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Preparation method of paraphthaloyl chloride with high purity

A technology of terephthaloyl chloride and terephthalic acid, which is applied in the field of preparation of high-purity terephthaloyl chloride by chlorination, can solve the problems of tail gas environmental pollution, long production cycle, complicated process, etc., and achieve the production process The effect of simplicity, shortened production cycle and convenient operation

Active Publication Date: 2009-10-21
SHANDONG KAISHENG NEW MATERIALS
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The present invention is aimed at the deficiencies of the above methods, and proposes a new production and preparation method, which solves the problems of complex process, long production cycle, large tail gas pollution to the environment, low yield, and low purity.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0012] Add 100kg of terephthalic acid, 250L of thionyl chloride and 0.2kg of N,N-dimethylformamide into the reaction tank. Turn on the stirring on the reactor, start to gradually raise the temperature to 60°C, turn on the reflux condensed water on the reactor, open the reflux valve, and control the tail gas volume to 80-100L / h. As the end point of the reaction, the reaction time was 12 hours. After the reaction, the thionyl chloride is recovered at 75-80°C, and the solution containing the catalyst is recovered at 80-155°C. Open the vacuum system and tail gas absorption system, after the vacuum degree is -0.095MPa, the temperature in the kettle is 170-180°C to collect terephthaloyl chloride. The tail gas is condensed through the first stage of low-temperature condensation, and a large amount of sulfur dioxide is condensed to obtain sulfur dioxide liquid. The remaining tail gas is absorbed by falling film in the secondary absorption tower, and the low-concentration sulfur dioxi...

Embodiment 2

[0014] Add 100kg of terephthalic acid, 250L of thionyl chloride and 0.1kg of pyridine into the reaction tank. Turn on the stirring on the reactor, start to gradually raise the temperature to 60°C, turn on the reflux condensed water on the reactor, open the reflux valve, and control the tail gas volume to 80-100L / h. As the end point of the reaction, the reaction time was 10 hours. After the reaction, the thionyl chloride is recovered at 75-80°C, and the solution containing the catalyst is recovered at 80-120°C. Open the vacuum system and tail gas absorption system, after the vacuum degree is -0.095MPa, the temperature in the kettle is 170-180°C to collect terephthaloyl chloride. The tail gas is condensed through the first stage of low-temperature condensation, and a large amount of sulfur dioxide is condensed to obtain sulfur dioxide liquid. The remaining tail gas is absorbed by falling film in the secondary absorption tower, and the low-concentration sulfur dioxide continues ...

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Abstract

The invention discloses a preparation method of paraphthaloyl chloride with high purity, which takes terephthalic acid and a chlorinating agent as materials to prepare the paraphthaloyl chloride with high purity by reflux reaction and distillating separation for one time under the condition of catalysts, and then the method conducts treatment on byproducts to obtain additional products which can be utilized. The method has the advantages of being capable of improving the yield of the product to over 90-95 percent, realizing closed cycle for tail gas absorption and utilization, having no pollution to environment and being capable of achieving over 99.95 percent of product purity.

Description

1. Technical field [0001] The invention relates to the fields of production technology and by-product utilization of terephthaloyl chloride, and mainly relates to a preparation method for producing high-purity terephthaloyl chloride by a chlorination method. 2. Background technology [0002] With the demand of domestic and foreign aramid fiber industries, especially the rapid development of aramid fiber 1414, terephthaloyl chloride, one of the important raw materials for the synthesis of aramid fiber 1414, also develops rapidly thereupon. In addition, terephthaloyl chloride can be As a monomer of insulating materials, dyes, pigments, polyamides, polyesters, polyarylates, polyester amides, polyarylamides, liquid crystal polymers, etc., it can also be used as a modifier for high polymers, and as an agent for pesticides and pharmaceutical processes. Intermediates, etc., the current domestic annual output is about 2,000 tons, and the annual demand is increasing at a rate of 70%....

Claims

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Application Information

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IPC IPC(8): C07C51/60C07C63/30B01D53/50
CPCY02P20/584
Inventor 李云永粱伟王荣海李云龙李志忠李文娟
Owner SHANDONG KAISHENG NEW MATERIALS
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