Method for preparing methyl mercaptan through reaction of methyl chloride and hydrogen sulfide

A technology of hydrogen sulfide and methyl chloride, applied in mercaptan preparation, organic chemistry, etc., can solve the problems of many by-products, low yield, difficult to handle, etc., and achieve the effects of great economic significance, high product purity, and simple operation

Inactive Publication Date: 2018-08-24
山东祥维斯生物科技股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0010] At the same time, the method of preparing methyl mercaptan with sodium hydrosulfide and dimethyl sulfate is widely used at present, and a large amount of waste water is generated in the production process, which is difficult to treat and does not conform to the concept of "green chemistry"
[0011] In small-scale production, there is a reaction between methyl chloride and hydrogen sulfide in sodium hydroxide solution, but there are many by-products, low yield and pollution.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0042] A method for producing methyl mercaptan from methyl chloride hydrogen sulfide, said method comprising the steps of:

[0043] (1) Add catalyst, replace and remove the air in the reactor with nitrogen, wherein the reactor adopts a fixed bed reactor, which is equipped with gamma-alumina as a carrier impregnated with a tungsten-containing metal ion solution, and calcined at high temperature to fix the catalyst bed, the calcination temperature is 800°C;

[0044] (2) feed reaction gas chloromethane and gas hydrogen sulfide, gas chloromethane and hydrogen sulfide mol ratio are CH 3 Cl:H 2 S=1:1.1, control reaction temperature 260 ℃, pressure 0.8MPa, carry out reaction, the reaction time of mixed gas in the reactor is 13min;

[0045] (2) After the reaction, adjust the pressure to 0.7 MPa, lower the temperature to 20° C., separate the product, and obtain high-purity methyl mercaptan and by-product hydrogen chloride through gas-liquid separation.

[0046] 821g of methyl mercapta...

Embodiment 2

[0048] A method for producing methyl mercaptan from methyl chloride hydrogen sulfide, said method comprising the steps of:

[0049] (1) Add catalyst, replace and remove the air in the reactor with nitrogen, wherein the reactor adopts a fixed bed reactor, which is equipped with gamma-alumina as a carrier impregnated with a tungsten-containing metal ion solution, and calcined at high temperature to fix the catalyst bed, the calcination temperature is 1200°C;

[0050] (2) feed reaction gas chloromethane and gas hydrogen sulfide, gas chloromethane and hydrogen sulfide mol ratio are CH 3 Cl:H 2 S=1:1.2, control reaction temperature 320 ℃, pressure 1.5MPa, carry out reaction, the reaction time of mixed gas in reactor is 1min;

[0051] (2) After the reaction, adjust the pressure to 0.9MPa, lower the temperature to 30°C, separate the product, and obtain high-purity methyl mercaptan and by-product hydrogen chloride through gas-liquid separation.

[0052] 827g of methyl mercaptan, 61...

Embodiment 3

[0054] A method for producing methyl mercaptan from methyl chloride hydrogen sulfide, said method comprising the steps of:

[0055] (1) Add catalyst, replace and remove the air in the reactor with nitrogen, wherein the reactor adopts a fixed bed reactor, which is equipped with gamma-alumina as a carrier impregnated with a tungsten-containing metal ion solution, and calcined at high temperature to fix the catalyst bed, the calcination temperature is 1000°C;

[0056] (2) Raise the temperature to 100°C, feed methyl chloride gas into the reactor, continue to heat up to 150°C, and start feeding hydrogen sulfide gas; the molar ratio of methyl chloride to hydrogen sulfide is 1:1, control the reaction temperature to 290°C, and the pressure 1.1MPa, for reaction, the reaction time of the mixed gas in the reactor is 15min;

[0057] (2) After the reaction, adjust the pressure to 0.8MPa, lower the temperature to 25°C, separate the product, and obtain high-purity methyl mercaptan and by-pr...

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Abstract

The invention discloses a method for preparing methyl mercaptan through a reaction of methyl chloride and hydrogen sulfide. The method comprises the following steps: inflating quantitative methyl chloride and hydrogen sulfide gas into a reactor in which a catalyst is added, and performing a chemical reaction at a certain temperature and under a certain pressure, cooling after the completion of thereaction, and separating to obtain the methyl mercaptan. By the method, the gas-gas reaction is adopted, the operation is simple, a target product has high selectivity and high purity, no waste wateris produced in the process, the pollution is low and a byproduct is mainly hydrogen chloride which can be sold as a product, so that the method has a relatively great economic significance.

Description

technical field [0001] The invention relates to the technical field of preparation methods of methyl mercaptan, in particular to a method for preparing methyl mercaptan by reacting methyl chloride and hydrogen sulfide. Background technique [0002] Methyl mercaptan is a colorless gas at normal temperature and pressure. It has an unpleasant smell. It is insoluble in water and soluble in organic solvents such as ethanol and ether. It is used as a raw material and catalyst for organic synthesis and pesticides. The market demand big. In industry, it is often produced by the action of methanol and hydrogen sulfide, or by the reaction of sodium hydrogen sulfide and dimethyl sulfate, but both production methods produce a large amount of waste water, and the treatment cost is high. [0003] The patent application No. 97123454.X relates to a method for continuous production of methyl mercaptan, comprising making a feed gas mixture of methanol and hydrogen sulfide in an atmosphere co...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C319/02C07C321/04
CPCC07C319/02C07C321/04
Inventor 马琳李越王守忠张钦太韩强毛秀立孟东霞梁新新
Owner 山东祥维斯生物科技股份有限公司
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