A kind of preparation method of ternary polyacrylonitrile copolymer for carbon fiber precursor

A technology of carbon fiber precursors and polyacrylonitrile, which is applied in the field of preparation of ternary polyacrylonitrile copolymers for carbon fiber precursors. It can solve the problems of inability to obtain high-performance carbon fibers and difficult control, and achieve easy control of exothermic reactions and reduce flexibility. , performance and the effect of carbonization yield improvement

Inactive Publication Date: 2016-09-07
DONGHUA UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The macromolecular chain structure of homopolymerized polyacrylonitrile is relatively regular, and the crystallinity is high. It reacts by free radical mechanism during pre-oxidation and cyclization, which is difficult to control and cannot obtain carbon fibers with good performance.

Method used

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  • A kind of preparation method of ternary polyacrylonitrile copolymer for carbon fiber precursor
  • A kind of preparation method of ternary polyacrylonitrile copolymer for carbon fiber precursor
  • A kind of preparation method of ternary polyacrylonitrile copolymer for carbon fiber precursor

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] The polymerization reactor was evacuated and circulated with nitrogen for 3 times. 22.31g of acrylonitrile, 0.46g of itaconic acid, 0.23g of polyvinyl alcohol (1755) and 60g of deionized water were added to the 5L glass reactor at 35°C. Blow nitrogen for 30min, heat up to 60℃ and hold at this temperature for 0.5h, then add ammonium persulfate (0.23g / 10gH 2 O) Aqueous solution and completed within 0.5h. After the initiator is added, acrylamide (0.23g / 7gH 2 O) Aqueous solution and finished in 1h. At the same time, keep the reaction at 60℃ for 24 hours, the prepared polyacrylonitrile has a viscosity average molecular weight of 3.4×10 5 g / mol, molecular weight distribution is 2.98. The polymer slurry was filtered, removed from the order, and dried to obtain a white granular powder. The measured copolymer conversion rate was 87.7%. DSC test under nitrogen atmosphere (using TA Company’s Q20 differential scanning calorimeter, rising from 30°C to 310°C at a rate of 5°C / min) show...

Embodiment 2

[0033] The polymerization reactor was evacuated and circulated with nitrogen for 3 times. 22.54g of acrylonitrile, 0.23g of itaconic acid, 0.23g of polyvinyl alcohol (1788) and 60g of deionized water were added to the 5L glass reactor at 35°C. Blow nitrogen for 30min, heat up to 60℃ and hold at this temperature for 0.5h, then add ammonium persulfate (0.23g / 10gH 2 O) Aqueous solution and completed within 0.5h. After the initiator is added, acrylamide (0.23g / 7gH 2 O) Aqueous solution and finished in 1h. At the same time, keep the reaction at 60℃ for 24 hours, the prepared polyacrylonitrile has a viscosity average molecular weight of 3.8×10 5 g / mol, the molecular weight distribution is 3.02. The polymer slurry was filtered, removed from the order, and dried to obtain a white granular powder. The measured copolymer conversion rate was 89.1%. DSC test under nitrogen atmosphere (using TA Company’s Q20 differential scanning calorimeter, rising from 30°C to 310°C at a rate of 5°C / min) ...

Embodiment 3

[0035] The polymerization reactor was evacuated and circulated with nitrogen for 3 times. 22.08g of acrylonitrile, 0.69g of itaconic acid, 0.23g of polyvinyl alcohol (1799) and 60g of deionized water were added to the 5L glass reactor at 35°C. Blow nitrogen for 30min, heat up to 60℃ and hold at this temperature for 0.5h, then add ammonium persulfate (0.23g / 10gH 2 O) Aqueous solution and completed within 0.5h. After the initiator is added, acrylamide (0.23g / 7gH 2 O) Aqueous solution and finished in 1h. At the same time, keep the reaction at 60℃ for 24 hours, the prepared polyacrylonitrile has a viscosity average molecular weight of 4.1×10 5 g / mol, molecular weight distribution is 2.98. The polymer slurry was filtered, removed, and dried to obtain a white granular powder. The measured copolymer conversion rate was 92.4%. DSC test under nitrogen atmosphere (using TA Company’s Q20 differential scanning calorimeter, rising from 30°C to 310°C at a rate of 5°C / min) shows that the init...

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Abstract

The invention relates to a method for preparing a ternary polyacrylonitrile copolymer applicable to a carbon fiber precursor; the method comprises the steps: under the protection of nitrogen gas, mixing acrylonitrile, itaconic acid, dispersant and water and heating to 60-75 DEG C; dropwise adding initiator aqueous solution and acrylamide aqueous solution in sequence; after dropwise adding, timing and reacting for 3-24h, washing, denitrifying, filtering, drying and obtaining the ternary polyacrylonitrile copolymer. A water-phase suspension polymerization process is adopted to polymerization; the polymerization heat is easy to be removed and the polymerization temperature is easily controlled; the average molecular weight of the ternary polyacrylonitrile copolymer is higher and the molecular weight distribution is narrow; the prepared ternary polyacrylonitrile copolymer is capable of effectively improving thermal stability performance at a high-temperature pre-oxidation stage and has certain actual application prospects.

Description

Technical field [0001] The invention belongs to the field of preparing copolymers for carbon fiber precursors, and particularly relates to a method for preparing a ternary polyacrylonitrile copolymer for carbon fiber precursors. Background technique [0002] Carbon fiber has a series of excellent properties such as high specific strength, high specific modulus, high temperature resistance, corrosion resistance, fatigue resistance, electrical conductivity, shock absorption, heat transfer, radiation resistance and small specific gravity. It is widely used in aerospace, military defense, and environmental protection. , Medical equipment and sporting goods industries. [0003] The macromolecular chain structure of homopolyacrylonitrile is relatively regular, and the crystallinity is high. When pre-oxidized and cyclized, it reacts with a free radical mechanism, which is difficult to control and cannot obtain carbon fibers with good performance. When preparing the polyacrylonitrile-base...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08F220/48C08F222/02C08F220/56C08F2/20D01F9/22
Inventor 曾照坡肖茹吕永根
Owner DONGHUA UNIV
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