Synthetic method for poly terephthalyl terephaldiamine polymer

A technology of poly(p-phenylene terephthalamide) and its synthesis method, which is applied in the field of synthesis of poly(p-phenylene terephthalamide) polymers, and can solve the problem of large amount of solvent recovery, large resin ash content, and complex production equipment and other problems, to achieve the effects of reducing investment cost and production cost, smooth polymerization reaction, and narrow molecular weight distribution

Inactive Publication Date: 2007-10-31
邢哲
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

This method requires a large investment cost for production equipment, a large amount of solvent recovery, and high requirements for the control accuracy of the production process. It is difficult to achieve precise control of reaction conditions, resulting in high production and operation costs, production equipment and control system investment.
[0004] Low-temperature solution polycondensation is to polymerize p-phenylenediamine and terephthaloyl chloride in strong polar solvents such as dimethylacetamide and N-methylpyrrolidone under low temperature conditions. In USP3,884,881, hexamethylphosphorus The amide is used as a solvent, and the jet mixer is used for mixing materials, and the twin-screw reactor is used for continuous polycondensation of low-temperature solution. The solvent hexamethylphosphoramide in this method has carcinogenic effect, and the jet mixer is easy to block, which affects the continuity of production; Zhao 53-133,296 uses N-methylpyrrolidone as a solvent and calcium chloride as a co-solvent, and p-phenylenediamine, calcium chloride and N-methylpyrrolidone are prepared into solutions and slurries respectively, and are mixed with molten terephthalamide After the acid chloride is mixed inside the S-1 mixer, it enters into the twin-screw kneader for polycondensation. The amount of calcium chloride used in this method is as high as 40%, and the resulting resin has a large ash content, and the S-1 mixer is easy to block; in the domestic open patent 90105870.x, Self-cleaning twin-shaft mixer and twin-screw reactor ar

Method used

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  • Synthetic method for poly terephthalyl terephaldiamine polymer
  • Synthetic method for poly terephthalyl terephaldiamine polymer

Examples

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Example Embodiment

[0021] Example 1:

[0022] Dissolve 0.20 kg of p-phenylenediamine and 0.23 kg of lithium chloride in 5.30 kg of dimethylacetamide with a water content below 100ppm, and prepare the weight of p-phenylenediamine in a reactor with a double-helix belt stirrer. The percentage concentration is 3.5%, and the lithium chloride weight percentage concentration is a solution of 4%. Cool the solution to -10°C, add 0.1 kg of terephthaloyl chloride to the reactor for the first time, and after 15 minutes of reaction, pass 0.016 kg of pure ammonia into the reactor to neutralize the hydrogen chloride produced by the reaction to obtain polycondensation intermediate The pH of the product solution is 6. For the second time, 0.1 kg of terephthaloyl chloride is added to the reactor. After 20 minutes of reaction, 0.016 kg of pure ammonia is passed into the reactor to neutralize the hydrogen chloride produced by the reaction, and the polycondensation intermediate product solution pH is obtained. 0.1 ...

Example Embodiment

[0027] Example 2:

[0028] Dissolve 0.30 kg of p-phenylenediamine and 0.30 kg of lithium chloride in 5.00 kg of N-methylpyrrolidone with a water content below 100ppm, and prepare the weight of p-phenylenediamine in a reactor with a double-helix belt stirrer. The percentage concentration is 6%, and the lithium chloride weight percentage concentration is a solution of 6%. Cool the solution to -10°C, add 0.2 kg of terephthaloyl chloride to the reactor for the first time, and after 15 minutes of reaction, pass 0.031 kg of pure ammonia into the reactor to neutralize the hydrogen chloride produced by the reaction to obtain polycondensation intermediate The pH of the product solution is 5. For the second time, 0.1 kg of terephthaloyl chloride is added to the reactor, and after 20 minutes of reaction, 0.017 kg of pure ammonia is passed into the reactor to neutralize the hydrogen chloride produced by the reaction to obtain the polycondensation intermediate product solution pH 0.1 kg o...

Example Embodiment

[0029] Example 3:

[0030]Dissolve 0.25 kg of p-phenylenediamine with a purity of more than 99.9% and 0.35 kg of calcium chloride with a purity of more than 99.9% in 5.00 kg of dimethylacetamide with a water content of less than 100ppm in a double-helix belt stirrer In the reactor, it is prepared as a solution containing 5% by weight of p-phenylenediamine and 7% by weight of calcium chloride. Cool the solution to -10°C, add 0.18 kg of terephthaloyl chloride to the reactor for the first time, and after 20 minutes of reaction, pass 0.029 kg of pure ammonia into the reactor to neutralize the hydrogen chloride produced by the reaction to obtain polycondensation intermediate The pH of the product solution is 6. For the second time, 0.15 kg of terephthaloyl chloride is added to the reactor, and after 25 minutes of reaction, 0.025 kg of pure ammonia is passed into the reactor to neutralize the hydrogen chloride produced by the reaction to obtain the polycondensation intermediate prod...

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Abstract

The present invention relates to the synthesis of polyterephthalyl phenyldiamine and belongs to the field of polymer material. The present invention synthesizes polyterephthalyl phenyldiamine polymer with p-phenyldiamine and paraththaolyl choride and through several reaction steps, and during the reaction, alkali matter is added continuously to produce hydrogen chloride to make the reaction mild and controllable to obtain high molecular weight polymer with narrow molecular weight distribution and high product homogeneity. The produced polymer may be used in many application fields.

Description

technical field [0001] The invention relates to a synthesis method of poly(p-phenylene terephthalamide) polymer, which belongs to the field of polymer materials. Background technique [0002] At present, the synthesis of poly-p-phenylene terephthalamide polymer mainly includes two processes: interfacial polycondensation and low-temperature solution polycondensation. [0003] Interfacial polycondensation is to dissolve p-phenylenediamine and terephthaloyl chloride in two immiscible solvents to prepare a solution of a certain concentration, and then quantitatively mix the two solutions under high-speed stirring, and then The interface is polymerized, and then the by-product hydrogen chloride is neutralized with an alkaline substance, and then the obtained poly-p-phenylene terephthalamide polymer is separated. This method requires a large investment in production equipment, a large amount of solvent recovery, and high requirements for the control accuracy of the production pro...

Claims

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Application Information

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IPC IPC(8): C08G69/32
Inventor 邢哲李吉东郭润栋
Owner 邢哲
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