Preparation and purification method of paraphthaloyl chloride with high purity

A terephthaloyl chloride and purification method technology, applied in the field of organic chemistry, can solve the problems of high energy consumption and low material utilization rate, and achieve the effects of improving product purity, convenient operation, and saving energy and material consumption

Inactive Publication Date: 2014-08-27
TECH CENT CHINA PINGMEI SHENMA ENERGY & CHEM GRP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The purpose of the embodiments of the present invention is to provide a method for preparing and purifying terephthaloyl dichloride, which aims to solve the defects of low material utiliza

Method used

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  • Preparation and purification method of paraphthaloyl chloride with high purity

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Experimental program
Comparison scheme
Effect test

Example Embodiment

[0015] Example 1.

[0016] Into a three-necked flask equipped with a reflux condenser, a thermometer and an exhaust gas absorption device, add 50 g terephthalic acid, 90 mL thionyl chloride, and 3.0 g 1-hexyl-3-methylimidazole tetrafluoroborate. The exhaust gas is absorbed by NaOH alkali solution, electromagnetic stirring is started, and heated to 79 o C refluxed for 10 h, the reactant changed from a white turbid suspension to a light yellow transparent solution, the reaction was ended, and the product was cooled to precipitate. Filter, analyze and detect the content of terephthalic acid, thionyl chloride and catalyst in the filtrate, and make corresponding supplements according to the amount of reactants to carry out a cyclic reaction. Put the filtered crude product into the melting crystallizer, 65-72 o Program C to increase the temperature for 4 hours, release sweat, and increase the temperature to 85 o C, release the product. Obtained 55.2 g of white product, product pur...

Example Embodiment

[0018] Example 2.

[0019] Into a three-necked flask equipped with reflux condenser, thermometer and exhaust gas absorption device, add 50 g terephthalic acid, 80 mL thionyl chloride, 4.5 g 1-hexyl-3-methylimidazole hexafluorophosphate, and tail gas. Absorb with NaOH alkali solution, start electromagnetic stirring, and heat to 89 o C was refluxed for 4 hours, the reactant changed from a white turbid suspension to a light yellow transparent solution, the reaction was ended, and the product was cooled to precipitate. Filter, analyze and detect the content of terephthalic acid, thionyl chloride and catalyst in the filtrate, and make corresponding supplements according to the amount of reactants to carry out a cyclic reaction. Put the filtered crude product into the melting crystallizer, 72-78 o C program heats up for 4h, releases sweat, and raises the temperature to 90 o C, release the product. Obtained 56.1 g of white product, product purity 99.9%, melting point: 82.0-82.5 o C...

Example Embodiment

[0021] Example 3.

[0022] To a three-necked flask equipped with a reflux condenser, a thermometer and an exhaust gas absorption device, add 50 g terephthalic acid, 80 mL thionyl chloride, and 3.5 g 1-butyl-3-methylimidazole tetrafluoroborate. , The tail gas is absorbed by NaOH alkali solution, electromagnetic stirring is started, and heated to 80 o C refluxed for 10 h, the reactant changed from a white turbid suspension to a light yellow transparent solution, the reaction was ended, and the product was cooled to precipitate. Filter, analyze and detect the content of terephthalic acid, thionyl chloride and catalyst in the filtrate, and make corresponding supplements according to the amount of reactants to carry out a cyclic reaction. The filtered crude product was distilled under reduced pressure, the vacuum degree was 133 Pa, and the distillate at 105-110℃ was received to obtain 58.0 g of white product with a purity of 99.9%. Melting point: 82.5-83.0 o C, the yield is 94.9%.

[0...

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Abstract

The invention discloses a preparation and purification method of paraphthaloyl chloride with a high purity, and belongs to the field of organic chemistry. The method comprises the following steps: carrying out a reflux reaction in the presence of a catalyst by taking terephthalic acid and thionyl chloride as raw materials, cooling and precipitating so as to obtain a crude product; filtering the crude product and then purifying the crude product in a melting crystallization or reduced pressure distillation manner; analyzing the contents of phthalic acid, thionyl chloride and catalyst in a filtrate; replenishing a proper amount of the terephthalic acid, thionyl chloride and catalyst according to the analysis result; then carrying out a circular reaction. Compared with the prior art, the method disclosed by the invention has the main advantage that the excess thionyl chloride does not need to be steamed out after the reaction is finished, but the crude product is obtained in a cooling and filtering manner, so that the filtrate is recycled. Thus, the consumption of energy and materials is decreased.

Description

technical field [0001] The invention belongs to the field of organic chemistry, in particular to a method for preparing and purifying terephthaloyl dichloride. Background technique [0002] Aramid fiber is one of the main high-tech fibers. Together with carbon fiber and high-strength and high-modulus polyethylene fiber, it is called the world's three high-performance fibers. It is not only an indispensable new material for aerospace, national defense and high-tech industries, but also gradually becomes Civil industry and living materials are widely used in advanced composite materials, life protection products, transportation and ultra-light structures, and are important basic raw materials related to national security and national economic development. According to reports, at present, aramid products are used in body armor, helmets, etc., accounting for about 7% to 8%, aerospace materials, sports materials account for about 40%; tire frame materials, conveyor belt material...

Claims

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Application Information

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IPC IPC(8): C07C63/30C07C51/60C07C51/64
CPCC01B17/4584C07C51/60C07C51/64C07C63/30Y02P20/582
Inventor 王俊伟海国栋胡延韶陈茜茹王丽杰李中贤刘小培靳鹏崔强
Owner TECH CENT CHINA PINGMEI SHENMA ENERGY & CHEM GRP
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