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High-value utilization method of sodium 2-mercaptoacetate in thionocarbamate production tail liquid

A technology of sodium thioglycolate and sodium thioacetate, which is applied in organic chemistry, solid separation, flotation, etc., can solve the problems that cannot completely solve the problem of 2-thioglycolate tail liquid accumulation and limited market, and achieve excellent extraction performance , Increase the effect of chelating ability

Active Publication Date: 2021-08-10
HUNAN UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although the above two methods can consume a certain amount of sodium 2-thioglycolate tail liquid, due to the limited market of copper-molybdenum separation inhibitor and isooctyl thioglycolate, they still cannot completely solve the accumulation of sodium 2-thioglycolate tail liquid question

Method used

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  • High-value utilization method of sodium 2-mercaptoacetate in thionocarbamate production tail liquid
  • High-value utilization method of sodium 2-mercaptoacetate in thionocarbamate production tail liquid
  • High-value utilization method of sodium 2-mercaptoacetate in thionocarbamate production tail liquid

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0079] Example 1: Preparation of sodium 2-mercaptoacetate during the preparation of O-isopropyl-N-ethylthiocarbamate (Z-200)

[0080] Add 9.5 parts of 2-chloroacetic acid with a purity of 99% into the reaction vessel, then add 30 parts of distilled water to completely dissolve the 2-chloroacetic acid, and add 5.9 parts of Na with a purity of 99.8% in batches 2 CO 3 When the pH of the solution is about 8.0 (±0.1), add 18.59 parts of sodium isopropylxanthate with a purity of 85.0%, stir magnetically while adding, and heat up to 80°C for 2 hours after the addition. Cool the reaction solution below 20°C, add 6.76 g of ethylamine aqueous solution with a purity of 68% to 72% dropwise with a constant pressure dropping funnel, stir magnetically while adding, raise the temperature to 70°C after the dropwise addition, and react for 1 hour , cooled to room temperature, and separated to obtain 14.38 parts of the Z-200 product as a light yellow oil in the upper layer, and 55.64 parts of a...

Embodiment 2

[0081]Embodiment 2: Preparation of S-carboxyethyl-N-benzoyl dithiocarbamate

[0082] Add 1.15 parts of PEG-400 with a purity of 99%, 11.83 parts of KSCN with a purity of 98.5% and 80 parts of dichloromethane with a purity of 99% into a 250mL three-necked flask, stir at 10°C for 10 minutes, and then add 13.63 A portion of benzoyl chloride with a purity of 99% was heated up to 25° C. for 3.5 hours. After the reaction, the salt was removed by filtration, the dichloromethane was recovered by rotary evaporation, and 55.64 parts of the aqueous solution of sodium 2-mercaptoacetate with a purity of 19.66% obtained in Example 1 were transferred to a reaction vessel, and the temperature was raised to 35° C. for 4 hours. After the reaction, add concentrated sulfuric acid to acidify, and filter to obtain a yellow solid that is the crude product of S-carboxyethyl-N-benzoyl dithiocarbamate. The product purity is 83.34%, based on the yield of sodium 2-mercaptoacetate was 85.21%. The crude ...

Embodiment 3

[0083] Embodiment 3: Preparation of S-carboxyethyl-N-octanoyl dithiocarbamate

[0084] Add 1.15 parts of PEG-400 with a purity of 99%, 11.83 parts of KSCN with a purity of 98.5% and 80 parts of dichloromethane with a purity of 99% into a 250mL three-necked flask, stir at 10°C for 10 minutes, and then add 15.77 A portion of octanoyl chloride with a purity of 99% was heated to 40° C. for 3.5 hours. After the reaction, the salt was removed by filtration, the dichloromethane was recovered by rotary evaporation, and 55.64 parts of the aqueous solution of sodium 2-mercaptoacetate with a purity of 19.66% obtained in Example 1 were transferred to a reaction vessel, and the temperature was raised to 35° C. for 4 hours. After the reaction, add concentrated sulfuric acid to acidify, and filter to obtain a yellow solid, which is the crude product of S-carboxyethyl-N-octanoyl dithiocarbamate. The product purity is 82.22%, and the yield based on 2-mercaptoacetate sodium is 83.92%. The cru...

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Abstract

The invention belongs to wastewater treatment, and particularly discloses a high-value utilization method of sodium 2-mercaptoacetate in thionocarbamate production tail liquid. According to the method, sodium 2-mercaptoacetate in the thionocarbamate production tail liquid is used as a raw material and reacts with thiocyanate and a halogenating reagent to obtain the S-carboxyethyl-N-alkanoyl dithiocarbamate. The method is simple to operate and high in efficiency, solves the problem that the sodium 2-mercaptoacetate in the thionocarbamate production tail liquid is difficult to recover, and can realize high-value utilization of the sodium 2-mercaptoacetate.

Description

technical field [0001] The invention belongs to the field of waste water utilization, and relates to a method for high-value utilization of sodium 2-mercaptoacetate in the tail liquid of thiourethane production. Background technique [0002] Thiurethane is currently one of the most widely used copper-sulfur separation collectors. Compared with traditional xanthate and black medicine, thiourethane has better selectivity to minerals, and can realize flotation separation of minerals in a lower pH medium, which can reduce the flotation pH in the flotation process and avoid high Corrosion of equipment and inhibition of precious metal minerals by alkaline conditions. Therefore, thiourethane is a very valuable sulfide ore flotation collector. [0003] There are many synthetic methods of thiourethane. Among them, the esterification and ammonolysis of xanthate are the main methods for the production of thiourethane due to the advantages of wide sources of raw materials, simple pro...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C333/26B03D1/012B03D101/02
CPCC07C333/26B03D1/012B03D2201/02Y02P10/20
Inventor 黄小平曾坚贤周虎薛建荣刘国清
Owner HUNAN UNIV OF SCI & TECH
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