Method for treating aluminum-containing wastewater in preparation process of 6-oxo-8-chloro ethyl caprylate

A technology for the preparation of ethyl chlorooctanoate, which is applied in the field of treating aluminum-containing wastewater, can solve the problems of large amount of aluminum-containing wastewater, difficulty in resource treatment, low aluminum ion content, etc., and achieves production cost reduction, obvious advantages in resource utilization, The effect of simple process

Inactive Publication Date: 2015-06-03
JIANGSU TOHOPE PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] However, the above-mentioned prior art still has a large amount of aluminum-containing wastewater (for example, throwing 100 kg of ethyl 6-chloro-6-oxohexanoate to participate in the reaction, producing 1.4 to 1.6 tons of wastewater), and low aluminum ion content (the Baume specific gravity is about 13 ), resource processing difficult defects

Method used

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  • Method for treating aluminum-containing wastewater in preparation process of 6-oxo-8-chloro ethyl caprylate
  • Method for treating aluminum-containing wastewater in preparation process of 6-oxo-8-chloro ethyl caprylate
  • Method for treating aluminum-containing wastewater in preparation process of 6-oxo-8-chloro ethyl caprylate

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Embodiment 1

[0039] According to the similar preparation method of 6-oxo-8-chlorooctanoic acid ethyl ester described in CN102731307A, put 1050kg water into 3M 3 In the hydrolysis kettle, ice salt water is passed into the jacket of the hydrolysis kettle. The hydrolysis kettle is equipped with a circulation pump and a circulation pipeline. The circulation pipeline is connected to a graphite condenser. Brine, the material is cooled and then recycled back to the hydrolysis tank. Use a jacket and a graphite condenser to circulate and cool the water in the hydrolysis tank to below 10°C for later use.

[0040] Add 1280Kg of dichloroethane into a 1500L reaction kettle, put in 450Kg of aluminum trichloride, stir, cool down to 10°C-18°C with an ice-salt water jacket, add dropwise 360kg of ethyl 6-chloro-6-oxohexanoate, and The temperature was controlled at 20°C to 25°C, and ethylene was passed through for 3 hours to obtain an addition reaction solution. Put the reaction solution into the spare 105...

Embodiment 2

[0043] Put the last batch of distilled water into 3M 3 In the hydrolysis kettle, add water to 1050kg, put ice salt water into the jacket of the hydrolysis kettle, install a circulation pump and a circulation pipeline in the hydrolysis kettle, and connect a graphite condenser to the circulation pipeline, and the materials in the hydrolysis kettle enter the graphite condenser through the circulation pump, and the graphite condenser The ice brine is passed into the water, and the material is cooled and then circulated back to the hydrolysis kettle. Use a jacket and a graphite condenser to circulate and cool the water in the hydrolysis tank to below 10°C for later use.

[0044]Add 1280Kg of dichloroethane into a 1500L reaction kettle, add 450Kg of aluminum trichloride, stir, cool down to 10°C-18°C with an ice-salt water jacket, add dropwise 360kg of ethyl 6-chloro-6-oxohexanoate, and Control the temperature at 20°C to 25°C, and pass through ethylene for 3 hours to obtain the addi...

Embodiment 3

[0047] Put 1350kg of water into 3M 3 In the hydrolysis kettle, ice salt water is passed into the jacket of the hydrolysis kettle. The hydrolysis kettle is equipped with a circulation pump and a circulation pipeline. The circulation pipeline is connected to a graphite condenser. Brine, the material is cooled and then recycled back to the hydrolysis tank. Use a jacket and a graphite condenser to circulate and cool the water in the hydrolysis tank to below 10°C for later use.

[0048] Add 1280Kg of dichloroethane into a 1500L reaction kettle, put in 450Kg of aluminum trichloride, stir, cool down to 10°C-18°C with an ice-salt water jacket, add dropwise 360kg of ethyl 6-chloro-6-oxohexanoate, and The temperature was controlled at 20°C to 25°C, and ethylene was passed through for 3 hours to obtain an addition reaction solution. Put the reaction solution into the spare 1350kg water in the hydrolysis kettle, stir it, and then enter the graphite condenser through the circulating pump...

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Abstract

The invention relates to a method for treating aluminum-containing wastewater in a preparation process of 6-oxo-8-chloro ethyl caprylate, and belongs to the field of industrial wastewater treatment and green production. The technical problem to be solved in the invention is to provide the method for treating aluminum-containing wastewater in a preparation process of 6-oxo-8-chloro ethyl caprylate. The method comprises the following steps: by taking aluminum trichloride as a catalyst, performing addition reaction on 6-oxo-6-oxo ethyl caproate and ethylene in a dichloroethane solution, and hydrolyzing the aluminum trichloride to prepare a target product. According to the technical scheme adopted by the invention, compared with the prior art, direction wastewater emission is avoided, and aluminum trichloride hexahydrate solids can be recycled, so that the method is very remarkable in saving water resources and achieving environmental friendliness.

Description

technical field [0001] The invention relates to a method for treating aluminum-containing wastewater in the preparation process of ethyl 6-oxo-8-chlorooctanoate, belonging to the fields of industrial wastewater treatment and green production. Background technique [0002] One of the synthetic methods of lipoic acid is to use adipic acid as the starting material, and the synthetic process includes processes such as esterification, acyl chloride, addition, reduction, chlorination, cyclization, hydrolysis and acidification. Among them, the addition reaction is 6-chloro-6-oxohexanoic acid ethyl ester obtained by esterification and acyl chloride of adipic acid, and ethylene addition reaction to prepare 6-oxo-8-chlorooctanoic acid ethyl ester, and then through Reduction and chlorination yield the intermediate 6,8-dichlorooctanoic acid ethyl ester. [0003] The addition reaction in the above process usually uses ethyl 6-chloro-6-oxohexanoate and ethylene as raw materials, uses alu...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C02F9/10C01F7/56C07C69/675C07C67/31C02F103/36
Inventor 袁跃华殷屹峰钱振青周小军陆惠刚
Owner JIANGSU TOHOPE PHARMA
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