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Ammonification method of polyacrylonitrile polymerization liquid and device for realizing same

A technology of polyacrylonitrile and polymerization liquid, which is applied in the fields of fiber chemical characteristics, textiles and papermaking, etc., and can solve problems such as difficulty in stably controlling the ammoniation degree of PAN polymerization liquid, affecting the quality stability of PAN precursor, and difficulty in obtaining PAN polymerization liquid, etc. , to achieve the effect of overcoming the difficult measurement of ammonia gas, improving controllability and uniformity, and simple structure

Inactive Publication Date: 2013-08-28
ZHEJIANG TAIXIAN NEW MATERIAL
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

But, this method has following shortcoming: the one, because ammonia has hindering effect to free radical polymerization reaction, directly pass ammonia gas in polymerization kettle, can pollute polymerization kettle, and residual ammonia can hinder the carrying out of next polymerization reaction; The 2nd, because The PAN polymerization liquid is a viscous system, and it is very difficult to mix ammonia gas with it, so it is difficult to obtain a uniformly ammoniated PAN polymerization liquid; third, because only a small amount of ammonia gas is absorbed by the polymerization liquid, it is difficult to stably control the PAN polymerization liquid The degree of ammoniation, which in turn affects the quality stability of PAN precursor

Method used

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  • Ammonification method of polyacrylonitrile polymerization liquid and device for realizing same

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Experimental program
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Effect test

Embodiment 1

[0031] DMSO is input in the spray tower 1, and the ammonia gas in the ammonia cylinder 2 is passed into the spray tower 1 to obtain NH 3 The mass percent concentration is 1% NH 3 / DMSO dilute solution;

[0032]DMSO is used as a solvent, azobisisobutyl is used as an initiator, and acrylonitrile and itaconic acid are used as comonomers (wherein, itaconic acid accounts for 1% by mass of the total monomers) and reacted in a polymerization tank 3 for 20 hours to prepare A PAN / DMSO polymer solution with a solid content of 19% was obtained;

[0033] Use the first metering gear pump 4 and the second metering gear pump 5 to separate the PAN / DMSO polymerization liquid in the polymerization kettle 3 and the NH in the spray tower 1 3 / DMSO dilute solution is delivered in the static mixer 6, the two are mixed evenly;

[0034] The mixed material directly enters the single-removal tank to remove unreacted acrylonitrile and soluble ammonia; finally, the material is transported to the defoa...

Embodiment 2

[0040] DMSO is input into the spray tower 1, and the ammonia gas in the ammonia cylinder 2 is passed into the spray tower 1 to obtain NH 3 The mass percent concentration is 1% NH 3 / DMSO dilute solution;

[0041] DMSO is used as a solvent, azobisisobutyl is used as an initiator, and acrylonitrile and itaconic acid are used as comonomers (wherein, itaconic acid accounts for 1% by mass of the total monomers) and reacted in a polymerization tank 3 for 20 hours to prepare To obtain a PAN / DMSO polymerization solution with a solid mass percent content of 20%;

[0042] Use the first metering gear pump 4 and the second metering gear pump 5 to separate the PAN / DMSO polymerization liquid in the polymerization kettle 3 and the NH in the spray tower 1 3 / DMSO dilute solution is delivered in the static mixer 6, the two are mixed evenly;

[0043] The mixed material directly enters the single-removal tank to remove unreacted acrylonitrile and soluble ammonia; finally, the material is tran...

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Abstract

The invention discloses an ammonification method of polyacrylonitrile polymerization liquid and a device for realizing the same. The method comprises the following steps: (1) dissolving acrylonitrile, copolymerization monomers and an initiator in a solvent in a polymerization kettle by adopting a solution polymerization process, and carrying out copolymerization reaction in a solution state to obtain the polyacrylonitrile polymerization liquid; (2) adding a certain amount of solvent to a container, and introducing ammonia gas to the solvent to obtain NH3 solution, wherein the solvent is same as that used in the step (1); and (3) adding a proper amount of the polyacrylonitrile polymerization liquid obtained in the step (1) and a proper amount of the NH3 solution obtained in the step (2) toa mixer, and uniformly mixing to realize uniform ammonification of the polyacrylonitrile polymerization liquid. Compared with the existing ammonia gas bubbling method, the ammonification method overcomes the defects that ammonia gas is difficult to meter and mix and generates pollution to the polymerization kettle, improves the ammonification controllability and uniformity, and lays a foundation for production of stable and high-performance PAN (polyacrylonitrile) protofilament.

Description

technical field [0001] The invention relates to the technical field of polyacrylonitrile precursor preparation, in particular to a method for ammoniating polyacrylonitrile polymerization liquid and a device for realizing the method. Background technique [0002] Carbon fiber has many excellent properties such as low density, high specific strength, high specific modulus, high temperature resistance and corrosion resistance, and has been widely used in various fields of aerospace, national defense and civilian industries. According to the raw material route, carbon fiber can be divided into three types: polyacrylonitrile (PAN)-based, pitch-based and viscose-based. Among them, PAN-based carbon fiber has become a carbon fiber with the fastest development, the highest output, the most varieties and the widest application due to its simple production process, low production cost and excellent mechanical properties. [0003] It is well known that high-performance PAN precursors a...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08F220/46C08F222/02C08F6/06D01F9/22
Inventor 杨建行欧阳琴陈友汜莫高明黄显雯马洪波
Owner ZHEJIANG TAIXIAN NEW MATERIAL