Polyacrylonitrile copolymer spinning solution and preparation method thereof

A technology of polyacrylonitrile and copolymer, which is applied in the field of polyacrylonitrile copolymer spinning solution and its rapid and stable preparation, can solve problems such as mass transfer, heat transfer difficulties, affecting fiber performance, and prone to implosion, etc., to achieve Enhanced mass transfer and heat transfer, narrow molecular weight distribution, no need for mechanical stirring

A technology of polyacrylonitrile and copolymer, which is applied in the field of polyacrylonitrile copolymer spinning solution and its rapid and stable preparation, can solve problems such as mass transfer, heat transfer difficulties, affecting fiber performance, and prone to implosion, etc., to achieve Enhanced mass transfer and heat transfer, narrow molecular weight distribution, no need for mechanical stirring

CN103421141AActive Publication Date: 2013-12-04INST OF CHEM CHINESE ACAD OF SCI
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  • Polyacrylonitrile copolymer spinning solution and preparation method thereof
  • Polyacrylonitrile copolymer spinning solution and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0050] Such as figure 1 As shown, the tubular reactor containing the static mixer assembly includes a circular pipe with a static mixer assembly 2 installed in a circular pipe made of stainless steel, and a circular pipe with a ring jacket 1 installed outside the circular pipe and an internal circulation pump 3, etc.; and connect four circular tubes in series through a flange installed on the circular tube in the tubular reactor to form a four-section tubular reaction containing a static mixer assembly device.

[0051] One end of the first circular tube in the tubular reactor containing the static mixer assembly combined into four sections is connected with one end of the internal circulation pump 3 through a pipeline, and a pressure gauge; the second circular tube connected in series with the first circular tube is equipped with a temperature control sensor, and is provided with a raw material inlet a; the other end of the internal circulation pump 3 passes through the tube ...

Embodiment 2

[0062] The preparation of the polyacrylonitrile copolymer spinning solution was carried out using the tubular reactor containing the static mixer assembly of Example 1.

[0063] (1) Accurately weigh 28.4Kg of solvent dimethylformamide, 9.408Kg of acrylonitrile, and 192g of methacrylic acid into a stainless steel batching kettle with a mechanical stirring device, and stir and mix at room temperature for about 30 minutes. During the process, nitrogen bubbles are used to evacuate and remove oxygen;

[0064] (2) Accurately weigh 2Kg of the solvent dimethylformamide and 57.6g of the free radical initiator azobisisobutyronitrile into the container, and stir rapidly at room temperature to dissolve;

[0065] (3) Under nitrogen protection and stirring, put the free radical initiator solution prepared in step (2) into the batching kettle of step (1) at one time, stir and mix rapidly at room temperature for 2 minutes to obtain a reaction solution;

[0066] (4) Use the external circulati...

Embodiment 3

[0069] The preparation of the polyacrylonitrile copolymer spinning solution was carried out using the tubular reactor containing the static mixer assembly of Example 1.

[0070] (1) Accurately weigh 26.8Kg of solvent dimethyl sulfoxide, 10.864Kg of acrylonitrile, 224g of acrylamide, and 112g of itaconic acid into a stainless steel batching kettle with a mechanical stirring device, stir and mix at room temperature for about 30 minutes, and In the process of stirring and mixing, use nitrogen bubbles to evacuate and remove oxygen;

[0071] (2) Accurately weigh 2Kg of the solvent dimethylformamide and 67.2g of the free radical initiator azobisisoheptanonitrile and add them to the container, stir and dissolve quickly at room temperature;

[0072] (3) Under nitrogen protection and stirring, put the free radical initiator solution prepared in step (2) into the batching kettle of step (1) at one time, stir and mix rapidly at room temperature for 2 minutes to obtain a reaction solution...

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Abstract

The invention relates to a polyacrylonitrile copolymer spinning solution and a preparation method thereof. In the invention, copolymerization reaction is performed on acrylonitrile in a tubular reactor containing a static mixer component; the tubular reactor, which contains the static mixer component and has the characteristics of mass transfer, efficient heat transfer, continuous and stable reaction and no mechanical stirring, is adopted to prepare the polyacrylonitrile copolymer spinning solution with high molecular weight and narrow molecular weight distribution. The polyacrylonitrile copolymer spinning solution is obtained after copolymerization reaction is performed on reaction liquid composed of monomers, a radical initiator and a solvent, wherein the percent concentration by weight of the monomers in the reaction liquid is 15% to 20%; the weight of the radical initiator is 0.4% to 1% of that of the monomers; the solvent is in balancing amount; the monomers are an acrylonitrile monomer and a comonomer. The dynamic viscosity of the polyacrylonitrile copolymer spinning solution provided by the invention is 200 to 800 Pa.S, and the molecular weight distribution is 1.5 to 2.6.

Description

technical field [0001] The invention belongs to the field of polyacrylonitrile preparation, in particular to a polyacrylonitrile copolymer spinning solution with uniform viscosity and narrow molecular weight distribution and a rapid and stable preparation method thereof. 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. Polyacrylonitrile-based carbon fiber has outstanding mechanical properties and is a hot spot in carbon fiber research and industrialization 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 polyacrylonitri...

Claims

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Application Information

Patent Timeline
04 Dec 2013
Publication
CN103421141A
IPC
C08F220/46; C08F220/48; C08F220/44; C08F2/01; D01F9/22; D01D1/02
Inventors
肖耀南; 李春成