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Method for continuously producing dimethyl disulfide

A technology of dimethyl disulfide and dimethyl trisulfide, which is applied in the field of petroleum fine chemical industry and can solve problems such as difficult recovery of methyl mercaptan

Active Publication Date: 2014-06-18
CNOOC TIANJIN CHEM RES & DESIGN INST +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0010] The present invention mainly solves the problem of difficult recovery of methyl mercaptan existing in the prior art and provides a method for continuous production of dimethyl disulfide

Method used

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  • Method for continuously producing dimethyl disulfide

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Effect test

Embodiment 1

[0030] 433.2kg / h sulfur is melted and pumped to a tubular reactor with a diameter of 1m and a length of 10m, made of 304 stainless steel, and circulating 2999.9kg / h dimethyl disulfide (88.5wt% dimethyl disulfide, Dimethyl trisulfide 11.5wt%) mixed, by adjusting the circulating flow rate of dimethyl disulfide to control the reactor inlet temperature is 20 ℃, the stoichiometric ratio of dimethyl disulfide and sulfur (calculated as sulfur element) is 2.1, The reaction pressure is 0.2MPaA, the outlet temperature of the reactor is 30°C, the excess dimethyl disulfide makes the sulfur completely converted, and basically no dimethyl polysulfide is generated during the reaction.

[0031] 3433.1kg / h of reaction products (40.3wt% dimethyl disulfide and 59.7wt% dimethyl trisulfide) are mixed with 1298.9kg / h methyl mercaptan, and enter a tubular reactor with a diameter of 1.2m and a length of 12m , The material is 304 stainless steel, the stoichiometric ratio of dimethyl trisulfide to meth...

Embodiment 2

[0035] 434.2kg / h sulfur is melted and pumped to a tubular reactor with a diameter of 1m and a length of 10m, made of 304 stainless steel, and circulating 4500.3kg / h dimethyl disulfide (composed of dimethyl disulfide 75.9wt%, Dimethyl trisulfide 24.1wt%) mixed, by adjusting the circulating flow rate of dimethyl disulfide to control the reactor inlet temperature is 30 ℃, the stoichiometric ratio of dimethyl disulfide and sulfur (calculated as sulfur element) is 2.7, The reaction pressure is 0.4MPaA, the outlet temperature of the reactor is 35°C, the excess dimethyl disulfide makes the sulfur completely converted, and basically no dimethyl polysulfide is generated during the reaction.

[0036] 4934.5kg / h of reaction products (43.4wt% dimethyl disulfide and 56.6wt% dimethyl trisulfide) are mixed with 1298.9kg / h methyl mercaptan, and enter a tubular reactor with a diameter of 1.2m and a length of 12m , The material is 304 stainless steel, the stoichiometric ratio of dimethyl trisul...

Embodiment 3

[0040] 433.7kg / h of sulfur is melted and pumped to a tubular reactor with a diameter of 1m and a length of 10m, made of 304 stainless steel, and circulating 5000.3kg / h dimethyl disulfide (87.1wt% dimethyl disulfide, Dimethyl trisulfide 12.9wt%) mixed, by adjusting the circulating flow rate of dimethyl disulfide to control the reactor inlet temperature is 35 ° C, the stoichiometric ratio of dimethyl disulfide and sulfur (calculated as sulfur element) is 3.4, The reaction pressure is 0.6MPaA, the outlet temperature of the reactor is 40°C, the excess dimethyl disulfide makes the sulfur completely converted, and basically no dimethyl polysulfide is generated during the reaction.

[0041] 5434kg / h of reaction products (56.7wt% dimethyl disulfide and 43.3wt% dimethyl trisulfide) are mixed with 1298.9kg / h methyl mercaptan, and enter a tubular reactor with a diameter of 1.2m and a length of 12m. The material is 304 stainless steel, the stoichiometric ratio of dimethyl trisulfide to me...

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Abstract

The invention discloses a method for continuously producing dimethyl disulfide. The method is characterized in that after being molten, a material sulfur is fed into a dimethyl trisulfide reactor by virtue of a feeding pump so as to react with recycled dimethyl disulfide to generate dimethyl trisulfide; dimethyl trisulfide and methyl mercaptan are feed into a dimethyl disulfide reactor so as to react to generate dimethyl disulfide; a dimethyl disulfide crude product is fed into a separating tank, so that most of hydrogen sulfide is separated out, a liquid-phase product is fed into a rectifying tower, a dimethyl disulfide product is condensed and recycled at a tower top, hydrogen sulfide is exhausted as a non-condensable gas, and the dimethyl disulfide and dimethyl trisulfide in a tower kettle are returned and recycled. A method of enabling dimethyl trisulfide to be excessive is adopted, so that methyl mercaptan is completely converted, separating requirements are lowered and a separating process is simplified, and therefore, not only can the dimethyl disulfide yield be improved to 90%, but also the product purity is up to 99wt%.

Description

Technical field: [0001] The invention relates to the technical field of petroleum fine chemicals, and relates to a method for continuously producing dimethyl disulfide, in particular to a method for continuously producing dimethyl disulfide with methyl mercaptan and sulfur as raw materials. Background of the invention: [0002] Dimethyl disulfide is an important organic chemical product, which can be widely used as an intermediate for preparing pesticides and insecticides; Vulcanizing machine in hydrogen catalysis and inhibitor of hydrocracking in benzene ring dehydroxylation reaction; in rubber industry, it can be used as solvent, regeneration agent, softener and plasticizer; in addition, dimethyl disulfide can also be used As fuel and lubricating oil additives. [0003] Most of the dimethyl disulfide production methods reported in China are based on dimethyl sulfate, sodium sulfide and sulfur as raw materials, including CN1075955, CN1031838 and CN1211568, etc., wherein di...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C321/14C07C319/24C07C319/28
Inventor 舒畅于海斌汲银平沙喜江李世松王春雷张健
Owner CNOOC TIANJIN CHEM RES & DESIGN INST
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