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Method for preparing polyaramide resin modified by aromatic heterocycle and chloromonomer

The technology of a polyaramide and a manufacturing method is applied in the field of special synthetic fiber production, and can solve the problems of difficult molecular weight, difficult recovery, and high price of lithium chloride

Inactive Publication Date: 2009-10-21
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] Example 1: 100 parts by weight of NMP with a content of 97% and 17.7 parts of CaCl with a content of 35% 2 After mixing evenly, it was heated to 200 ℃ by a preheater, and then input into a rectifying tower to remove water, and 103.2 parts of CaCl were obtained. 2 The NMP solution with a content of 6% (water content≤150ppm) was 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 (5% concentration of diamine in NMP). Then, the dissolved diamine solution was cooled to 2-5° C., and 50% molar terephthaloyl chloride was added under vigorous stirring to form an amine-terminated low-molecular oligomer. Then, the low-molecular oligomer was cooled to 2-5° C., and the remaining 50% mole of terephthaloyl chloride was gradually added to obtain a resin solution with a dynamic viscosity of 700 poise.

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

Embodiment 2

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

[0025] 40% moles of 2-chloro-p-phenylenediamine and 60% moles of 2-(4aminophenyl)-5(6)aminophenylbenzimidazole were dissolved in 6% by weight CaCl as in Example 1 2 in NMP solvent. Then, the dissolved diamine solution is cooled to 2-5° C., and 50% mol of terephthaloyl chloride is added under vigorous stirring to form a low molecular oligomer capped with an amine group. Then, the low molecular weight oligomer was cooled to 2-5° C., and the remaining 50% mole of terephthaloyl chloride was gradually added to obtain a resin solution with a dynamic viscosity of 900 poise.

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

[0027] Monofilament strength 6.0GPa

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

[0029] Elastic modulus 172GPa,

[...

Embodiment 3

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

[0032] 80% moles of 2-chloro-p-phenylenediamine and 20% moles of 2-(4aminophenyl)-5(6)aminophenylbenzimidazole were dissolved in 6% by weight CaCl as in Example 1 2 in NMP solvent. Then, the dissolved diamine solution is cooled to 2-5° C., and 50% mol of terephthaloyl chloride is added under vigorous stirring to form a low molecular oligomer capped with an amine group. Then, the low molecular weight oligomer was cooled to 2-5° C., and the remaining 50% mole of terephthaloyl chloride was gradually added to obtain a resin solution with a dynamic viscosity of 800 poise.

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

[0034] Monofilament strength 6.0GPa

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

[0036] Elastic modulus 180GPa,

[...

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Abstract

The invention discloses a preparation method of a polyaramide resin modified with aromatic heterocycles and chlorinated monomers. 6) aminophenyl benzimidazole is a monomer, wherein terephthaloyl chloride and p-phenylenediamine are input material by calculated equivalent, 2-(4-aminophenyl)-5(6) aminophenyl benzimidazole is by Calculate the equivalent 20-80% of the input materials, and use a two-step process to synthesize the resin solution in the NMP / CaCl solvent system. The two-step method refers to first letting part of terephthaloyl chloride and all p-phenylenediamine in the solvent system. react to form a low molecular weight oligomer terminated with an amine group; then the remaining terephthaloyl chloride is further reacted with the low molecular weight oligomer terminated with an amine group, and finally a high molecular weight resin is obtained. The product produced by the method has the advantages of good flame retardancy, high mechanical strength and relatively 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 precipitating fibers. At the same time, the fibers made of this resin cannot meet the needs of certain applications in terms of tensile strength, tensile modulus, flame retardancy, and fatigue resistance. Therefore, a lot of modification studies have been carried out on the synthesis of the above-mentioned resins. [0003] Teijin Corporation of Japan obtained a solution-like resin by introducing the third monomer-3,4'-diam...

Claims

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Application Information

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Patent Type & Authority Patents(China)
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