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Method for preparing aromatic polyamide

A polyarylamide and copolymer technology, which is applied in the field of polyarylamide preparation, can solve the problems of large fluctuations in performance indicators, influence on enlarged production, and performance degradation, and achieve stable quality indicators, good repeatability of parts performance, and thermal stability. The effect of excellent stability

Active Publication Date: 2015-04-22
SHANGHAI PLASTICS RES INST CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] Prior art (CN100432120C, November 12, 2008) adopts emulsion polymerization method to prepare, and application sodium dodecyl sulfonate, sodium methylene dinaphthalene sulfonate and sodium dibutyl naphthalene sulfonate are used as emulsifiers, with its It is very difficult to completely separate the emulsifier during the post-treatment process of the prepared polyaramid copolymer
The presence of a small amount of emulsifier in the copolymer will reduce its performance. The performance of polyaramid copolymer molded parts produced in different batches is not stable, and the performance index fluctuates greatly. Users often report product quality problems
In addition, adding a large amount of salt-forming agent sodium carbonate aqueous solution affects the problem of enlarged production

Method used

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  • Method for preparing aromatic polyamide
  • Method for preparing aromatic polyamide

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Experimental program
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Embodiment 1

[0017] Add 1500g N,N'-dimethylformamide and 108g (1.0mol) m-phenylenediamine to a 3L reactor equipped with a stirrer, a thermometer, a cooler, and an inert gas protection device, and wait until it is completely dissolved at room temperature , Add a homogeneous powder mixture of isophthaloyl dichloride and terephthaloyl dichloride in 10 batches. Among them, 101.5 g (0.5 mol) of isophthaloyl dichloride and 101.5 g (0.5 mol) of terephthaloyl dichloride. The time interval between each batch of addition is 10 minutes, and the reaction is 4 hours after the addition is completed. After the polymerization reaction is completed, add 3000ml of deionized water, stir and precipitate the copolymer, filter, wash with water, dry, crush, and sieve to obtain 216g of polyaramide Copolymer powder. Dissolve 2.16g of combined antioxidant in 300g of dimethyl carbonate, mix evenly with polyaramid copolymer powder, bake at 90°C for 4h after natural ventilation for 12h, and sieve. The composition of...

Embodiment 2

[0020] Add 1500g N,N'-dimethylformamide and 108g (1.0mol) m-phenylenediamine to a 3L reactor equipped with a stirrer, a thermometer, a cooler, and an inert gas protection device, and wait until it is completely dissolved at room temperature , Add a homogeneous powder mixture of isophthaloyl dichloride and terephthaloyl dichloride in 10 batches. Among them, 142g (0.7mol) of isophthaloyl chloride and 61g (0.3mol) of terephthaloyl chloride. The time interval between each batch of addition is 10 minutes, and the reaction is carried out for 4 hours after the addition is completed. tert-butyl-4-hydroxybenzyl) combined antioxidant composed of isocyanuric acid, after stirring evenly, precipitate polyaramid copolymer in 3000ml deionized water; filter, wash with water, dry, pulverize, sieve to obtain 219g Polyarylamide copolymer powder, measured polyarylamide copolymer, its specific viscosity is 1.2, the performance of molded sample is: unnotched impact strength 150kJ / m 2 , other perf...

Embodiment 3

[0022] In addition to adding a combined antioxidant composition of 0.86g triphenyl phosphite and 1.30g 1,3,5-tris(3,5-di-tert-butyl-4-hydroxybenzyl) isocyanuric acid, other formulas and steps Same as Example 1. The obtained polyaramid copolymer has a specific viscosity of 1.1, and the performance of the molded sample is: unnotched impact strength of 125kJ / m 2 , other performance indexes are all with embodiment 1.

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Abstract

The invention relates to a method for preparing aromatic polyamide. The method comprises the following steps: carrying out a solution polymerization reaction on m-phenylenediamine, paraphthaloyl chloride and isophthaloyl dichloride in an aprotic polar solvent at 0-10 DEG C for 5-8 hours, wherein the usage of the aprotic polar solvent is 10-12 times of the mass of m-phenylenediamine, and the molar ratio of paraphthaloyl chloride to isophthaloyl dichloride is (70-50):(30-50); adding a combined antioxidant into the reaction liquid, uniformly stirring the reaction liquid, and adding into stirring water to precipitate a copolymer; and filtering, washing and drying the copolymer to obtain an aromatic polyamide copolymer which has a specific viscosity of 0.8-1.6, wherein the addition amount of the antioxidant is 0.5-1.0 percent of the weight of copolyamide. The product processing sample performance indexes include more than or equal to 35kJ / m<2> of unnotched impact strength, 0.5-0.6 percent of molding shrinkage, more than or equal to 1.8*10<16> omega.cm of volume resistivity and more than or equal to 19kV / mm of dielectric strength.

Description

technical field [0001] The invention relates to a preparation method of polyarylamide, more specifically to a method for preparing polyarylamide copolymer by reacting m-phenylenediamine with isophthaloyl chloride and terephthaloyl chloride. technical background [0002] Poly(m-phenylene isophthalamide terephthalamide) copolymer is a copolymer with high strength, high modulus, dimensional stability and high temperature resistance. It has been adopted by high-tech enterprises and widely used in civilian and military industries. It is also a leader in alternating cold and heat aging, and has become an indispensable new material. [0003] The prior art (CN100432120C, November 12, 2008) was prepared by emulsion polymerization, using sodium dodecyl sulfonate, sodium methylene dinaphthalene sulfonate and sodium dibutyl naphthalene sulfonate as emulsifiers, with its It is very difficult to completely separate the emulsifier during the post-treatment process of the prepared polyara...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G69/32C08G69/28
Inventor 张梦宇胡存雷邱孜学
Owner SHANGHAI PLASTICS RES INST CO LTD
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