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Method for synthesizing high-viscosity polyphenylene terephthalamide

A technology of poly-p-phenylene terephthalamide and terephthaloyl chloride, which is applied in the field of polymer synthesis, can solve the problems of high cost and difficult solvent recovery and treatment, and achieve the effect of eliminating influence and facilitating stability

Active Publication Date: 2011-08-17
TSINGHUA UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] The purpose of the present invention is to propose a synthetic method of high-viscosity poly-p-phenylene terephthalamide, which overcomes the disadvantages of difficult solvent recovery and high cost caused by the use of pyridine and amine acid absorbents in the PPTA polymerization process. Considering the Factors Affecting the Polymerization of PPTA, Provide a Synthetic Method Using a New Acid Absorbent

Method used

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preparation example Construction

[0013] The synthetic method of the high-viscosity poly-p-phenylene terephthalamide that the present invention proposes comprises the following steps:

[0014] The synthetic method of the high-viscosity poly-p-phenylene terephthalamide that the present invention proposes comprises the following steps:

[0015] (1) Add the solvent N-methylpyrrolidone into the dissolution kettle, and add the solubilizing salt under nitrogen protection and stirring, and heat at 70-110°C to dissolve the solubilizing salt, and the solubilizing salt is calcium chloride Or lithium chloride, or the mixture of calcium chloride and lithium chloride mixed in any proportion, the weight percentage of solvent and solubilizing salt is: solvent: solubilizing salt=1: 0.04~0.12;

[0016] (2) Cool the solvent system obtained in (1) to 0-25°C, add p-phenylenediamine under stirring to dissolve, and the molar concentration of p-phenylenediamine in the solvent system is 0.3-0.7mol / L;

[0017] (3) Add terephthaloyl c...

Embodiment 1

[0022] (1) Add 100ml of solvent N-methylpyrrolidone into the dissolution kettle, and add 10 g of calcium chloride as a solubilizing salt under nitrogen protection and stirring, and heat at 100° C. to dissolve the solubilizing salt. Percentage by weight is: solvent: solubilizing salt=1: 0.097;

[0023] (2) Cool the solvent system obtained in (1) to 15° C., add 4.326 g of p-phenylenediamine under stirring to dissolve, and the molar concentration of p-phenylenediamine in the solvent system is 0.4 mol / L;

[0024] (3) add terephthaloyl chloride in above-mentioned system and carry out polymerization, the addition molar ratio of terephthaloyl chloride is: p-phenylenediamine: terephthaloyl chloride=1: 1.007; Then the above-mentioned step (2) Add the system into the tank reactor, and cool it to 0°C, add 4.089g of terephthaloyl chloride powder accounting for 50% of the total amount under stirring conditions, react for 10 minutes, and then add the remaining 50% of the total amount of ter...

Embodiment 2

[0027] (1) Add 100ml of solvent N-methylpyrrolidone in the dissolution kettle, and add 8g of calcium chloride as a solubilizing salt under nitrogen protection and stirring, and heat at 100°C to dissolve the solubilizing salt, and the solvent and the solubilizing salt Percentage by weight is: solvent: solubilizing salt=1: 0.078;

[0028] (2) Cool the solvent system obtained in (1) to 5° C., add 5.407 g of p-phenylenediamine to dissolve under stirring, and the molar concentration of p-phenylenediamine in the solvent system is 0.5 mol / L;

[0029](3) Add terephthaloyl chloride to the above-mentioned system to polymerize, and the adding molar ratio of terephthaloyl chloride is: p-phenylenediamine: terephthaloyl chloride=1: 1.006; the system of above-mentioned steps (2) Add to the tank reactor, and add 0.526g of calcium hydride powder to it, then cool the system temperature to 0°C; then add 5.106g of terephthaloyl chloride powder accounting for 50% of the total amount under stirring...

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Abstract

The invention relates to a method for synthesizing high-viscosity polyphenylene terephthalamide, and belongs to the technical field of polymer synthesis. The method comprises the following steps of: adding dissolution-helping salt into N-methyl pyrrolidone first, adding p-phenylenediamine for dissolution, adding paraphthaloyl chloride for polymerization, and washing and drying an obtained reaction product to obtain the polyphenylene terephthalamide. An acid absorbent used by the synthesis method is calcium hydride, the calcium hydride can react with hydrogen chloride produced in a polymerization reaction, and generated calcium chloride is a cosolvent in a solvent system and is favorable for the stability of a reaction system; and the calcium hydride can remove trace water in the reaction system, so that the influence of water on polyphenylene terephthalamide (PPTA) polymerization is eliminated. Moreover, the unreacted calcium hydride can be easily removed in the subsequent washing step after the PPTA polymerization is finished.

Description

technical field [0001] The invention relates to a synthesis method of high-viscosity poly-p-phenylene terephthalamide, in particular to a method for synthesizing poly-p-phenylene terephthalamide with calcium hydride as an acid absorbent, which belongs to polymer synthesis technology field. Background technique [0002] Polyparaphenylene terephthalamide (hereinafter referred to as PPTA) fiber has many excellent properties, such as high strength, high modulus, high temperature resistance and solvent resistance, etc. PPTA fiber is made by dissolving PPTA polymer in concentrated sulfuric acid to form a liquid crystal solution, and then through dry spray wet spinning. The performance of the PPTA polymer has a direct impact on the final performance of the PPTA fiber. To obtain high-performance fibers, the PPTA polymer must first have a high molecular weight. It is generally believed that the logarithmic viscosity must be above 5.5dl / g. [0003] There are many ways to synthesize ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G69/32
Inventor 庹新林孙力力王晓工
Owner TSINGHUA UNIV
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