Method for preparing methane chloride by dimethyl sulfate

A technology of dimethyl sulfate and monochloromethane, which is applied in the preparation of halogenated hydrocarbons, chemical instruments and methods, organic chemistry, etc., can solve the problems of low economic benefit, low concentration, influence on utilization, etc., and achieves remarkable economic benefits, Simple process and low energy consumption

Inactive Publication Date: 2010-01-27
HANERGY TECH
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Although the present invention has processed dimethyl sulfate and carried out resource recovery, the concentrations of the obtained

Method used

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  • Method for preparing methane chloride by dimethyl sulfate

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Experimental program
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Effect test

Embodiment 1

[0017] Mix 1 mol of dimethyl sulfate with 98.3wt% concentrated sulfuric acid, and the ratio of dimethyl sulfate to sulfuric acid is 1:1. Put the mixture into a flask, heat it to 100°C, and then pass in hydrogen chloride gas to react for 8 hours. The generated gas is washed with water, washed with alkali, and dried to obtain the product gas. Wherein the rate of the hydrogen chloride that feeds is 1mol / h, and the used lye of alkali washing is the sodium hydroxide solution of 5wt%.

[0018] The generated gas was detected, and the conversion rate of dimethyl sulfate was calculated to be 54.6%, the yield of monochloromethane was 54.6%, and the purity of monochloromethane was 99.1%.

Embodiment 2

[0020] Mix 0.5mol dimethyl sulfate with 95wt% concentrated sulfuric acid, the ratio of dimethyl sulfate to sulfuric acid is 1:1. Put the mixture into a three-necked flask, heat it to 120°C, and then pass in hydrogen chloride gas to react for 10 hours. The generated gas is washed with water, washed with alkali, and dried to obtain the product gas. Wherein the rate of the hydrogen chloride that feeds is 1mol / h, and the lye used for alkali washing is 10wt% sodium hydroxide solution.

[0021] The generated gas was detected, and the conversion rate of dimethyl sulfate was calculated to be 76.7%, the yield of monochloromethane was 76.7%, and the purity of monochloromethane was 99.4%.

Embodiment 3

[0023] Put 0.8 mol of dimethyl sulfate into a three-necked flask, heat it to 60°C, and inject hydrogen chloride gas to react for 0.5 h. The generated gas is washed with water, washed with alkali, and dried to obtain product gas. Wherein the rate of the hydrogen chloride that feeds is 8mol / h, and the used lye of alkali washing is the sodium hydroxide solution of 15wt%.

[0024] The generated gas was detected, and the conversion ratio of dimethyl sulfate was calculated to be 32.3%, the yield of monochloromethane was 32.3%, and the purity of monochloromethane was 99.5%.

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Abstract

The invention discloses a method for preparing methane chloride by dimethyl sulfate, dimethyl sulfate is taken as a raw material, hydrogen chloride gas is led into dimethyl sulfate solution, and methane chloride is generated by reacting for 0.5-10h at 60-180 DEG C; and the amount of substance of hydrogen chloride gas led into dimethyl sulfate solution per hour is 1-10 times that of substance of dimethyl sulfate. The invention has the advantages of mild reaction condition, simple technical process, capability of carrying out effective harmless treatment on dimethyl sulfate and higher economic benefit, belonging to the field of preparation of methane chloride.

Description

technical field [0001] The invention relates to a method for preparing monochloromethane, in particular to a method for preparing monochloromethane using dimethyl sulfate as a raw material. Background technique [0002] From the perspective of the preparation of monochloromethane, there are currently two main methods for the industrial production of monochloromethane: methane chlorination and methanol hydrochlorination. [0003] The methane chlorination method is to chlorinate methane and chlorine at a high temperature of 400 ° C. The chlorination product is absorbed by water to remove hydrogen chloride, and then the unreacted methane is separated by compression and condensation, and then the methyl chloride and polychloride are fractionated. The methane chlorination method is suitable for the production of polychlorides, and this method is generally not used for the single production of methyl chloride. [0004] The methanol hydrochlorination method is to mix hydrogen chlo...

Claims

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Application Information

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IPC IPC(8): C07C19/03C07C17/093
Inventor 肖钢侯晓峰李波王波
Owner HANERGY TECH
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