Preparation method of thiodiethanethiol

A technology of thiodiglycol and thiodiglycol, applied in thioether preparation, organic chemistry and other directions, can solve the problems of low product quality, difficult treatment, large amount of waste water, etc., to maximize resource value, The effect of maximizing comprehensive utilization and low energy consumption

Inactive Publication Date: 2018-05-04
SHANDONG EFIRM BIOCHEMISTRY & ENVIRONMENTAL PROTECTION CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the synthesis process of the prior art has shortcomings such as low product quality, low reaction yield, and a large amount of three wastes, especially a large amount of waste water, which is difficult to handle.

Method used

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  • Preparation method of thiodiethanethiol
  • Preparation method of thiodiethanethiol
  • Preparation method of thiodiethanethiol

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preparation example Construction

[0028] The invention provides a kind of preparation method of thiodiglycolyl mercaptan, comprises the following steps:

[0029] a) mixing thiodiglycol, thiourea and hydrochloric acid to perform a salt-forming reaction, and then adding an alkali solution to perform a hydrolysis reaction to obtain a reaction mixture;

[0030] b) Separating the reaction mixture obtained in step a) to obtain the crude thiodiglycol mercaptan and reaction waste water respectively; waste water;

[0031] c) performing flocculation treatment on the reaction waste water and washing waste water obtained in step b), respectively, to obtain recycled water.

[0032] In the invention, the thiodiglycol, thiourea and hydrochloric acid are firstly mixed for a salt-forming reaction, and then an alkali solution is added for a hydrolysis reaction to obtain a reaction mixture. In the present invention, the hydrochloric acid is preferably concentrated hydrochloric acid with a mass concentration of 37%. In the pre...

Embodiment 1

[0059] (1) The preparation of isothiourea hydrochloride: add 34g thiourea in the 250mL four-neck flask that thermometer, agitator, ventilation device are housed, start stirring, then add 34g mass concentration and be the concentrated hydrochloric acid of 37%, be warming up to Dissolve, then directly add 25g of thiodiethylene glycol, and heat up to reflux after adding; keep warm after reflux, take samples every 2h to follow up, if there is raw material thiodiethylene glycol, continue the heat preservation reaction, if there is no thiodiethylene glycol, then Stop the reaction, cool down;

[0060] (2) Hydrolysis of isothiourea hydrochloride: lower the temperature to below 60°C, add dropwise 300mL of 10% sodium hydroxide solution into the flask, then raise the temperature to 70°C, keep warm for 3h, and the reaction is completed to obtain a reaction mixture.

[0061] (3) Pour the reaction mixture obtained in step (2) into a separatory funnel and let stand for 30min to separate liqu...

Embodiment 2

[0066] (1) The preparation of isothiourea hydrochloride: add 35g thiourea in the 250mL four-neck flask that thermometer, agitator, ventilation device are housed, start stirring, then add 35g mass concentration and be the concentrated hydrochloric acid of 37%, be warming up to Dissolve, then directly add 25g of thiodiethylene glycol, and heat up to reflux after adding; keep warm after reflux, take samples every 2h to follow up, if there is raw material thiodiethylene glycol, continue the heat preservation reaction, if there is no thiodiethylene glycol, then Stop the reaction, cool down;

[0067] (2) Hydrolysis of isothiourea hydrochloride: lower the temperature to below 60°C, add dropwise 300mL of 10% sodium hydroxide solution into the flask, then raise the temperature to 70°C, keep warm for 3h, and the reaction is completed to obtain a reaction mixture.

[0068](3) Pour the reaction mixture obtained in step (2) into a separatory funnel and let stand for 30min to separate liqui...

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Abstract

The invention provides a preparation method of thiodiethanethiol. The preparation method comprises the following steps: a) mixing thiodiglycol, thiourea and hydrochloric acid to carry out a salt forming reaction and then adding an alkaline solution for hydrolysis reaction to obtain a reaction mixture; b) skimming the reaction mixture obtained in the step a) to separately obtain a thiodiethanethiolcoarse product and reaction wastewater; and then washing the thiodiethanethiol coarse product to separately obtain thiodiethanethiol and washing waste water; and c) separately flocculating the reaction waste water and the washing waste water obtained in the step b) to obtain circulating water. Compared with the prior art, the preparation method provided by the invention has relatively high product quality and yield, and can achieve circular use of waste water. Experimental results verify that the content of thiodiethanethiol prepared by the preparation method is stabilized at over 99%, and the yield is over 98%, and zero discharge of the waste water is achieved.

Description

technical field [0001] The invention relates to the technical field of organic synthesis, and more specifically, relates to a preparation method of thiodiglycol mercaptan. Background technique [0002] Thiodiglycol mercaptan is a kind of organic compound with special unpleasant smell, and its structure is shown in formula (I): [0003] [0004] It is often used as an intermediate product in the synthesis of other sulfur-containing organic compounds, and is especially suitable for the synthesis of thioethers, thioesters, maple and maple. Thiodiglycol thiol is widely used in chemical reagents, fine chemicals, pharmaceutical intermediates, material intermediates, etc. in industry. [0005] The application fields of thiodiglycol mercaptan mainly include: sulfur-containing organic compound intermediates, chemical reagents, dye cosolvent printing and dyeing industry, optical resin for lenses, etc. Application of sulfur-containing organic compound intermediates: Thiodiglycol m...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C319/20C07C321/14
CPCC07C319/20C07C321/14
Inventor 高德振马韵升陈梅梅张建林常忠臣郭龙龙易先君
Owner SHANDONG EFIRM BIOCHEMISTRY & ENVIRONMENTAL PROTECTION CO LTD
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