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Method for continuous production of polyisophthaloyl metaphenylene diamine spinning stock solution

A technology of poly-m-phenylene isophthalamide spinning and isophthaloyl chloride is applied in the directions of single-component polyamide rayon, dry spinning, wet spinning, etc., and can solve the problem of unfavorable fiber product stability. , polymer batch differences, etc.

Inactive Publication Date: 2012-06-27
YANTAI TAYHO ADVANCED MATERIALS CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the patent US3063966 and other related patents are not related to the use of batch polymerization or continuous polymerization
[0009] Major domestic manufacturers of meta-aramid fibers mostly use intermittent low-temperature solution polymerization, resulting in large differences between polymer batches, which is not conducive to the stability of fiber products. In the patent CN1443882, a two-step polymerization method is used, which mentions One-step semi-continuous solution polymerization process

Method used

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  • Method for continuous production of polyisophthaloyl metaphenylene diamine spinning stock solution

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] First, dissolve m-phenylenediamine in the polar solvent NMP with a concentration of 1.0mol / L. After cooling down, it enters the main polymerization reactor, and then adds a certain amount of isophthaloyl chloride, which is 60% of the total amount. %, the temperature is 0°C; after a certain period of reaction, add a total of 30% of isophthaloyl chloride in the second section of the reactor; the remaining 10% of isophthaloyl chloride is added in the third section of the reactor, and the reaction is completed The final polymer solution enters the next process. By controlling the reaction time and the ratio of the two reactants, polymers with different molecular weights can be obtained. The closer the reaction ratio is to 1, the larger the molecular weight of the polymer.

[0023] After the polymerization is completed, the hydrogen chloride produced by the polymerization is neutralized with metal hydroxide, and the produced metal chloride is dissolved in the polymer solutio...

Embodiment 2

[0026] First, dissolve m-phenylenediamine in the polar solvent DMAC with a concentration of 0.9mol / L. After cooling down, it enters the main polymerization reactor, and then adds a certain amount of isophthaloyl chloride, which is 70% of the total amount. %, the temperature is -5°C; after reacting for a certain period of time, add a total amount of 25% isophthaloyl chloride in the second section of the reactor; the remaining 5% of isophthaloyl chloride is added in the third section of the reactor, and the reaction After completion, the polymer solution enters the next process.

[0027] After the polymerization is completed, the hydrogen chloride produced by the polymerization is neutralized with metal hydroxide, and the produced metal chloride is dissolved in the polymer solution without filtering out, and contributes to the stability of the polymer solution. The polymer content in the polymer solution was 15.8%.

[0028] The polymer solution is directly used for spinning aft...

Embodiment 3

[0030] First, dissolve m-phenylenediamine in the polar solvent DMAC with a concentration of 1.2mol / L. After cooling down, it enters the main polymerization reactor, and then adds a certain amount of isophthaloyl chloride, which is 80% of the total amount. %, the temperature is 0°C; after a certain period of reaction, add a total of 18% of isophthaloyl chloride in the second section of the reactor; the remaining 2% of isophthaloyl chloride is added in the third section of the reactor, and the reaction is completed The final polymer solution enters the next process.

[0031] After the polymerization is completed, the hydrogen chloride produced by the polymerization is neutralized with metal hydroxide, and the produced metal chloride is dissolved in the polymer solution without filtering out, and contributes to the stability of the polymer solution. The polymer content in the polymer solution was 19.2%.

[0032] The polymer solution is directly used for spinning after filtering,...

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Abstract

The invention relates to a method for continuous production of polyisophthaloyl metaphenylene diamine spinning stock solution, which mainly comprises the steps of polymerization, neutralization, filtration and other steps. The polymerization process adopts one-step polymerization and batch feed, firstly, metaphenylene diamine is dissolved in a polar solvent, cooled down, introduced into a polymerization main reactor, and then isophthaloyl dichloride is fed in a batch mannerl; after polymerization is completed, a metal hydroxide neutralizes hydrogen chloride generated during polymerization, and the generated metal chloride dissolves in a polymer solution so as to dispense with filtration and be helpful for the stability of the polymer solution; the polymer solution is directly used for spinning after filtration, debubbling and other steps. The method provided by the invention adopts a continuous low-temperature solution polymerization, and the polymerization process has the advantages of simplicity in process, stability in polymerization condition, high quality of polymer and the like, improves the uniformity of polymer, and is helpful for producing high-quality fiber products.

Description

technical field [0001] The invention relates to a method for preparing fiber spinning stock solution, in particular to a method for preparing polym-phenylene isophthalamide spinning solution by solution polymerization. Background technique [0002] Polym-phenylene isophthalamide fiber has excellent high temperature resistance and flame retardancy, as well as excellent electrical insulation, radiation resistance and chemical corrosion resistance. It is used in the manufacture of fireproof materials and high temperature insulation materials. Important basic materials for the development of high-tech industries such as aerospace, energy industry, and environmental protection. [0003] Existing methods for preparing polym-phenylene isophthalamide usually include: [0004] 1. Interface aggregation [0005] m-Phenylenediamine reacts with isophthaloyl dichloride in a poor solvent of polym-phenylene isophthalamide, and then mixes it with an aqueous solution containing an acid abso...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): D01F6/90D01F1/10C08G69/32D01D1/02D01D1/10D01D5/04D01D5/06
Inventor 宋翠艳吕继平宋金苓
Owner YANTAI TAYHO ADVANCED MATERIALS CO LTD
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