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A kind of method for continuously synthesizing thiodiglycol

A technology for synthesizing thiodiethylene glycol and hydrogen sulfide, which is applied in the fields of sulfide preparation and organic chemistry, can solve the problems of long vacuum distillation time and low reaction yield, achieve short reaction residence time, high reaction efficiency, The effect of shortening the production cycle

Active Publication Date: 2017-08-04
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

[0027] A method for continuously synthesizing thiodiglycol, characterized in that the reaction is carried out in a tubular reactor, and the specific steps include:

[0028] Install and debug the reaction device, fill 30 mL of activated carbon-supported sodium bicarbonate catalyst in a 100 mL reaction tube, wet the catalyst with 50 g of solvent, prepare 500 g of a 20% mass fraction of ethylene oxide-thiodiglycol solution, and control the reaction temperature to 20 °C , the pressure is 0MPa, and ethylene oxide and hydrogen sulfide are fed at the same time, with a molar ratio of 1:2.05. The product passes through a tubular reactor equipped with a catalyst, and the temperature of the gas-liquid separation tank is controlled to 20 °C, and the ring is recovered in the gas-liquid separation tank. 4.1 g of oxyethane with a purity of 99.9%; purging with nitrogen to obtain 582.31 g of thiodiglycol with a content of 99.5% and a yield of 99.02% in terms of hydrogen sulfide.

Embodiment 2

[0030] A method for continuously synthesizing thiodiglycol, characterized in that the reaction is carried out in a tubular reactor, and the specific steps include:

[0031] 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 a 20% mass fraction of ethylene oxide-thiodiglycol solution, and control the reaction temperature to 40°C, The pressure is 0MPa, and ethylene oxide and hydrogen sulfide are introduced at the same time, and the molar ratio is 1:2.0. The product passes through a tubular reactor equipped with a catalyst, and the temperature of the gas-liquid separation tank is controlled to 20 °C, and the epoxy resin 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% in terms of hydrogen sulfide.

Embodiment 3

[0033] A method for continuously synthesizing thiodiglycol, characterized in that the reaction is carried out in a tubular reactor, and the specific steps include:

[0034] Install and debug the reaction device, fill 30 mL of activated carbon-supported potassium carbonate catalyst in a 100 mL reaction tube, wet the catalyst with 50 g of solvent, prepare 500 g of a 20% mass fraction of ethylene oxide-thiodiglycol solution, and control the reaction temperature to 0 °C. The pressure is 0MPa, and ethylene oxide and hydrogen sulfide are introduced at the same time, and the molar ratio is 1:2.3. The product passes through a tubular reactor equipped with a catalyst, and the temperature of the gas-liquid separation tank is controlled to 20 °C, and the epoxy resin is recovered in the gas-liquid separation tank. Ethane 9.9g, with a purity of 99.9%, was purged with nitrogen to obtain 574.31g 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. [0002] technical background [0003] Thiodiethylene glycol, molecular formula: C 4 H 10 SO 2 , From the perspective of molecular structure, thiodiglycol is not only a diol, 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 an intermediate for organic synthesis raw materials, thiodiglycol can be used to prepare plasticizers, rubber accelerators, antioxidants, preservatives, pesticides, herbicides, repellents, dye auxiliaries, inks and printing and dyeing auxiliaries agent, etc. It is widely used in industry as dye auxiliaries and antioxidants for rubber and plastics. In addition, it is also used in optical resin materials, metal surface treatment fluids, photographic film film developing and...

Claims

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Application Information

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Patent Type & Authority Patents(China)
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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