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Method for continuously synthesizing thiodiglycol

A technology for synthesizing thiodiglycol and hydrogen sulfide, which is applied in sulfide preparation, organic chemistry and other directions, can solve the problems of low reaction yield, long vacuum distillation time, etc., and achieves high reaction efficiency, short reaction residence time, The effect of reducing production costs

Active Publication Date: 2016-03-16
SHANDONG EFIRM BIOCHEMISTRY & ENVIRONMENTAL PROTECTION CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

But this method also has its limitations, for example: adjust the pH value with concentrated hydrochloric acid after the reaction is completed, and concentrated hydrochloric acid and thiodiglycol will react under certain conditions to generate a kind of erosive poison, which is harmful to the eyes, respiratory tract and skin. Effect; the reaction uses water as a solvent. After the reaction is completed, there is more water in the solution, and the vacuum distillation time is longer; the reaction yield is only 79% to 86%. Diethylene glycol, the yield increased to 85% to 90%

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] A method for continuously synthesizing thiodiglycol is characterized in that it reacts in a tubular reactor, and the specific steps include:

[0027] Install and debug the reaction device, fill 30mL of activated carbon-supported sodium bicarbonate catalyst in a 100mL reaction tube, use 50g of solvent to wet the catalyst, prepare 500g of ethylene oxide-thiodiglycol solution with a mass fraction of 20%, and control the reaction temperature at 20°C , pressure 0MPa, feed ethylene oxide and hydrogen sulfide at the same time, the molar ratio is 1:2.05, the product passes through a tubular reactor equipped with a catalyst, the temperature of the gas-liquid separation tank is controlled at 20°C, and the ring is recovered in the gas-liquid separation tank Oxyethane 4.1g, purity 99.9%; thiodiglycol 582.31g, content 99.5%, yield 99.02% based on hydrogen sulfide was obtained by purging with nitrogen.

Embodiment 2

[0029] A method for continuously synthesizing thiodiglycol is characterized in that it reacts in a tubular reactor, and the specific steps include:

[0030] Install and debug the reaction device, fill 36mL of activated carbon-supported sodium carbonate catalyst in a 100mL reaction tube, use 50g of solvent to wet the catalyst, prepare 500g of ethylene oxide-thiodiglycol solution with a mass fraction of 20%, and control the reaction temperature at 40°C. The pressure is 0MPa, feed ethylene oxide and hydrogen sulfide at the same time, the molar ratio is 1:2.0, the product passes through the tubular reactor equipped with catalyst, the temperature of the gas-liquid separation tank is controlled at 20°C, and epoxy is recovered in the gas-liquid separation tank 8.6 g of ethane, with a purity of 99.9%, was purged with nitrogen to obtain 568.67 g of thiodiglycol, with a content of 98.4%, and a yield of 92.15% based on hydrogen sulfide.

Embodiment 3

[0032] A method for continuously synthesizing thiodiglycol is characterized in that it reacts in a tubular reactor, and the specific steps include:

[0033] Install and debug the reaction device, fill 30mL of activated carbon-supported potassium carbonate catalyst in a 100mL reaction tube, use 50g of solvent to wet the catalyst, prepare 500g of ethylene oxide-thiodiglycol solution with a mass fraction of 20%, and control the reaction temperature at 0°C. The pressure is 0MPa, feed ethylene oxide and hydrogen sulfide at the same time, the molar ratio is 1:2.3, the product passes through the tubular reactor equipped with catalyst, the temperature of the gas-liquid separation tank is controlled at 20°C, and epoxy is recovered in the gas-liquid separation tank 9.9 g of ethane, with a purity of 99.9%, was purged with nitrogen to obtain 574.31 g of thiodiglycol, with a content of 98.0%, and a yield of 97.53% in terms of hydrogen sulfide.

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Abstract

The invention discloses a method for continuously synthesizing thiodiglycol. The method is based on a tubular reactor, ethylene oxide and sulfureted hydrogen serve as raw materials, the reaction is performed at 0-40 DEG C, and thiodiglycol is synthesized by liquid phase catalysis at normal temperature and normal pressure. The operation is simple, the conditions are mild, the method is green, environmentally friendly and free of three wastes, and a catalyst can be reused; the reaction standing time is short, no back-mixing occurs, no by-product is generated, slightly excessive ethylene oxide can be recycled, the production cycle is shortened, and the production cost is reduced. The tubular reactor can react continuously, the product purity can reach 98-99.5%, and the yield of thiodiglycol can reach 92-99% according to hydrogen sulfide.

Description

technical field [0001] The invention belongs to the technical field of organic synthesis, and relates to a method for continuously synthesizing thiodiglycol. technical background [0002] Thiodiethylene glycol, molecular formula: C 4 h 10 SO 2 , From the perspective of molecular structure, thiodiethylene glycol is not only a glycol, but also a water-soluble thioether, so it can be used to synthesize functional solvents, surfactants, or new materials with several functions at the same time. As a solvent and organic synthesis raw material intermediate, thiodiethylene glycol can be used to prepare plasticizers, rubber accelerators, antiaging agents, preservatives, insecticides, herbicides, repellents, dye auxiliaries, inks and printing and dyeing auxiliaries agent etc. It is widely used in dyeing auxiliaries and antioxidants of rubber and plastics in industry. In addition, it is also used in optical resin materials, metal surface treatment fluids, photosensitizers for deve...

Claims

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Application Information

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IPC IPC(8): C07C323/12C07C319/14
CPCC07C319/14C07C323/12
Inventor 高艳丽刘龙飞袁新洁张建林常忠臣韩立霞
Owner SHANDONG EFIRM BIOCHEMISTRY & ENVIRONMENTAL PROTECTION CO LTD
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