Method of preparing acrylonitrile-based polymer for producing carbon fiber

Patent metadata

Field	Value
Publication number	US-11427659-B2
Application number	US-201816481395-A
Country	US
Kind code	B2
Filing date	Sep 18, 2018
Priority date	Sep 29, 2017
Publication date	Aug 30, 2022
Grant date	Aug 30, 2022

Abstract

A method of preparing an acrylonitrile-based copolymer for a carbon fiber. The method includes: preparing a reaction solution including a (meth)acrylonitrile-based monomer and a first reaction solvent; adding a first portion of a radical polymerization initiator to the reaction solution to initiate polymerization; and adding a second portion of the radical polymerization initiator to the reaction solution when a polymerization conversion ratio is between 70 to 80%.

First claim

The invention claimed is:

1. A method of preparing a copolymer for a carbon fiber, comprising:
preparing a reaction solution comprising a (meth)acrylonitrile-containing monomer chosen from the group consisting of acrylonitrile and methacrylonitrile and a first reaction solvent;
primarily adding an initiator to the reaction solution to initiate polymerization; and
secondarily adding an initiator when a polymerization conversion rate reaches between 70 to 80% to perform polymerization,
wherein the initiator added in the primary and secondary stages has the same composition, and is selected from one or more of: azobisisobutyronitrile, 2,2′-azobis(4-methoxy-2,4-dimethylvaleronitrile, 2,2′-azobis(2,4-dimethylvaleronitrile), dimethyl 2,2′-azobis(2-methylpropionate), 2,2′-azobis (2-methylbutyronitrile), 1,1′-azobis(cyclohexane-1-carbonitrile), 2,2′-azobis [N-(2-propenyl)-2-methylpropionamide], [(cyano-1-methylethyl)azo]formamide, 2,2′-azobis(N-butyl-2-methylpropionamide) and 2,2′-azobis(N-cyclohexyl-2 methylpropionamide), and
wherein a weight ratio of the primarily-added initiator and the secondarily-added initiator is 2:1 to 8:1.

2. The method of claim 1 , wherein the secondarily-added initiator is added while mixed with a second reaction solvent.

3. The method of claim 2 , wherein the second reaction solvent is the same as the first reaction solvent.

4. The method of claim 2 , wherein the secondarily-added initiator and the second reaction solvent are mixed in a weight ratio of 1:15 to 1:35.

5. The method of claim 2 , wherein the second reaction solvent is added in an amount of 1 to 10 parts by weight with respect to 100 parts by weight of the first reaction solvent.

6. The method of claim 1 , wherein the total content of the primarily-added initiator and the secondarily-added initiator is 0.2 to 2 parts by weight with respect to 100 parts by weight of the (meth)acrylonitrile-containing monomer.

7. The method of claim 1 , further comprising:
raising a temperature of the reaction solution to 50 to 70° C. before the first addition of the initiator.

8. The method of claim 1 , wherein the reaction solution further comprises one or more comonomers selected from the group consisting of a carboxylic acid-containing monomer and a (meth)acrylate-containing monomer.

9. The method of claim 8 , wherein the one or more comonomer(s) is/are included in an amount of 1 to 10 parts by weight with respect to 100 parts by weight of the (meth)acrylonitrile-containing monomer.

10. The method of claim 1 , wherein the initiator added in the primary and secondary stages has the same composition, and is selected from one or more of: azobisisobutyronitrile, dimethyl 2,2′-azobis(2-methylpropionate) and 2,2′-azobis(2-methylbutyronitrile).

11. The method of claim 1 , wherein preparing the reaction solution comprises preparing the reaction solution within a reactor, and wherein both the primary and secondary additions of the initiator are made to the same reactor.

Assignees

• Lg Chemical Ltd

Inventors

• Kim Chang Hun
• Kim Hyun Min
• Cho Jeong Hun
• Cho Joon Hee

Classifications

• C08F220/44

  Acrylonitrile · CPC title

• C08F20/44 Primary

  Acrylonitrile · CPC title

• C08F2/04

  Polymerisation in solution (C08F2/32 takes precedence) · CPC title

• D01F9/22

  from polyacrylonitriles · CPC title

• C08F220/46

  with carboxylic acids, sulfonic acids or salts thereof · CPC title