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Preparation method for long carbon chain nylon PA1313 and product

A long carbon chain, nylon technology, applied in the field of polymer material synthesis, can solve problems such as low solubility and inability to form salt, and achieve the effects of low recovery cost, reduced equipment investment, and low requirements for equipment safety grades

Active Publication Date: 2019-01-11
ZHENGZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] At present, ethanol is mostly used as the salt-forming solvent and polymerization medium in the synthesis of long carbon chain nylon, because the solubility of long carbon chain dibasic acids and diamines in ethanol is high, but the solubility in water is extremely low, and cannot be realized in water. Salt formation by crystallization

Method used

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  • Preparation method for long carbon chain nylon PA1313 and product
  • Preparation method for long carbon chain nylon PA1313 and product

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] A preparation method of long carbon chain nylon PA1313, comprising the following steps:

[0034] (1) Preparation of PA1313 nylon salt: Add 1,13-tridecanediamine to water with 5 times the mass number, heat to 80°C, and then follow the steps of 1,13-tridecanedibasic acid and 1,13- The molar ratio of thirteen carbon diamine is 1:1.1, add the metered 1,13-tridecanyl diamine, heat to 130°C in an inert gas atmosphere (nitrogen), keep the pressure in the kettle at 0.5MPa, measure the pH of the system According to the measured pH value, add an appropriate amount of 1,13-tridecanedibasic acid or 1,13-tridecanediamine, adjust the pH value of the system at 7.2, and continue the reaction for 25 minutes to obtain PA1313 salt. After centrifugation and dehydration, the PA1313 salt with a water content of 20 wt% was obtained;

[0035] (2) Polymerization of PA1313: Add PA1313 salt with a water content of 20wt% into the polymerization kettle, replace the gas in the kettle with nitrogen ...

Embodiment 2

[0043] A preparation method of long carbon chain nylon PA1313, comprising the following steps:

[0044] (1) Preparation of PA1313 nylon salt: Add 1,13-tridecanediamine to water with 3 times the mass number, heat to 60°C, and then follow the steps of 1,13-tridecanedibasic acid and 1,13- The molar ratio of tridecanyl diamine is 1:1.2. Add the metered 1,13-tridecyl diamine, heat to 120°C in an inert gas atmosphere, keep the pressure in the kettle at 0.4MPa, measure the pH value of the system, according to Add an appropriate amount of 1,13-tridecanedibasic acid or 1,13-tridecanediamine to the measured pH value, adjust the pH value of the system to 7.4, and continue the reaction for 30 minutes to obtain PA1313 salt. After centrifugation and dehydration Obtaining water content is the PA1313 salt of 15wt%;

[0045] (2) Polymerization of PA1313: Add PA1313 salt with a water content of 15wt% into the polymerization kettle, replace the gas in the kettle with inert gas nitrogen to ensur...

Embodiment 3

[0053] A preparation method of long carbon chain nylon PA1313, comprising the following steps:

[0054] 1) Preparation of PA1313 nylon salt: add 1,13-tridecanediamine to water with 8 times the mass number, heat to 80°C, and then follow the steps of 1,13-tridecanedioic acid and 1,13-deca The molar ratio of three-carbon diamine is 1:1.05. Add metered 1,13-tridecyl diamine, heat to 180°C in an inert gas atmosphere, keep the pressure in the kettle at 1.2MPa, and measure the pH value of the system. Add an appropriate amount of 1,13-tridecanedibasic acid or 1,13-tridecanediamine to adjust the pH of the system to 7.1, and continue the reaction for 20 minutes to obtain PA1313 salt, which is obtained after centrifugation and dehydration PA1313 salt with a water content of 30% by weight;

[0055](2) Polymerization of PA1313: Add PA1313 salt with a water content of 30wt% into the polymerization kettle, and replace the gas in the kettle with nitrogen gas to ensure that the reaction kettl...

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Abstract

The invention discloses a preparation method for long carbon chain nylon PA1313. The preparation method comprises the following steps: taking 1,13-tridecanedioic acid as a raw material; preparing 1,13-tridecylamine through cyanation and amination; preparing PA1313 salt by taking 1,13-tridecylamine and 1,13-tridecanedioic acid as raw materials and water as a solvent; putting PA1313 salt and water at a certain ratio into a polymerizing kettle; performing melt polymerization, thereby acquiring PA1313 with a certain molecular weight. In the cyanation step of the method, an ammonia gas recycling technique is adopted, so that the use ratio of ammonia gas is greatly increased and the emission of wastewater and exhaust gas is reduced; in the salt forming and polymerizing process, water is used forreplacing ethyl alcohol as a reaction medium, so that the safety of industrial production is promoted, the safety level of equipment is reduced, the investment in equipment is reduced and the recycling cost of solvent is lowered.

Description

technical field [0001] The invention belongs to the technical field of polymer material synthesis, and in particular relates to a preparation method and product of long carbon chain nylon PA1313. Background technique [0002] Since the industrialized production of nylon 66 by DuPont Company in the United States in 1939, the current industrially produced nylon varieties in the world mainly include nylon 66, nylon 6, nylon 46, nylon 610, nylon 1010, nylon 612, nylon 11, nylon 12, etc. Among them, nylon 11 and nylon 12 are long carbon chain nylon varieties, which have the advantages of low water absorption, good solvent resistance and low temperature resistance, wear resistance and impact resistance, and excellent dimensional stability. Melt glue, 3D printing and other fields are irreplaceable nylon varieties. However, the synthesis technology of nylon 11 and nylon 12 has long been monopolized by large foreign companies such as French Akema, American DuPont, and Japanese Ube I...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G69/26C08G69/28C07C209/48C07C211/09C07C253/22C07C255/04
CPCC07C209/48C07C253/22C08G69/26C08G69/28C07C255/04C07C211/09
Inventor 赵清香刘民英付鹏崔喆
Owner ZHENGZHOU UNIV
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