CN103864650A - Method for continuously producing dimethyl disulfide - Google Patents
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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:
The present invention relates to oil fine chemistry industry technical field, is a kind of method of continuous production Methyl disulfide, relates in particular to a kind of method take thiomethyl alcohol and sulphur as the continuous production Methyl disulfide of raw material.
Background of invention:
Methyl disulfide is a kind of important Organic chemical products, can be widely used in the intermediate of producing agricultural chemical insecticide; In petroleum industry, can be used as the inhibitor of hydrocracking in vulcanizer in anticorrosion and scorch retarder, the gasoline hydrogenation catalysis of ethane cracking furnace and phenyl ring decarboxylation reaction; In rubber industry, can be used as solvent, regenerator, tenderizer and softening agent etc.; In addition, Methyl disulfide also can be used as fuel and lubricated oil additives.
The Methyl disulfide production method great majority of current domestic report are take methyl-sulfate, sodium sulphite and sulphur as raw material, comprise CN1075955, CN1031838 and CN1211568 etc., wherein methyl-sulfate severe toxicity, operator is in peril of one's life, and discharge the sodium sulfate wastewater of a large amount of sulfur acid dimethyl esters and sulfide, severe contamination environment.
The external method production Methyl disulfide that adopts thiomethyl alcohol oxidation more, oxygenant comprises oxygen, hydrogen peroxide, sulphur and Sodium Nitrite etc., the method has not only been avoided the use of methyl-sulfate, and production process is without the discharge of waste water.
CN102816093A discloses a kind of method of thiomethyl alcohol oxidation production Methyl disulfide, oxygenant is oxygen or sulphur, catalyzer is nitrogen peroxide, emulsifying agent is acetone, dimethyl formamide and dimethyl sulfoxide (DMSO), successive reaction in tower reactor, product obtains Methyl disulfide finished product through the separation of liquid liquid, rectifying.Thiomethyl alcohol is very easy to blast, and it is beyond doubt extremely dangerous that the method adopts oxygen to make oxygenant, and the emulsifying agent of introducing obviously increased operation easier, has improved production cost.
GB1094782A discloses a kind of method of thiomethyl alcohol and the continuous production Methyl disulfide of sulphur, sulphur and Methyl disulfide are reacted and are generated dimethyltrisulfide in reactor A, then enter reactor B and thiomethyl alcohol reaction generation Methyl disulfide, the product of reactor B enters knockout tower I and takes off excessive hydrogen sulfide and thiomethyl alcohol, then enter knockout tower II and reclaim Methyl disulfide product, Methyl disulfide yield based on thiomethyl alcohol is 85%, and product purity is 90wt%.The hydrogen sulfide that the method produces is discharged from reactor B, not only caused a large amount of thiomethyl alcohol losses, and loss has also occurred Methyl disulfide.
EP0202420 discloses a kind of method take hydrogen sulfide, sulphur and methyl alcohol as raw material production Methyl disulfide, sulphur and the reaction of part Methyl disulfide generate dimethyltrisulfide, methyl alcohol and hydrogen sulfide reaction generate thiomethyl alcohol, separate after water and excessive hydrogen sulfide, thiomethyl alcohol and dimethyltrisulfide reaction generate Methyl disulfide, Methyl disulfide crude product is taken off hydrogen sulfide, thiomethyl alcohol through 3 knockout towers, thereby obtains Methyl disulfide sterling, and the Methyl disulfide product yield based on methyl alcohol reaches 90%.The method has been used excessive thiomethyl alcohol, and internal circulating load is large, and separating technology complexity.
US4721813 discloses the method for a kind of alkyl sulfhydryl dioxygen oxidation production dialkyl disulfides, but thiomethyl alcohol explosive, the method does not indicate and is applicable to Methyl disulfide.
On the basis of our research, we find all to adopt in method in the past the excessive method production Methyl disulfide of thiomethyl alcohol, and Methyl disulfide to remove thiomethyl alcohol be a very complicated job, therefore not only yield is low, and product purity is not high.We have broken through forefathers' thinking set, adopt the excessive method of dimethyltrisulfide, and thiomethyl alcohol is transformed completely, thereby reduce separation requirement, simplified separating technology, not only the yield of Methyl disulfide is increased to 90%, and has obtained purity and reach the Methyl disulfide product of 99wt%.
Summary of the invention:
The present invention mainly solves that the thiomethyl alcohol existing in prior art reclaims difficult problem and a kind of method that continuous production Methyl disulfide is provided.
The present invention is a kind of method of continuous production Methyl disulfide, it is characterized in that:
A) sulphur reacts and generates dimethyltrisulfide with excessive Methyl disulfide in dimethyltrisulfide reactor, the stoichiometric ratio of Methyl disulfide and sulphur is 1～4, excessive Methyl disulfide has guaranteed the conversion completely of sulphur, has also reduced the generation of the many sulphur of dimethyl simultaneously; 0～80 ℃ of temperature of reaction; Reaction pressure 0～1MPaA;
B) excessive dimethyltrisulfide reacts in Methyl disulfide reactor with thiomethyl alcohol and generates Methyl disulfide, the stoichiometric ratio of dimethyltrisulfide and thiomethyl alcohol is 0.5～1, excessive dimethyltrisulfide has guaranteed the conversion completely of thiomethyl alcohol, thereby has avoided thiomethyl alcohol in follow-up workshop section to be difficult to the problem reclaiming; 0～60 ℃ of temperature of reaction; Reaction pressure 0～1MPaA;
C) the thick product of the Methyl disulfide after adiabatic flash adopts single tower rectification under vacuum to refine Methyl disulfide product, tower top pressure 10～500mmHg, a small amount of hydrogen sulfide discharges as non-condensable gas, the Methyl disulfide of tower reactor and dimethyltrisulfide return to dimethyltrisulfide reactor cycles through recycle pump and use, tower top Methyl disulfide product purity reaches 99wt%, and yield is greater than 90%.
According to the method described in the present invention, it is characterized in that:
A) sulphur reacts and generates dimethyltrisulfide with excessive Methyl disulfide in dimethyltrisulfide reactor, the stoichiometric ratio of Methyl disulfide and sulphur is 2.1～3.4, excessive Methyl disulfide has guaranteed the conversion completely of sulphur, has also reduced the generation of the many sulphur of dimethyl simultaneously; 20～40 ℃ of temperature of reaction; Reaction pressure 0.2～0.6MPaA;
B) excessive dimethyltrisulfide reacts in Methyl disulfide reactor with thiomethyl alcohol and generates Methyl disulfide, the stoichiometric ratio of dimethyltrisulfide and thiomethyl alcohol is 0.6～0.8, excessive dimethyltrisulfide has guaranteed the conversion completely of thiomethyl alcohol, thereby has avoided thiomethyl alcohol in follow-up workshop section to be difficult to the problem reclaiming; 10～30 ℃ of temperature of reaction, reaction pressure 0.2～0.5MPaA;
C) the thick product of the Methyl disulfide after adiabatic flash adopts single tower rectification under vacuum to refine Methyl disulfide product, tower top pressure 50～200mmHg, a small amount of hydrogen sulfide discharges as non-condensable gas, the Methyl disulfide of tower reactor and dimethyltrisulfide return to dimethyltrisulfide reactor cycles through recycle pump and use, tower top Methyl disulfide product purity reaches 99wt%, and yield is greater than 90%.
Concrete technology flow process of the present invention comprises: after raw material sulphur melts, send into dimethyltrisulfide reactor through fresh feed pump, react and generate dimethyltrisulfide (S+C2H6S2 → C2H6S3) with the Methyl disulfide of circulation, dimethyltrisulfide and thiomethyl alcohol enter Methyl disulfide reactor, reaction generates Methyl disulfide (CH4S+C2H6S3 → 2C2H6S2+H2S), the thick product introduction separating tank of Methyl disulfide, separate most hydrogen sulfide, liquid product enters rectifying tower, overhead condensation reclaims Methyl disulfide product, hydrogen sulfide discharges as non-condensable gas, the Methyl disulfide of tower reactor and dimethyltrisulfide return and recycle.
Sulphur reacts in dimethyltrisulfide reactor with Methyl disulfide and generates dimethyltrisulfide, the stoichiometric ratio of Methyl disulfide and sulphur is 1～4, preferably 2.1～3.4, excessive Methyl disulfide has guaranteed the conversion completely of sulphur, has also reduced the generation of the many sulphur of dimethyl simultaneously; 0～80 ℃ of temperature of reaction, preferably 20～40 ℃; Reaction pressure 0～1MPaA, preferably 0.2～0.6MPaA; Those skilled in the art can skillfully select applicable type of reactor as required.
Dimethyltrisulfide reacts in Methyl disulfide reactor with thiomethyl alcohol and generates Methyl disulfide, the stoichiometric ratio of dimethyltrisulfide and thiomethyl alcohol is 0.5～1, preferably 0.6～0.8, excessive dimethyltrisulfide has guaranteed the conversion completely of thiomethyl alcohol, thereby has avoided thiomethyl alcohol in follow-up workshop section to be difficult to the problem reclaiming; 0～60 ℃ of temperature of reaction, preferably 10～30 ℃; Reaction pressure 0～1MPaA, preferably 0.2～0.5MPaA; Those skilled in the art's type of reactor of skilled choice for use as required.
The thick product of Methyl disulfide adiabatic flash in separating tank, working pressure 0.15MPaA, separates approximately 70% hydrogen sulfide.
Liquid-phase product after flash distillation enters rectifying tower, Methyl disulfide product is refined in rectification under vacuum, tower top pressure 10～500mmHg, preferably 50～200mmHg, a small amount of hydrogen sulfide discharges as non-condensable gas, the Methyl disulfide of tower reactor and dimethyltrisulfide return to dimethyltrisulfide reactor cycles through recycle pump and use, and tower top Methyl disulfide product purity reaches 99wt%, and yield is greater than 90%.
The hydrogen sulfide that system produces can skillfully be processed by those skilled in the art, and the one, adopt ripe Claus unit sulfur recovery unit to be reclaimed, the 2nd, return to thiomethyl alcohol synthesis system by compressor cycle and recycle.
Accompanying drawing explanation:
Fig. 1 is schematic flow sheet used in the present invention
1-sulphur melting tank; 2-sulphur fresh feed pump; 3-dimethyltrisulfide reactor; 4-Methyl disulfide reactor; 5-divides
From tank; 6-rectifying tower; 7-overhead condenser; 8-tower reactor reboiler; 9-Methyl disulfide recycle pump.
Embodiment:
According to the flow process of Fig. 1, take sulphur and thiomethyl alcohol as raw material, production Methyl disulfide continuously.
Embodiment 1
433.2kg/h sulphur melts rear with being pumped to a tubular reactor, diameter 1m, long 10m, material 304 stainless steels, 2999.9kg/h Methyl disulfide (composition Methyl disulfide 88.5wt% with circulation, dimethyltrisulfide 11.5wt%) mix, it is 20 ℃ by the circular flow control reactor inlet temperature of adjusting Methyl disulfide, the stoichiometric ratio of Methyl disulfide and sulphur (take sulphur simple substance) is 2.1, reaction pressure 0.2MPaA, 30 ℃ of reactor outlet temperature, excessive Methyl disulfide transforms sulphur completely, and in reaction process, substantially do not produce the many sulphur of dimethyl.
The reaction product (composition Methyl disulfide 40.3wt%, dimethyltrisulfide 59.7wt%) of 3433.1kg/h is mixed with 1298.9kg/h thiomethyl alcohol, enter a tubular reactor, diameter 1.2m, long 12m, material 304 stainless steels, the stoichiometric ratio of dimethyltrisulfide and thiomethyl alcohol is 0.6,10 ℃ of reaction inlet temperature, 23.1 ℃ of reaction temperature outs, reaction pressure 0.2MPaA.
The thick product of 4732kg/h Methyl disulfide (hydrogen sulfide 9.7wt%, Methyl disulfide 83wt%, dimethyltrisulfide 7.3wt%) enters separating tank adiabatic flash, working pressure 0.15MPaA, the gas (hydrogen sulfide 94.63wt%, Methyl disulfide 5.34wt%, dimethyltrisulfide 0.03wt%) of 354.5kg/h is discharged from gas phase, and 4377.5kg/h liquid product (hydrogen sulfide 2.8wt%, Methyl disulfide 89.2wt%, dimethyltrisulfide 7.9wt%) enters rectifying tower.
Rectifying tower vacuum operation, tower top pressure 100mmHg, tower bottoms is 3012.6kg/h(Methyl disulfide 88.5wt%, dimethyltrisulfide 11.5% altogether), wherein 2999.9kg/h recycles, and discharges to maintain system Compositional balance on a small quantity, and tower top is cooled to 10 ℃, the hydrogen sulfide (hydrogen sulfide 71.8wt%, Methyl disulfide 28.2wt%) of 168.3kg/h discharges as non-condensable gas, tower top obtains 1196.7kg/h Methyl disulfide product, and purity is 99.7wt%, and the yield based on thiomethyl alcohol reaches 93.8%.
Embodiment 2
434.2kg/h sulphur melts rear with being pumped to a tubular reactor, diameter 1m, long 10m, material 304 stainless steels, 4500.3kg/h Methyl disulfide (composition Methyl disulfide 75.9wt% with circulation, dimethyltrisulfide 24.1wt%) mix, it is 30 ℃ by the circular flow control reactor inlet temperature of adjusting Methyl disulfide, the stoichiometric ratio of Methyl disulfide and sulphur (take sulphur simple substance) is 2.7, reaction pressure 0.4MPaA, 35 ℃ of reactor outlet temperature, excessive Methyl disulfide transforms sulphur completely, and in reaction process, substantially do not produce the many sulphur of dimethyl.
The reaction product (composition Methyl disulfide 43.4wt%, dimethyltrisulfide 56.6wt%) of 4934.5kg/h is mixed with 1298.9kg/h thiomethyl alcohol, enter a tubular reactor, diameter 1.2m, long 12m, material 304 stainless steels, the stoichiometric ratio of dimethyltrisulfide and thiomethyl alcohol is 0.8,20 ℃ of reaction inlet temperature, 30 ℃ of reaction temperature outs, reaction pressure 0.3MPaA.
The thick product of 6233.4kg/h Methyl disulfide (hydrogen sulfide 7.4wt%, Methyl disulfide 75.1wt%, dimethyltrisulfide 17.5wt%) enters separating tank adiabatic flash, working pressure 0.15MPaA, the gas (hydrogen sulfide 93.7wt%, Methyl disulfide 6.2wt%, dimethyltrisulfide 0.1wt%) of 336.6kg/h is discharged from gas phase, and 5896.8kg/h liquid product (hydrogen sulfide 2.5wt%, Methyl disulfide 79.1wt%, dimethyltrisulfide 18.5wt%) enters rectifying tower.
Rectifying tower vacuum operation, tower top pressure 50mmHg, tower bottoms is 4524.8kg/h(Methyl disulfide 75.9wt%, dimethyltrisulfide 24.1% altogether), wherein 4500.3kg/h recycles, and discharges to maintain system Compositional balance on a small quantity, and tower top is cooled to 10 ℃, the hydrogen sulfide (hydrogen sulfide 64wt%, Methyl disulfide 36wt%) of 223.7kg/h discharges as non-condensable gas, tower top obtains 1148.2kg/h Methyl disulfide product, and purity is 99.9wt%, and the yield based on thiomethyl alcohol reaches 90%.
Embodiment 3
433.7kg/h sulphur melts rear with being pumped to a tubular reactor, diameter 1m, long 10m, material 304 stainless steels, 5000.3kg/h Methyl disulfide (composition Methyl disulfide 87.1wt% with circulation, dimethyltrisulfide 12.9wt%) mix, it is 35 ℃ by the circular flow control reactor inlet temperature of adjusting Methyl disulfide, the stoichiometric ratio of Methyl disulfide and sulphur (take sulphur simple substance) is 3.4, reaction pressure 0.6MPaA, 40 ℃ of reactor outlet temperature, excessive Methyl disulfide transforms sulphur completely, and in reaction process, substantially do not produce the many sulphur of dimethyl.
The reaction product (composition Methyl disulfide 56.7wt%, dimethyltrisulfide 43.3wt%) of 5434kg/h is mixed with 1298.9kg/h thiomethyl alcohol, enter a tubular reactor, diameter 1.2m, long 12m, material 304 stainless steels, the stoichiometric ratio of dimethyltrisulfide and thiomethyl alcohol is 0.7,20 ℃ of reaction inlet temperature, 28 ℃ of reaction temperature outs, reaction pressure 0.5MPaA.
The thick product of 6732.9kg/h Methyl disulfide (hydrogen sulfide 6.8wt%, Methyl disulfide 83.5wt%, dimethyltrisulfide 9.6wt%) enters separating tank adiabatic flash, working pressure 0.15MPaA, the gas (hydrogen sulfide 92.8wt%, Methyl disulfide 7.1wt%, dimethyltrisulfide 0.1wt%) of 329.5kg/h is discharged from gas phase, and 6403.4kg/h liquid product (hydrogen sulfide 2.4wt%, Methyl disulfide 87.5wt%, dimethyltrisulfide 10.1wt%) enters rectifying tower.
Rectifying tower vacuum operation, tower top pressure 200mmHg, tower bottoms is 5026.4kg/h(Methyl disulfide 87.1wt%, dimethyltrisulfide 12.9% altogether), wherein 5000.3kg/h recycles, and discharges to maintain system Compositional balance on a small quantity, and tower top is cooled to 10 ℃, the hydrogen sulfide (hydrogen sulfide 84.7wt%, Methyl disulfide 15.3wt%) of 172.7kg/h discharges as non-condensable gas, tower top obtains 1204.3kg/h Methyl disulfide product, and purity is 99.3wt%, and the yield based on thiomethyl alcohol reaches 94%.
Claims (2)
1. a method for continuous production Methyl disulfide, is characterized in that:
A) sulphur reacts and generates dimethyltrisulfide with excessive Methyl disulfide in dimethyltrisulfide reactor, the stoichiometric ratio of Methyl disulfide and sulphur is 1～4, excessive Methyl disulfide has guaranteed the conversion completely of sulphur, has also reduced the generation of the many sulphur of dimethyl simultaneously; 0～80 ℃ of temperature of reaction; Reaction pressure 0～1MPaA;
B) excessive dimethyltrisulfide reacts in Methyl disulfide reactor with thiomethyl alcohol and generates Methyl disulfide, the stoichiometric ratio of dimethyltrisulfide and thiomethyl alcohol is 0.5～1, excessive dimethyltrisulfide has guaranteed the conversion completely of thiomethyl alcohol, thereby has avoided thiomethyl alcohol in follow-up workshop section to be difficult to the problem reclaiming; 0～60 ℃ of temperature of reaction; Reaction pressure 0～1MPaA;
C) the thick product of the Methyl disulfide after adiabatic flash adopts single tower rectification under vacuum to refine Methyl disulfide product, tower top pressure 10～500mmHg, a small amount of hydrogen sulfide discharges as non-condensable gas, the Methyl disulfide of tower reactor and dimethyltrisulfide return to dimethyltrisulfide reactor cycles through recycle pump and use, tower top Methyl disulfide product purity reaches 99wt%, and yield is greater than 90%.
2. it is characterized in that in accordance with the method for claim 1:
A) sulphur reacts and generates dimethyltrisulfide with excessive Methyl disulfide in dimethyltrisulfide reactor, the stoichiometric ratio of Methyl disulfide and sulphur is 2.1～3.4, excessive Methyl disulfide has guaranteed the conversion completely of sulphur, has also reduced the generation of the many sulphur of dimethyl simultaneously; 20～40 ℃ of temperature of reaction; Reaction pressure 0.2～0.6MPaA;
B) excessive dimethyltrisulfide reacts in Methyl disulfide reactor with thiomethyl alcohol and generates Methyl disulfide, the stoichiometric ratio of dimethyltrisulfide and thiomethyl alcohol is 0.6～0.8, excessive dimethyltrisulfide has guaranteed the conversion completely of thiomethyl alcohol, thereby has avoided thiomethyl alcohol in follow-up workshop section to be difficult to the problem reclaiming; 10～30 ℃ of temperature of reaction, reaction pressure 0.2～0.5MPaA;
C) the thick product of the Methyl disulfide after adiabatic flash adopts single tower rectification under vacuum to refine Methyl disulfide product, tower top pressure 50～200mmHg, a small amount of hydrogen sulfide discharges as non-condensable gas, the Methyl disulfide of tower reactor and dimethyltrisulfide return to dimethyltrisulfide reactor cycles through recycle pump and use, tower top Methyl disulfide product purity reaches 99wt%, and yield is greater than 90%.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201410105544.4A CN103864650B (en) | 2014-03-20 | A kind of method of continuous production Methyl disulfide |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410105544.4A CN103864650B (en) | 2014-03-20 | A kind of method of continuous production Methyl disulfide |
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| CN103864650A true CN103864650A (en) | 2014-06-18 |
| CN103864650B CN103864650B (en) | 2016-11-30 |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104592071A (en) * | 2015-01-13 | 2015-05-06 | 湖北兴发化工集团股份有限公司 | Method of adding sulfur in dissolved state in dimethyl disulfide production process |
| CN104592070A (en) * | 2015-01-13 | 2015-05-06 | 湖北兴发化工集团股份有限公司 | Preparation method of dimethyl disulfide |
| CN104610106A (en) * | 2015-01-13 | 2015-05-13 | 湖北兴发化工集团股份有限公司 | Method for producing dimethyl disulfide by using methyl mercaptan and sulfur vaporization method |
| CN106565568A (en) * | 2016-11-08 | 2017-04-19 | 辽宁广汇有机硫化工研究院有限公司 | Method of selectively synthesizing di-tert-butyl trithioether |
| CN106928105A (en) * | 2017-04-24 | 2017-07-07 | 湖北兴发化工集团股份有限公司 | One-step method continuously produces the Processes and apparatus of DMDS |
| 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 |
| 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 |
| 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 |
| CN116651020A (en) * | 2023-07-31 | 2023-08-29 | 民勤县鑫达化工有限公司 | Separation device for dimethyl disulfide production and manufacturing and application method thereof |
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| US3299146A (en) * | 1964-03-26 | 1967-01-17 | Pennsalt Chemicals Corp | Preparation of dimethyl disulfide |
| US5068445A (en) * | 1988-04-14 | 1991-11-26 | Societe Nationale Elf Aquitaine (Production) | Process for the preparation of organic disulphides and polysulphides |
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| US3299146A (en) * | 1964-03-26 | 1967-01-17 | Pennsalt Chemicals Corp | Preparation of dimethyl disulfide |
| US5068445A (en) * | 1988-04-14 | 1991-11-26 | Societe Nationale Elf Aquitaine (Production) | Process for the preparation of organic disulphides and polysulphides |
| US5312993A (en) * | 1990-03-05 | 1994-05-17 | Elf Atochem S.A. | Process for the manufacture of dimethyl disulphide |
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Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104592071A (en) * | 2015-01-13 | 2015-05-06 | 湖北兴发化工集团股份有限公司 | Method of adding sulfur in dissolved state in dimethyl disulfide production process |
| CN104592070A (en) * | 2015-01-13 | 2015-05-06 | 湖北兴发化工集团股份有限公司 | Preparation method of dimethyl disulfide |
| CN104610106A (en) * | 2015-01-13 | 2015-05-13 | 湖北兴发化工集团股份有限公司 | Method for producing dimethyl disulfide by using methyl mercaptan and sulfur vaporization method |
| CN106565568A (en) * | 2016-11-08 | 2017-04-19 | 辽宁广汇有机硫化工研究院有限公司 | Method of selectively synthesizing di-tert-butyl trithioether |
| CN106565568B (en) * | 2016-11-08 | 2018-06-08 | 辽宁广汇有机硫化工研究院有限公司 | A kind of method of selectivity synthesis di-t-butyl trithioether |
| CN106928105A (en) * | 2017-04-24 | 2017-07-07 | 湖北兴发化工集团股份有限公司 | One-step method continuously produces the Processes and apparatus of DMDS |
| CN106928105B (en) * | 2017-04-24 | 2019-06-04 | 湖北兴发化工集团股份有限公司 | The Processes and apparatus of one-step method continuous production dimethyl disulfide |
| 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 |
| 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 |
| 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 |
| CN116651020A (en) * | 2023-07-31 | 2023-08-29 | 民勤县鑫达化工有限公司 | Separation device for dimethyl disulfide production and manufacturing and application method thereof |
| CN116651020B (en) * | 2023-07-31 | 2023-09-19 | 民勤县鑫达化工有限公司 | Separation device for dimethyl disulfide production and manufacturing and application method thereof |
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