Method for preparing polyacrylonitrile spinning stoste

A technology of polyacrylonitrile spinning and acrylonitrile, which is applied in the direction of single-component synthetic polymer rayon, textiles and papermaking, fiber chemical characteristics, etc., to achieve the effects of simple process, improved oxidation and reduced probability of defects

Inactive Publication Date: 2005-12-21
SHANXI INST OF COAL CHEM CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

But so far there is no report about the continuous addition of acrylamide and acrylonitrile solution copolymerization at home and abroad to prepare polyacrylonitrile spinning stock solution

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0016] In a 500ml four-neck flask, add 60.935g of purified acrylonitrile (AN), 0.183g of azobisisobutyronitrile (AIBN) and 260g of dimethyl sulfoxide (DMSO), and stir until they are completely dissolved. Nitrogen was then purged for 1.5 hours to purge the air. Afterwards, nitrogen was continuously fed in as a gas protection, and when the temperature of the water bath was 52° C., the reaction was started, and the stirring speed was 280 rpm. At the same time, through the metering pump, the ratio of the feed rate per minute to the volume of the container is 2×10 -5 min -1 Speed, 0.138g / ml (acrylamide / dimethyl sulfoxide) acrylamide solution was continuously put into the reactor. After 12 hours, the reaction was terminated. Then vacuum remove residual monomer and sulfoxide at 60°C and 0.080Mpa. Stand at 50° C. for 24 hours, defoam, and obtain spinning dope. It was determined that the polymerization conversion rate was 68%, the molecular weight measured by gel permeation chroma...

Embodiment 2

[0018] In a 500ml four-neck flask, add 62.539g of purified acrylonitrile (AN), 0.222g of azobisisobutyronitrile (AIBN) and 258g of dimethyl sulfoxide (DMSO), and stir until all of them are dissolved. Nitrogen was then purged for 1.5 hours to purge the air. Then continue to pass nitrogen protection. When the temperature of the water bath rose to 55° C., the reaction was started, and the stirring speed was 260 rpm. At the same time, through the metering pump, the volume ratio of the feed amount per minute to the container is 4×10 -5 min -1 Speed, 0.172g / ml (acrylamide / dimethyl sulfoxide) acrylamide solution was continuously put into the reactor. After reacting for 10 hours, the reaction was stopped. Then vacuum remove residual monomer and sulfoxide at 65°C and 0.088Mpa. Stand at 40° C. for 30 hours, defoam, and obtain spinning dope. The reaction conversion rate as measured by weighing method is 64%, the molecular weight as measured by GPC is 260,000, and the molecular weig...

Embodiment 3

[0020] In a 500ml four-neck flask, add 67.35g of purified acrylonitrile (AN), 0.337g of azobisisobutyronitrile (AIBN) and 253g of dimethyl sulfoxide (DMSO), and stir until they are completely dissolved. Nitrogen was then purged for 2 hours to purge the air. Then continue to pass nitrogen protection. When the temperature of the water bath rose to 60° C., the reaction was started, and the stirring speed was 230 rpm. At the same time, through the metering pump, the ratio of the feed rate per minute to the volume of the container is 1×10 -1 min -1 Speed, 0.170g / ml (acrylamide / dimethyl sulfoxide) acrylamide solution was continuously put into the reactor. After 11 hours of reaction, the reaction was stopped. Then vacuum remove residual monomer and sulfoxide at 75°C and 0.082Mpa. Stand at 30° C. for 48 hours, defoam, and obtain spinning dope. The reaction conversion rate as measured by weighing method is 61%, the molecular weight as measured by GPC is 220,000, and the molecular...

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Abstract

The poly-acrylonitrile spinning stost is prepared by mixing acrylonitrile, azobisisobutyronitrile and dimethyl sulfoxide according to a certain weight proportion, stirring uniformly, leading in nitrogen gas under the stirring speed of 230-290 turn / min., making them react under reaction temp. of 52-65 degree C, continuously feeding in acryamide solution to react for 8-13 hours in which the ratio of feed amount per min. to container volume is 2x10-5 -1x10-4 min-1 , then demonomorizing and defoaming. Advantages: obviously reduced poly-acrylonitrile molecular weight distribution, improved spinning property of polymer and the oxidisability of raw yarn and simple process etc..

Description

technical field [0001] The invention belongs to a method for preparing a carbon fiber precursor, in particular to a method for preparing a polyacrylonitrile spinning stock solution for carbon fibers. Background technique [0002] In the preparation process of carbon fiber, the synthesis of polyacrylonitrile resin is the basis. The development of high-performance carbon fiber requires that the acrylonitrile polymer has a suitable molecular weight and distribution and a chain structure with uniform distribution of comonomers. A regular, uniform and reasonable molecular chain structure can lay the foundation for the spinning of precursors with few defects and uniform structure and the preparation of high-performance carbon fibers. Under the premise of maintaining good spinnability and solubility, the oligomers and macromolecules in the fiber-forming polymer should be reduced as much as possible, that is, the molecular weight distribution is suitable. Oligomers not only destro...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): D01F6/18
Inventor 吕春祥吴雪平凌立成
Owner SHANXI INST OF COAL CHEM CHINESE ACAD OF SCI
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