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A kind of preparation method of ternary polyacrylonitrile copolymer

A technology for polyacrylonitrile and copolymers, which is applied in the field of preparation of ternary polyacrylonitrile copolymers, can solve problems such as narrow exothermic peaks and concentrated exothermic peaks, achieve narrow distribution, smooth polymerization process, and improve thermal stability Effect

Inactive Publication Date: 2017-01-11
DONGHUA UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the exothermic peak is narrow during the pre-oxidation of homopolymerized polyacrylonitrile, and the exothermic heat is concentrated, and the peak temperature is about 282 ° C, which is easy to burn the fiber

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] Under the protection of nitrogen, first raise the temperature of the aqueous solution of maleic anhydride, acrylamide and polyvinyl alcohol to 65 ° C, then add acrylonitrile monomer to keep the temperature for 30 minutes, and finally add the dimethyl sulfoxide solution dissolved in azobisisobutyronitrile, After reacting for 6 hours, the conversion rate was 91.7%, and the viscosity-average molecular weight was 2.97×10 5 , a polyacrylonitrile copolymer with a molecular weight distribution of 1.56. According to the DSC test under nitrogen atmosphere (Using the Q20 differential scanning calorimeter of American TA company, rising from 30°C to 310°C at a rate of 5°C / min), it can be seen that the cyclization initiation temperature is higher than that of homopolyacrylonitrile (the same Prepared under polymerization conditions, the viscosity-average molecular weight (molecular weight: 302,000) decreased by 27.6°C; the exothermic heat of cyclization was 567.3J / g, which was 54.4J / ...

Embodiment 2

[0031] According to the formula in Table 2, under the protection of nitrogen, the aqueous solution of maleic anhydride, acrylamide and polyvinyl alcohol was first heated to 65°C, then the acrylonitrile monomer was added to keep the temperature for 30 minutes, and finally the diisobutyronitrile dissolved in azobisisobutyronitrile was added. Methyl sulfoxide solution was reacted for 6 hours to obtain a conversion rate of 90.3% and a viscosity-average molecular weight of 2.89×10 5 , a polyacrylonitrile copolymer with a molecular weight distribution of 1.74. According to the DSC test under nitrogen atmosphere (Using the Q20 differential scanning calorimeter of American TA company, rising from 30°C to 310°C at a rate of 5°C / min), it can be seen that the cyclization initiation temperature is higher than that of homopolyacrylonitrile (the same Prepared under polymerization conditions, the viscosity-average molecular weight (molecular weight: 308,000) decreased by 29.0°C; the exotherm...

Embodiment 3

[0035] According to the formula in Table 3, under the protection of nitrogen, the aqueous solution of maleic anhydride, acrylamide and polyvinyl alcohol was first heated to 65 °C, then the acrylonitrile monomer was added to keep the temperature for 30 minutes, and finally the dimethyl solution dissolved in azobisisobutyronitrile was added. The base sulfoxide solution was reacted for 6 hours to obtain a conversion rate of 94.6% and a viscosity-average molecular weight of 3.06×10 5 , a polyacrylonitrile copolymer with a molecular weight distribution of 1.91. According to the DSC test under nitrogen atmosphere (Using the Q20 differential scanning calorimeter of American TA company, rising from 30°C to 310°C at a rate of 5°C / min), it can be seen that the cyclization initiation temperature is higher than that of homopolyacrylonitrile (the same Prepared under polymerization conditions, the viscosity-average molecular weight is 325,000) decreased by 31.4°C; the exothermic heat of cyc...

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Abstract

The invention relates to a preparation method of a ternary polyacrylonitrile copolymer, which comprises the steps of heating an aqueous solution of maleic anhydride, acrylamide and a dispersing agent to 55-75 DEG C under a nitrogen shielding condition, adding acrylonitrile to keep constant temperature for 20-30min, adding an initiator solution for reaction for 3-12h, and carrying out washing, demonomerisation, filtration and drying. The method employs a mixed solvent precipitation polymerization method for polymerization and has the advantages of high reaction yield, high viscosity average molecular weight, narrow distribution, easiness in temperature control, stable product quality and the like. The thermal property of the polyacrylonitrile copolymer prepared by the method can be effectively improved, and the copolymer has certain practical application prospects.

Description

technical field [0001] The invention belongs to the field of preparation of polyacrylonitrile for carbon fiber precursors, in particular to a preparation method of a ternary polyacrylonitrile copolymer. 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. Homopolyacrylonitrile seems to be the most ideal in terms of structural uniformity and carbon yield. However, the exothermic peak is narrow and concentrated during the preoxidation of homopolyacrylonitrile, and the peak temperature is about 282 ° C, which is easy to burn the fiber. Therefore, it is necessary to add a certain copolymeriza...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08F220/48C08F222/06C08F220/56D01F9/22D01F6/38
Inventor 曾照坡肖茹吕永根晏珊
Owner DONGHUA UNIV
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