CN102659648A - 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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- CN102659648A CN102659648A CN201210132039XA CN201210132039A CN102659648A CN 102659648 A CN102659648 A CN 102659648A CN 201210132039X A CN201210132039X A CN 201210132039XA CN 201210132039 A CN201210132039 A CN 201210132039A CN 102659648 A CN102659648 A CN 102659648A
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- pressure distillation
- dimethyl sulfide
- thiomethyl alcohol
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- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
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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 widely and use.With the thiomethyl alcohol is that raw material synthetic methionine(Met) has been widely used in fields such as fodder industry, medicine industry, foodstuffs industry, health care industry.The compound method of thiomethyl alcohol is a lot, in the industry generally the gas-phase reaction of the heterogeneous catalyst through methyl alcohol and hydrogen sulfide prepare thiomethyl alcohol.Except thiomethyl alcohol, also contain the reaction by-product dimethyl sulfide and the material benzenemethanol etc. of complete reaction not in the product that in the preparation process, obtains; Because thiomethyl alcohol and methyl alcohol, dimethyl sulfide and methyl alcohol are prone to form azeotrope, can not realize purifying its effective separation with the conventional distillation method.Part thiomethyl alcohol and dimethyl sulfide are directly regarded waste treatment, well do not recycle; Or it is purified, thereby increased cost through the technology of more complicated.
Summary of the invention
The objective of the invention is to one of problem that solves above-mentioned existence, the method that provides a kind of separation to contain the mixed solution of dimethyl sulfide and thiomethyl alcohol through hanging down the high pressure two stage rectification and optimizing processing parameter etc., is separated purification dimethyl sulfide and thiomethyl alcohol.
According to a first aspect of the invention, the method that provides a kind of separation to contain the mixed solution of 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, and 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 ℃; Obtain containing the product of dimethyl sulfide and thiomethyl alcohol from the top of low-pressure distillation column, and obtain containing the mixture of first alcohol and water from the bottom of low-pressure distillation column; And the product that will contain dimethyl sulfide pumps 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 ℃, obtain containing the discharging of thiomethyl alcohol from the top of high pressure distillation tower, and obtain the dimethyl sulfide product from the bottom of high pressure distillation tower.
Preferably, wherein the working pressure of low-pressure distillation column is 0.2-0.4MPaA, 0.33MPaA more preferably, and service temperature is 60-90 ℃, more preferably 78 ℃; The working pressure of this high pressure distillation tower is 0.6-0.8MPaA, 0.72MPaA more preferably, and service temperature is 70-120 ℃, more preferably 98 ℃.
Preferably, wherein the content of the dimethyl sulfide from the product that contains dimethyl sulfide and thiomethyl alcohol that the top of low-pressure distillation column obtains is 50-70%wt.
Preferably, wherein obtaining the dimethyl sulfide product gas purity from the bottom of high pressure distillation tower is more than the 99.5%wt.
Preferably, wherein from the mixture that contains the first alcohol and water that the bottom of low-pressure distillation column obtains methanol content be more than the 70%wt.
Preferably, wherein from the discharging that contains thiomethyl alcohol that the top of high pressure distillation tower obtains thiomethyl alcohol content more than 80%wt.
Preferably, wherein also obtain containing the material of dimethyl sulfide from the side line of high pressure distillation tower, this material that contains dimethyl sulfide is recycled the opening for feed that is back to low-pressure distillation column.Preferably, wherein from the material that contains dimethyl sulfide that the side line of high pressure distillation tower obtains the content of dimethyl sulfide be 50-60%wt.
Preferably, wherein this mixed solution comes from the thiomethyl alcohol building-up process, and the mixture that contains the first alcohol and water that obtains from the bottom of low-pressure distillation column is recycled to send into as raw material and is used for the synthetic of thiomethyl alcohol the thiomethyl alcohol synthesizer.
Preferably, wherein this mixed solution comes from the thiomethyl alcohol building-up process, and the discharging that contains thiomethyl alcohol that obtains from the top of high pressure distillation tower is recycled the opening for feed of sending into the thiomethyl alcohol distillation tower distills purification.
According to a second aspect of the invention, provide a kind of separation to contain the system of the mixed solution of dimethyl sulfide and thiomethyl alcohol, having comprised:
The thiomethyl alcohol distillation tower receives thiomethyl alcohol and sub product thereof from the thiomethyl alcohol synthesizer, discharges the thiomethyl alcohol product and at the bottom of tower, discharges the mixed solution that contains dimethyl sulfide and thiomethyl alcohol from cat head;
Low-pressure distillation column; The mixed solution that contains dimethyl sulfide and thiomethyl alcohol that reception is discharged at the bottom of the tower of thiomethyl alcohol distillation tower; Discharge the product that contains dimethyl sulfide and thiomethyl alcohol from the top of low-pressure distillation column, and discharge the mixture that contains the first alcohol and water from the bottom of low-pressure distillation column; And
The 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 that contains thiomethyl alcohol from the top of high pressure distillation tower, and discharges the dimethyl sulfide product from the bottom of high pressure distillation tower,
The material that contains 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 the first alcohol and water of discharging from the bottom of low-pressure distillation column is recycled to send into as raw material and is used for the synthetic of thiomethyl alcohol the thiomethyl alcohol synthesizer; And the discharging that contains thiomethyl alcohol of discharging from the top of high pressure distillation tower is recycled the opening for feed of sending into the thiomethyl alcohol distillation tower.
Separation of the present invention contains the method for mixed solution of dimethyl sulfide and thiomethyl alcohol through rationally setting technology and parameter etc.; Can effectively separate purification dimethyl sulfide and thiomethyl alcohol, and technology is simple, is easy to realize; Both reduced environmental pollution; Abundant again recycle starting material have been practiced thrift cost, can also obtain the high dimethyl sulfide product of purity simultaneously.
Description of drawings
Fig. 1 contains the exemplary process flow figure of the mixed solution of dimethyl sulfide and thiomethyl alcohol for separation of the present invention.
Embodiment
Below in conjunction with accompanying drawing and specific embodiment, describe content of the present invention in detail.
The exemplary process flow figure that contains the mixed solution of dimethyl sulfide and thiomethyl alcohol referring to the separation of Fig. 1.Thiomethyl alcohol and the sub product thereof 11 that comes from thiomethyl alcohol synthesizer 1 is through being admitted to the opening for feed of thiomethyl alcohol distillation tower 2 after the separate hydrogen sulfide; After the ordinary method distillation; Cat head discharging at thiomethyl alcohol distillation tower 2 obtains the higher thiomethyl alcohol of purity 12; At the bottom of the tower of thiomethyl alcohol distillation tower 2, obtain containing the mixed solution 13 of dimethyl sulfide and thiomethyl alcohol, 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 in this mixed solution 13.Reclaim thiomethyl alcohol and methyl alcohol in this mixed solution 13 through following technology, and purification dimethyl sulfide wherein, make various resources not be wasted, not only economy but also environmental protection.
Mixed solution 13 pumps into the opening for feed of low-pressure distillation column 3 after the surge tank (not shown); At the bottom of the tower of low-pressure distillation column 3, obtain containing the mixture 14 of first alcohol and water; Wherein methanol content can reach more than the 70%wt, and mixture 14 can deliver to that the raw material as synthesis of methyl mercaptan recycles in the thiomethyl alcohol synthesizer 1.
Cat head at low-pressure distillation column 3 obtains the product 15 that dimethyl sulfide content is 50-70%wt, and this product 15 is pumped into the opening for feed of high pressure distillation tower 4, and at the bottom of the tower of high pressure distillation tower 4, can obtain purity is the dimethyl sulfide product 16 more than the 99.5%wt.Cat head at high pressure distillation tower 4 has a small amount of discharging 17, and wherein thiomethyl alcohol content reaches more than the 80%wt, discharging 17 is recycled in the thiomethyl alcohol distillation tower 2 purifies.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 the foregoing description only is used to explain the present invention but not is used for it is made any restriction.
Claims (10)
1. a separation contains the method for the mixed solution of 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, and 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 ℃; Obtain containing the product of dimethyl sulfide and thiomethyl alcohol from the top of low-pressure distillation column, and obtain containing the mixture of first alcohol and water from the bottom of low-pressure distillation column; And the product that will contain dimethyl sulfide pumps 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 ℃, obtain containing the discharging of thiomethyl alcohol from the top of high pressure distillation tower, and obtain the dimethyl sulfide product from the bottom of high pressure 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 ℃; The working pressure of this high pressure distillation tower is 0.6-0.8MPaA, and service temperature is 70-120 ℃.
3. the process of claim 1 wherein that the content of the dimethyl sulfide from the product that contains dimethyl sulfide and thiomethyl alcohol that the top of low-pressure distillation column obtains is 50-70%wt.
4. the process of claim 1 wherein that obtaining the dimethyl sulfide product gas purity from the bottom of high pressure distillation tower is more than the 99.5%wt.
5. the process of claim 1 wherein that methanol content is more than the 70%wt from the mixture that contains the first alcohol and water that the bottom of low-pressure distillation column obtains.
6. the process of claim 1 wherein that thiomethyl alcohol content is more than 80%wt from the discharging that contains thiomethyl alcohol that the top of high pressure distillation tower obtains.
7. the process of claim 1 wherein the material that also obtains containing dimethyl sulfide from the side line of high pressure distillation tower, this material that contains dimethyl sulfide is recycled the opening for feed that is back to low-pressure distillation column.
8. the process of claim 1 wherein that this mixed solution comes from the thiomethyl alcohol building-up process, the mixture that contains the first alcohol and water that obtains from the bottom of low-pressure distillation column is recycled to send into as raw material and is used for the synthetic of thiomethyl alcohol the thiomethyl alcohol synthesizer.
9. the process of claim 1 wherein that this mixed solution comes from the thiomethyl alcohol building-up process, the discharging that contains thiomethyl alcohol that obtains from the top of high pressure distillation tower is recycled the opening for feed of sending into the thiomethyl alcohol distillation tower distills purification.
10. a separation contains the system of the mixed solution of dimethyl sulfide and thiomethyl alcohol, comprising:
The thiomethyl alcohol distillation tower receives thiomethyl alcohol and sub product thereof from the thiomethyl alcohol synthesizer, discharges the thiomethyl alcohol product and at the bottom of tower, discharges the mixed solution that contains dimethyl sulfide and thiomethyl alcohol from cat head;
Low-pressure distillation column; The mixed solution that contains dimethyl sulfide and thiomethyl alcohol that reception is discharged at the bottom of the tower of thiomethyl alcohol distillation tower; Discharge the product that contains dimethyl sulfide and thiomethyl alcohol from the top of low-pressure distillation column, and discharge the mixture that contains the first alcohol and water from the bottom of low-pressure distillation column; And
The 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 that contains thiomethyl alcohol from the top of high pressure distillation tower, and discharges the dimethyl sulfide product from the bottom of high pressure distillation tower,
The material that contains 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 the first alcohol and water of discharging from the bottom of low-pressure distillation column is recycled to send into as raw material and is used for the synthetic of thiomethyl alcohol the thiomethyl alcohol synthesizer; And the discharging that contains thiomethyl alcohol of discharging from the top of high pressure distillation tower is recycled the opening for feed of sending into the thiomethyl alcohol distillation tower.
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| 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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| CN102659648B CN102659648B (en) | 2014-07-30 |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112552217A (en) * | 2020-12-26 | 2021-03-26 | 查都(海南)科技有限公司 | Methyl mercaptan purification device |
| CN114478334A (en) * | 2022-02-25 | 2022-05-13 | 新疆广汇陆友硫化工有限公司 | Method for producing dimethyl disulfide by methyl mercaptan vulcanization method |
| 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)
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|---|---|---|---|---|
| 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 | Separation method of product gas mixture for 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 | Separation method of product gas mixture for 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 |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112552217A (en) * | 2020-12-26 | 2021-03-26 | 查都(海南)科技有限公司 | Methyl mercaptan purification device |
| CN114478334A (en) * | 2022-02-25 | 2022-05-13 | 新疆广汇陆友硫化工有限公司 | Method for producing dimethyl disulfide by methyl mercaptan vulcanization method |
| 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 |
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| CN102659648B (en) | 2014-07-30 |
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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. |