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Method for preparing semi aromatic copolymer nylon

A technology of aromatic copolymerized nylon and semi-aromatic, which is applied in the field of preparation of semi-aromatic copolymerized nylon, which can solve the problems of difficult curing and achieve the effects of not easy to oxidize, low equipment requirements, and mild polymerization process conditions

Active Publication Date: 2014-07-16
ZHUZHOU TIMES NEW MATERIALS TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] In order to solve the above-mentioned technical problems, the present invention provides a preparation method of semi-aromatic nylon copolymer. By controlling factors such as temperature, deflation time, and initial water content, the prepolymer can be discharged in a fluid state, which is convenient for discharging, not easy to solidify and There is no material residue in the kettle, white particles after crushing, no yellowing and blackening phenomenon

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0037] Step 1: Mix terephthalic acid and an appropriate amount of deionized water evenly, heat to 70 oC, start stirring, add hexamethylenediamine aqueous solution, adjust the pH to 7.5-7.7, continue stirring for 1 hour, cool to room temperature, filter and dry to obtain White powder PA6T salt.

[0038] Step 2: 1350 grams of PA6T salt, 1650 grams of PA66 salt, 6 grams of catalyst sodium hypophosphite and 1615 grams of deionized water

[0039] Add it into a 10 L high-temperature and high-pressure reactor, replace the air in the reactor with high-purity nitrogen three times successively, and keep the nitrogen pressure at 0.15 MPa, start stirring, and raise the temperature to 170 oC within 1 hour. The pressure was 0.7 MPa, and the pressure was maintained for 1 hour, then the gas was released slowly, the solution was concentrated to 80%, and the gas release valve was closed.

[0040] Step 3: Continue to raise the temperature to 225 oC, the pressure of the reactor reaches 2.1 MPa, ...

Embodiment 2

[0043] Step 1: Prepare PA6T salt according to step 1 of Example 1, mix isophthalic acid and an appropriate amount of deionized water evenly, heat to 70 oC, start stirring, add hexamethylenediamine aqueous solution, adjust pH to 7.5-7.7, continue to stir 1 hour, cooled to room temperature, filtered and dried to give PA6I salt as a white powder.

[0044] Step 2: 1650 grams of PA6T salt, 1350 grams of PA6I salt, 6 grams of catalyst sodium hypophosphite and 1615 grams of deionized water were added to a 10 L high-temperature and high-pressure reaction kettle, and the air in the kettle was replaced with high-purity nitrogen. Retain the nitrogen pressure of 0.15 MPa, start stirring, and within 1 hour, raise the temperature to 170 oC, at this time the pressure of the reactor is 0.7 MPa, maintain this pressure for 1 hour, then slowly vent, concentrate the solution to 80%, close the vent valve.

[0045] Step 3: According to Step 3 of Example 1, white particles were obtained.

[0046] ...

Embodiment 3

[0048] Step 2: 2142 grams of PA6T salt, 858 grams of caprolactam, 6 grams of catalyst sodium hypophosphite and 750 grams of deionized water obtained in the first step of Example 1 were added to a 10 L high-temperature and high-pressure reaction kettle, and replaced with high-purity nitrogen in the kettle. Air, successively three times, and keep the nitrogen pressure at 0.15 MPa, and start stirring.

[0049] Step 3: Within 2 hours, increase the temperature to 225 oC, the pressure of the reactor reaches 2.1 MPa, keep under this condition for 4 hours, and then release the pressure to normal pressure within 0.75 hours, open the bottom valve of the reactor, and the prepolymer is The liquid was discharged into a nitrogen protection tank, cooled and broken into white particles with a particle size of not more than 2 mm, and vacuum-dried at 100 oC for 10 hours to obtain a prepolymer with an intrinsic viscosity [η] of 0.18 dl / g, and the reaction was started. There is no residual materi...

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Abstract

The invention relates to a method for preparing semi aromatic copolymer nylon, belonging to the technical field of preparation materials for high temperature resistant nylon with high strength and high stability. According to the method, nylon salt is firstly synthesized, then semi aromatic copolymer nylon prepolymer is mainly synthesized at lower temperature and lower pressure, the semi aromatic copolymer nylon prepolymer is prevented from yellowing due to oxidization at high temperature in discharging so as to affect the quality, due to the requirement of lower pressure, the requirement on preparation equipment is lowered, and the production cost is greatly lowered.

Description

technical field [0001] The invention discloses a method for preparing semi-aromatic copolymerized nylon, which belongs to the field of preparing nylon with high temperature resistance, high strength and high stability. Background technique [0002] Semi-aromatic nylon has excellent high temperature stability, outstanding toughness, excellent fluidity and high crystallinity, so semi-aromatic nylon is increasingly used in microelectronic components. The peripheral parts of the engine require the plastics used to have high temperature resistance, high strength, dimensional stability, and chemical resistance. Semi-aromatic nylon can meet the requirements and is an ideal material. [0003] Semi-aromatic nylon is a difficult production process due to its high melting point. At present, the synthesis of semi-aromatic copolymerized nylon adopts a two-step method: pre-polymerization and tackifying polymerization. The pre-polymerization of semi-aromatic nylon can be divided into high...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G69/28C08G69/26C08G69/36
Inventor 曹凯凯王文志胡天辉黄安民邓凯桓姜其斌
Owner ZHUZHOU TIMES NEW MATERIALS TECH
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