# US 5,708,111 A · Process for the preparation of an acrylonitrile copolymer and product prepared therefrom

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- Number: US 5,708,111 A
- Document ID: US5708111A
- Status: Granted
- Kind: A
- Application number: 08/731,160
- Filed: 1996-10-10
- Granted: 1998-01-13
- Earliest claimed: 1993-05-06
- Inventors: Kenneth Wilkinson
- Web page: https://patentgrep.com/patent/US5708111A

## CPC

- D01F 9/22: from polyacrylonitriles
- C08F 2/14: Organic medium
- C08F 2/38: Polymerisation using regulators, e.g. chain terminating agents {, e.g. telomerisation}
- C08F 220/44: Acrylonitrile
- D01F 6/18: from polymers of unsaturated nitriles, e.g. polyacrylonitrile, polyvinylidene cyanide
- D01F: CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- C08F: MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS

## Abstract

A process for the rapid precipitation polymerization of acrylonitrile and a minor amount of a vinyl carboxylic acid comonomer in an environment of less than 10 ppm metal-ions to produce an acrylonitrile copolymer which, when pyrolyzed in an oxidizing atmosphere, produces a high quality carbon fiber.

## Claims

### Claim 1

An acrylonitrile copolymer fiber prepared according to a precipitation polymerization process comprising the steps of:
maintaining in a reaction zone a solvent system consisting essentially of water and a co-solvent which is a member selected from the group consisting of sodium thiocyanate and zinc chloride,
adding to the reaction zone a vinyl sulfonic acid comonomer-free feedstock comprising a major amount of acrylonitrile monomer and a minor amount of a vinyl carboxylic acid comonomer,
adding to the reaction zone an initiator mixture comprising a peroxide, a low molecular weight organic mercaptan, and less than 10 ppm of metal ion,
polymerizing the acrylonitrile monomer and vinyl carboxylic acid monomer under suitable conditions of temperature and pressure to obtain an acrylonitrile copolymer,
stripping off water and excess monomer and comonomer to obtain a spinnable solution of acrylonitrile copolymer, and
wet spinning the solution to produce a round fiber.

### Claim 2 (depends on 1)

A process according to claim 1 wherein the vinyl carboxylic acid comonomer is a member selected from the group consisting of itaconic acid, acrylic acid and methacrylic acid.

### Claim 3 (depends on 1)

A process according to claim 1 wherein the peroxide is a member selected from the group consisting of hydrogen peroxide, t-butyl hydroperoxide, t-butyl peroxide and lauroyl peroxide.

### Claim 4 (depends on 1)

A process according to claim 1 wherein the low molecular weight organic mercaptan is a member selected from the group consisting of 1-thioglycerol, mercapto ethanol and butyl mercaptan isomers.