dispersing said isocyanate-terminated prepolymer either before or after dispersing the prepolymer therein, in an amount sufficient to displace at least a portion of the volatile tertiary amines as the neutralizing agent for said carboxylic acid groups, (c) chain extending said isocyanate-terminated prepolymer to form said aqueous polyurethane-urea dispersion and (d) removing the volatile teritary amines by distillation either before and/or after step (c).

Claim 12

Dependent Claim 13 words

The process of claim 2 wherein said distillation is conducted under reduced pressure.

Claim 13

Dependent Claim 18 words

The process of claim 9 wherein said weak organic or inorganic acids have a pKa greater than 5.

Claim 14

Dependent Claim 24 words

The process of claim 9 wherein said alkali metal salt comprises a member selected from the group consisting of sodium carbonate and sodium bicarbonate.

Claim 15

Dependent Claim 13 words

The process of claim 9 wherein said volatile organic bases are tertiary amines.

Claim 16

Dependent Claim 13 words

The process of claim 11 wherein said volatile organic bases are tertiary amines.

Claim 17

Dependent Claim 13 words

The process of claim 7 wherein said distillation is conducted under reduced pressure.

Claim 18

Dependent Claim 13 words

The process of claim 8 wherein said distillation is conducted under reduced pressure.

Claim 19

Dependent Claim 171 words

A process for the preparation of an aqueous polyurethane-urea dispersion with improved hydrolytic stability which comprises (a) forming an aqueously dispersed isocyanate-terminate prepolymer containing (i) about 5 to 120 milliequivalents per 100 grams of polyurethane-urea of chemically incorporated anionic groups wherein at least about 50% of said anionic groups are carboxylic acid groups neutralized with volatile organic bases and (ii) up to about 10% by weight, based on the weight of said polyurethane-urea, of lateral and/or terminal hydrophilic chains containing ethylene oxide units and (b) converting the volatile organic base-neutralized carboxylic acid groups to non-volatile cation-neutralized carboxylate groups by adding an alkali metal salt of an organic or inorganic acid having a pKa greater than 0 to the aqueous medium used for dispersing the isocyanate-terminated prepolymer either before or after dispersing the prepolymer therein, in an amount sufficient to displace at least a portion of said volatile organic bases as the neutralizing agent for said carboxylic acid groups and (c) chain extending said isocyanate-terminated prepolymer to form said aqueous polyurethane-urea disperson.

Claim 20

Dependent Claim 171 words

A process for the preparation of an aqueous polyurethane-urea dispersion with improved hydrolytic stability which comprises (a) forming an aqueously dispersed isocyanate-terminate prepolymer containing (i) about 5 to 120 milliequivalents per 100 grams of polyurethane-urea of chemically incorporated anionic groups wherein at least about 50% of said anionic groups are carboxylic acid groups neutralized with volatile organic bases and (ii) up to about 10% by weight, based on the weight of said polyurethane-urea, of lateral and/or terminal hydrophilic chains containing ethylene oxide units and (b) converting the volatile organic base-neutralized carboxylic acid groups to non-volatile cation-neutralized carboxylate groups by adding an alkali metal salt of an organic or inorganic acid having a pKa greater than 0 to the aqueous medium used for dispersing the isocyanate-terminated prepolymer either before or after dispersing the prepolymer therein, in an amount sufficient to displace at least a portion of said volatile organic bases as the neutralizing agent for said carboxylic acid groups and (c) chain extending said isocyanate-terminated prepolymer to form said aqueous polyurethane-urea disperson.

Claim 21

Dependent Claim 25 words

The process of claim 16 which comprises removing at least a portion of the volatile organic bases by distillation either before and/or after step (c).

Claim 22

Dependent Claim 17 words

The process of claim 16 wherein said organic or inorganic acids have a pKa greater than 5.

Claim 23

Dependent Claim 24 words

The process of claim 16 wherein said alkali metal salt comprises a member selected from the group consisting of sodium carbonate and sodium bicarbonate.

Claim 24

Dependent Claim 23 words

The process of claim 16 wherein at least about 80% of said anionic groups are carboxylic acid groups neutralized with volatile organic bases.

Claim 25

Dependent Claim 13 words

The process of claim 16 wherein said volatile organic bases are tertiary amines.

Annuity Stage	Window Opens	Payment Deadline	Surcharge Period Until	Estimated Fee	Status
3.5 Years (Year 4)	1990-10-19	1991-04-20	1991-10-20	$2000.00	Window Closed / Lapsed
7.5 Years (Year 8)	1994-10-19	1995-04-20	1995-10-20	$3760.00	Window Closed / Lapsed
11.5 Years (Year 12)	1998-10-19	1999-04-20	1999-10-20	$7700.00	Window Closed / Lapsed

Stable, aqueous dispersions of polyurethane-ureas

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