CN104610106A - Method for producing dimethyl disulfide by using methyl mercaptan and sulfur vaporization method - Google Patents
Method for producing dimethyl disulfide by using methyl mercaptan and sulfur vaporization method Download PDFInfo
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- CN104610106A CN104610106A CN201510014815.XA CN201510014815A CN104610106A CN 104610106 A CN104610106 A CN 104610106A CN 201510014815 A CN201510014815 A CN 201510014815A CN 104610106 A CN104610106 A CN 104610106A
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- thiomethyl alcohol
- sulphur
- methyl disulfide
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Abstract
The invention discloses a novel process for producing dimethyl disulfide by using a methyl mercaptan and sulfur vaporization method. According to the process, sulfur is vaporized and is subsequently subjected to homogeneous reaction with methyl mercaptan so as to generate dimethyl disulfide. The process has the characteristics of simple production process, low energy consumption, low production cost, production environment protection, high product purity and the like.
Description
Technical field
The present invention relates to a kind of production method of novel synthesization of dimethyl disulfide, its principal character produces without the three wastes.
Background technology
methyl disulfide is a kind of broad-spectrum organic compounds containing sulfur, is used as the anticorrosion of ethane cracking furnace and scorch retarder in petroleum technology, the vulcanizing agent of gasoline hydrogenation catalysis, the inhibitor of hydrocracking in benzene nucleus decarboxylation reaction.In rubber industry, can be used as solvent, regenerator, tenderizer, softening agent etc.In addition, Methyl disulfide also can be used as the additive of fuel and lubrication, produces the intermediate of agricultural chemical insecticide.
Producing more ripe production method both at home and abroad is at present dimethyl sulfate ester process: take methyl-sulfate, sodium sulphite, sulphur certain mol proportion, sulphur powder is joined in the sodium sulfide solution of 18% one 22%, stirring reaction is after 1 hour, in mixed solution, drip methyl-sulfate be obtained by reacting the thick product of Methyl disulfide, then obtain smart two sulphur through rectifying.
Also there are relevant report and the patent of thiomethyl alcohol and sulfur reaction production Methyl disulfide in China.Method is in the past all adopt powder or Molten sulphur and thiomethyl alcohol to react to generate Methyl disulfide, and after not having thiomethyl alcohol and sulphur vaporization, reaction generates the operational path of Methyl disulfide.
On the basis of our research, we determine the novel method of thiomethyl alcohol and sulphur gasification production Methyl disulfide according to response characteristic and reaction mechanism.
Summary of the invention
The invention provides a kind of method of thiomethyl alcohol and sulphur gasification production Methyl disulfide, comprise the steps:
1) mix after Molten sulphur and gas thiomethyl alcohol being gasified respectively by tubular oven, high-temperature gas mixture body after gasification enters adiabatic reactor, under the effect of catalyzer preset in adiabatic reactor, generate the mixed gas of Methyl disulfide, dimethyl thioether, thiomethyl alcohol, dimethyltrisulfide, dimethyl polysulfide and hydrogen sulfide;
2) crude product Methyl disulfide is obtained by after mixed gas desulfurization, separation, condensation in step 1), uncooled hydrogen sulfide returns thiomethyl alcohol reactor and the methyl alcohol Reactive Synthesis thiomethyl alcohol raw material as step 1), crude product Methyl disulfide is by obtaining Methyl disulfide product after rectifying, condensed by product dimethyl thioether, thiomethyl alcohol, dimethyltrisulfide, dimethyl polysulfide intermittent type squeeze into molten sulfur mixing tank, enter adiabatic reactor through tubular oven after mixing with methyl mercaptan gas, form periodic cycle and produce.
The mass ratio of sulphur and thiomethyl alcohol is 1:1.03-1.1.
Molten sulphur and gas thiomethyl alcohol gasification temperature in tubular oven is 470-650 DEG C, and meanwhile, tubular oven internal pressure controls as 0.1-0.65MPa, and adiabatic reactor internal pressure controls as 0.1-0.65MPa.
After Molten sulphur, thiomethyl alcohol are passed into and vaporize in tubular oven, be sent in adiabatic reactor and react, then obtain the pure Methyl disulfide of content more than 99.5% through measures such as desulfurization, condensation, rectifying.
Embodiment
embodiment 1
After sulphur is melted, be transported in tubular oven by fluid pump, have burner in tubular oven, fuel (Sweet natural gas, diesel oil, biogas etc.) produces flare by burner spray burning, and flare heat is used for feed vaporization through radiation delivery to heating furnace tube and heats up.Sulphur mixes with methyl mercaptan gas in tubular oven, sulphur and thiomethyl alcohol mass ratio are 1:1.03-1.1, by tubular oven heating, sulphur and thiomethyl alcohol are vaporized to 470-650 DEG C, then the mixed gas after heating enters into adiabatic reactor, control adiabatic reactor and tubular oven pressure are at 0.1-0.65MP, the special catalyst that thiomethyl alcohol-sulphur gasification generates Methyl disulfide is filled with in adiabatic reactor, adiabatic reactor inwall is built thermal insulation material and is prevented calorific loss simultaneously, sulphur, after thiomethyl alcohol carries out the homogeneous catalytic reaction of gas phase in adiabatic reactor, obtain Methyl disulfide, dimethyl thioether, thiomethyl alcohol, dimethyltrisulfide, the gas mixture of the many sulphur of dimethyl, gas mixture is through the desulfurization of sulphur cooler, after the measures such as separation, crude product Methyl disulfide is obtained through condensation, do not obtain the H of condensation
2s desulfuration alcohol reactor and methanol-fueled CLC generate thiomethyl alcohol.Crude product Methyl disulfide is obtained the pure Methyl disulfide of purity >=99.5% after rectifying by tower top, still liquid interval containing dimethyltrisulfide, the many sulphur of dimethyl at the bottom of tower squeezes into molten sulfur mixing tank, then in the presence of thiomethyl alcohol, enters tubular oven enter adiabatic reactor and start the circulation of next production cycle.
Claims (3)
1. a method for thiomethyl alcohol and sulphur gasification production Methyl disulfide, is characterized in that, comprise the steps:
Mix after Molten sulphur and gas thiomethyl alcohol are gasified respectively by tubular oven, high-temperature gas mixture body after gasification enters adiabatic reactor, generates the mixed gas of Methyl disulfide, dimethyl thioether, thiomethyl alcohol, dimethyltrisulfide, dimethyl polysulfide and hydrogen sulfide in adiabatic reactor;
Crude product Methyl disulfide is obtained by after mixed gas desulfurization, separation, condensation in step 1), uncooled hydrogen sulfide returns thiomethyl alcohol reactor and the methyl alcohol Reactive Synthesis thiomethyl alcohol raw material as step 1), crude product Methyl disulfide is by obtaining Methyl disulfide product after rectifying, condensed by product dimethyl thioether, thiomethyl alcohol, dimethyltrisulfide, dimethyl polysulfide intermittent type squeeze into molten sulfur mixing tank, enter adiabatic reactor through tubular oven after mixing with methyl mercaptan gas, form periodic cycle and produce.
2. method according to claim 1, is characterized in that: the mass ratio of sulphur and thiomethyl alcohol is 1:1.03-1.1.
3. method according to claim 1, it is characterized in that: Molten sulphur and gas thiomethyl alcohol gasification temperature in tubular oven is 470-650 DEG C, meanwhile, tubular oven internal pressure controls as 0.1-0.65MPa, and adiabatic reactor internal pressure controls as 0.1-0.65MPa.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510014815.XA CN104610106A (en) | 2015-01-13 | 2015-01-13 | Method for producing dimethyl disulfide by using methyl mercaptan and sulfur vaporization method |
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| CN201510014815.XA CN104610106A (en) | 2015-01-13 | 2015-01-13 | Method for producing dimethyl disulfide by using methyl mercaptan and sulfur vaporization method |
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| CN104610106A true CN104610106A (en) | 2015-05-13 |
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| CN201510014815.XA Pending CN104610106A (en) | 2015-01-13 | 2015-01-13 | Method for producing dimethyl disulfide by using methyl mercaptan and sulfur vaporization method |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107759501A (en) * | 2017-12-07 | 2018-03-06 | 查都（上海）科技有限公司 | A kind of device for producing DMDS coproduction dimethyltrisulfide |
| CN107827793A (en) * | 2017-12-07 | 2018-03-23 | 查都（上海）科技有限公司 | A kind of DMDS refining separation device |
| CN107827794A (en) * | 2017-12-07 | 2018-03-23 | 查都（上海）科技有限公司 | A kind of device of methyl mercaptan vulcanization method production DMDS |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1037331A (en) * | 1988-04-14 | 1989-11-22 | 埃尔夫阿奎垣国家石油(制造)公司 | The method for preparing lower dialkyl disulphides |
| US5659086A (en) * | 1995-06-06 | 1997-08-19 | Phillips Petroleum Company | Production of organic disulfides |
| CN103864650A (en) * | 2014-03-20 | 2014-06-18 | 中国海洋石油总公司 | Method for continuously producing dimethyl disulfide |
| CN103910661A (en) * | 2013-02-26 | 2014-07-09 | 湖北兴发化工集团股份有限公司 | Method for producing dimethyl disulfide from methyl mercaptan and sulphur by employing sulfuration process |
-
2015
- 2015-01-13 CN CN201510014815.XA patent/CN104610106A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1037331A (en) * | 1988-04-14 | 1989-11-22 | 埃尔夫阿奎垣国家石油(制造)公司 | The method for preparing lower dialkyl disulphides |
| US5659086A (en) * | 1995-06-06 | 1997-08-19 | Phillips Petroleum Company | Production of organic disulfides |
| CN103910661A (en) * | 2013-02-26 | 2014-07-09 | 湖北兴发化工集团股份有限公司 | Method for producing dimethyl disulfide from methyl mercaptan and sulphur by employing sulfuration process |
| CN103864650A (en) * | 2014-03-20 | 2014-06-18 | 中国海洋石油总公司 | Method for continuously producing dimethyl disulfide |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107759501A (en) * | 2017-12-07 | 2018-03-06 | 查都（上海）科技有限公司 | A kind of device for producing DMDS coproduction dimethyltrisulfide |
| CN107827793A (en) * | 2017-12-07 | 2018-03-23 | 查都（上海）科技有限公司 | A kind of DMDS refining separation device |
| CN107827794A (en) * | 2017-12-07 | 2018-03-23 | 查都（上海）科技有限公司 | A kind of device of methyl mercaptan vulcanization method production DMDS |
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Application publication date: 20150513 |
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