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Semi-aromatic polyamide production method and semi-aromatic polyamide

A semi-aromatic and production method technology, which is applied in the production method of semi-aromatic polyamide and the field of semi-aromatic polyamide, can solve problems such as long lag time, stable prepolymerization reaction, and lower product quality, and achieves wide application fields, The effect of low gel content and excellent performance

Active Publication Date: 2017-05-24
ZHEJIANG NHU SPECIAL MATERIALS +2
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0009] (1) Because the fusing point of aromatic dibasic acid exceeds its decomposition temperature, therefore, in the technique of existing literature report, the salt-forming reaction is all carried out in batches, and the ratio of dibasic acid and diamine in each batch of salt solution is different It is necessary to take samples for analysis and measurement, and then adjust according to the measurement results, which makes the prepolymerization reaction impossible to achieve true continuity
[0010] (2) The existing on-line test method can only quantitatively analyze the content of carboxyl-terminated and amino-terminated groups, but cannot analyze the composition of raw materials. Therefore, automatic control of the feeding process cannot be realized
[0011] (3) The amine and acid lost in the dehydration process cannot be continuously quantified, so it cannot be automatically adjusted according to the actual amine-acid ratio of the dehydrated material to stabilize the prepolymerization reaction
[0012] (4) The lag time for adjustment according to the end group content of the prepolymerization or polycondensation reaction outlet is long, and the amino acid ratio is prone to fluctuations during the adjustment process
However, if the amino acid ratio is too high, it is easy to cause side reactions of gelation, thereby reducing the quality of the product

Method used

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Experimental program
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Effect test

Embodiment 1

[0117] According to the ratio of the initial feeding amine acid molar ratio of 0.95, 4.15Kg / h (25mol / h) terephthalic acid, 3.65Kg / h (25mol / h) adipic acid, 5.51Kg / h (47.5Kmol / h) adipic acid Diamine, 0.04Kg / h of 20% sodium hypophosphite aqueous solution and 3.2Kg / h of water are put into the beating kettle 9 together, and the slurry is formed by continuous beating at 60°C. The slurry is transported by pump 10 to multi-stage stirring dissolution tank 14 and heated to 150° C. to dissolve into salt with the steam generated in the dehydration process. According to the composition of the dibasic acid in the salt solution detected by the on-line Raman spectrum 18, the amount of the aliphatic dibasic acid is adjusted by using molten adipic acid through the metering pump 23, so that the aromatic dibasic acid and the aliphatic dibasic acid in the salt-forming kettle 19 are dissolved. The ratio of basic acid remains stable. After the composition of the above-mentioned salt solution is det...

Embodiment 2

[0119] According to the proportion of the initial feeding amine acid molar ratio of 0.92, 3.32Kg / h (20mol / h) terephthalic acid, 6.06Kg / h (30mol / h) sebacic acid, 7.91Kg / h (46mol / h) sebacic acid Amine, 0.47Kg / h of 20% potassium hypophosphite aqueous solution and 5.46Kg / h of water are put into the beating kettle 9, and beating continuously at 70°C to form a slurry. The slurry is transported to the multi-stage stirring dissolution tank 14 through the pump 10, heated to 160°C with the steam generated in the dehydration process to dissolve into salt, and the composition of the dibasic acid in the salt solution is detected according to the online Raman spectrum 18. The amount of the aliphatic dibasic acid is adjusted by using the molten sebacic acid through the metering pump 23, so that the ratio of the aromatic dibasic acid to the aliphatic dibasic acid in the dissolution and salt-forming tank 19 is kept stable. After the composition of the above-mentioned salt solution is detected ...

Embodiment 3

[0121] According to the proportion of the initial feeding amine acid molar ratio of 0.98, 6.64Kg / h (40mol / h) terephthalic acid, 2.30Kg / h (10mol / h) dodecanedioic acid, 5.68Kg / h (49mol / h) Hexamethylenediamine, 0.2Kg / h of 20% sodium phosphite aqueous solution and 2.42Kg / h of water are put into the beating kettle 9, and the slurry is formed by continuous beating at 60°C. The slurry is transported by the pump 10 to the multi-stage stirring dissolution tank 14 and heated to 160° C. by the steam generated in the dehydration process to dissolve into salt. According to the composition of the dibasic acid in the salt solution detected by the online Raman spectrum 18, the amount of the aliphatic dibasic acid is adjusted by using molten dodecanedioic acid through the metering pump 23, so that the aromatic dibasic acid and the fatty acid in the salt-forming kettle 19 are dissolved. The ratio of family dibasic acids remains stable. After the above-mentioned salt solution is detected by the...

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Abstract

The invention provides a semi-aromatic polyamide production method and semi-aromatic polyamide. The semi-aromatic polyamide production method includes the steps that firstly, diamine and binary acid are primarily charged in the amino-acid molar ratio smaller than 1.0, diamine, binary acid, water and a catalyst form slurry, and the slurry is heated and dissolved to form a salt solution; secondly, after it is detected that the salt solution is formed, the salt solution is dehydrated, the content of diamine in steam condensed water from a dehydration device is detected, the amino-acid molar ratio is adjusted to be larger than 1.0 by melting diamine and a molecular weight regulator, namely monoacid, and a pre-polymerization reaction is conducted; thirdly, a pre-polymerization reaction solution is subjected to vacuum flashing and then a post-polycondensation reaction is conducted. The content of gel in a semi-aromatic polyamide product is low, properties are excellent, and the application range is wide.

Description

technical field [0001] The invention relates to a production method of semi-aromatic polyamide and semi-aromatic polyamide, in particular to a continuous production method of low-gel semi-aromatic polyamide. Background technique [0002] Semi-aromatic polyamide is usually a polyamide with benzene ring structure obtained by polycondensation reaction of aromatic dibasic acid, aliphatic diacid and aliphatic diamine. Due to the introduction of the aromatic ring structure in the main chain, semi-aromatic polyamide has good heat resistance and mechanical properties, low water absorption, and has a more suitable cost performance, filling the general engineering plastic nylon and high temperature engineering The gap between plastic PEEK can be used in electronics, electrical appliances, automobiles, clothing fibers and other fields. [0003] The preparation of semi-aromatic polyamides usually adopts a prepolymerization-finishing reaction process. The prepolymerization reaction usu...

Claims

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Application Information

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IPC IPC(8): C08G69/26C08G69/28
CPCC08G69/265C08G69/28C08L77/00C08L77/08
Inventor 陈志荣尹红张琴吴笑笑洪文刚宋恩峰邓杭军周贵阳王昌泽
Owner ZHEJIANG NHU SPECIAL MATERIALS