US4460751A — Crosslinking composition and method of preparation

Claim 1

Independent Claim 148 words

A crosslinking composition comprising: (a) water; (b) a zirconium compound selected from the group consisting of zirconium oxychloride, zirconium acetate, zirconium tetrachloride, zirconium ortho-sulfate, zirconium carbonate, zirconium ammonium carbonate, and mixtures thereof; (c) an alpha-hydroxy acid represented by the following formula: ##STR7## wherein: R is selected from the group consisting of hydrogen and an alkyl group having 1 to about 3 carbon atoms; and, (d) an amine compound represented by the formula: ##STR8## wherein: R 1 is an hydroxyalkyl group having 1 to about 3 carbon atoms; R 2 is selected from the group consisting of an alkyl group having 1 to about 3 carbon atoms and a hydroxyalkyl group having 1 to about 3 carbon atoms; and, R 3 is selected from the group consisting of hydrogen, an alkyl group having 1 to about 3 carbon atoms, and a hydroxyalkyl group 1 to about 3 carbon atoms.

Claim 2

Dependent Claim 148 words

A crosslinking composition comprising: (a) water; (b) a zirconium compound selected from the group consisting of zirconium oxychloride, zirconium acetate, zirconium tetrachloride, zirconium ortho-sulfate, zirconium carbonate, zirconium ammonium carbonate, and mixtures thereof; (c) an alpha-hydroxy acid represented by the following formula: ##STR7## wherein: R is selected from the group consisting of hydrogen and an alkyl group having 1 to about 3 carbon atoms; and, (d) an amine compound represented by the formula: ##STR8## wherein: R 1 is an hydroxyalkyl group having 1 to about 3 carbon atoms; R 2 is selected from the group consisting of an alkyl group having 1 to about 3 carbon atoms and a hydroxyalkyl group having 1 to about 3 carbon atoms; and, R 3 is selected from the group consisting of hydrogen, an alkyl group having 1 to about 3 carbon atoms, and a hydroxyalkyl group 1 to about 3 carbon atoms.

Claim 3

Dependent Claim 24 words

The composition recited in claim 1 wherein the alpha-hydroxy acid is selected from the group consisting of lactic acid, glycolic acid and mixtures thereof.

Claim 4

Dependent Claim 23 words

The composition recited in claim 1 wherein the amine compound is selected from the group consisting of diethanolamine, triethanolamine, dimethylethanolamine, and mixtures thereof.

Claim 5

Dependent Claim 13 words

The composition recited in claim 1 wherein the zirconium compound is zirconium oxychloride.

Claim 6

Dependent Claim 38 words

The composition recited in claim 1 wherein the crosslinking composition comprises about 1 mole of zirconium metal ion, about 2 to about 5 moles of the alpha-hydroxy acid, and about 1 to 5 moles of the amine compound.

Claim 7

Dependent Claim 47 words

The composition recited in claim 1 further comprising an ingredient selected from the group consisting of citric acid, malic acid and mixtures thereof and said ingredient is present in the range of about 0.25 moles to about 2 moles to about 1 mole of zirconium metal ion.

Claim 8

Dependent Claim 25 words

The composition recited in claim 1 further comprising a water dispersible hydrophilic organic polymer having a molecular weight greater than 100,000 and containing carboxyl functionality.

Claim 9

Dependent Claim 108 words

The composition recited in claim 7 wherein said water dispersible hydrophilic organic polymer is selected from the group consisting of carboxyalkyl guar wherein the alkyl group has 1 to about 3 carbon atoms, carboxyalkylhydroxyalkyl quar wherein the alkyl groups have 1 to about 3 carbon atoms, xanthan gum, polyacrylamide wherein about 5 to about 75 percent of the carboxamide groups are hydrolyzed to carboxyl groups, polymethacrylamide wherein about 5 to about 75 percent of the carboxamide groups are hydrolyzed to carboxyl groups, cellulose ethers, a copolymer of about 5 to about 70 percent by weight acrylic acid or methacrylic acid copolymerized with acrylamide or methacrylamide, and mixtures thereof.

Claim 10

Dependent Claim 44 words

The composition recited in claim 8 wherein said polymer is selected from the group consisting of polyacrylamide wherein 7 percent of the carboxamide groups are hydrolyzed to carboxyl groups, polyacrylamide wherein 30 percent of carboxamide groups are hydrolyzed to carboxyl groups, and mixtures thereof.

Claim 11

Independent Claim 213 words

A method of preparing a crosslinking composition comprising: (a) adding an alpha-hydroxy acid to water to form a first mixture and adjusting the pH of the first mixture from about 5 to about 8 wherein said alpha-hydroxy acid has the following formula; ##STR9## wherein: R is selected from the group consisting of hydrogen and an alkyl group having 1 to about 3 carbon atoms; (b) adding a zirconium compound selected from the group consisting of zirconium oxychloride, zirconium acetate, zirconium tetrachloride, zirconium ortho-sulfate and mixtures thereof to the first mixture to form a second mixture; (c) adding an amine compound to the second mixture to form a third mixture wherein said amine compound is represented by the following formula: ##STR10## wherein: R 1 is hydroxyalkyl group having 1 to about 3 carbon atoms; R 2 is selected from the group consisting of an alkyl group having 1 to about 3 carbon atoms and a hydroxyalkyl group having 1 to about 3 carbon atoms; and, R 3 is selected from the group consisting of hydrogen, an alkyl group having 1 to about 3 carbon atoms, and a hydroxyalkly group having 1 to about 3 carbon atoms; and, (d) adjusting the pH of the third mixture of step (c) from about 5 to about 8.

Claim 12

Independent Claim 213 words

A method of preparing a crosslinking composition comprising: (a) adding an alpha-hydroxy acid to water to form a first mixture and adjusting the pH of the first mixture from about 5 to about 8 wherein said alpha-hydroxy acid has the following formula; ##STR9## wherein: R is selected from the group consisting of hydrogen and an alkyl group having 1 to about 3 carbon atoms; (b) adding a zirconium compound selected from the group consisting of zirconium oxychloride, zirconium acetate, zirconium tetrachloride, zirconium ortho-sulfate and mixtures thereof to the first mixture to form a second mixture; (c) adding an amine compound to the second mixture to form a third mixture wherein said amine compound is represented by the following formula: ##STR10## wherein: R 1 is hydroxyalkyl group having 1 to about 3 carbon atoms; R 2 is selected from the group consisting of an alkyl group having 1 to about 3 carbon atoms and a hydroxyalkyl group having 1 to about 3 carbon atoms; and, R 3 is selected from the group consisting of hydrogen, an alkyl group having 1 to about 3 carbon atoms, and a hydroxyalkly group having 1 to about 3 carbon atoms; and, (d) adjusting the pH of the third mixture of step (c) from about 5 to about 8.

Claim 13

Dependent Claim 35 words

The method recited in claim 10 wherein the second mixture of step (b) is adjusted to a pH of from about 5 to about 8 before the addition of the amine compound of step (c).

Claim 14

Dependent Claim 24 words

The method recited in claim 10 wherein the alpha-hydroxy acid is selected from the group consisting of lactic acid, glycolic acid and mixtures thereof.

Claim 15

Dependent Claim 23 words

The method recited in claim 10 wherein the amine compound is selected from the group consisting of diethanolamine, triethanolamine, dimethylethanolamine, and mixtures thereof.

Claim 16

Dependent Claim 36 words

The method recited in claim 10 wherein the complexing composition comprises about 1 mole of zirconium metal ion, about 2 to about 5 moles of the alpha-hydroxy acid, and about 1 to 5 moles of amine.

Claim 17

Dependent Claim 28 words

The method recited in claim 10 wherein the first mixture is adjusted to a pH of about 7 before the addition of the zirconium compound of step (b).

Claim 18

Dependent Claim 30 words

The method recited in claim 10 wherein the second mixture of step (b) is adjusted to a pH of 7 with ammonium hydroxide prior to the addition of the amine.

Claim 19

Dependent Claim 24 words

The mixture recited in claim 10 wherein said zirconium compound is zirconium oxychloride, the alpha-hydroxy acid is lactic acid and the amine is triethanolamine.

Claim 20

Independent Claim 210 words

A method of preparing a crosslinking composition comprising: (a) adding a zirconium compound selected from the group consisting of zirconium carbonate, zirconium ammonium carbonate and mixtures thereof to water to form a first mixture; (b) adding an amine compound to the first mixture to form a second mixture wherein said amine compound is represented by the following formula: ##STR11## wherein: R 1 is hydroxyalkyl group having 1 to about 3 carbon atoms; R 2 is selected from the group consisting of an alkyl group having 1 to about 3 carbon atoms and a hydroxyalkyl group having 1 to about 3 carbon atoms; and, R 3 is selected from the group consisting of hydrogen, an alkyl group having 1 to about 3 carbon atoms, and a hydroxyalkyl group having 1 to about 3 carbon atoms; (c) adjusting the pH of the second mixture of step (b) from about 5 to about 8; and, (d) adding an alpha-hydroxy acid to the second mixture to form a third mixture and adjusting the pH of the third mixture from about 5 to about 8 wherein said alpha-hydroxy acid has the following formula; ##STR12## wherein: R is selected from the group consisting of hydrogen and an alkyl group having 1 to about 3 carbon atoms.

Claim 21

Independent Claim 210 words

A method of preparing a crosslinking composition comprising: (a) adding a zirconium compound selected from the group consisting of zirconium carbonate, zirconium ammonium carbonate and mixtures thereof to water to form a first mixture; (b) adding an amine compound to the first mixture to form a second mixture wherein said amine compound is represented by the following formula: ##STR11## wherein: R 1 is hydroxyalkyl group having 1 to about 3 carbon atoms; R 2 is selected from the group consisting of an alkyl group having 1 to about 3 carbon atoms and a hydroxyalkyl group having 1 to about 3 carbon atoms; and, R 3 is selected from the group consisting of hydrogen, an alkyl group having 1 to about 3 carbon atoms, and a hydroxyalkyl group having 1 to about 3 carbon atoms; (c) adjusting the pH of the second mixture of step (b) from about 5 to about 8; and, (d) adding an alpha-hydroxy acid to the second mixture to form a third mixture and adjusting the pH of the third mixture from about 5 to about 8 wherein said alpha-hydroxy acid has the following formula; ##STR12## wherein: R is selected from the group consisting of hydrogen and an alkyl group having 1 to about 3 carbon atoms.

Claim 22

Dependent Claim 24 words

The method recited in claim 18 wherein the alpha-hydroxy acid is selected from the group consisting of lactic acid, glycolic acid and mixtures thereof.

Claim 23

Dependent Claim 18 words

The method recited in claim 18 wherein the amine-compound is triethanolamine and the alpha-hydroxy acid is lactic acid.

Annuity Stage	Window Opens	Payment Deadline	Surcharge Period Until	Estimated Fee	Status
3.5 Years (Year 4)	1987-07-17	1988-01-16	1988-07-17	$2000.00	Window Closed / Lapsed
7.5 Years (Year 8)	1991-07-17	1992-01-16	1992-07-17	$3760.00	Window Closed / Lapsed
11.5 Years (Year 12)	1995-07-17	1996-01-16	1996-07-17	$7700.00	Window Closed / Lapsed

Crosslinking composition and method of preparation

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