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Preparation method of acrylonitrile copolymer spinning solution with low molecular weight distribution

A technology of molecular weight distribution and acrylonitrile, which is applied in the preparation of spinning solutions, etc., can solve the problems of small molecular weight of high molecular weight and increase of molecular weight distribution index of polymers, and achieve the effect of easy realization and simple method

Active Publication Date: 2015-04-22
NINGBO INST OF MATERIALS TECH & ENG CHINESE ACADEMY OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the actual polymerization process is very complicated, and there are often situations beyond the range of the four basic assumptions, especially when the conversion rate is high, the concentration of the monomer and the concentration of the initiator are constantly decreasing, and due to the half-life of the initiator, the monomer The concentration decreases faster than the initiator concentration, and as a result, the molecular weight of newly generated polymers becomes smaller and smaller, resulting in an exponential increase in the molecular weight distribution of the overall polymer

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] In the present embodiment, the preparation method of acrylonitrile copolymer spinning solution comprises the following steps:

[0029] (1) Accurately take by weighing 13.30kg dimethyl sulfoxide, 0.088kg itaconic acid, 4.3kg acrylonitrile, 0.044kg azobisisobutyronitrile, join successively in the reactor with condenser and mechanical stirring device, Under the protection of nitrogen, stir at room temperature for 20 minutes, then raise the temperature of the system to 60°C to allow the polymerization reaction of acrylonitrile and itaconic acid, which is used as the starting point of the polymerization reaction;

[0030] (2) After the reaction starts, the temperature of the reaction system is rapidly reduced by 0.5° C. every 1 hour, so that after 10 hours from the start of the reaction, the temperature of the reaction system drops to 55° C., and then the reaction system is stirred and reacted at a constant temperature of 55° C. for 12 hours, and then Residual monomers and a...

Embodiment 2

[0033] In the present embodiment, the preparation method of acrylonitrile copolymer spinning solution comprises the following steps:

[0034] (1) Accurately take by weighing 13.30kg dimethyl sulfoxide, 0.088kg itaconic acid, 4.3kg acrylonitrile, 0.044kg azobisisobutyronitrile, join successively in the reactor with condenser and mechanical stirring device, Under the protection of nitrogen, stir at room temperature for 20 minutes, then raise the temperature of the system to 60°C to allow the polymerization reaction of acrylonitrile and itaconic acid, which is used as the starting point of the polymerization reaction;

[0035] (2) After the reaction starts, within 10 hours, the temperature of the reaction system is continuously lowered to 53°C, and then the reaction system is stirred and reacted at a constant temperature of 53°C for 12 hours, and then the residual monomers and bubbles in the system are removed to obtain acrylonitrile Copolymer spinning solution C.

[0036]Measur...

Embodiment 3

[0038] In the present embodiment, the preparation method of acrylonitrile copolymer spinning solution comprises the following steps:

[0039] (1) Accurately take by weighing 13.30kg dimethyl sulfoxide, 0.088kg itaconic acid, 4.3kg acrylonitrile, 0.044kg azobisisobutyronitrile, join successively in the reactor with condenser and mechanical stirring device, Under the protection of nitrogen, stir at room temperature for 20 minutes, then raise the temperature of the system to 60°C to allow the polymerization reaction of acrylonitrile and itaconic acid, which is used as the starting point of the polymerization reaction;

[0040] (2) After the reaction starts, stir the reaction system at a constant temperature of 60°C for 5 hours, then quickly cool down the temperature of the reaction system to 50°C, continue to stir the reaction system at a constant temperature of 50°C for 17 hours, and then remove the residual monomers in the system and air bubbles to obtain an acrylonitrile copol...

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Abstract

The invention discloses a preparation method of an acrylonitrile copolymer spinning solution with low molecular weight distribution. According to the invention, in a solution polymerization process between acrylonitrile monomers and comonomers, the weight-average molecular weight and number-average molecular weight of a copolymer are regulated in a continuous or intermittent cooling manner so as to reduce the molecular weight distribution index of the copolymer. Compared with other methods, the preparation method is simple and feasible and is stronger in process operability, the molecular weight distribution index of an acrylonitrile copolymer obtained according to the method can be controlled to be 2.3-2.8, and an acrylonitrile copolymer solution can be used as a high-performance polyacrylonitrile-based carbon fiber spinning solution after residual monomers and air bubbles are removed.

Description

technical field [0001] The invention belongs to the technical field of carbon fiber material preparation, and in particular relates to a method for preparing a spinning solution for reducing the molecular weight distribution of an acrylonitrile copolymer. Background technique [0002] Carbon fiber has the characteristics of high specific strength, high specific modulus, heat resistance, corrosion resistance, fatigue resistance, and creep resistance. It is a high-performance fiber material and has been widely used in aerospace, national defense construction, sports and leisure products, and medical equipment. and construction industries. According to the different raw materials used, carbon fiber can be divided into polyacrylonitrile-based carbon fiber, pitch-based carbon fiber, viscose-based carbon fiber, etc. Among them, polyacrylonitrile-based carbon fiber has become a carbon fiber with the fastest development, the highest output, the most varieties and the widest applica...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): D01F6/38D01F9/22D01D1/02C08F220/44
Inventor 莫高明王艳菲渠丽景陈友汜欧阳琴张若愚杨建行
Owner NINGBO INST OF MATERIALS TECH & ENG CHINESE ACADEMY OF SCI
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