CN104275132A - Thioether oxidation tower for producing dimethyl sulfoxide - Google Patents
Thioether oxidation tower for producing dimethyl sulfoxide Download PDFInfo
- Publication number
- CN104275132A CN104275132A CN201410561491.7A CN201410561491A CN104275132A CN 104275132 A CN104275132 A CN 104275132A CN 201410561491 A CN201410561491 A CN 201410561491A CN 104275132 A CN104275132 A CN 104275132A
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- tower
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- thioether
- sub
- dimethyl sulfoxide
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J10/00—Chemical processes in general for reacting liquid with gaseous media other than in the presence of solid particles, or apparatus specially adapted therefor
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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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- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention discloses a thioether oxidation tower for producing dimethyl sulfoxide, for solving the problems of the existing oxidation tower that liquid level in the tower is not stable, safety is poor, the content of nitric oxide in tail gas is high, and the control difficulty is high. According to the technical scheme of the invention, the thioether oxidation tower comprises a tower body; the tower body is divided into a heating area, a reaction area, a sub-cooling area and a cooling area from bottom to top; each of the reaction area, the sub-cooling area and the cooling area is internally provided with a cooling water coil pipe and a cooling water jacket on the wall of the tower; the heating area is provided with an oxidation air inlet; the reaction area is provided with a thioether feeding point; a tail gas outlet is formed at the upper section of the cooling area; the sub-cooling area is provided with a sulfoxide outlet under the liquid level; the upper section of the sub-cooling area is provided with a compressed air inlet. The thioether oxidation tower is simple in structure, simple and convenient to operate, good in reliability and low in oxidizing temperature; in addition, the liquid level in the tower is stable, no gas-phase reaction is generated and the content of nitric oxide in the tail gas is low.
Description
Technical field
The present invention relates to a kind of reaction tower of chemical industry, specifically a kind of production dimethyl sulfoxide (DMSO) sulfide oxidation tower.
Background technology
It is mainly raw material synthesizing dimethyl thioether (abbreviation thioether) under the effect of catalyst with hydrogen sulfide (or carbon disulfide) with methyl alcohol that the dimethyl sulfoxide (DMSO) (abbreviation sulfoxide) of current industrial comparative maturity is produced, thioether carries out oxidation reaction with oxic gas (gaseous mixture of oxygen and nitrogen oxide, nitrogen oxide is the gaseous mixture of nitrogen dioxide or nitric oxide and nitrogen dioxide) again and generates sulfoxide.
Existing sulfide oxidation tower is deposited following with problem: the outlet of (1) sulfoxide is arranged at the bottom of tower, generally outside tower, all arranges an inverted U pipe, and sulfoxide is sulfoxide outlet at the bottom of tower, then discharges oxidizing tower through inverted U pipe.If discharge nozzle blocking or the fluctuation of tower pressure, all can cause liquid level instability (even void tower) in tower; (2) in tail gas, content of nitric oxide is high, causes follow-up vent gas treatment operation difficulty; (3) oxidizing temperature is high, and temperature reaches more than 75 DEG C, easily causes the generation of gas-phase reaction, and the risk of thus blasting is higher.(5) reaction zone temperature control difficulty is larger.
Summary of the invention
The object of the invention is to solve the problems of the technologies described above, there is provided that a kind of structure is simple, easy and simple to handle, level stability in good reliability, tower, oxidizing temperature is low, without the production dimethyl sulfoxide (DMSO) sulfide oxidation tower that content of nitric oxide in gas-phase reaction generation, tail gas is low.
Technical scheme comprises tower body, described tower body is divided into heating region, reaction zone, sub-cold-zone and cooling zone from the bottom to top, cooling water jecket on cooling water coil and tower wall is equipped with in described reaction zone, sub-cold-zone and cooling zone, described heating region is provided with oxic gas import, reaction zone is provided with thioether charging layer, cooling zone epimere is provided with offgas outlet, the position that described sub-cold-zone is positioned at below liquid level is provided with sulfoxide outlet, and described sub-cold-zone epimere is provided with compressed air inlet.
Described sulfoxide outlet is positioned at below liquid level 100 ~ 500mm.
Be provided with gas distributor in the epimere tower of described sub-cold-zone, described compressed air inlet is connected with described gas distributor.
Described sub-cold-zone hypomere is provided with packing layer.
The thickness of described packing layer is 300mm ~ 500mm.
Described reaction zone hypomere has the upper and lower two-layer thioether feed points of different vertical height.
The vertical range of described lower thioether charging layer distance heating region end face is 150mm ~ 300mm, and the vertical drop of upper thioether charging layer and lower thioether charging layer is at 300mm ~ 600mm.
Described heating region temperature controls between 43 ~ 55 DEG C, and the temperature of described reaction zone controls between 38 ~ 50 DEG C; The temperature of described sub-cold-zone controls between 35 ~ 47 DEG C; The temperature of described cooling zone controls between 28 ~ 38 DEG C.
Described heating region tower wall is provided with hot water jacket.
Inventor analyses in depth existing sulfide oxidation tower Problems existing, and it is improved, first sulfoxide is exported by being changed to the liquid level of sub-cold-zone at the bottom of tower with upper/lower positions, export under moving to fluid level by making sulfoxide, effectively can solve the problem of liquid level instability in tower, also without the need to using inverted U pipe, the generation of inverted U blockage problem is avoided.Liquid level 100 ~ 500mm in preferred described sulfoxide outlet distance tower, higher apart from liquid level in excessive then tower, make the separated space of tail gas less than normal, in too small then tower, liquid level is on the low side, makes reaction mother liquor amount on the low side, is unfavorable for absorption and the reaction of nitrogen dioxide; Inventor sets up compressed air inlet at sub-cold-zone epimere simultaneously, pass into air and can make bubbling and oxidation reaction occurs further for the nitric oxide in the tail gas gone out and the oxygen in air, content of nitric oxide in tail gas is declined, for follow-up vent gas treatment is provided convenience, nitrogen simultaneously in air reduces the concentration of nitrogen dioxide and thioether in tail gas, reduce the generation of gas-phase reaction, add the security of oxidizing process.In order to ensure to enter being uniformly distributed of tower compressed air, compressed air inlet being connected with gas distributor, making compressed air and tail gas Homogeneous phase mixing by gas distributor, fast fully reaction.
Further, inventor sets up packing layer at sub-cold-zone hypomere, makes gas-liquid mixture from reaction zone through packing layer, gas under the help of packing layer better by liquid in separate out, improve gas-liquid separation effect, described packing layer can select stainless steel Pall ring filler.The height of described packing layer preferably controls at 300mm ~ 500mm, packing layer thickness crosses the pressure drop that conference strengthens gas, packing layer thickness is too small, can not ensure the separating effect of gas-liquid, makes to discharge nitrogen dioxide content in sulfoxide bigger than normal, strengthens the load of subsequent handling.
Further, because reaction zone is reaction generating region, it is large that its temperature controls difficulty, in order to ensure that temperature controls in scope of design, under the prerequisite that original control device is constant, inventor provide the temperature control means newly increased, namely the upper and lower two-layer thioether feed points of different vertical height is set at reaction zone hypomere.During normal production; the charging simultaneously of upper and lower thioether charging layer; often oxidizing tower reaction zone temperature can be caused to raise due to the impact of upstream process aborning; upper thioether charging layer can be just utilized to adjust the inlet amount of thioether like this; reduce the carrying out of oxidation reaction; thus reduce reaction liberated heat, thus reach the object reducing tower temperature.Can control the inlet amount of upper thioether charging layer according to the temperature of reaction zone, the temperature as reaction zone is too high, then can turn down thioether charging layer, inlet amount is declined, if desired all right complete shut-down, otherwise then can open thioether charging layer.By said structure and simple adjustment method, the method for another effective regulation and control reaction zone temperature can be increased, avoid the excessive safety problem brought of temperature fluctuation in reaction zone.
Inventor Hai Duige district temperature adjusts, each district temperature entire lowering, the control of temperature controls by the cooling water inflow adjusting cooling water coil and the cooling water jecket arranged in each district, the maximum temperature of reaction zone controls below 50 DEG C, avoids overheatedly causing the generation of gas-phase reaction and the danger of blast.
Beneficial effect:
Structure of the present invention is simple, can carry out simple transformation to existing equipment can produce obvious technique effect, level stability in tower, and oxidizing temperature is low, and low without content of nitric oxide in gas-phase reaction generation, tail gas, security is good.
Accompanying drawing explanation
Fig. 1 is structural representation of the present invention.
Wherein, thioether feed points, 6-compressed air inlet, the outlet of 7-sulfoxide, 8-air gas distributor, 9-packing layer, 10-hot water jacket, 11-cooling water jecket, 12-demister, 13-oxic gas gas distributor under 1-tower body, 2-cooling water coil, the import of 3-oxic gas, 4-offgas outlet, the upper thioether feed points of 5.1-, 5.2-.A-oxic gas, B-thioether, C-sulfoxide, D-compressed air, E-tail gas, F-heating region, G-reaction zone, the sub-cold-zone of H-, I-cooling zone.
Detailed description of the invention
Below in conjunction with accompanying drawing, explanation is further explained to the present invention:
See Fig. 1, tower body is followed successively by heating region F, reaction zone G, sub-cold-zone H and cooling zone I from the bottom to top, cooling water coil is equipped with in described reaction zone G, sub-cold-zone H and cooling zone I, tower wall is provided with cooling water jecket 11, is provided with the hot water jacket 10 on oxic gas gas distributor 13 and tower wall in described heating region.
Described heating region F is provided with the oxic gas import 3 be connected with oxic gas gas distributor 13, described reaction zone G hypomere has the upper thioether charging layer 5.1 of different vertical height and lower thioether charging layer 5.2, described lower thioether charging layer 5.2 is 150mm ~ 300mm apart from the vertical range of heating region F end face, and the vertical drop of upper thioether charging layer 5.1 and lower thioether charging layer 5.2 is between 300mm ~ 600mm.Cooling zone I epimere is provided with offgas outlet 4, and the position that described sub-cold-zone H is positioned at below liquid level is provided with sulfoxide outlet 7, distance liquid level 100 ~ 500mm.Described sub-cold-zone H epimere is provided with compressed air inlet 6, and described compressed air inlet 6 is connected with air gas distributor 8.Described sub-cold-zone H hypomere is provided with packing layer 9, and the thickness of described packing layer 9 is 300mm ~ 500mm.
Operation principle:
Oxic gas (the gaseous mixture of oxygen and nitrogen oxide, described nitrogen oxide is the gaseous mixture of nitrogen dioxide or nitric oxide and nitrogen dioxide) A enters in oxidizing tower through oxic gas import 3 and oxic gas gas distributor 13, be uniformly distributed in tower, heat up in heating region, enter reaction zone G subsequently, thioether is through upper, lower thioether charging layer 5.1, 5.2 enter reaction zone G hypomere, the two co-current contact in reaction zone G carries out chemical reaction and generates sulfoxide, reacted gas-liquid mixture rises and enters the packing layer 9 of sub-cold-zone H hypomere, under the effect of filler, gas-liquid is separated rapidly, gas rises at sub-cold-zone H liquid level bubbling and forms tail gas, the liquid sulfoxide be separated discharges oxidizing tower (without the need to using inverted U pipe) from the sulfoxide outlet 7 below liquid level, from tower body top, sub-cold-zone H discharges sulfoxide and can well ensure the stable of liquid level in tower.Compressed air (pressure is 0.2MPa ~ 0.5MPa gauge pressure) through being positioned at sub-cold-zone H epimere compressed air inlet 6 again through air gas distributor 8 be uniformly distributed in Ta Nei and cooling zone I and rising tail gas Homogeneous phase mixing and react, reduce the content of nitric oxide in tail gas, the tail gas after compressed air-treatment removes after mist through demister 8 and discharges oxidizing tower by the offgas outlet 4 of cooling zone I epimere.
The tower wall of described heating region F is provided with hot water jacket 10 for heating materials at bottom of tower, ensures that heating region F temperature maintains between 43-55 DEG C;
Other each district is equipped with cooling water jecket 11 on cooling water coil 2 and tower wall for controlling reaction temperature and being reacted gas-liquid mixture cooling, and reaction zone G can adopt segmentation (three sections or multistage) to cool, the method for temperature control to be separately to ensure that the temperature of reaction zone maintains between 38 ~ 50 DEG C; The temperature of sub-cold-zone H maintains between 35 ~ 47 DEG C; The temperature of cooling zone I maintains between 28 ~ 38 DEG C.
When the temperature of reaction zone G is more than 50 DEG C, the flow of upper thioether feed points 5.1 can be reduced, when the temperature of reaction zone G is more than 55 DEG C, can closes and close temperature in thioether feed points 5.1 to tower and return back in design temperature, avoid the too high risk of explosion brought of temperature.
Claims (9)
1. produce dimethyl sulfoxide (DMSO) sulfide oxidation tower for one kind, comprise tower body, described tower body is divided into heating region, reaction zone, sub-cold-zone and cooling zone from the bottom to top, cooling water jecket on cooling water coil and tower wall is equipped with in described reaction zone, sub-cold-zone and cooling zone, described heating region is provided with oxic gas import, reaction zone is provided with thioether charging, cooling zone epimere is provided with offgas outlet, it is characterized in that, the position that described sub-cold-zone is positioned at below liquid level is provided with sulfoxide outlet, and described sub-cold-zone epimere is provided with compressed air inlet.
2. production dimethyl sulfoxide (DMSO) sulfide oxidation tower as claimed in claim 1, is characterized in that, described sulfoxide outlet is positioned at below liquid level 100 ~ 500mm.
3. production dimethyl sulfoxide (DMSO) sulfide oxidation tower as claimed in claim 1 or 2, it is characterized in that, be provided with gas distributor in the epimere tower of described sub-cold-zone, described compressed air inlet is connected with described gas distributor.
4. production dimethyl sulfoxide (DMSO) sulfide oxidation tower as claimed in claim 1 or 2, it is characterized in that, described sub-cold-zone hypomere is provided with packing layer.
5. production dimethyl sulfoxide (DMSO) sulfide oxidation tower as claimed in claim 4, it is characterized in that, the thickness of described packing layer is 300mm ~ 500mm.
6. production dimethyl sulfoxide (DMSO) sulfide oxidation tower as claimed in claim 1 or 2, it is characterized in that, described reaction zone hypomere has the upper and lower two-layer thioether feed points of different vertical height.
7. production dimethyl sulfoxide (DMSO) sulfide oxidation tower as claimed in claim 6, it is characterized in that, the vertical range of described lower thioether charging layer distance heating region end face is between 150mm ~ 300mm, and the vertical drop of upper thioether charging layer and lower thioether charging layer is between 300mm ~ 600mm.
8. production dimethyl sulfoxide (DMSO) sulfide oxidation tower as claimed in claim 6, it is characterized in that, described heating region temperature controls between 43 ~ 55 DEG C, and the temperature of described reaction zone controls between 38 ~ 50 DEG C; The temperature of described sub-cold-zone controls between 35 ~ 47 DEG C; The temperature of described cooling zone controls between 28 ~ 38 DEG C.
9. production dimethyl sulfoxide (DMSO) sulfide oxidation tower as claimed in claim 1 or 2, it is characterized in that, described heating region tower wall is provided with hot water jacket.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410561491.7A CN104275132A (en) | 2014-10-21 | 2014-10-21 | Thioether oxidation tower for producing dimethyl sulfoxide |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410561491.7A CN104275132A (en) | 2014-10-21 | 2014-10-21 | Thioether oxidation tower for producing dimethyl sulfoxide |
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| CN104275132A true CN104275132A (en) | 2015-01-14 |
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| CN201410561491.7A Pending CN104275132A (en) | 2014-10-21 | 2014-10-21 | Thioether oxidation tower for producing dimethyl sulfoxide |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111039262A (en) * | 2020-01-02 | 2020-04-21 | 黎明化工研究设计院有限责任公司 | Oxidation tower for preparing hydrogen peroxide by anthraquinone process |
Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3647884A (en) * | 1970-03-11 | 1972-03-07 | Toray Industries | Liquid-vapor phase oxidation method for producing dialkyl sulfoxides |
| DE69400047D1 (en) * | 1993-02-22 | 1996-02-15 | Wladimiro Bizzotto | High pressure melamine reactor |
| LT2006089A (en) * | 2004-07-13 | 2007-02-26 | Research & Design Institute Of Urea And Organic Synthesis Products, Joint Stock Company (Oao Niic) | Reactor internal design |
| CN201006419Y (en) * | 2007-01-29 | 2008-01-16 | 煤炭科学研究总院 | Bubbling type heterogemeous reactor |
| CN101460239A (en) * | 2006-06-03 | 2009-06-17 | 鲁奇有限责任公司 | Reactor for the production of C2 to C8 olefins from an oxygenate, water vapor, and one or more material flows containing hydrocarbon |
| CN202490608U (en) * | 2012-02-20 | 2012-10-17 | 兖矿鲁南化肥厂 | Safety production device of dimethyl sulfide oxidizing reaction |
| KR20130132395A (en) * | 2010-07-08 | 2013-12-04 | 아이에프피 에너지스 누벨 | Column with gas distribution and method for characterising an element for bringing gas and liquid into contact |
| CN204182376U (en) * | 2014-10-21 | 2015-03-04 | 武汉江汉化工设计有限公司 | Produce dimethyl sulfoxide (DMSO) sulfide oxidation tower |
-
2014
- 2014-10-21 CN CN201410561491.7A patent/CN104275132A/en active Pending
Patent Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3647884A (en) * | 1970-03-11 | 1972-03-07 | Toray Industries | Liquid-vapor phase oxidation method for producing dialkyl sulfoxides |
| DE69400047D1 (en) * | 1993-02-22 | 1996-02-15 | Wladimiro Bizzotto | High pressure melamine reactor |
| LT2006089A (en) * | 2004-07-13 | 2007-02-26 | Research & Design Institute Of Urea And Organic Synthesis Products, Joint Stock Company (Oao Niic) | Reactor internal design |
| CN101460239A (en) * | 2006-06-03 | 2009-06-17 | 鲁奇有限责任公司 | Reactor for the production of C2 to C8 olefins from an oxygenate, water vapor, and one or more material flows containing hydrocarbon |
| CN201006419Y (en) * | 2007-01-29 | 2008-01-16 | 煤炭科学研究总院 | Bubbling type heterogemeous reactor |
| KR20130132395A (en) * | 2010-07-08 | 2013-12-04 | 아이에프피 에너지스 누벨 | Column with gas distribution and method for characterising an element for bringing gas and liquid into contact |
| CN202490608U (en) * | 2012-02-20 | 2012-10-17 | 兖矿鲁南化肥厂 | Safety production device of dimethyl sulfide oxidizing reaction |
| CN204182376U (en) * | 2014-10-21 | 2015-03-04 | 武汉江汉化工设计有限公司 | Produce dimethyl sulfoxide (DMSO) sulfide oxidation tower |
Non-Patent Citations (1)
| Title |
|---|
| 天津市跃进化工厂: "《二甲基亚砜的制造》", 30 April 1973, 天津人民出版社 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111039262A (en) * | 2020-01-02 | 2020-04-21 | 黎明化工研究设计院有限责任公司 | Oxidation tower for preparing hydrogen peroxide by anthraquinone process |
| CN111039262B (en) * | 2020-01-02 | 2024-06-04 | 黎明化工研究设计院有限责任公司 | Oxidation tower for preparing hydrogen peroxide by anthraquinone process |
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Application publication date: 20150114 |