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High-molecular-weight para-aramid pulp and preparation method thereof

A para-aramid pulp, high molecular weight technology, applied in the direction of single-component polyamide rayon, single-component synthetic polymer rayon, fiber chemical characteristics, etc., can solve the problem of low pulp strength modulus, product Small molecular weight, complex process flow and other problems, to achieve the effect of improving strength and tear performance, dimensional stability, and short process flow

Active Publication Date: 2021-02-19
BLUESTAR CHENGDU NEW MATERIALS
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] The purpose of the present invention is to solve the problem in the prior art that in the production of para-aramid fibrids, the process flow is complicated, the cost is high, or the preparation method is easy to operate and control, and the obtained product has small molecular weight, small fibril aspect ratio, and pulp To solve the problem of low strength modulus, the present invention provides a method for preparing high molecular weight para-aramid pulp, which can effectively solve the above problems

Method used

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  • High-molecular-weight para-aramid pulp and preparation method thereof

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Embodiment 1

[0031] A preparation method of high molecular weight para-aramid fiber pulp, comprising the following steps:

[0032] A. refer to figure 1 The schematic diagram of the process in 2 Add 90 mL of pure N-methylpyrrolidone solvent, stir, dissolve and shake well to obtain a solvent system, then add 3.78 g of p-phenylenediamine and 0.2 g of calcium hydride into the solvent system to fully dissolve to obtain a solution of p-phenylenediamine, and then add p-phenylenediamine. The diamine solution was cooled under normal pressure to -10°C;

[0033] B. Dissolve 7.14 g of terephthaloyl chloride powder in 10 mL of pure N-methylpyrrolidone solvent at 80°C to obtain a terephthaloyl chloride solution,

[0034] C, the terephthaloyl chloride solution is gradually added in the p-phenylenediamine solution to carry out the polycondensation reaction, and stirring, the stirring speed is 1500 r / min;

[0035] D. During the reaction for 2 min, 0.4 g of polyvinylpyrrolidone solubilizer was added, and...

Embodiment 2

[0043] A preparation method of high molecular weight para-aramid fiber pulp, comprising the following steps:

[0044]A. Under nitrogen drying atmosphere, first add 2.0g LiCl into 90mL pure N-ethylpyrrolidone solvent, stir, dissolve and shake to obtain a solvent system, then add 4.11g p-phenylenediamine and 0.35g calcium hydride into the solvent system to fully dissolve , to obtain a p-phenylenediamine solution, and then the p-phenylenediamine solution was cooled under normal pressure to -5°C;

[0045] B. Dissolve 7.79g of terephthaloyl chloride powder in 10mL of amide solvent at 80°C to obtain a terephthaloyl chloride solution,

[0046] C, the terephthaloyl chloride solution is gradually added in the p-phenylenediamine solution to carry out the polycondensation reaction, and stirring, the stirring speed is 2000r / min;

[0047] D. During the reaction for 1min, add 0.6g of alkylphenol polyoxyethylene ether solubilizer, continue the polycondensation reaction, when the mixed solut...

Embodiment 3

[0055] A preparation method of high molecular weight para-aramid fiber pulp, comprising the following steps:

[0056] A. In a nitrogen dry atmosphere, first add 1.2g CaCl 2 and 0.5g LiCl were added into 90mL pure N,N-dimethylacetamide solvent, stirring, dissolving and shaking to obtain a solvent system, and then 3.46g p-phenylenediamine and 0.4g calcium hydride were added into the solvent system to fully dissolve to obtain terephthalic acid. amine solution, and then the p-phenylenediamine solution was cooled under normal pressure to -8°C;

[0057] B. Dissolve 6.63 g of terephthaloyl chloride powder in 10 mL of pure N,N-dimethylacetamide solvent at 80°C to obtain a terephthaloyl chloride solution,

[0058] C, the terephthaloyl chloride solution is gradually added in the p-phenylenediamine solution to carry out the polycondensation reaction, and stirring, the stirring speed is 2500r / min;

[0059] D, during the reaction for 3min, add 0.6g polyvinylpyrrolidone solubilizer, conti...

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Abstract

The invention discloses high-molecular-weight para-aramid pulp and a preparation method thereof, and belongs to the technical field of polymer synthetic fibers. P-phenylenediamine and paraphthaloyl chloride are used as reaction monomers, a low-temperature solution polycondensation method is utilized, paraphthaloyl chloride is gradually added for polycondensation reaction, a solubilizer and an acidabsorbent are used as auxiliary materials for promoting polycondensation reaction, a poly-paraphthaloyl-p-phenylenediamine product with high relative molecular weight is obtained, and further fiber forming is performed through precipitation by using solidification liquid, and the para-aramid pulp fiber with the intrinsic viscosity eta inh of 3.5-6.5 is obtained. The method is simple in technological process, the para-aramid pulp stable in performance and size can be obtained by regulating and controlling technological parameters, the para-aramid pulp can be applied to aramid paper, high-performance reinforced composite materials and asbestos substitutes, and the strength and tearing performance of the aramid paper and the composite materials are remarkably improved.

Description

technical field [0001] The invention belongs to the technical field of polymer synthetic fibers, and relates to a high molecular weight para-aramid fiber pulp and a preparation method thereof. Background technique [0002] Para-aramid fiber, namely polyparaphenylene terephthalamide (PPTA), also known as aramid 1414, aramid Ⅱ, is one of the three major high-performance fibers in the world, with high strength and high modulus, light weight and flame retardant, With the characteristics of high temperature resistance, acid and alkali resistance and good electrical insulation, it is widely used in defense and military industry, aerospace, optical cable communication, personal protection and other fields. [0003] Para-aramid pulp is a differentiated product developed by PPTA in recent years. Its chemical structure is the same as that of PPTA, and it retains the excellent properties of PPTA, such as high tensile strength, heat resistance, abrasion resistance and dimensional stabil...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G69/32C08G69/28D01F6/60
CPCC08G69/32C08G69/28D01F6/605Y02E60/10
Inventor 崔晓静孙潜毛亚丽李林
Owner BLUESTAR CHENGDU NEW MATERIALS