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Isophthaloyl dichloride production process and production equipment

A technology of isophthaloyl chloride and production process, applied in the field of isophthaloyl chloride production process and production devices thereof, can solve the problems of unfavorable product quality stability and yield improvement, difficulty in meeting the rapid development of the aramid fiber industry, and difficulty in product quality Guarantee and other issues, to achieve the effect of shortening the distillation and purification time, high product yield and convenient operation

Inactive Publication Date: 2016-06-01
SHANDONG KAISHENG NEW MATERIALS
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The refining process of this method usually adopts vacuum rectification, which takes a long time and high temperature, and the product quality is difficult to guarantee. At the same time, it has high requirements on the vacuum device, and the fore distillation and rectification residue need to be removed, which is not conducive to the stability of product quality and the improvement of yield, and it is difficult to Meet the rapid development of my country's aramid fiber industry

Method used

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  • Isophthaloyl dichloride production process and production equipment
  • Isophthaloyl dichloride production process and production equipment
  • Isophthaloyl dichloride production process and production equipment

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1-3

[0024] Embodiment 1-3 of the present invention all adopts following device:

[0025] The described production device consists of a reaction kettle 1, a reaction liquid storage tank 2, a first metering pump 3, a primary thin film evaporator 4, a crude product storage tank 5, a second metering pump 6, a secondary thin film evaporator 7, The condenser 8 and the product tank 9 are composed.

Embodiment 1

[0027] Put 1000kg of isophthalic acid and 2500kg of thionyl chloride into the reaction kettle, add 5kg of N,N-dimethylformamide, and gradually raise the temperature to react to release sulfur dioxide and hydrochloric acid gas. When the temperature rises to 90°C, no gas comes out, and the reaction After the end, continue to keep warm for 1 hour, and recover most of the unreacted thionyl chloride by distillation under normal pressure and under reduced pressure in the reaction kettle, and put the remaining reaction solution into the reaction solution storage tank.

[0028] The temperature of the primary thin film evaporator is maintained at 120°C and the vacuum degree is 660mmHg, the temperature of the secondary thin film evaporator is maintained at 165°C and the vacuum degree is 750mmHg. The reaction solution continuously enters the first-stage thin-film evaporator at a feed rate of 5 kg / min to remove the residual thionyl chloride and the catalyst, and the crude product enters th...

Embodiment 2

[0033] Put 1000kg of isophthalic acid and 2500kg of thionyl chloride into the reaction kettle, add 1kg of N,N-dimethylacetamide, and gradually raise the temperature to react to release sulfur dioxide and hydrochloric acid gas. When the temperature rises to 95°C, no gas comes out, and the reaction is over. , continue to keep warm for 1 hour, and recover most of the unreacted thionyl chloride by distillation under normal pressure and under reduced pressure in the reaction kettle, and put the remaining reaction solution into the storage tank.

[0034] Keep the temperature of the first-stage thin film evaporator at 100°C and the vacuum degree of 720mmHg, and the reaction liquid enters the first-stage thin-film evaporator intermittently at a feed rate of 4.5kg / min to remove the residual thionyl chloride and the catalyst, and the crude product enters the crude product storage tank .

[0035] Keep the temperature of the secondary thin-film evaporator at 180°C, and the vacuum degree i...

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Abstract

The invention relates to an m-phthaloyl chloride production process and a production device thereof, and belongs to the technical field of organic synthesis. According to the production process, a reflux reaction is performed on m-phthalic acid and excessive sulfoxide chloride in the presence of a catalyst; after the reaction ends, most of non-reacted sulfoxide chloride is recovered by virtue of atmospheric distillation and reduced pressure distillation, and then the residual sulfoxide chloride and catalyst are distilled off under reduced pressure by use of a primary film evaporator, and finally, the m-phthaloyl chloride is obtained by virtue of distillation purification by use of a secondary film evaporator under a high vacuum condition. The m-phthaloyl chloride production process has the characteristics of simple process, convenient operations, short production period, high product yield, low impurity content, recyclable excessive sulfoxide chloride and the like, and is suitable for industrial production. The m-phthaloyl chloride produced by use of the m-phthaloyl chloride production process has the purity of more than 99.95% and the yield of greater than 99.5%.

Description

technical field [0001] The invention relates to a production process of isophthaloyl dichloride and a production device thereof, belonging to the technical field of organic synthesis. Background technique [0002] Isophthaloyl chloride, also known as isophthaloyl dichloride or isophthaloyl dichloride, referred to as IPC, is a white crystal at room temperature, with a melting point of 43-45°C and a boiling point of 276-278°C. It is easy to decompose or change in air. yellow. High-quality isophthaloyl chloride is the main raw material for the production of high-performance meta-aramid fiber (aramid 1313), and can also be used as a monomer for the synthesis of polyamide, polyester, polyarylate, polyaramid, liquid crystal polymer, etc. , Modifier of high polymer, intermediate of pesticide and pharmaceutical industry. At present, the industrial production of isophthaloyl dichloride mainly involves the thionyl chloride method and the phosgene method, among which the thionyl chlo...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C63/24C07C51/60
CPCC07C51/60C07C63/24
Inventor 张泰铭孙丰春张善民王荣海毕义霞薛居强王军孙庆民
Owner SHANDONG KAISHENG NEW MATERIALS
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