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Method and device for producing dimethyl disulfide through oxidation of methyl mercaptan salt solution

A technology of dimethyl disulfide and methyl mercaptan, which is applied in the field of organic chemical industry, can solve the problems of high product purification cost, complex operating conditions, difficulty in controlling the degree of oxidation, etc., achieves continuous production and automatic control, and simple process flow , the effect of easy continuous production and automatic control

Inactive Publication Date: 2015-12-23
HUBEI XINGFA CHEM GRP CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The operating conditions of this method are complicated in actual production, and it is difficult to control the degree of oxidation, so excessive oxidation products such as sulfate radicals and methanesulfonic acid will be generated, resulting in high product purification costs
In addition, there is a certain safety risk in the direct contact and mixing of methyl mercaptan and oxygen

Method used

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  • Method and device for producing dimethyl disulfide through oxidation of methyl mercaptan salt solution

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] In a 1000ml four-necked flask equipped with a magnetic stirrer, add 500ml of an aqueous solution containing 10% to 20%wt of sodium methyl mercaptide, 0.1% to 5%wt of free alkali (calculated as NaOH), and 50 to 150ppm of a Co catalyst, Under the conditions of heating and stirring in a water bath at 50°C to 100°C, pure oxygen was continuously introduced into the solution through the gas distribution head, and the reaction stopped after 60 minutes. g oil. After chromatographic analysis, the components of the oily substance are: 99.7% of dimethyl disulfide, 0.1% of methyl sulfide, and 0.2% of water.

Embodiment 2

[0030] In a simulated tower with a height of 4.5 meters, an inner diameter of 50 mm, and filled with saddle ring fillers and a hot water jacket, 5000 ml of industrial liquid caustic soda with 10% to 30% wt of sodium hydroxide is charged from the bottom of the tower to the liquid Methyl mercaptan gas is passed into the alkali to carry out absorption reaction, and the aeration is stopped when methyl mercaptan components appear in the tail gas at the top of the tower, and then 0.5-5g of Co-containing catalyst is dissolved in the solution, and then the gas is passed into the jacket of the simulated tower. Warm up the solution to 70°C with hot water, continuously feed oxygen-enriched air with an oxygen content of 25% to 80%wt into the solution from the bottom of the tower, keep the reaction pressure at 0.1 to 0.3MPa, and the temperature at 70 to 90°C; stop after 30 minutes Introduce oxygen-enriched air, cool down the simulated tower, take out the liquid in the tower and let it stand...

Embodiment 3

[0032] The remaining solution after the oxidation reaction in Example 2 was left to stand for stratification and liquid separation was reacted with an appropriate amount of methyl mercaptan to obtain an aqueous solution containing 5% to 25% wt of sodium methyl mercaptan and 10% to 20% wt of free alkali. This solution is sent in the simulated tower described in embodiment 2, under the condition of 80 ℃, 0.1MPa, pass through the oxygen-enriched air of oxygen content 25%~99%wt, after oxidation reaction 15 minutes, the simulated tower is cooled , The liquid in the tower was taken out and allowed to stand for stratification to obtain 471.0 g of oily substance, the components of which were 99.6% of dimethyl disulfide, 0.2% of methyl sulfide, and 0.2% of water. After rectification of the oil, a light yellow transparent liquid is obtained, and the components are 99.9% of dimethyl disulfide and 0.1% of water.

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Abstract

The invention discloses a method and device for producing dimethyl disulfide through oxidation of methyl mercaptan salt solution. The method comprises the following steps: firstly, methyl mercaptan is inputted into an alkaline solution, a reaction is carried out, a methyl mercaptan salt solution is obtained, then the methyl mercaptan salt solution is reacted with an oxidizing agent to generate a dimethyl disulfide crude product, finally the crude product is purified and refined and a dimethyl disulfide finished product is obtained. The employed raw materials have low toxicity or no toxicity and are cheap and easily available. Through oxidation of a methyl mercaptan salt solution, the safety risk is avoided that methyl mercaptan and oxygen are reacted directly and an explosive mixture is easy to generate.

Description

technical field [0001] The invention belongs to the technical field of organic chemical industry, and in particular relates to a method and a device for producing dimethyl disulfide by oxidation of methyl mercaptan solution, especially sodium methyl mercaptide or ammonium methyl mercaptide solution. Background technique [0002] Dimethyl disulfide (DMDS) is an important chemical product with a wide range of uses. In the pesticide industry, it is used as an intermediate for the preparation of pesticides; in the petroleum industry, it can be used as an anti-corrosion and anti-scorch agent for ethane cracking furnaces, a vulcanizing agent for oil hydrogenation catalysts, and dehydroxylation of benzene nuclei. Inhibitor of hydrocracking in medium; in rubber industry, it can be used as solvent, regenerant, softener and plasticizer; in addition, DMDS can also be used as fuel, lubricant additive and inhibitor of some organic chemical reactions. It is mainly used in pesticide, dyes...

Claims

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Application Information

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IPC IPC(8): C07C319/24C07C321/14
Inventor 王杰方兴田云清杨军敖含李修兵易晓明
Owner HUBEI XINGFA CHEM GRP CO LTD
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