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Preparation method of thiodiethanethiol

A technology of thiodiglycol thiol and thiodiglycol, which is applied in the preparation of thioether, organic chemistry, etc., can solve the problems of high waste water treatment cost, large amount of waste water generation, low atom utilization rate, etc., and achieve easy operation , sufficient reaction and high synthesis efficiency

Active Publication Date: 2020-01-07
SHANDONG EFIRM BIOCHEMISTRY & ENVIRONMENTAL PROTECTION CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The existing technology needs to convert thiodiethylene glycol into isothiouronium salt first, and then carry out alkaline hydrolysis with alkali to generate a crude product. The crude product is washed with water, distilled, adsorbed, and filtered to obtain the final product. This process is complicated and uses more raw materials. , the utilization rate of atoms is extremely low; the amount of waste water is relatively large, about 6 tons of waste water per ton of product, the cost of waste water treatment is high, and the pressure on environmental protection is great

Method used

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  • Preparation method of thiodiethanethiol

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] Fill the fixed bed reactor with 20ml of prepared cobalt catalyst, fill evenly, connect the pipeline, open the hydrogen sulfide cylinder, control the pressure to 0.6MPa through the pressure reducing valve, and control the flow rate to 20L / h (the space velocity is 1000h -1 ), replaced for 10 minutes, opened the thiodiglycol feed pump, and the flow control was 21.8g / hour (the mol ratio of hydrogen sulfide to thiodiglycol was 5), and the reaction temperature was controlled by the reactor jacket to be 120°C. Sampling was started after 60 minutes of reaction, and the detected product content was 99.6%, and the product yield from the first hour to the second hour was 98.6%.

Embodiment 2

[0022] Fill the fixed-bed reactor with 20ml of prepared molybdenum catalyst, fill evenly, connect the pipeline, open the hydrogen sulfide cylinder, control the pressure to 0.2MPa through the pressure reducing valve, and control the flow rate to 20L / h (the space velocity is 1000h -1 ), replaced for 10 minutes, opened the thiodiglycol feed pump, and the flow control was 21.8g / hour (the mol ratio of hydrogen sulfide to thiodiglycol was 4), and the reaction temperature was controlled by the reactor jacket to be 120°C. Sampling was started after 60 minutes of reaction, the detected product content was 99.0%, and the product yield from the first hour to the second hour was 97.2%.

Embodiment 3

[0024] Fill the cobalt and molybdenum catalyst prepared by 20ml in the fixed-bed reactor, fill evenly, connect the pipeline, open the hydrogen sulfide cylinder, control the pressure to be 0.6MPa through the pressure reducing valve, flow control 40L / h (space velocity is 2000h -1 ), replacement for 10 minutes, open the thiodiglycol feed pump, flow control is 43.6g / hour (hydrogen sulfide and thiodiglycol mol ratio is 5), the reaction temperature is 120 ℃ by reactor jacket control, Sampling began after 60 minutes of reaction, and the detected product content was 98.7%, and the product yield from the first hour to the second hour was 96.9%.

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Abstract

The invention belongs to the technical field of organic synthesis, and particularly relates to a preparation method of thiodiethanethiol, wherein the preparation method particularly comprises the steps: introducing thiodiethylene glycol and hydrogen sulfide into a mixer, sufficiently mixing, carrying out pressurized introduction of the thiodiethylene glycol by a pump, and introducing the hydrogensulfide under the reduced pressure by a steel cylinder; enabling the uniformly mixed raw materials to pass through a fixed bed reactor filled with a catalyst from bottom to top, and carrying out a reaction of thiodiethylene glycol with hydrogen sulfide to generate thiodiethanethiol; and enabling the reacted product and unreacted hydrogen sulfide to enter a separator, pressurizing the hydrogen sulfide from the upper part of the separator for recycling, and producing the product from the lower part of the separator. The hydrogen sulfide is adopted to replace thiourea, hydrochloric acid, alkali and other chemicals in the original process, the cost is reduced, no three wastes are generated, the fixed bed reactor is adopted, the device is a continuous reaction device, the operation is simple, the reaction is sufficient, and side reactions are reduced.

Description

technical field [0001] The invention belongs to the technical field of organic synthesis, and more specifically relates to a preparation method of thiodiglycol mercaptan. Background technique [0002] Thiodiglycol thiol is an organic compound containing two mercapto groups, which is mainly used to prepare optical resin materials, and its structural formula is The existing synthesis of thiodiglycol mercaptan is realized by the following technology: the raw material thiodiglycol is refluxed with a certain ratio of thiourea and hydrochloric acid, the temperature is about 110°C, and the reaction time is 2-5 hours. Generate isothiourea salt of thiodiethylene glycol, add lye to the generated isothiourea salt, carry out alkaline hydrolysis reaction at 40-80°C to generate the target product, and then separate the product from the water phase through liquid separation , The product is prepared through the process of washing, distillation, adsorption, filtration and other processes ...

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 梁万根张超崔卫华孙志利费潇瑶许倩倩周芳晶靖培培刘龙飞
Owner SHANDONG EFIRM BIOCHEMISTRY & ENVIRONMENTAL PROTECTION CO LTD
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