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Method for preparing polyacrylonitrile spinning solution

A technology of polyacrylonitrile spinning and acrylonitrile, which is used in the preparation of spinning solutions, single-component synthetic polymer rayon, textiles and papermaking, etc., can solve problems such as the conversion rate of only 37.4% and the inability to meet industrial application requirements. , to achieve the effect of low gel content, stable control and good repeatability

Active Publication Date: 2012-11-14
KINGFA SCI & TECH CO LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In the patent CN 200810054411.3, the temperature range of azobisisoheptanonitrile is reduced to 25-45 degrees. In the implementation example, it is mentioned that the polymerization is carried out at 25 degrees for 24 hours, but the conversion rate is only 37.4%, which cannot meet the requirements of industrial applications; the patent The use range of azobisisoheptanonitrile in CN 200910045219.2 is 30~40 degrees, but this process is obviously different from the traditional process, the system does not contain solvent, and what is obtained after polymerization is polymer powder, which belongs to the two-step process
[0005]Although azobisisoheptanonitrile is more reactive than azobisisobutyronitrile, the ten hour half-life of this initiator corresponds to a decomposition temperature of 50 degrees, which is much higher than room temperature, the polymerization device still needs to be equipped with a heat source to preheat the reaction materials and control the temperature of the reaction process

Method used

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  • Method for preparing polyacrylonitrile spinning solution

Examples

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Comparison scheme
Effect test

Embodiment 1

[0022] Add 10kg of acrylonitrile, 40kg of dimethyl sulfoxide, 200g of methyl acrylate, and 100g of itaconic acid into a 100L reaction kettle, set the temperature inside the kettle to 20°C, pass nitrogen for 30min, and then add α, α'-formazan Base-γ, γ'-Ethoxy-γ, γ'-Carboxyl-Azobisvaleronitrile (R is ethoxy, R1 is carboxyl). The polymerization was stopped after 24 hours, and the obtained polymer had a molecular weight of 205,000, a molecular weight distribution of 2.3, and a monomer conversion rate of 82%.

Embodiment 2

[0024] Add 10kg of acrylonitrile, 40kg of dimethyl sulfoxide, and 150g of itaconic acid into a 100L reaction kettle, set the temperature inside the kettle to 20 degrees, and add α, α', γ, γ'-formazan after 30 minutes of nitrogen flow Base-γ, γ'-methoxy-azobisisovaleronitrile (R is methyl, R1 is methoxy). Set the temperature to 25 degrees after 2 hours, set the temperature to 30 degrees after 4 hours, set the temperature to 40 degrees after 5 hours, stop the polymerization after 24 hours, and obtain a polymer with a molecular weight of 196,000, a molecular weight distribution of 2.3, and a monomer conversion rate 90%

Embodiment 3

[0026] Add 10kg of acrylonitrile, 40kg of dimethyl sulfoxide, 200g of acrylamide, and 150g of itaconic acid into a 100L reaction kettle, set the temperature inside the kettle to 20°C, and add α, α'-methyl -γ, γ'-Ethyl-γ, γ'-Butoxy-Azobisisovaleronitrile (R is ethyl, R1 is butoxy). Set the temperature to 25 degrees after 2 hours, set the temperature to 30 degrees after 4 hours, set the temperature to 40 degrees after 5 hours, stop the polymerization after 24 hours, and obtain a polymer with a molecular weight of 206,000, a molecular weight distribution of 2.4, and a monomer conversion rate 92%

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Abstract

The invention discloses a method for preparing polyacrylonitrile spinning solution. Initiator is adopted in the polymerization process, and the initiator is alpha, alpha'-methyl-gamma, gamma'-disubstituted azo-bis valeronitrile with higher activity, thus the polymerization of acrylonitrile is initiated at low temperature of 10-40 DEG C. The polymerization heat can be fully utilized in the polymerization process to control the viscosity of the system. The temperature of the system can be controlled stably by adjusting cooling water. The polymerization solution contains less gel and has good reproducibility. The polyacrylonitrile spinning solution prepared by using the method disclosed by the invention can be used for preparing polyacrylonitrile fiber or acrylonitrile-based carbon fiber.

Description

technical field [0001] The invention relates to a preparation method of polyacrylonitrile spinning stock solution. Background technique [0002] The performance and quality of polyacrylonitrile spinning solution will directly affect the fiber coagulation forming and drawing orientation, and high-performance spinning solution is a necessary condition for preparing high-performance carbon fibers. [0003] According to the characteristics of free radical solution polymerization, the higher the polymerization temperature, the greater the probability of side reactions such as branching and crosslinking. The traditional one-step PAN spinning solution preparation process usually uses azobisisobutyronitrile as the initiator, and its ten-hour half-life corresponds to a decomposition temperature of 64 degrees. Due to the high polymerization temperature, how to control the microgel content in the system has become a problem for many production One of the problems faced by businessmen....

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08F220/44C08F4/04D01D1/02D01F6/38D01F9/22
Inventor 辛伟马雷黄险波宋威叶丹滢曾祥斌蔡彤旻
Owner KINGFA SCI & TECH CO LTD