CN110229086A - A kind of dimethyl disulfide synthesis waste gas treatment process - Google Patents
A kind of dimethyl disulfide synthesis waste gas treatment process Download PDFInfo
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- CN110229086A CN110229086A CN201910549963.XA CN201910549963A CN110229086A CN 110229086 A CN110229086 A CN 110229086A CN 201910549963 A CN201910549963 A CN 201910549963A CN 110229086 A CN110229086 A CN 110229086A
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- dmso
- acetone
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- oil reservoir
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C315/00—Preparation of sulfones; Preparation of sulfoxides
- C07C315/02—Preparation of sulfones; Preparation of sulfoxides by formation of sulfone or sulfoxide groups by oxidation of sulfides, or by formation of sulfone groups by oxidation of sulfoxides
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C315/00—Preparation of sulfones; Preparation of sulfoxides
- C07C315/06—Separation; Purification; Stabilisation; Use of additives
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C319/00—Preparation of thiols, sulfides, hydropolysulfides or polysulfides
- C07C319/26—Separation; Purification; Stabilisation; Use of additives
- C07C319/28—Separation; Purification
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- Organic Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention discloses a kind of dimethyl disulfides to synthesize waste gas treatment process, and the step for the treatment of process is as follows: step 1, condensation: the waste gas condensation that will be generated in dimethyl disulfide synthesis process is at waste liquid；Step 2, separation: waste liquid is separated into oil reservoir and water layer；Step 3, distillation: the oil reservoir liquid that step 2 obtains is distilled；Step 4, oxidation: acetone and hydrogen peroxide is added into the oil reservoir liquid after above-mentioned distillation, the oil reservoir liquid oxygen after distillation is turned into DMSO with hydrogen peroxide using acetone as solvent；Step 5, rectifying: rectifying is carried out to reaction solution, the acetone and vapor that Fractional Collections rectifying goes out obtain sticky oily transparency liquid；Step 6, vacuum distillation: fraction is collected, crude product DMSO is obtained；Step 7, decompression filter: a certain amount of calcium oxide decompression being added into crude product DMSO and filters, fine work DMSO is made.The present invention realizes exhaust gas and is effectively treated, and in exhaust gas DMSO the rate of recovery up to 88.6%, be not necessarily to acid-base neutralization, reached the standard of industrial discharge.
Description
Technical field
The present invention relates to a kind of dimethyl disulfides to synthesize waste gas treatment process, belongs to technical field of waste gas treatment.
Background technique
Dimethyl disulfide is a kind of artificial synthesized, not soluble in water, colourless or pale yellow virose chemical reagent of band.Diformazan
Base disulfide is important chemical products, be widely used as solvent, pesticide intermediate, coking agent, catalyst vulcanizing agent and subtract
Fast agent.In recent years, as people are to the understanding of DMDS and using it as the research and development of waste methylsufonyl chloride and methane sulfonic acid etc.,
Cause both at home and abroad to sharply increase the demand of DMDS.
The method for producing DMDS has: methyl mercaptan method, halogenated hydrocarbons method, dimethyl sulfate method.Original used in dimethyl sulfate method
Material is easy to get, and process flow is simpler, and product cost is lower, is the method generallyd use both at home and abroad, and principle is: first with Na2S and
Sulphur is waste Na2S2, then in Na2S2Solution in be added dimethyl suflfate, etherificate produces DMDS.Due to Na2S2Easily
In the reasons such as decomposing, there is side reaction in DMDS production process, generates useless containing dimethyl sulfide and dimethyl mercaptan
Gas seriously pollutes environment.It is solved for this reason, it may be necessary to design corresponding technical solution and give.
Summary of the invention
The present invention be directed to the shortcomings of the prior art, provide a kind of dimethyl disulfide synthesis waste gas treatment process,
It solves the problems, such as above-mentioned background technique, meets actual operation requirements.
To solve the above problems, the technical solution used in the present invention is as follows:
A kind of the step of dimethyl disulfide synthesis waste gas treatment process, the treatment process, is as follows:
Step 1, condensation: the exhaust gas generated in dimethyl disulfide synthesis process is carried out to be condensed into waste liquid；
Step 2, separation: waste liquid is separated into oil reservoir and water layer, and (wherein, oil reservoir contains a large amount of DMS and a small amount of dimethyl
Mercaptan, DMDS), collect its water layer liquid being directly separated away；
Step 3, distillation: distilling the oil reservoir liquid that step 2 obtains, collect the DMS distilled out, spare；
Step 4, oxidation: the addition acetone and hydrogen peroxide into above-mentioned fraction, using acetone as solvent, with hydrogen peroxide by fraction
(main component are as follows: dimethyl sulfide) is oxidized to DMSO, and main chemical reactions formula is as follows:
CH3SCH3+H2O2-- acetone -- CH3SOCH3+H2O；
Step 5, rectifying: carrying out rectifying to the reaction solution of step 4, the acetone and vapor that then Fractional Collections rectifying goes out,
Obtain sticky oily transparency liquid；
Step 6, vacuum distillation: fraction is collected, crude product DMSO is obtained；
Step 7, decompression filter: a certain amount of calcium oxide be added into the crude product DMSO that step 6 obtains and carries out decompression suction filtration,
Fine work DMSO is made.
Compared with prior art, implementation result of the invention is as follows by the present invention:
This programme, using hydrogen peroxide as oxidant, not only realizes and exhaust gas is effectively treated using acetone as solvent, and in exhaust gas
The recycling yield of DMSO reaches 88.6%, is not necessarily to acid-base neutralization, and directly distillation obtains, and circulation can be recycled using the low boiling point of acetone
It uses, makes to be preferably minimized environment, reached the standard of industrial discharge.
Detailed description of the invention
Fig. 1 is waste-gas treatment process flow schematic diagram of the present invention.
Specific embodiment
Illustrate the contents of the present invention below in conjunction with specific embodiments.
The method for producing DMDS in the prior art has: methyl mercaptan method, halogenated hydrocarbons method, dimethyl sulfate method.Dimethyl suflfate
Raw material used in method is easy to get, and process flow is simpler, and product cost is lower, is the method generallyd use both at home and abroad, and principle is:
First with Na2S and sulphur are waste Na2S2, then in Na2S2Solution in be added dimethyl suflfate, etherificate produces DMDS.By
In Na2S2The reasons such as easily decomposes have side reaction in DMDS production process, generate and contain dimethyl sulfide and dimethyl
The exhaust gas of mercaptan, seriously pollutes environment.To solve above-mentioned exhaust pollution problems, adopt the following technical solutions, as shown in Figure 1: for
Waste-gas treatment process flow schematic diagram of the present invention.
Embodiment: dimethyl disulfide synthesizes waste gas treatment process, and the step for the treatment of process is as follows:
Step 1, condensation: the exhaust gas generated in dimethyl disulfide synthesis process is passed through in drainer, then will be passed through
Waste liquid is condensed under the drainer merging liquid nitrogen environment of exhaust gas, usual liquid nitrogen environment temperature is -48 DEG C-(- 72) DEG C, condensation time
For until exhaust gas becomes waste liquid completely；
Step 2, separation: above-mentioned waste liquid being placed in knockout drum, stands 10-30min after stirring, lower section oil reservoir and upper occurs
Square water layer, then using separatory funnel separation oil-yielding stratum and water layer, (wherein, oil reservoir contains a large amount of DMS and a small amount of dimethyl disulfide
Alcohol, DMDS)；
Step 3, distillation: the oil reservoir liquid that step 2 obtains is distilled using cucurbit (in distillation process, using ice
Salt water is condensed back), usual vapo(u)rizing temperature is 42 DEG C -72 DEG C, and collecting the fraction that distills out, (temperature of fraction is usually 38
DEG C -42 DEG C), i.e., are as follows: DMS, it is spare；
Step 4, oxidation: (thermometer and blender will be housed) on flask in above-mentioned spare fraction merging flask, then
Acetone is added, it, under agitation will burning using acetone as solvent, then with constant pressure funnel with suitable flow instillation hydrogen peroxide
Bottle is placed in ice water under cooling using collet mode, is controlled certain reaction temperature and time, is reacted it, work as hydrogen peroxide
It is added dropwise and continues stirring until reaction temperature drops to 10 DEG C hereinafter, stopping stirring；Wherein, main with hydrogen peroxide oxidation fraction
Chemical equation is as follows:
CH3SCH3+H2O2-- acetone -- CH3SOCH3+H2O；
Step 5, rectifying: rectifying is carried out to the reaction solution of step 4 and (has been built into capillary in flask, has been prevented instead of zeolite
There is bumping phenomenon), it is then condensed back using brine ice, the acetone and vapor that Fractional Collections rectifying goes out obtain sticky
Oily transparency liquid；
Step 6, vacuum distillation: vacuum collecting fraction, obtain crude product DMSO (vacuum degree are as follows: 0.086MPa, temperature are as follows:
100-110℃)；
Step 7, decompression filter: a certain amount of calcium oxide be added into the crude product DMSO that step 6 obtains and carries out decompression suction filtration,
Fine work DMSO is made.
This programme, using hydrogen peroxide as oxidant, not only realizes and exhaust gas is effectively treated using acetone as solvent, and in exhaust gas
The recycling yield of DMSO reaches 88.6%, is not necessarily to acid-base neutralization, and directly distillation obtains, and circulation can be recycled using the low boiling point of acetone
It uses, makes to be preferably minimized environment, reached the standard of industrial discharge.
The foregoing is a detailed description of the present invention in conjunction with specific embodiments, and it cannot be said that the present invention is specifically real
It applies and is only limitted to these explanations.For those skilled in the art to which the present invention belongs, before not departing from present inventive concept
It puts, a number of simple deductions or replacements can also be made, all shall be regarded as belonging to the scope of protection of the invention.
Claims (1)
1. a kind of the step of dimethyl disulfide synthesis waste gas treatment process, the treatment process, is as follows:
Step 1, condensation: the exhaust gas generated in dimethyl disulfide synthesis process is carried out to be condensed into waste liquid；
Step 2, separation: by waste liquid be separated into oil reservoir and water layer (wherein, oil reservoir contain a large amount of DMS and a small amount of dimethyl mercaptan,
DMDS), its water layer liquid being directly separated away is collected；
Step 3, distillation: distilling the oil reservoir liquid that step 2 obtains, collect the DMS distilled out, spare；
Step 4, oxidation: acetone and hydrogen peroxide being added into above-mentioned fraction, with hydrogen peroxide that fraction is (main using acetone as solvent
Ingredient are as follows: dimethyl sulfide) it is oxidized to DMSO, main chemical reactions formula is as follows:
CH3SCH3+H2O2-- acetone -- CH3SOCH3+H2O；
Step 5, rectifying: rectifying is carried out to the reaction solution of step 4, the acetone and vapor that then Fractional Collections rectifying goes out obtain
Sticky oily transparency liquid；
Step 6, vacuum distillation: fraction is collected, crude product DMSO is obtained；
Step 7, decompression filter: a certain amount of calcium oxide is added into the crude product DMSO that step 6 obtains and carries out decompression suction filtration, is made
Fine work DMSO.
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| CN201910549963.XA CN110229086A (en) | 2019-06-24 | 2019-06-24 | A kind of dimethyl disulfide synthesis waste gas treatment process |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113979906A (en) * | 2021-11-16 | 2022-01-28 | 北京工商大学 | Simple method for preparing dimethyl disulfide and deuterated dimethyl disulfide |
-
2019
- 2019-06-24 CN CN201910549963.XA patent/CN110229086A/en active Pending
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113979906A (en) * | 2021-11-16 | 2022-01-28 | 北京工商大学 | Simple method for preparing dimethyl disulfide and deuterated dimethyl disulfide |
| CN113979906B (en) * | 2021-11-16 | 2023-10-27 | 北京工商大学 | Simple and convenient method for preparing dimethyl disulfide and deuterated dimethyl disulfide |
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