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Method for preparing high molecular weight acrylonitrile copolymer with narrow molecular weight distribution

A technology with narrow molecular weight distribution and high molecular weight, applied in the field of acrylonitrile copolymer spinning solution, can solve the problems of low adjustment ability, reduced monomer conversion rate, complex structure, etc. Easy, less toxic effect

Inactive Publication Date: 2008-03-19
CHANGZHOU INST OF ENERGY STORAGE MATERIALS &DEVICES
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  • Abstract
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  • Application Information

AI Technical Summary

Problems solved by technology

But because the molecular weight of the synthetic acrylonitrile homopolymer is too big, and monomer conversion rate is low, can not be used as the spinning liquid of polyacrylonitrile-based carbon fiber
Using dodecyl mercaptan-based mercaptans or isopropanol as chain transfer agents for free radical polymerization can effectively adjust the molecular weight of acrylonitrile copolymers, but will reduce the conversion rate of monomers
In addition, the strong pungent smell and strong toxicity of mercaptan are unfavorable factors restricting industrial production, while isopropanol has no pungent smell and is less toxic, but its adjustment ability is not high
Chinese patents 94194602.9 and 01140852.9 report that allyl compounds can regulate free radical polymerization and reduce the molecular weight of polymers, but such allyl compounds have complex structures and difficult synthesis, and are not suitable for molecular weight adjustment of acrylonitrile-based carbon fiber spinning solutions agent

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] Weigh 19.62 gram of acrylonitrile, 0.20 gram of itaconic acid, 0.20 gram of methyl acrylate, 80 gram of dimethyl sulfoxide, 0.1001 gram of azobisisoheptanonitrile, and add the weighed raw materials into the polymerization device under nitrogen protection, Polymerize at 35°C for 24 hours, then remove residual monomers and air bubbles to obtain an acrylonitrile copolymer spinning solution. The monomer conversion rate was 99.8%, the weight average molecular weight of the copolymer was 580,000, and the molecular weight distribution was 2.04.

Embodiment 2

[0025] Weigh 19.61 grams of acrylonitrile, 0.20 grams of acrylic acid, 0.20 grams of ethyl acrylate, 0.3 grams of propylene alcohol, 80 grams of dimethyl sulfoxide, 0.1002 grams of azobisisoheptanonitrile, and add the weighed raw materials to the polymerization under the protection of nitrogen. In the device, polymerize at 35°C for 24 hours, and then remove residual monomers and air bubbles to obtain an acrylonitrile copolymer spinning solution. The monomer conversion rate was 96.4%, the weight average molecular weight of the copolymer was 171,000, and the molecular weight distribution was 2.06.

Embodiment 3

[0032] Weigh 19.90 g of acrylonitrile, 0.05 g of itaconic acid, 0.05 g of isobutyl acrylate, 80 g of dimethyl sulfoxide, and 0.1605 g of azobisisoheptanonitrile, and add the weighed raw materials into the polymerization device under nitrogen protection , polymerized at 35° C. for 6 hours, and then removed residual monomers and air bubbles to obtain an acrylonitrile copolymer spinning solution. The monomer conversion rate was 47.9%, the weight average molecular weight of the copolymer was 515,000, and the molecular weight distribution was 2.13.

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Abstract

The present invention initiates the copolymerization reaction of acrylonitrile and a comonomer with azo-bis-iso-heptonitrile in the dimethyl sulphoxide solution, and can adjust the molecular weight of an acrylonitrile copolymer with a bit of acrylonitrile, under the condition of 30 to 45 DEG C, the acrylonitrile copolymer having high molecular weight and narrow molecular weight. The present invention is characterized in that by adopting a traditional free radical polymerization method, the azo-bis-iso-heptonitrile is initiating agent, the molecular weight of a copolymer is adjusted with propenol, the synthetic molecular weight can be adjusted and controlled in 100 thousands to 900 thousands, the molecular weight distributes an acrylonitrile copolymer with an index smaller than 2.3, and the acrylonitrile copolymer solution can be used for preparing the spinning liquid of high performance carbon fiber.

Description

[0001] Field [0002] The invention relates to a method for preparing an acrylonitrile copolymer spinning solution with high molecular weight and narrow molecular weight distribution. Background technique [0003] 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. Polyacrylonitrile-based carbon fiber has outstanding mechanical properties and is a hot spot in carbon fiber research in recent years. The key to restricting the development of polyacrylonitrile-based carbon fibers is the quality of polyacrylonitrile precursors, and to obtain high-quality polyacrylonitrile precursors must start from the synthesis of high-quality acrylonitrile copolymer spinning solutions and the o...

Claims

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Application Information

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IPC IPC(8): D01F6/38C08F220/44C08F2/38C08F4/04
Inventor 李悦生李百祥张贵宝刘晓辉白云刚
Owner CHANGZHOU INST OF ENERGY STORAGE MATERIALS &DEVICES
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