IP Library Granted Patent US 9,732,442
Granted Patent B2
US 9,732,442 · App. 14/371,746 · Granted Aug 15, 2017

Process for preparing aramid copolymer yarn having low residual sulfur

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Quick Facts
Patent No.
US 9,732,442
App. No.
14/371,746
Granted
Aug 15, 2017
Kind
B2
Abstract

The present invention concerns methods for producing a yarn comprising the steps of: (a) producing a plurality of dope filaments by spinning a polymer solution in sulfuric acid through a multi-hole spinneret, the polymer comprising imidazole groups; (b) coagulating the plurality of dope filaments into an as-spun yarn; (c) contacting the yarn with an aqueous base having a pKa less than or equal to 11; and (d) rinsing the yarn.

Claims (21)

1. A process for producing a yarn comprising the steps of:

(a) producing a plurality of dope filaments by spinning a polymer solution through a multi-hole spinneret, the polymer solution being formed from sulfuric acid and a polymer in the form of a neutralized polymer crumb, said polymer comprising residues of 5(6)-amino-2-(p-aminophenyl)benzimidazole, terephthaloyl dichloride, and para-phenylenediamine;

(b) coagulating the plurality of dope filaments into an as-spun yarn;

(c) contacting the yarn with an aqueous base having a pKa less than or equal to 11;

(d) rinsing the yarn; and

(e) heating the yarn to a temperature of at least 350° C.

2. The process of claim 1 , wherein in step c) the yarn is contacted with aqueous base comprising ammonium hydroxide, sodium bicarbonate, sodium carbonate, or mixtures thereof.

3. The process of claim 1 , wherein said polymer comprises copolymer derived from the copolymerization of para-phenylenediamine, 5(6)-amino-2-(p-aminophenyl)benzimidazole; and terephthaloyl dichloride wherein the molar ratio of 5(6)-amino-2-(p-aminophenyl)benzimidazole to aromatic diamine is 30/70 to 85/15.

4. The process of claim 3 wherein the molar ratio of 5(6)-amino-2-(p-aminophenyl)benzimidazole to aromatic diamine is 45/55 to 85/15.

5. The process of claim 1 , wherein in step d) the yarn is rinsed with additional quantities of aqueous base, said base being the same or different than the base used in step c).

6. The process of claim 1 , wherein in step d) the yarn is rinsed with an aqueous solution.

7. The process of claim 1 , wherein in step d) the yarn is rinsed with water.

8. The method of claim 1 , where after step b), the yarn has a sulfur content of 0.01 to 3 percent, based on the weight of the yarn.

9. The method of claim 8 , where after step b), the yarn has a sulfur content of 0.1 to 2.5 percent, based on the weight of the yarn.

10. The method of claim 8 , where after step b), the yarn has a sulfur content of 0.05 to 1.75 percent, based on the weight of the yarn.

11. The method of claim 10 , where after step b), the yarn has a sulfur content of 0.05 to 1.0 percent, based on the weight of the yarn.

12. The method of claim 8 , where after step b), the yarn has a sulfur content of 0.01 to 0.08 percent, based on the weight of the yarn.

13. The method of claim 12 , where after step b), the yarn has a sulfur content of 0.01 to 0.05 percent, based on the weight of the yarn.

14. The process of claim 1 , wherein the yarn, after heating, has a tenacity of 32 cN/dtex (35.6 gpd) or higher.

15. The process of claim 14 , wherein the yarn, after heating, has a tenacity of 34 cN/dtex (37.8 gpd) or higher.

16. The process of claim 15 , wherein the yarn, after heating, has a tenacity of 36 cN/dtex (40 gpd) or higher.

Assignments (2)
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Jun 25, 2019
From: E. I. DU PONT DE NEMOURS AND COMPANY
To: DUPONT SAFETY & CONSTRUCTION, INC.
Reel/Frame 049585/0450 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Jul 22, 2014
From: ALLEN, STEVEN R.; GABARA, VLODEK; LOWERY, JOSEPH LENNING; LUSTIG, STEVEN RAYMOND; NEWTON, CHRISTOPHER WILLIAM; RODINI, DAVID J.; SITTER, ANDREW J.
To: E. I. DUPONT DE NEMOURS AND COMPANY
Reel/Frame 033363/0251 →