Method for preparing high-temperature-resistant nylon by utilizing amidation reaction of polyester

A technology of amidation reaction and high temperature resistance, which is applied in the field of nylon preparation, can solve the problems of many residues on the wall of the kettle, high melt viscosity, side reactions, etc., so as to improve heat resistance, physical and mechanical properties, physical and mechanical properties. The effect of stable and lower production cost

Pending Publication Date: 2021-09-24
ZHENGZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

CN103360598 A, CN 107383365 A, CN 109970968 B introduced the use of "one-step" melt polymerization in a polymerization kettle to prepare semi-aromatic nylon, but this preparation method has many disadvantages, such as high polymerization temperature, high energy consumption, and side reactions , the product is easy to form gel, yellow, the melt viscosity is high, it is difficult to discharge, and there are many residues on the wall of the kettle; if things go on like this, black spots will be generated, which seriously affects its appearance quality and performance
CN 104327265 A and CN 101768266 A introduce the use of "one-step" solid-phase polymerization in a polymerization kettle to prepare semi-aromatic nylon, but during the polymerization process, there will be lumpy products due to the melting of part of the raw materials, which will block the discharge pipe, resulting in failure to discharge normally. material, so it cannot be applied to industrial production
CN 105339415 A introduces the preparation of semi-aromatic nylon by "one-step" solid-state polymerization using a closed small cup (the small cup cover has a small opening for balancing the environmental pressure), but when the temperature is raised under normal pressure, the nylon salt will be decomposed into two Amines and dibasic acids, and part of the diamines will be discharged in the form of steam, resulting in an imbalance in the molar ratio of the two, unable to increase the molecular weight of the product
CN 104817693 A introduces the use of drum reactors for salt formation and polymerization to prepare PA11T, but nylon 11T salt is easily soluble in water, that is, the essence of this reaction is solution polymerization, and the product is easy to stick to the wall and cannot be discharged

Method used

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  • Method for preparing high-temperature-resistant nylon by utilizing amidation reaction of polyester
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  • Method for preparing high-temperature-resistant nylon by utilizing amidation reaction of polyester

Examples

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Effect test

Embodiment 1

[0028] A kind of method utilizing the amidation reaction of polyester to prepare high temperature resistant nylon, comprises the following steps:

[0029] 1) Weigh 192g of polyethylene terephthalate (PET), 116g of hexamethylenediamine, 0.92g of sodium hypophosphite and 924g of sulfolane into an autoclave. Wherein, the mol ratio of hexamethylenediamine and PET is 1:1, the amount of sodium hypophosphite is 0.3% of the PET quality, and the mass ratio of the total mass of raw materials to the solvent is 1:3; 2 Replace the gas 3 times, turn on the stirring and heating device, when the temperature rises to 200°C, keep it warm for 1h, release the steam for 2h, vacuumize for 1h, turn off the heating, cool to room temperature, and take out the product;

[0030] 2) Add 924g of acetone to the product for washing and suction filtration, and repeat the operation 3 times; put the product in a vacuum drying oven and dry it at 60°C for 24 hours to finally obtain white powdery high-temperature...

Embodiment 2

[0032] A kind of method utilizing the amidation reaction of polyester to prepare high temperature resistant nylon, comprises the following steps:

[0033] 1) Weigh 256g of polytrimethylene 2,6-naphthalate (PPN), 172g of decanediamine, 1.28g of phosphorous acid and 1284g of trichloroacetic acid into an autoclave. Wherein, the mol ratio of decyl diamine and PEN is 1:1, and the sodium hypophosphite consumption is 0.3% of the PPN quality, and the mass ratio position of raw material total mass and solvent is 1:3; 2 Replace the gas 3 times, turn on the stirring and heating device, when the temperature rises to 200°C, keep the temperature and pressure for 1 hour, release the steam for 2 hours, and vacuum for 1 hour; turn off the heating, cool to room temperature, and take out the product;

[0034] 2) Add 1284g of ethanol to the product for washing and suction filtration, and repeat the operation 3 times; put the product in a vacuum drying oven and dry it at 60°C for 24 hours to final...

Embodiment 3

[0036] A kind of method utilizing the amidation reaction of polyester to prepare high temperature resistant nylon, comprises the following steps:

[0037] 1) Weigh 226g of polybutylene 1,4-cyclohexanedicarboxylate (PBC), 200g of dodecyl diamine, 1.28g of H10 and 1278g of chlorophenol into an autoclave. Wherein, the mol ratio of decyl diamine and PEN is 1:1, and the sodium hypophosphite consumption is 0.3% of the PBC quality; 2 Replace the gas 3 times, turn on the stirring and heating device, when the temperature rises to 200°C, keep the temperature and pressure for 1 hour, release the steam for 2 hours, and vacuum for 1 hour; turn off the heating, cool to room temperature, and take out the product;

[0038]2) Add 1278g of methanol to the product for washing and suction filtration, and repeat the operation 3 times; put the product in a vacuum drying oven and dry it at 60°C for 24 hours to finally obtain white powdery high-temperature-resistant nylon PA12C.

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Abstract

The invention belongs to the field of preparation of nylon, and particularly relates to a method for preparing high-temperature-resistant nylon by utilizing an amidation reaction of polyester. The preparation method comprises the following steps of: adding a macromolecular polyester raw material and diamine into a solvent, heating to a heat preservation temperature, reacting, and washing the obtained product to obtain the high-temperature-resistant nylon. The preparation method is mild in reaction condition and simple in process, the used solvent can be recycled, and the cost is relatively low. Meanwhile, recycled polyester can be used as a reaction raw material in the method, so that the waste polyester plastic can be converted into another high-added-value product while the white pollution is reduced, and the waste is turned into wealth. The obtained product has stable physical and mechanical properties and excellent quality, can be widely applied to the fields of automobile industry, electronic and electrical industry, mechanical industry and the like, and is a new material with good application prospects.

Description

technical field [0001] The invention belongs to the field of nylon preparation, and in particular relates to a method for preparing high-temperature-resistant nylon by using polyester amidation reaction. Background technique [0002] High temperature resistant nylon can be a kind of high temperature resistant nylon prepared by polycondensation of diamine and cyclic dicarboxylic acid. This kind of nylon not only has good heat resistance, mechanical properties, solvent resistance and chemical resistance, good insulation and low moisture absorption rate; it also has good toughness and low melting point, so it has good processing performance and high cost performance. The excellent comprehensive properties of high-temperature-resistant nylon make it widely used in the automotive and electrical and electronic industries. The market demand continues to increase and the application field is gradually expanding. [0003] The commonly used preparation method of high-temperature-resi...

Claims

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Application Information

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IPC IPC(8): C08G69/44
CPCC08G69/44
Inventor 付鹏雪冰峰刘民英赵清香崔喆张晓朦庞新厂
Owner ZHENGZHOU UNIV
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