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Method for simultaneously preparing 5-chlorovaleryl chloride and adipoyl chloride by using one-pot method

A technology of chlorovaleryl chloride and adipoyl chloride, applied in chemical instruments and methods, nitrile preparation, carboxylate preparation and other directions, can solve the problems of waste of raw materials, low single-pot production capacity, low cyanation reaction yield and the like

Inactive Publication Date: 2018-03-23
常州润联化工有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This results in low yield of cyanidation reaction, large amount of solvent circulation, low single-pot production capacity and large energy consumption
[0006] In addition, when the raw material 1,4-dichlorobutane was separated by rectification and 5-chlorovaleronitrile was collected, the by-product adiponitrile was heated in the kettle for a long time, and finally turned into a tar-like substance, which could not be recovered and could only be used as Waste disposal
This not only wastes raw materials, but also increases the cost of "three wastes" treatment

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] Put 1270Kg of 1,4-dichlorobutane and 9.5Kg of tetrabutylammonium bromide catalyst into a 3000L reactor, raise the temperature to 80-85°C under stirring, and evenly add 730Kg of 30% sodium cyanide aqueous solution dropwise within 5 hours. After the addition, react at 80-85°C for 1 hour.

[0031] Cool the liquid in the kettle to 25°C, and pump it into a high-position 3000L phase-separation tank with vacuum suction or a transfer pump. The lower organic phase is a solution of 5-chlorovaleronitrile and adiponitrile in 1,4-dichlorobutane. The organic phase was separated and returned to the kettle. The upper aqueous phase is discharged into the wastewater system for treatment.

[0032] Add 820Kg of 30% industrial hydrochloric acid into the reaction kettle, heat up to 55-70°C for 5 hours under stirring. After the reaction, cool to 45°C, add 110Kg of water to completely dissolve the solid ammonium chloride, and separate the lower organic phase to be a 1,4-dichlorobutane solut...

Embodiment 2

[0034] Put 1270Kg of 1,4-dichlorobutane and 12Kg of tetrabutylammonium bromide catalyst into a 3000L reactor, raise the temperature to 80-85°C under stirring, and evenly add 950Kg of 30% sodium cyanide aqueous solution dropwise within 5 hours. After the addition, react at 80-85°C for 1 hour.

[0035] Cool the liquid in the kettle to 25°C, and pump it into a high-position 3000L phase-separation tank with vacuum suction or a transfer pump. The lower organic phase is a solution of 5-chlorovaleronitrile and adiponitrile in 1,4-dichlorobutane. The organic phase was separated and returned to the kettle. The upper aqueous phase is discharged into the wastewater system for treatment.

[0036] Add 1400Kg of 30% industrial hydrochloric acid into the reaction kettle, and heat up to 55-70° C. for 5 hours under stirring. After the reaction, cool to 45°C, add 110Kg of water to completely dissolve the solid ammonium chloride, and separate the lower organic phase to be a 1,4-dichlorobutane...

Embodiment 3

[0038]Put 1270Kg of 1,4-dichlorobutane and 16.5Kg of tetrabutylammonium bromide catalyst into a 3000L reactor, heat up to 80-85°C under stirring, and evenly add 1060Kg of 30% sodium cyanide aqueous solution dropwise within 5 hours. After the addition, react at 80-85°C for 1 hour.

[0039] Cool the liquid in the kettle to 25°C, and pump it into a high-position 3000L phase-separation tank with vacuum suction or a transfer pump. The lower organic phase is a solution of 5-chlorovaleronitrile and adiponitrile in 1,4-dichlorobutane. The organic phase was separated and returned to the kettle. The upper aqueous phase is discharged into the wastewater system for treatment.

[0040] Add 1740Kg of 30% industrial hydrochloric acid into the reaction kettle, and heat up to 55-70°C for 5 hours under stirring. After the reaction, cool to 45°C, add 110Kg of water to completely dissolve the solid ammonium chloride, and separate the lower organic phase to be a 1,4-dichlorobutane solution of 5...

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Abstract

The invention discloses a method for simultaneously preparing 5-chlorovaleryl chloride and adipoyl chloride by using a one-pot method. Using 1,4-dichlorobutane as a raw material, sodium cyanide is gradually added dropwise into a reaction kettle in the presence of a phase transfer catalyst 1,4-dichlorobutane solution of 5-chlorovaleronitrile and adiponitrile; the obtained organic phase is separated from the aqueous phase, and hydrolyzed to generate 5-chlorovaleric acid and adipic acid 1,4-di Chlorobutane solution; the obtained ammonium chloride solid is added with water to dissolve completely, and the aqueous phase is separated; the 1,4 dichlorobutane solution of the obtained 5-chlorovaleric acid and adipic acid is added to sulfur oxychloride to carry out acid chloride reaction, Obtain the 1,4-dichlorobutane solution of 5-chlorovaleryl chloride and adipoyl chloride; the 1,4-dichlorobutane solution of the above-obtained 5-chlorovaleryl chloride and adipoyl chloride is dropped into a vacuum distillation column Adipoyl chloride products with a distillate temperature of 105-107°C are distilled out of the kettle. The present invention uses 1,4-dichlorobutane as a raw material, adopts "one-pot method" to simultaneously produce two intermediate products of 5-chlorovaleryl chloride and adipoyl chloride, the method has high yield, large single-pot production capacity, and solvent circulation Small amount, low energy consumption, less "three wastes".

Description

technical field [0001] The invention relates to the fields of medicine and pesticide intermediates, and more specifically relates to a method for simultaneously preparing 5-chlorovaleryl chloride and adipoyl chloride by a one-pot method. Background technique [0002] 5-Chlorovaleryl Chloride, CAS: [1575-61-7], English name 5-Chlorovaleryl Chloride is an important pharmaceutical and pesticide intermediate. 5-Chlorovaleryl chloride is mainly used in medicine to manufacture Cilostazol, a drug that resists platelet aggregation, protects vascular endothelial cells, and prevents atherosclerosis. 5-chlorovaleryl chloride is also used to produce Pyraclonil, a new broad-spectrum herbicide for rice. [0003] Adipoyl chloride, CAS: [111-50-2], English name: Adipoyl Chloride, is a pharmaceutical intermediate used in the manufacture of water-soluble intravenous contrast agent (Iodipamide), which is widely used in X-rays Diagnosis of various diseases with CT. [0004] In the existing t...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C51/60C07C51/64C07C53/46C07C55/36C07C253/14C07C255/09C07C255/10C07C51/08C07C53/19C07C55/14
CPCC07C51/60C07C51/08C07C51/64C07C253/14C07C53/46C07C55/36C07C255/09C07C255/10C07C53/19C07C55/14
Inventor 言兆福
Owner 常州润联化工有限公司
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