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Semi-aromatic polyamide and preparation method thereof

A semi-aromatic and polyamide technology, applied in the field of semi-aromatic polyamide preparation, can solve the problem of inaccurate control of the molar ratio of dicarboxylic acid and diamine, affecting the quality of the final semi-aromatic polyamide, purification Solve the problems of semi-aromatic polyamide salts, etc., and achieve the effects of good processing stability, low content of active end groups, and high crystallinity

Active Publication Date: 2009-06-17
KINGFA SCI & TECH CO LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0013] But, there is such a problem in the prior art, both when using water or alcohol as solvent to prepare semi-aromatic polyamide salt, because the solubility of aromatic dicarboxylic acid and semi-aromatic polyamide salt in these solvents is very Small, the purification of semi-aromatic polyamide salt becomes very difficult, it is difficult to obtain pure semi-aromatic polyamide salt, and then the molar ratio of dicarboxylic acid and diamine cannot be accurately controlled, which affects the final product semi-aromatic polyamide salt. Amide quality

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0054] Mix 16.61Kg terephthalic acid (100mol) and 40Kg dimethylformamide evenly, heat to 120°C while stirring to form A solution; then mix 17.23Kg 1,10-decanediamine (100mol) with 20Kg di Mix methylformamide evenly and heat to 80°C while stirring to make solution B; mix solution A and solution B evenly and heat to 120°C while stirring continuously to make the reaction fully; after centrifugation, the obtained The precipitate was washed with dimethylformamide and then with deionized water several times to obtain 32.28 kg of terephthalic acid decanediamine salt with a yield of 95.4% and a melting point of 260°C.

[0055] Add 6769g (20mol) decyl diamine terephthalate, 73.27g (0.6mol) benzoic acid, 6.77g ( 0.1% by weight based on the total weight of the raw materials) sodium hypophosphite, 2283g (25% by weight based on the total weight of the reaction system) deionized water, and the temperature was raised after purging with nitrogen. The temperature was raised to 220°C with stir...

Embodiment 2

[0057] The preparation steps of Example 1 were repeated, except that the method of thickening was changed to melt thickening, the thickening temperature was 330° C., and the thickening time was 5 minutes. The results are shown in Table 1.

Embodiment 3

[0059] Repeat the preparation steps of Example 1, except that the raw materials are changed to terephthalic acid, isophthalic acid and 1,10-decanediamine, thereby making decanediamine terephthalate and isophthalic acid decanediamine amine salt.

[0060] 5754 g (17 mol) of decyl diamine terephthalate and 1015 g (3 mol) of decyl diamine isophthalate were subjected to prepolymerization and viscosity-increasing reaction, and the steps were the same as in Example 1. The results are shown in Table 1.

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Abstract

The invention relates to semi-aromatic polyamide and a preparation method thereof. The semi-aromatic polyamide is prepared by: adding aromatic dicarboxylic acids and the fatty diamine with 4-14 carbon atoms to an organic solvent to undergo neutralization reaction to prepare high-purification salt; pre-polymerizing by taking the high-purification salt as the raw material with the existence of water; preparing the semi-aromatic polyamide by the further tackification reaction of the prepolymer. By using high-purification salt, the preparation method can accurately control the molar ratio of dicarboxylic acids and diamine, and avoid the loss of the diamine. By purifying monomers in the salifying process, the preparation method also improves the quality of the semi-aromatic polyamide and obtains the semi-aromatic polyamide with high inherent viscosity, high crystallinity, high melting point and good mechanical performance.

Description

technical field [0001] The invention relates to the technical field of polyamide resins, in particular to a method for preparing semi-aromatic polyamides. Background technique [0002] Aliphatic polyamides, such as PA6 and PA66, have excellent mechanical strength, heat resistance, chemical resistance, wear resistance and self-lubricating properties, and low coefficient of friction. Their applications include electronic appliances, automotive parts, furniture , building materials and fibers, has become one of the most important engineering plastics. [0003] Semi-aromatic polyamide is a polyamide resin prepared by polycondensation of diamines or dicarboxylic acids with aromatic rings and aliphatic dicarboxylic acids or diamines, and is one of the aromatic polyamides. Due to the introduction of aromatic rings into the main chain of polyamide molecules, the heat resistance and mechanical properties are improved, the water absorption rate is reduced, and it has a more suitable ...

Claims

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Application Information

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IPC IPC(8): C08G69/26
CPCC08G69/28C08G69/26
Inventor 曹民夏世勇黄险波曾祥斌罗湘安史振国陈健
Owner KINGFA SCI & TECH CO LTD
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