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Preparation method of polyacrylonitrile precursor

A technology of polyacrylonitrile and acrylonitrile, which is applied in the field of preparation of polyacrylonitrile precursors, can solve the problems of low strength and unstable performance of carbon fiber precursors, and achieve the effects of high density, guaranteed stability and good technical effects

Inactive Publication Date: 2016-06-15
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] The invention mainly solves the problem of low strength and unstable performance of the carbon fiber precursor obtained by spinning in the prior art by using an ordinary oil agent device

Method used

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  • Preparation method of polyacrylonitrile precursor
  • Preparation method of polyacrylonitrile precursor
  • Preparation method of polyacrylonitrile precursor

Examples

Experimental program
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Effect test

Embodiment 1

[0024] 1. Preparation of stock solution: Distilled acrylonitrile (AN) and itaconic acid (IA) in a ratio of 97:3, with a solid content of 20%, and azobisisobutyronitrile (AIBN) accounts for 0.4wt% of the comonomer, Add dimethyl sulfoxide (DMSO) as a solvent into the reactor, and react at a constant temperature of 38° C. for 20 hours under the protection of nitrogen to obtain a binary acrylonitrile copolymer spinning solution. Then the spinning solution is decompressed to remove residual monomers and air bubbles, and then filtered through a 5 μm filter material to obtain a high-performance polyacrylonitrile copolymer spinning solution.

[0025] 2. Coagulation molding: Extrude through the spinneret and enter the first coagulation bath, the temperature of the coagulation bath is 20°C, the concentration is 50%, the draft ratio is -30%, the second coagulation bath is 40°C, the concentration is 40% %, the draft ratio is 100%, the third coagulation bath is 60°C, the concentration is 3...

Embodiment 2

[0033] 1. Preparation of stock solution: Distilled acrylonitrile (AN) and itaconic acid (IA) in a ratio of 97:3, with a solid content of 20%, and azobisisobutyronitrile (AIBN) accounts for 0.4wt% of the comonomer, Add dimethyl sulfoxide (DMSO) as a solvent into the reactor, and react at a constant temperature of 38° C. for 20 hours under the protection of nitrogen to obtain a binary acrylonitrile copolymer spinning solution. Then the spinning solution is decompressed to remove residual monomers and air bubbles, and then filtered through a 5 μm filter material to obtain a high-performance polyacrylonitrile copolymer spinning solution.

[0034] 2. Coagulation molding: Extrude through the spinneret and enter the first coagulation bath, the temperature of the coagulation bath is 20°C, the concentration is 50%, the draft ratio is -30%, the second coagulation bath is 40°C, the concentration is 40% %, the draft ratio is 100%, the third coagulation bath is 60°C, the concentration is 3...

Embodiment 3

[0040] 1. Preparation of stock solution: Distilled acrylonitrile (AN) and itaconic acid (IA) in a ratio of 97:3, with a solid content of 20%, and azobisisobutyronitrile (AIBN) accounts for 0.4wt% of the comonomer, Add dimethyl sulfoxide (DMSO) as a solvent into the reactor, and react at a constant temperature of 38° C. for 20 hours under the protection of nitrogen to obtain a binary acrylonitrile copolymer spinning solution. Then the spinning solution is decompressed to remove residual monomers and air bubbles, and then filtered through a 5 μm filter material to obtain a high-performance polyacrylonitrile copolymer spinning solution.

[0041] 2. Coagulation molding: Extrude through the spinneret and enter the first coagulation bath, the temperature of the coagulation bath is 20°C, the concentration is 50%, the draft ratio is -30%, the second coagulation bath is 40°C, the concentration is 40% %, the draft ratio is 100%, the third coagulation bath is 60°C, the concentration is 3...

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Abstract

The present invention relates to a preparation method of a polyacrylonitrile precursor, and mainly solves the problems that in the prior art a carbon fiber precursor obtained by spinning by use of a common oil device is low in strength and unstable in performance. The preparation method well solves the problems, and the preparation method includes the following steps: 1) a spinning stock solution is prepared by binary copolymerization, a high performance polyacrylonitrile copolymer spinning stock solution is obtained by filtering after demonomerisation and defoaming of the spinning stock solution; and a high density high strength carbon fiber precursor can be obtained by solidification, drawing, water washing, oiling by use of an oil agent groove with an ultrasound device, compacting by drying, steam stretching, steam heat-setting and collection; and the method can be used for the industrial production of the carbon fiber precursor.

Description

technical field [0001] The invention relates to a preparation method of polyacrylonitrile precursor. Background technique [0002] Polyacrylonitrile (PAN)-based carbon fiber is a new type of material developed rapidly in the 1960s, because of its light weight, high specific strength, high specific modulus, high temperature resistance, corrosion resistance, wear resistance, fatigue resistance, electrical conductivity, thermal conductivity, etc. It is widely used in military industries such as satellites, launch vehicles, tactical missiles, and spacecraft, and has become an indispensable material in the aerospace industry. Excellent carbon fiber precursors should have the characteristics of high heat resistance, less pore structure, less surface defects, dense structure, and good stretchability. [0003] Pre-filament is the prerequisite for producing high-performance carbon fiber, and in the spinning process, the uniformity of oiling often determines the fiber breakage rate a...

Claims

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Application Information

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IPC IPC(8): D01F6/38D01F11/06D01F9/22D01D5/06D01D5/14D01D10/06D01D11/00
Inventor 张静缪金根沈志刚赵微微
Owner CHINA PETROLEUM & CHEM CORP
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