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Preparation method of high-purity isophthaloyl dichloride

An isophthaloyl chloride and high-purity technology, which is applied in the field of preparation of high-purity isophthaloyl chloride, can solve the problems of large environmental pollution, long production cycle, low purity and the like, and achieves low environmental pollution, short production cycle, high purity effect

Inactive Publication Date: 2012-02-08
X FIPER NEW MATERIAL CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] At present, there are phosgene method, phosphorus trichloride method, phosphorus pentachloride method, ester chlorination method, p-xylene chlorination method to the common method of preparing isophthaloyl chloride, and above method has long production cycle, for its Large environmental pollution, low yield, low purity and other defects

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] a. Feeding: At room temperature (usually around 25°C), add 650kg of inert solvent chlorobenzene into the reflux reactor, start stirring, then add 150kg of isophthalic acid and 15kg of catalyst N,N-dimethylformamide, stir, Add 330 kg of chlorinating agent thionyl chloride, and stir evenly;

[0025] b. Reaction: Gradually raise the temperature to 50°C, open the reflux valve of the reflux reactor, and open the reflux condensed water on the reflux reactor, and react for 10 hours to obtain the reaction liquid;

[0026] c. Separation and recovery: the reaction liquid is separated by atmospheric distillation, the chlorinating agent thionyl chloride is recovered at 80°C, the solution containing the catalyst is recovered at the top of the tower at 150°C, and the remaining liquid is collected. The recovered chlorinating agent thionyl chloride can continue to be reused, and the solution containing the catalyst can be recovered, and the catalyst can also be continuously reused afte...

Embodiment 2

[0030] a. Feeding: at room temperature, add 650 kg of inert solvent xylene into the reflux reactor, turn on the stirring, then add 150 kg of isophthalic acid and 15 kg of catalyst N,N-dimethylacetamide, stir, and add chlorinating agent Thionyl chloride 330 kg, stirred evenly;

[0031] b. Reaction: Gradually raise the temperature to 80°C, open the reflux valve of the reflux reactor, and open the reflux condensed water on the reflux reactor, and react for 5 hours to obtain the reaction liquid;

[0032] c. Separation and recovery: the reaction solution is separated by atmospheric distillation, the chlorinating agent thionyl chloride is recovered at 70°C, the solution containing the catalyst is recovered at the top of the tower at 80°C, and the remaining liquid is collected. The recovered chlorinating agent thionyl chloride can continue to be reused, and the solution containing the catalyst can be recovered, and the catalyst can also be continuously reused after further extraction...

Embodiment 3

[0036] a. Feeding: At room temperature, add 420 kg of inert solvent dichlorobenzene into the reflux reactor, turn on the stirring, then add 100 kg of isophthalic acid and 11 kg of catalyst N,N-dimethylacetamide, stir, add chlorine Chemical agent thionyl chloride 260 kg, stir evenly;

[0037] b. Reaction: Gradually raise the temperature to 70°C, open the reflux valve of the reflux reactor, and open the reflux condensed water on the reflux reactor, and react for 7.5 hours to obtain the reaction liquid;

[0038] c. Separation and recovery: the reaction liquid is separated by atmospheric distillation, the chlorinating agent thionyl chloride is recovered at 75°C, the solution containing the catalyst is recovered at the top of the tower at 120°C, and the remaining liquid is collected. The recovered chlorinating agent thionyl chloride can continue to be reused, and the solution containing the catalyst can be recovered, and the catalyst can also be continuously reused after further ex...

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PUM

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Abstract

The invention discloses a preparation method of high-purity isophthaloyl dichloride, which comprises the following steps of: a. at room temperature, adding an inert solvent into a reactor, adding m-phthalic acid, a catalyst and a chlorinating agent, and evenly stirring; b. gradually heating to 50-80 DEG C to react for 5-10 hours, thereby obtaining a reaction liquid; c. carrying out atmospheric distillation separation on the reaction liquid, recycling the chlorinating agent at 70-80 DEG C, recycling the catalyst-containing solution on the tower top at 80-150 DEG C, and collecting the residual kettle liquid; d. carrying out rectification on the residual kettle liquid under vacuum, and recycling isophthaloyl dichloride at the kettle liquid temperature of 170-190 DEG C while keeping the vacuum; and e. under vacuum conditions, carrying out secondary vacuum distillation on the isophthaloyl dichloride, and recycling the isophthaloyl dichloride at 185-190 DEG C. The invention has the advantages of simple technique, short production cycle, low environmental pollution and high yield; and particularly, the purity of the isophthaloyl dichloride subjected to rectification twice is high, up to over 99.98%.

Description

technical field [0001] The invention relates to a preparation method of isophthaloyl dichloride, in particular to a preparation method of high-purity isophthaloyl dichloride. Background technique [0002] At present, isophthaloyl chloride can be used as a monomer of polyamide, polyester, polyarylate, polyarylamide, liquid crystal polymer, etc., and can also be used as a modifier of high polymer, an intermediate of pesticide and pharmaceutical industry . With the rapid development of high-performance fiber aramid 1313, the demand for isophthaloyl chloride, one of the important raw materials of aramid 1313, is growing rapidly. [0003] At present, there are phosgene method, phosphorus trichloride method, phosphorus pentachloride method, ester chlorination method, p-xylene chlorination method to the common method of preparing isophthaloyl chloride, and above method has long production cycle, for its Large environmental pollution, low yield, low purity and other defects. Con...

Claims

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Application Information

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IPC IPC(8): C07C63/24C07C51/60C07C51/44
CPCY02P20/584
Inventor 钟洲胡祖明陈蕾
Owner X FIPER NEW MATERIAL CO LTD
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