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Method for preparing polyaramide resin modified by aromatic heterocycle and chloromonomer

A technology of polyaramid and manufacturing method, which is applied in the field of special synthetic fiber production, and can solve problems such as difficult molecular weight, difficult recycling, and high price of lithium chloride

Inactive Publication Date: 2008-04-23
四川华通特种工程塑料研究中心有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Lithium chloride is not conducive to cost reduction due to its high price, high toxicity, and difficulty in recycling
In addition, the synthetic process equipment of resin is not involved in the Russian patent, and it is difficult to ensure that the resin solution with high molecular weight and uniform molecular weight distribution is obtained during implementation.

Method used

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  • Method for preparing polyaramide resin modified by aromatic heterocycle and chloromonomer
  • Method for preparing polyaramide resin modified by aromatic heterocycle and chloromonomer

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] Embodiment 1: be 97% NMP and 17.7 parts of content be the CaCl of 35% by 100 parts (weight) content 2 After mixing evenly, heat it to 200°C through a preheater, and then input it into a rectification tower to remove water, and obtain 103.2 parts of CaCl 2 A 6% NMP solution (water content≤150ppm) is used as a solvent. Then 40% moles of 2-5'dichloro-p-phenylenediamine and 60% moles of 2-(4aminophenyl)-5(6)aminophenylbenzimidazole were dissolved in 6% (by weight) CaCl 2 in NMP solvent (the concentration of diamine in NMP is 5%). Then the dissolved diamine solution is cooled to 2-5° C., and 50% mole of terephthaloyl chloride is added under vigorous stirring to form a low-molecular-weight oligomer terminated by an amino group. Then cool the low-molecular-weight oligomer to 2-5 DEG C, and gradually add the remaining 50% by mole of terephthaloyl chloride to obtain a resin solution with a kinetic viscosity of 700 poise.

[0019] After the resin solution is filtered, it is de...

Embodiment 2

[0024] Example 2: CaCl 2 The preparation method of the NMP solution (water content≤150ppm) with a content of 6% is the same as in Example 1.

[0025] 40% mole 2-chloro-p-phenylenediamine and 60% mole 2-(4 aminophenyl)-5(6) aminophenylbenzimidazole are dissolved in 6% (weight) CaCl by the method of embodiment 1 2 in the NMP solvent. Then the dissolved diamine solution is cooled to 2-5° C., and 50% mole of terephthaloyl chloride is added under vigorous stirring to form a low-molecular-weight oligomer terminated by an amino group. Then cool the low-molecular oligomer to 2-5 DEG C, and gradually add the remaining 50% mole terephthaloyl chloride to obtain a resin solution with a kinetic viscosity of 900 poise.

[0026] The properties of the fiber obtained after the resin solution is degassed and spun in a falling film evaporator are as follows:

[0027] Single filament strength 6.0GPa

[0028] The relative elongation at break is 1.9%;

[0029] Elastic modulus 172GPa,

[0030]...

Embodiment 3

[0031] Example 3: CaCl 2 The preparation method of the NMP solution (water content≤150ppm) with a content of 6% is the same as in Example 1.

[0032] 80% mole 2-chloro-p-phenylenediamine and 20% mole 2-(4 aminophenyl)-5(6) aminophenyl benzimidazole are dissolved in 6% (weight) CaCl by the method of embodiment 1 2 in the NMP solvent. Then the dissolved diamine solution is cooled to 2-5° C., and 50% mole of terephthaloyl chloride is added under vigorous stirring to form a low-molecular-weight oligomer terminated by an amino group. Then cool the low-molecular oligomer to 2-5 DEG C, and gradually add the remaining amount of 50% mole terephthaloyl chloride to obtain a resin solution with a dynamic viscosity of 800 poise.

[0033] The properties of the fiber obtained after the resin solution is degassed and spun in a falling film evaporator are as follows:

[0034] Single filament strength 6.0GPa

[0035] The relative elongation at break is 1.6%;

[0036] Elastic modulus 180GPa...

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Abstract

The present invention discloses process of producing aromatic heterocycle and chlorated monomer modified polyaramide resin. Monomers including paraphthaloyl chloride and p-phenylene diamine in the calculated equivalents and 2-(4-aminophenyl)-5(6) aminophenyl benzimidazole in 20-80 % the calculated equivalent are synthesized inside NMP / CaCl2 solvent system into high molecular weight resin through one two-step process including the first reaction between partial paraphthaloyl chloride and all the p-phenylene diamine to form amido group terminated low molecular weight oligomer and the subsequent reaction between the rest paraphthaloyl chloride and the amido group terminated low molecular weight oligomer to form the high molecular weight resin. The aromatic heterocycle and chlorated monomer modified polyaramide resin has the advantages of high fireproof performance, high mechanical strength and low cost.

Description

Technical field [0001] The invention belongs to the field of special synthetic fiber production. Background technique [0002] It is a well-known technology to use terephthaloyl chloride and p-phenylenediamine as raw materials to produce aromatic polyamide resin, and use this resin as a precursor for preparing aramid fibers and films, and a large number of patents have been published. However, this aromatic polyamide resin is in powder form and needs to be further dissolved in concentrated sulfuric acid before it can be used for spinning, film making and fibrids. At the same time, fibers made of this resin cannot meet the needs of some applications in terms of tensile strength, tensile modulus, flame retardancy, and fatigue resistance. Therefore, a large number of modification studies have been carried out on the synthesis of the above-mentioned resins. [0003] Japan's Teijin Corporation has obtained a solution-like resin by introducing the third monomer - 3,4'-diaminodip...

Claims

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Application Information

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IPC IPC(8): C08G69/32D01F6/60C09D177/06C08J5/18
Inventor 潘育英刘文良蔡兴明
Owner 四川华通特种工程塑料研究中心有限公司
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