CN102659648B - Method and system for separating mixed liquid containing dimethyl sulfide and methyl mercaptan - Google Patents
Method and system for separating mixed liquid containing dimethyl sulfide and methyl mercaptan Download PDFInfo
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- CN102659648B CN102659648B CN201210132039.XA CN201210132039A CN102659648B CN 102659648 B CN102659648 B CN 102659648B CN 201210132039 A CN201210132039 A CN 201210132039A CN 102659648 B CN102659648 B CN 102659648B
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- pressure distillation
- dimethyl sulfide
- thiomethyl alcohol
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/50—Improvements relating to the production of bulk chemicals
- Y02P20/582—Recycling of unreacted starting or intermediate materials
Abstract
The invention relates to a method and system for separating mixed liquid containing dimethyl sulfide and methyl mercaptan. The mixed liquid is composed of 1-10%wt of methyl mercaptan, 40-60%wt of dimethyl sulfide, 20-40%wt of methanol and the balance water. The method comprises the following steps: pumping the mixed liquid into a feeding port of a low-pressure distillation tower, wherein the operation pressure of the low-pressure distillation tower is 0.1-0.5MPaA and the operation temperature is 40-100 DEG C; obtaining a product containing dimethyl sulfide and methyl mercaptan from the top of the low-pressure distillation tower; obtaining a mixture containing methanol and water from the bottom of the low-pressure distillation tower; pumping the product containing dimethyl sulfide into the feeding port of a high-pressure distillation tower, wherein the operation pressure of the high-pressure distillation tower is 0.6-1.0MPaA and the operation temperature is 60-150 DEG C; obtaining the material containing methyl mercaptan from the top of the high-pressure distillation tower; and obtaining the dimethyl sulfide product from the bottom of the high-pressure distillation tower. According to the method provided by the invention, the dimethyl sulfide and the methyl mercaptan are effectively separated and purified; the process is simple; the environmental pollution is reduced; the raw materials are fully recycled; the cost is saved; and the dimethyl sulfide product with high purity is obtained.
Description
Technical field
The present invention relates to separate the mixed solution that contains dimethyl sulfide and thiomethyl alcohol.
Background technology
Thiomethyl alcohol is a kind of important organic synthesis intermediate, synthetic materials, feed, agricultural chemicals and medical aspect have a wide range of applications.Have been widely used in fields such as fodder industry, medicine industry, foodstuffs industry, health care industry taking thiomethyl alcohol as the synthetic methionine(Met) of raw material.The synthetic method of thiomethyl alcohol is a lot, and the gas-phase reaction of the industrial general heterogeneous catalyst by methyl alcohol and hydrogen sulfide is prepared thiomethyl alcohol.In the product obtaining, except thiomethyl alcohol, also contain reaction by-product dimethyl sulfide and the material benzenemethanol etc. of complete reaction not in preparation process, because thiomethyl alcohol and methyl alcohol, dimethyl sulfide and methyl alcohol easily form azeotrope, can not realize its effective separating-purifying by conventional distillation method.Part thiomethyl alcohol and dimethyl sulfide are directly regarded refuse processing, well do not recycle; Or purified by the technique of more complicated, thereby increase cost.
Summary of the invention
The object of the invention is to one of problem solving above-mentioned existence, provide the method for the mixed solution that a kind of separation contains dimethyl sulfide and thiomethyl alcohol, by low high pressure two stage rectification Optimizing Process Parameters etc., separating-purifying dimethyl sulfide and thiomethyl alcohol.
According to a first aspect of the invention, provide the method for the mixed solution that a kind of separation contains dimethyl sulfide and thiomethyl alcohol, the consisting of of this mixed solution: thiomethyl alcohol content 1-10%wt; Dimethyl sulfide content 40-60%wt; Methanol content 20-40%wt; And surplus is water, the method comprising the steps of:
This mixed solution is pumped into the opening for feed of low-pressure distillation column, the working pressure of this low-pressure distillation column is 0.1-0.5MPaA, service temperature is 40-100 DEG C, obtain the product that contains dimethyl sulfide and thiomethyl alcohol from the top of low-pressure distillation column, and obtain the mixture that contains first alcohol and water from the bottom of low-pressure distillation column; And the product that contains dimethyl sulfide is pumped into the opening for feed of high pressure distillation tower, the working pressure of this high pressure distillation tower is 0.6-1.0MPaA, service temperature 60-150 DEG C, obtains the discharging containing thiomethyl alcohol, and obtains dimethyl sulfide product from the bottom of high pressure distillation tower from the top of high pressure distillation tower.
Preferably, wherein the working pressure of low-pressure distillation column is 0.2-0.4MPaA, more preferably 0.33MPaA, and service temperature is 60-90 DEG C, more preferably 78 DEG C; The working pressure of this high pressure distillation tower is 0.6-0.8MPaA, more preferably 0.72MPaA, and service temperature is 70-120 DEG C, more preferably 98 DEG C.
The content of the dimethyl sulfide the product that contains dimethyl sulfide and thiomethyl alcohol preferably, wherein obtaining from the top of low-pressure distillation column is 50-70%wt.
Preferably, the purity that wherein obtains dimethyl sulfide product from the bottom of high pressure distillation tower is more than 99.5%wt.
Preferably, the mixture that contains first alcohol and water wherein obtaining from the bottom of low-pressure distillation column, methanol content is more than 70%wt.
Preferably, wherein obtain from the top of high pressure distillation tower containing thiomethyl alcohol content the discharging of thiomethyl alcohol more than 80%wt.
Preferably, wherein also obtain the material containing dimethyl sulfide from the side line of high pressure distillation tower, should be recycled the opening for feed that is back to low-pressure distillation column containing the material of dimethyl sulfide.Preferably, the content containing dimethyl sulfide the material of dimethyl sulfide wherein obtaining from the side line of high pressure distillation tower is 50-60%wt.
Preferably, wherein this mixed solution comes from thiomethyl alcohol building-up process, and the mixture that contains first alcohol and water obtaining from the bottom of low-pressure distillation column is recycled and sends into synthesizing for thiomethyl alcohol thiomethyl alcohol synthesizer as raw material.
Preferably, wherein this mixed solution comes from thiomethyl alcohol building-up process, and what obtain from the top of high pressure distillation tower is recycled and the opening for feed of sending into thiomethyl alcohol distillation tower, carries out distilation containing the discharging of thiomethyl alcohol.
According to a second aspect of the invention, provide the system of the mixed solution that a kind of separation contains dimethyl sulfide and thiomethyl alcohol, having comprised:
Thiomethyl alcohol distillation tower, receives thiomethyl alcohol and byproduct thereof from thiomethyl alcohol synthesizer, discharges thiomethyl alcohol product and discharge the mixed solution that contains dimethyl sulfide and thiomethyl alcohol at the bottom of tower from tower top;
Low-pressure distillation column, receive the mixed solution that contains dimethyl sulfide and thiomethyl alcohol of discharging from the bottom of the tower of thiomethyl alcohol distillation tower, discharge from the top of low-pressure distillation column the product that contains dimethyl sulfide and thiomethyl alcohol, and discharge from the bottom of low-pressure distillation column the mixture that contains first alcohol and water; And
High pressure distillation tower, receives the product that contains dimethyl sulfide and thiomethyl alcohol of discharging from the top of low-pressure distillation column, discharges the discharging containing thiomethyl alcohol from the top of high pressure distillation tower, and discharges dimethyl sulfide product from the bottom of high pressure distillation tower,
The material containing dimethyl sulfide of wherein discharging from the side line of high pressure distillation tower is recycled the opening for feed that is back to low-pressure distillation column; The mixture that contains first alcohol and water of discharging from the bottom of low-pressure distillation column is recycled and sends into synthesizing for thiomethyl alcohol thiomethyl alcohol synthesizer as raw material; And the discharging containing thiomethyl alcohol of discharging from the top of high pressure distillation tower is recycled the opening for feed of sending into thiomethyl alcohol distillation tower.
The method of the mixed solution that separation of the present invention contains dimethyl sulfide and thiomethyl alcohol is by rationally setting technique and parameter etc., effectively separating-purifying dimethyl sulfide and thiomethyl alcohol, and technique is simple, be easy to realize, both reduced environmental pollution, abundant recycle starting material, have saved cost again, can also obtain the dimethyl sulfide product that purity is high simultaneously.
Brief description of the drawings
Fig. 1 is the exemplary process flow figure of the separation of the present invention mixed solution that contains dimethyl sulfide and thiomethyl alcohol.
Embodiment
Below in conjunction with the drawings and specific embodiments, describe content of the present invention in detail.
The exemplary process flow figure of the mixed solution that contains dimethyl sulfide and thiomethyl alcohol referring to the separation of Fig. 1.Come from the opening for feed that the thiomethyl alcohol of thiomethyl alcohol synthesizer 1 and byproduct 11 thereof are admitted to thiomethyl alcohol distillation tower 2 after separate hydrogen sulfide, according to a conventional method after distillation, obtain in the tower top discharging of thiomethyl alcohol distillation tower 2 thiomethyl alcohol 12 that purity is higher, at the bottom of the tower of thiomethyl alcohol distillation tower 2, obtain the mixed solution 13 that contains dimethyl sulfide and thiomethyl alcohol, in this mixed solution 13, thiomethyl alcohol content is that 1-10%wt, dimethyl sulfide content are that 40-60%wt, methanol content are 20-40%wt, all the other are moisture.Reclaim thiomethyl alcohol and the methyl alcohol in this mixed solution 13 by following technique, and the dimethyl sulfide of purifying wherein, various resources are not wasted, not only economy but also environmental protection.
Mixed solution 13 pumps into the opening for feed of low-pressure distillation column 3 after surge tank (not shown), at the bottom of the tower of low-pressure distillation column 3, obtain the mixture 14 that contains first alcohol and water, more than wherein methanol content can reach 70%wt, mixture 14 can be delivered to the raw material as synthesis of methyl mercaptan in thiomethyl alcohol synthesizer 1 and recycle.
Obtain at the tower top of low-pressure distillation column 3 product 15 that dimethyl sulfide content is 50-70%wt, this product 15 is pumped into the opening for feed of high pressure distillation tower 4, at the bottom of the tower of high pressure distillation tower 4, can obtain purity is dimethyl sulfide product 16 more than 99.5%wt.There is a small amount of discharging 17 at the tower top of high pressure distillation tower 4, more than wherein thiomethyl alcohol content reaches 80%wt, discharging 17 is recycled in thiomethyl alcohol distillation tower 2 and is purified.In the material 18 of the side line extraction of high pressure distillation tower 4, the content of dimethyl sulfide can reach 50-60%wt, and the opening for feed that material 18 is turned back to low-pressure distillation column 3 continues fractionation by distillation.
It will be appreciated by those skilled in the art that above-described embodiment is only for explaining the present invention but not for making any restriction to it.
Claims (3)
1. a method for the mixed solution that separation contains dimethyl sulfide and thiomethyl alcohol, the consisting of of this mixed solution: thiomethyl alcohol content 1-10%wt; Dimethyl sulfide content 40-60%wt; Methanol content 20-40%wt; And surplus is water, the method comprising the steps of:
This mixed solution is pumped into the opening for feed of low-pressure distillation column, the working pressure of this low-pressure distillation column is 0.1-0.5MPaA, service temperature is 40-100 DEG C, obtain the product that contains dimethyl sulfide and thiomethyl alcohol from the top of low-pressure distillation column, wherein the content of dimethyl sulfide is 50-70%wt, and obtain the mixture that contains first alcohol and water from the bottom of low-pressure distillation column, wherein methanol content is more than 70%wt; And the product that contains dimethyl sulfide is pumped into the opening for feed of high pressure distillation tower, the working pressure of this high pressure distillation tower is 0.6-1.0MPaA, service temperature 60-150 DEG C, obtain the discharging containing thiomethyl alcohol from the top of high pressure distillation tower, in discharging, thiomethyl alcohol content is more than 80%wt, and obtain dimethyl sulfide product from the bottom of high pressure distillation tower, the purity of dimethyl sulfide product is more than 99.5%wt, wherein also obtain the material containing dimethyl sulfide from the side line of high pressure distillation tower, should be recycled the opening for feed that is back to low-pressure distillation column containing the material of dimethyl sulfide;
Wherein this mixed solution comes from thiomethyl alcohol building-up process, the mixture that contains first alcohol and water obtaining from the bottom of low-pressure distillation column is recycled and sends into thiomethyl alcohol synthesizer synthetic for thiomethyl alcohol as raw material, and the discharging containing thiomethyl alcohol obtaining from the top of high pressure distillation tower is recycled carries out distilation the opening for feed of sending into thiomethyl alcohol distillation tower.
2. the process of claim 1 wherein that the working pressure of low-pressure distillation column is 0.2-0.4MPaA, service temperature is 60-90 DEG C; The working pressure of this high pressure distillation tower is 0.6-0.8MPaA, and service temperature is 70-120 DEG C.
3. a device for the mixed solution that separation contains dimethyl sulfide and thiomethyl alcohol, comprising:
Thiomethyl alcohol distillation tower, receives thiomethyl alcohol and byproduct thereof from thiomethyl alcohol synthesizer, discharges thiomethyl alcohol product and discharge the mixed solution that contains dimethyl sulfide and thiomethyl alcohol at the bottom of tower from tower top;
Low-pressure distillation column, receive the mixed solution that contains dimethyl sulfide and thiomethyl alcohol of discharging from the bottom of the tower of thiomethyl alcohol distillation tower, discharge from the top of low-pressure distillation column the product that contains dimethyl sulfide and thiomethyl alcohol, and discharge from the bottom of low-pressure distillation column the mixture that contains first alcohol and water; And
High pressure distillation tower, receives the product that contains dimethyl sulfide and thiomethyl alcohol of discharging from the top of low-pressure distillation column, discharges the discharging containing thiomethyl alcohol from the top of high pressure distillation tower, and discharges dimethyl sulfide product from the bottom of high pressure distillation tower,
The material containing dimethyl sulfide of wherein discharging from the side line of high pressure distillation tower is recycled the opening for feed that is back to low-pressure distillation column; The mixture that contains first alcohol and water of discharging from the bottom of low-pressure distillation column is recycled and sends into synthesizing for thiomethyl alcohol thiomethyl alcohol synthesizer as raw material; And the discharging containing thiomethyl alcohol of discharging from the top of high pressure distillation tower is recycled the opening for feed of sending into thiomethyl alcohol distillation tower.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN201210132039.XA CN102659648B (en) | 2012-04-28 | 2012-04-28 | Method and system for separating mixed liquid containing dimethyl sulfide and methyl mercaptan |
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| CN201210132039.XA CN102659648B (en) | 2012-04-28 | 2012-04-28 | Method and system for separating mixed liquid containing dimethyl sulfide and methyl mercaptan |
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| CN102659648A CN102659648A (en) | 2012-09-12 |
| CN102659648B true CN102659648B (en) | 2014-07-30 |
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Families Citing this family (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN112552217A (en) * | 2020-12-26 | 2021-03-26 | 查都(海南)科技有限公司 | Methyl mercaptan purification device |
| CN114478334B (en) * | 2022-02-25 | 2023-11-10 | 新疆广汇陆友硫化工有限公司 | Method for producing dimethyl disulfide by methyl mercaptan vulcanization |
| CN114591205A (en) * | 2022-03-26 | 2022-06-07 | 河南君合新材料科技有限公司 | Process for joint production of methyl mercaptan and methyl sulfide |
| CN114702420A (en) * | 2022-05-07 | 2022-07-05 | 宁夏紫光天化蛋氨酸有限责任公司 | Method for separating methyl mercaptan and dimethyl sulfide |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3935276A (en) * | 1973-11-30 | 1976-01-27 | Rhone-Poulenc Industries | Process for the manufacture of methyl mercaptan |
| US4186061A (en) * | 1977-06-24 | 1980-01-29 | Phillips Petroleum Company | Fractionation of methyl-mercaptan reactor effluent |
| US4686009A (en) * | 1985-10-29 | 1987-08-11 | James W. Laney | Distillation system |
| CN1189487A (en) * | 1996-12-27 | 1998-08-05 | 底古萨股份公司 | Process for separating product gas mixture from catalytic synthesis of methyl mercaptan |
| CN1217326A (en) * | 1998-09-03 | 1999-05-26 | 田锡义 | Process for preparing dimethyl thio-ether and methylthio-alcohol |
-
2012
- 2012-04-28 CN CN201210132039.XA patent/CN102659648B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3935276A (en) * | 1973-11-30 | 1976-01-27 | Rhone-Poulenc Industries | Process for the manufacture of methyl mercaptan |
| US4186061A (en) * | 1977-06-24 | 1980-01-29 | Phillips Petroleum Company | Fractionation of methyl-mercaptan reactor effluent |
| US4686009A (en) * | 1985-10-29 | 1987-08-11 | James W. Laney | Distillation system |
| CN1189487A (en) * | 1996-12-27 | 1998-08-05 | 底古萨股份公司 | Process for separating product gas mixture from catalytic synthesis of methyl mercaptan |
| CN1217326A (en) * | 1998-09-03 | 1999-05-26 | 田锡义 | Process for preparing dimethyl thio-ether and methylthio-alcohol |
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Effective date of registration: 20160602 Address after: 755000 Ningxia central defence industrial park Patentee after: NINGXIA ZIGUANG TIANHUA METHIONINE CO., LTD. Address before: 408200, Chongqing County, Zhenjiang Town, Fengdu village Xiangjiaba Patentee before: Chongqing Unisplendour Tianhua Methionine Co., Ltd. |