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Preparation method of long-carbon chain semi-aromatic nylon salt

A semi-aromatic nylon and long carbon chain technology, which is applied in the field of preparation of long carbon chain semi-aromatic nylon salts, can solve the problems of high reaction temperature, low production efficiency, and long time consumption, and achieve mild reaction conditions and short production cycle , the effect of low energy consumption

Active Publication Date: 2014-03-05
JIANGMEN DENGZHONGTAI ENG PLASTICS CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] But there is following problem in existing nylon salt preparation technology: 1, when using water or ethanol as solvent preparation long carbon chain semi-aromatic nylon salt, because nylon salt and aromatic dibasic acid have little solubility in water, in the reaction process just A large amount of nylon salt is precipitated, which may wrap the unreacted aromatic dibasic acid, resulting in inaccurate determination of the end point and a decrease in the purity of the salt; 2. Choose dimethylformamide, N-methylpyrrolidone or dimethyl sulfoxide as the solvent When preparing semi-aromatic nylon salt, because the prepared nylon salt is not completely soluble in the sol

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] (1) Add 172g (1mol) 1,10-decanediamine and 400g deionized water into a 1L three-necked flask protected by nitrogen, stir and heat to 95°C;

[0027] (2) Mix 99.6g (0.6mol) terephthalic acid and 100g deionized water for beating, and heat to 80°C;

[0028] (3) Slowly add the slurry obtained in step (2) to the aqueous solution of 1,10-decanediamine obtained in step (1), and continue to react at 95°C for 0.5 h after the addition is completed;

[0029] (4) Cool down to 65°C, centrifuge, wash the obtained solid, and dry to obtain 138.1 g of PA10T salt, with a yield of 68.1%.

[0030] The formula for calculating yield is: yield = actual yield / theoretical yield.

[0031] Among them, the theoretical yield of the nylon salt is calculated based on the aromatic dibasic acid, and the mass of the nylon salt after drying in a vacuum oven at 105°C for 24 hours is the actual yield.

Embodiment 2

[0033] (1) Add 172g (1mol) 1,10-decanediamine and 500g deionized water into a 2L three-necked flask protected by nitrogen, stir and heat to 95°C;

[0034] (2) Mix 97g (0.5mol) terephthalic acid and 150g deionized water for beating and heat to 80°C;

[0035] (3) Slowly add the slurry obtained in step (2) into the aqueous solution of 1,10-decanediamine obtained in step (1), and continue to react at 90°C for 0.5 h after the addition is completed;

[0036] (4) Cool down to 55°C, centrifuge, wash the obtained solid, and dry to obtain 128.6 g of PA10P salt, with a yield of 70.3%.

Embodiment 3

[0038] (1) Add 172g (1mol) 1,10-decanediamine and 500g deionized water into a 2L three-necked flask protected by nitrogen, stir and heat to 95°C;

[0039] (2) Mix 96.9g (0.4mol) 4,4-biphenyldicarboxylic acid with 130g deionized water for beating, and heat to 80°C;

[0040] (3) Slowly add the slurry obtained in step (2) into the aqueous solution of 1,10-decanediamine obtained in step (1), and continue to react at 90°C for 0.5 h after the addition is completed;

[0041] (4) Cool down to 70°C, centrifuge, retain the filtrate, wash the obtained solid, and dry to obtain 114.1 g of PA10B salt, with a yield of 68.8%.

[0042] (5) After raising the temperature of 500g of filtrate to 90°C, add 25g of deionized water, 60g of 1,10-decanediamine and 60g of 4,4-biphenyldicarboxylic acid in turn, and continue to react at 90°C for 0.5h under the protection of nitrogen, and cool down to Centrifuge at 70°C, wash the obtained solid, and dry to obtain 101.1 g of PA10B salt, with a yield of 98.5...

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Abstract

The invention discloses a preparation method of long-carbon chain semi-aromatic nylon salt, which comprises the following steps of performing a neutralization reaction between aromatic diacid and excess aliphatic diamine in water, cooling, separating, washing and drying to obtain a product. Since the long-carbon chain semi-aromatic nylon salt has relatively high solubility in the mixed solution of water and corresponding aliphatic diamine, the method adopts a mode of performing a reaction between excess aliphatic diamine and aromatic diacid in water and completely dissolving the nylon salt generated by the reaction into the solution. The method can effectively prevent the nylon salt generated by the reaction from coating the water-insoluble aromatic diacid, the prepared semi-aromatic nylon salt has high purity, the operation cycle is short, the reaction conditions are mild, and the method is environment-friendly; moreover, the filtrate can be utilized repeatedly, the yield is high, and the production cost is low.

Description

technical field [0001] The invention belongs to the field of chemical synthesis, and in particular relates to a preparation method of long carbon chain semi-aromatic nylon salt. Background technique [0002] Polyamide, also known as nylon, is a general term for polymers containing amide groups in the repeating units of the main chain of macromolecules. It is the earliest and most widely used thermoplastic engineering plastic at home and abroad. Due to its excellent properties such as toughness, wear resistance, impact resistance, fatigue resistance, corrosion resistance, oil resistance, etc., especially excellent wear resistance and self-lubricating properties, and small friction coefficient, nylon has been steadily competing with other engineering plastics for forty years. Its demand has so far ranked first among the five major engineering plastics (polyamide, polyoxymethylene, polycarbonate, polyphenylene ether, polybutylene terephthalate). [0003] Semi-aromatic nylon is...

Claims

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Application Information

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IPC IPC(8): C07C51/41C07C63/28C07C57/34C07C63/333C07C63/38C07C209/00C07C211/09C08G69/26
CPCC07C51/412C07C209/00C08G69/26C07C63/28C07C57/34C07C63/333C07C63/38C07C211/09
Inventor 金良文曾建平严燕
Owner JIANGMEN DENGZHONGTAI ENG PLASTICS CO LTD