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A method and device for ammoniating polyacrylonitrile spinning dope

A technology of polyacrylonitrile spinning and polyacrylonitrile, which is applied in the chemical post-treatment of synthetic polymer rayon, single-component synthetic polymer rayon, and fiber chemical characteristics. Prolong the processing time and other problems to achieve the effect of overcoming the difficulty of metering, avoiding the presence of ammonia gas, and adjusting the solid content

Active Publication Date: 2017-03-01
GUANGZHOU KINGFA CARBON FIBER NEW MATERIALS DEV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Because ammonia is difficult to measure, its dissolved amount is difficult to measure, and after the ammoniation process, due to the residual ammonia gas, it is necessary to carry out the de-single and de-gassing process, thereby prolonging the processing time and affecting work efficiency , and there will also be a certain loss of ammonia in the process of single removal and defoaming, which leads to the difficulty in controlling the amount of ammoniation. Therefore, the stability of the PAN precursor obtained by this method is poor

Method used

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  • A method and device for ammoniating polyacrylonitrile spinning dope

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] 10kg of acrylonitrile, 0.2kg of itaconic acid, 0.3kg of methyl acrylate, 0.06kg of azobisisobutyronitrile and 40kg of dimethyl sulfoxide were copolymerized at 63°C, and the solid content of the obtained copolymer was 19.8%. The average molecular weight is 260,000, and it is placed in the storage kettle 1 for subsequent use after de-singling and defoaming.

[0034] 2.5kg of DMSO was placed in the liquid storage tank 4, and 51g of ammonia solution with a mass concentration of 25% was added to prepare a NH3 / DMSO solution with a mass percentage of 0.5% ammonia.

[0035] Use the gear metering pump 2 and the high-pressure liquid phase pump 3 to transport the polyacrylonitrile spinning stock solution in the storage tank 1 and the NH3 / DMSO solution in the liquid storage tank 4 to the static mixer 6 according to a certain ratio, and control the ammoniation The ratio is 20%, and the obtained homogeneously ammoniated polyacrylonitrile spinning dope is finely filtered and then prep...

Embodiment 2

[0038] The ratio of ammoniation is controlled at 80%, and other conditions are the same as example 1. The solid content of the homogeneous polyacrylonitrile spinning stock solution of gained ammoniation is 18.28%, and the polyacrylonitrile precursor fineness prepared by dry-jet wet spinning is 1.25dtex, density It is 1.184g / cm3, and this precursor obtains the polyacrylonitrile-based carbon fiber of density 1.823g / cm3, tensile strength 5.08GPa, tensile modulus of elasticity 290GPa after pre-oxidation carbonization.

Embodiment 3

[0040]The ammoniation ratio is controlled at 150%, and other conditions are the same as example 1. The polyacrylonitrile spinning stock solution with uniform ammoniation solid content is 17.15%, and the polyacrylonitrile precursor fineness prepared by dry-jet wet spinning is 1.25dtex, and the density It is 1.178g / cm3, and this precursor obtains the polyacrylonitrile base carbon fiber of density 1.819g / cm3, tensile strength 4.96GPa, tensile modulus of elasticity 286GPa after pre-oxidation carbonization.

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Abstract

The invention discloses an ammonification method and device of a polyacrylonitrile spinning solution. The method comprises the steps of 1, dissolving acrylonitrile and a comonomer into a solvent in a polymeric kettle, and carrying out complex solution copolymerization by feeding an initiating agent into the polymeric kettle to obtain a polyacrylonitrile polymerization solution; 2, carrying out demonomerisation on the polyacrylonitrile polymerization solution, carrying out deaeration to form the polyacrylonitrile spinning solution, and storing the obtained polyacrylonitrile spinning solution in a storage kettle for later use; 3, feeding a certain amount of solvent into a liquid storage tank, wherein the solvent is the same as that used in the step 1, mixing a certain amount of ammonia water into the solvent to obtain a solution with the known ammonia concentration; and 4, fully mixing the polyacrylonitrile spinning solution obtained in the step 2 and the solution with the known ammonia concentration obtained in the step 3 to realize the even ammonification of the polyacrylonitrile spinning solution. After the method is adopted, the ammoniation amount can be accurately controlled, the hydrophilia of polymerization liquid is obviously improved, the ammonification time is shortened, and the working efficiency is improved.

Description

technical field [0001] The invention relates to the technical field of polyacrylonitrile raw silk preparation, in particular to a method for ammonating polyacrylonitrile spinning stock solution and a device thereof. Background technique [0002] Carbon fiber has many advantages such as low density, high specific strength, high specific modulus, high temperature resistance, and corrosion resistance. It has been widely used in various fields such as aerospace, transportation, medical equipment, sporting goods, and new energy. There are many kinds of carbon fibers. Among them, PAN-based carbon fibers have developed into a carbon fiber with the largest output, the most varieties and the widest application due to its relatively simple production process, excellent mechanical properties and low cost. [0003] As we all know, high-quality PAN precursors are an important prerequisite for the preparation of high-performance PAN-based carbon fibers. Therefore, the coagulation process ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): D01F6/38D01F9/22D01F11/06
Inventor 黄险波陈大华辛伟马雷蔡华轮庄英斌宋威
Owner GUANGZHOU KINGFA CARBON FIBER NEW MATERIALS DEV