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

A low-molecular-weight, acrylonitrile technology, applied in the direction of single-component synthetic polymer rayon, textiles and papermaking, fiber chemical characteristics, etc., can solve the problems of increased molecular weight distribution index of polymers, small molecular weight of polymers, etc., to achieve the method Simple, easy-to-craft effect

Active Publication Date: 2013-04-10
NINGBO INST OF MATERIALS TECH & ENG CHINESE ACADEMY OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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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

[0027] In the present embodiment, the preparation method of acrylonitrile copolymer spinning solution comprises the following steps:

[0028] (1) Accurately take by weighing 13.30kg dimethyl sulfoxide, 0.088kg itaconic acid, 3.88kg acrylonitrile, 0.044kg azobisisobutyronitrile, and 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;

[0029] (2) After reacting the reaction system at a constant temperature of 60°C for 9 hours, add 0.42 kg of acrylonitrile to the reaction system, continue to stir and react at a constant temperature of 60°C for 13 hours, and then remove the residual monomers and bubbles in the system to obtain acrylonitrile copolymer Spinning solution B.

[0030] Measure the...

Embodiment 2

[0032] In the present embodiment, the preparation method of acrylonitrile copolymer spinning solution comprises the following steps:

[0033] (1) Accurately take by weighing 13.30kg dimethyl sulfoxide, 0.088kg itaconic acid, 3.67kg 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 65°C to allow the polymerization reaction of acrylonitrile and itaconic acid, which is used as the starting point of the polymerization reaction;

[0034] (2) After reacting the reaction system at a constant temperature of 60°C for 5 hours, add 0.63 kg of acrylonitrile in batches to the polymerization system within 3 hours, then stir the reaction system at a constant temperature of 65°C for 14 hours, and then remove the residual monomers in the system bodies and air bubbles to obtain acrylonitrile copolymer ...

Embodiment 3

[0043] In the present embodiment, the preparation method of acrylonitrile copolymer spinning solution comprises the following steps:

[0044] (1) Accurately weigh 13.30kg dimethyl sulfoxide, 0.066kg itaconic acid, 0.022kg methyl acrylate, 3.88kg acrylonitrile, 0.044kg azobisisobutyronitrile and add them to the In the reactor, under the protection of nitrogen, stir at room temperature for 20 minutes, then raise the temperature of the system to 65 ° C, so that acrylonitrile, itaconic acid, and methyl acrylate are polymerized, and this time is used as the starting point of the reaction;

[0045] (2) After reacting the reaction system at a constant temperature of 65°C for 8 hours, add 0.42 kg of acrylonitrile to the reaction system, continue to stir and react at a constant temperature of 65°C for 12 hours, and then remove the residual monomers and bubbles in the system to obtain acrylonitrile copolymer Textile spinning solution E.

[0046] Measure the weight-average molecular wei...

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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 preparation method, in a solution polymerization process of an acrylonitrile monomer and a comonomer, the acrylonitrile monomer is supplemented once or multiple times within certain reaction time to adjust a weight-average molecular weight and a number-average molecular weight of a copolymer so as to reduce a molecular weight distribution index of the copolymer. Compared with other methods, the preparation method is simple and easy to implement in process; the molecular weight distribution index of the acrylonitrile copolymer prepared by using the method can be controlled between 2.5 and 3.0; and after residual monomers and bubbles of an acrylonitrile copolymer solution are removed, the acrylonitrile copolymer solution can be used as a spinning solution of high-performance polyacrylonitrile-based carbon fibers.

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 an acrylonitrile copolymer spinning solution with low molecular weight distribution. Background technique [0002] Carbon fiber is an inorganic polymer fiber with a carbon content higher than 90%. 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 application due to its simple production process, low production cost and excellent mechanical properties. [0003] It is generally believed that the quality of polyacrylonitrile precursors determines the quality of polyacrylonitrile-based carbon fibers, and only acrylonitrile copolymer spinning ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F220/44C08F220/46C08F220/48D01F6/38D01F9/22
Inventor 莫高明张若愚王艳菲渠丽景陈友汜欧阳琴杨建行
Owner NINGBO INST OF MATERIALS TECH & ENG CHINESE ACADEMY OF SCI
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