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Method for treating boron-containing wastewater in 6-hydroxyl-8-chloro ethyl caprylate preparation process

A treatment method and waste water technology, applied in the direction of neutralized water/sewage treatment, natural water treatment, chemical instruments and methods, etc., can solve problems such as inability to form recycling, few application fields of potassium metaborate, and difficulties in market sales, etc., to achieve Avoid the direct discharge of waste water, easy to recycle, and the effect of simple method

Inactive Publication Date: 2018-05-29
JIANGSU TOHOPE PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Potassium metaborate has very few application fields, and is mainly used as an additive for lubricating oils. It is difficult to sell in the market and cannot be effectively recycled.

Method used

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  • Method for treating boron-containing wastewater in 6-hydroxyl-8-chloro ethyl caprylate preparation process

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] Dissolve 100Kg of ethyl 6-oxo-8-chlorooctanoate in 500Kg of dichloroethane, add 1kg of tetrabutylammonium bromide, add potassium borohydride ammonia solution dropwise below 35°C (16kg potassium borohydride+48g17% ammonia water ), control the internal temperature below 35°C, and keep warm for 3 hours. The organic layer was washed with water to neutrality, concentrated under reduced pressure at 0.1MPa, until the temperature was 110°C, and 95kg of 6-hydroxy-8-chlorooctanoic acid ethyl ester concentrate with a content of 91% was obtained.

[0023] Recover 35kg of 10% ammonia water in the water phase at 100°C, add 32kg of water, add 30% hydrochloric acid dropwise at 50-55°C, until pH 1, keep warm for 3 hours, filter to obtain 18Kg of boric acid, dry at 80°C to obtain 15Kg, with a purity of 99.2%. After filtering boric acid, distill 20kg of water from the solution, cool to 10°C, and keep warm for 2 hours to obtain 14.8Kg of potassium chloride by filtration, and dry at 90°C to...

Embodiment 2

[0025] Dissolve 100Kg of ethyl 6-oxo-8-chlorooctanoate in 500Kg of dichloroethane, add 1kg of tetrabutylammonium bromide, add potassium borohydride ammonia solution (16kg potassium borohydride+48kg17% ammonia water) dropwise below 35°C ), control the internal temperature below 35°C, and keep warm for 3 hours. The organic layer was washed with water to neutrality, concentrated under reduced pressure at 0.1MPa until the temperature reached 110°C, and 96kg of concentrated solution of 6-hydroxy-8-chlorooctanoic acid ethyl ester with a content of 92% was obtained.

[0026] Recover 30kg of 10% ammonia water in the water layer at 100°C, add 48kg of water, add 30% hydrochloric acid dropwise at 50-55°C to pH 2, keep warm for 2.5 hours, filter to obtain 18.4Kg of boric acid, and dry at 80°C to obtain 16Kg with a purity of 99.6%. After filtering the boric acid, distill 36kg of water from the solution, cool to 20°C, and keep warm for 2 hours to obtain 17.2Kg of potassium chloride by filtr...

Embodiment 3

[0028] Dissolve 100Kg of ethyl 6-oxo-8-chlorooctanoate in 500Kg of dichloroethane, add 1kg of tetrabutylammonium bromide, add potassium borohydride ammonia solution (16kg potassium borohydride+48kg17% ammonia water) dropwise below 35°C ), control the internal temperature below 35°C, and keep warm for 3 hours. The organic layer was washed with water to neutrality, concentrated under reduced pressure at 0.1MPa, until the temperature was 110°C, and 95kg of 6-hydroxy-8-chlorooctanoic acid ethyl ester concentrate with a content of 93% was obtained.

[0029] Recover 32kg of 10% ammonia water in the water layer at 100°C, add 40kg of water, add 30% hydrochloric acid dropwise at 50-55°C to pH 1.5, keep warm for 3 hours, filter to obtain 18Kg of boric acid, and dry at 80°C to obtain 15.6Kg with a purity of 99.8%. After filtering the boric acid, the solution was combined with 40 kg of potassium chloride mother liquor of Example 2, steamed off 48 kg of water, cooled to 15° C., kept warm f...

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Abstract

The invention relates to a method for treating boron-containing wastewater in a 6-hydroxyl-8-chloro ethyl caprylate preparation process. According to the method for treating boron-containing wastewater in a 6-oxo-8-chloro ethyl caprylate preparation process, tetrabutylammonium bromide is used as a catalyst, a 6-oxo-8-chloro ethyl caprylate dichloroethane solution and a potassium borohydride ammonia water solution are subjected to a mixed reaction, 6-hydroxyl-8-chloro ethyl caprylate is obtained from the organic layer after the reaction, and ammonia water is recovered by concentrating the layer; and the method for treating boron-containing wastewater comprises: 1, after recovering the ammonia water, adding a proper amount of water, and adding an inorganic acid in a dropwise manner to acidify until the pH value is 1-2; 2, precipitating boric acid solid, filtering, drying the solid, and recovering; 3, evaporating the filtered boric acid mother liquor to remove a proper amount of water, cooling to a temperature of less than 30 DEG C, precipitating a potassium salt solid, drying the solid, and recovering; and 4, applying the mother liquor obtained in the step 3.

Description

technical field [0001] The invention relates to a method for treating boron-containing wastewater in the preparation process of ethyl 6-hydroxy-8-chlorooctanoate, belonging to the fields of industrial wastewater treatment and green production. Background technique [0002] At present, the main method for preparing lipoic acid in the industry at home and abroad is to react cyclization of ethyl 6,8-dichlorooctanoate with sodium sulfide and sulfur, and obtain it through alkaline hydrolysis and acidification with hydrochloric acid. Therefore, ethyl 6,8-dichlorooctanoate is the key intermediate for the preparation of lipoic acid. Its synthesis is based on adipic acid as the starting material, and undergoes processes such as esterification, acyl chloride, addition, reduction, and chlorination. Among them, the reduction of 6-oxo-8-chlorooctanoic acid ethyl ester to prepare 6-hydroxy-8-chlorooctanoic acid ethyl ester process mainly uses 6-oxo-8-chlorooctanoic acid ethyl ester and se...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C02F9/10C01B35/10C01D3/06C02F101/10C02F103/36
CPCC01B35/1045C01D3/06C02F1/04C02F1/52C02F1/66C02F9/00C02F2101/108C02F2103/36
Inventor 陆惠刚周小军袁跃华
Owner JIANGSU TOHOPE PHARMA
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