CN1042883A - The method for separating and processing of resultant of reaction in the carbon disulphide production process - Google Patents
The method for separating and processing of resultant of reaction in the carbon disulphide production process Download PDFInfo
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- CN1042883A CN1042883A CN 89104115 CN89104115A CN1042883A CN 1042883 A CN1042883 A CN 1042883A CN 89104115 CN89104115 CN 89104115 CN 89104115 A CN89104115 A CN 89104115A CN 1042883 A CN1042883 A CN 1042883A
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- sulphur
- dithiocarbonic anhydride
- hydrogen sulfide
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Abstract
The present invention be a kind of with lower hydrocarbon and sulphur be in the synthetic dithiocarbonic anhydride process of raw material to the method for separating and processing of resultant of reaction, principal feature is to isolate sulphur continuously and once make all liquefaction and finish sepn process with hydrogen sulfide of dithiocarbonic anhydride under the condition of all using reacting system pressure.
Description
What the present invention relates to is to be to the method for separating and processing of resultant of reaction in the raw material production dithiocarbonic anhydride process with rudimentary hydro carbons and sulphur.
With lower hydrocarbon (as being the Sweet natural gas of main component with methane, contain the oil gas of saturated or unsaturated lower hydrocarbon etc.) and sulphur be the method that extensively adopts for raw material production dithiocarbonic anhydride, concrete reaction formation can have the branch of catalyzed reaction and uncatalyzed reaction.For making methane can fully finish conversion, no matter adopt which kind of form reaction in the actual production process, surpass the theoretical excessive sulphur that needs general usually the adding on proportioning raw materials.After resultant of reaction left reactor, the excessive sulphur that this is had neither part nor lot in reaction generally was by cooling, makes its liquefaction and at first separated removing, and isolated sulphur is sent back to as raw material and recycled.From the mixed gas that has separated remaining dithiocarbonic anhydride and hydrogen sulfide behind the sulphur, separate the method for removing hydrogen sulfide and have two kinds at present, a kind of is classical Tyke (Thacker) method, promptly utilize have absorb optionally that oil absorbs dithiocarbonic anhydride and not absorbing hydrogen sulphide the two is separated, do desorb and handle and obtain the dithiocarbonic anhydride product absorbing oil then.This method not only needs off-set facility such as special-purpose absorption, stripping apparatus and accessory heating, cooling, heat exchange, conveying, and owing to has increased the complicacy that absorbs oil and increased production process more significantly in process of production.Another kind of separation method can be described as " pressurization ",, mixed gas is sent into compressor rising pressure that is, makes dithiocarbonic anhydride liquefaction wherein and hydrogen sulfide still keeps gasiform two-phase difference and realize separating.
Generally speaking, resultant of reaction is impossible it is separated completely when the condensation process excessive separation sulphur of the above-mentioned the first step, still has a small amount of residual sulphur and is present in the mixed gas after the processing with mist or other form.These residual sulphur can not bring many adverse influences if do not remove to the process of later separate hydrogen sulfide, sometimes even can be very serious.For example, when " absorption-desorb " method of employing, can show as residual sulphur and in absorption oil, assemble, reduce pick up the oil efficient, and then can make it lose assimilation effect fully; When adopting " pressurization ", then show as residual sulphur and be cured and accumulate in the compressor, can cause compressor damage in various degree.For removing this part residual sulphur, once adopted deep fat washing method washing gas mixture in early days, recent then adopt turns part dithiocarbonic anhydride phlegma into methods that washings washs gas mixture more.The common drawback of these methods is all to need to be provided with specific equipment to finish washing operation.Just can send to the processing of making separate hydrogen sulfide through the gas mixture behind the residual sulphur of washing Ex-all.
The objective of the invention is for being in the raw material production dithiocarbonic anhydride process separating treatment of resultant of reaction to be proposed a kind of more simple and clear new and reasonable with lower hydrocarbon and sulphur.
Method of the present invention is such: with lower hydrocarbon and sulphur is raw material, after no matter adopting which kind of reaction formation to finish synthesizing of dithiocarbonic anhydride, resultant of reaction at first makes its cooling by general method under the condition of the pressure in all using former reactive system, for example can be cooled to about 130 ℃, make excessive sulphur condensation liquefaction separated going out from resultant of reaction wherein.To be the 1.5-10 kg/cm at the pressure that continue to keep being used directly do separating fully of dithiocarbonic anhydride and hydrogen sulfide under for-10-+20 ℃ condition with temperature to remaining mixed gas.Under such condition, dithiocarbonic anhydride is liquefied, and hydrogen sulfide is gas still then, utilizes its biphase difference just can realize that it separates fully.Here said separate to be fully to be different from present for washing residual sulphur only make the practice of a small amount of dithiocarbonic anhydride liquefaction.Requiring emphasis is pointed out that, the necessary pressure condition of separate hydrogen sulfide need not realized by pressure exerting devices such as compressors here, but the pressure of using fully in the former reactive system gets final product.Because the height of the pressure under the different building-up reactions modes in the system is different, according to the temperature and pressure relation as can be known, the pressure of the reactive system of being used in treating processes when this step is during in the 1.5-10 kg/cm, only needs suitably to adjust cooling temperature and can reach the dithiocarbonic anhydride that makes in the mixed gas and finish by gas and become liquid and obtain the purpose of high yield between-10-+20 ℃.And the adjusting of the cooling in this temperature range generally is not difficult to realize.
The operation of separate hydrogen sulfide can directly be carried out in the hydrogen sulfide knockout tower, and sepn process can be carried out continuously.Unsegregated mixed gas entered at the bottom of tower continuously, and the dithiocarbonic anhydride that has liquefied flows from top to bottom, emits at the bottom of tower, and gasiform hydrogen sulfide is separated from cat head.This process has not only been finished the separation of hydrogen sulfide, and since the dithiocarbonic anhydride that has liquefied with in tower, carried out counter current contact by the mixed gas that enters at the bottom of the tower, realize simultaneously the purpose of residual sulphur in the washing gas mixture again, killed two birds with one stone better effects if.
The thick dithiocarbonic anhydride that obtains after the separate hydrogen sulfide is carried out flash distillation according to a conventional method, after removing wherein remaining a small amount of hydrogen sulfide, carry out again refining and distilling get final product elaboration dithiocarbonic anhydride, have residual sulphur to exist in the high boiling point residue after the distillation, can send back to again and use as raw material.Isolated hydrogen sulfide restrains routinely and obtains chemical sulphur after Lloyd's (Claus) handles, and also can return and do the raw material use.
In sum, under the condition of using the synthesis reaction system internal pressure, separate the processing of sulphur and hydrogen sulfide continuously, and a step is realized dithiocarbonic anhydride and be separating of hydrogen sulfide the substantive features of the inventive method.Because needed pressure do not need pressure exerting devices such as ad hoc compressor fully, thus avoided residual sulphur the disadvantageous effect that may bring.Because of the inventive method makes treating processes and required equipment greatly simple, its reasonableness and significant superiority are self-evident.Should be noted that especially, the inventive method takes to use and keep certain pressure condition in the separate hydrogen sulfide stage, decapacitation makes outside the dithiocarbonic anhydride liquefaction separation, pass through pressurize, can also reduce the amount of the dithiocarbonic anhydride that is pulled away with hydrogen sulfide, thereby also be the important factor that improves the dithiocarbonic anhydride yield.According to the height difference of using pressure, can significantly improve the rate that changes of dithiocarbonic anhydride by the adjusting cooling temperature.These specific embodiments by following introduction can be clear that.
Example 1:
Under 680 ℃ and 3.5 kg/cm conditions, finish the dithiocarbonic anhydride building-up reactions with 16663 cubic metres of Sweet natural gases (methane 96.37%, ethane 1.62%, propane 0.45%, butane 0.33%) and excessive 10% sulphur.Reacted generation material is being cooled under the condition of all using reacting system pressure about 130 ℃ routinely, and condensation separation goes out excessive sulphur.Remaining mixed gas is sent into the hydrogen sulfide knockout tower, continues to use and keep the tower internal pressure to be not less than 3 kg/cm and to leave the overhead gas temperature under about-10 ℃ the condition, makes dithiocarbonic anhydride liquefaction, and by discharging at the bottom of the tower, hydrogen sulfide is left by cat head.With the carbon in the Sweet natural gas is that benchmark calculates (later on together), and gained dithiocarbonic anhydride yield is 93% at the bottom of the tower.
Example 2:
With 402 cubic metres of crude propylenes (propylene 92.5%, ethane 1.45%, propane 4.95%, propadiene 0.46%, butene-1 0.47%) and sulphur is raw material, finishes building-up reactions, sulphur excessive 75% under 735 ℃ and 2 kg/cm pressure conditions.Under the condition of all using reacting system pressure, make the excessive sulphur of resultant of reaction material condensation separation by general method, to remain mixed gas under the pressure condition and send into the hydrogen sulfide knockout tower continuing to keep to use, tower internal pressure 1.7 kg/cm, overhead gas temperature are-10 ℃.Gained dithiocarbonic anhydride yield 94.7% at the bottom of the tower.
Example 3:
Under 680 ° and 10 kg/cm pressure conditions, finish building-up reactions with 16 cubic metres of Sweet natural gases (methane 97.44%, ethane 1.08%, propane 0.27%, butane 0.04%, hydrogen sulfide 0.01%, nitrogen 0.56%) and excessive 40% sulphur.Under the condition of all using reacting system pressure, the resultant of reaction material is pressed the excessive sulphur of general method condensation separation.Continuing to keep under the pressure condition, will remain gas mixture and send into the hydrogen sulfide knockout tower, tower internal pressure 9.6 kg/cm, overhead gas temperature are not higher than 20 ℃.Gained dithiocarbonic anhydride yield 91% at the bottom of the tower.
Example 4:
Under 740 ℃ and 5.3 kg/cm conditions, finish building-up reactions with 8 cubic metres of crude propylenes (propylene 91.45%, ethane 0.91%, propane 5.67%, propadiene 0.77%, butene-1 0.66%, divinyl 0.56%) and excessive 160% sulphur.Under the condition of all using reacting system pressure, the resultant of reaction material is pressed the excessive sulphur of general method condensation separation, to remain mixed gas under the condition of pressure and directly send into the hydrogen sulfide knockout tower continuing to keep, the tower internal pressure is not less than 5 kg/cm, the overhead gas temperature is not higher than 20 ℃, and gained dithiocarbonic anhydride yield is 91.5% at the bottom of the tower.
Claims (2)
1, be that raw material generates in the dithiocarbonic anhydride process method for separating and processing to resultant of reaction with lower hydrocarbon and sulphur, what comprise the separation of excessive and remaining sulphur and hydrogen sulfide separates two portions process, it is characterized in that resultant of reaction makes the be condensed liquefaction and separate and remove of wherein sulphur under the condition of all using reacting system pressure, remaining mixed gas is in that continue to keep using pressure be 1.5-10 kg/cm and temperature under-10-+20 ℃ the condition, makes dithiocarbonic anhydride liquefaction and realizes and still be separated for the hydrogen sulfide of gas.
2, the method for claim 1, it is characterized in that said mixed gas is when the liquefaction separate hydrogen sulfide, make mixed gas and the dithiocarbonic anhydride liquid that has liquefied in advance do the counter current contact motion, reach the purpose of finishing the micro residue sulphur in the washing mixed gas simultaneously.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 89104115 CN1016599B (en) | 1989-10-17 | 1989-10-17 | Separation treatment of reaction product during production of carbon disulfide |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 89104115 CN1016599B (en) | 1989-10-17 | 1989-10-17 | Separation treatment of reaction product during production of carbon disulfide |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1042883A true CN1042883A (en) | 1990-06-13 |
| CN1016599B CN1016599B (en) | 1992-05-13 |
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 89104115 Expired CN1016599B (en) | 1989-10-17 | 1989-10-17 | Separation treatment of reaction product during production of carbon disulfide |
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| Country | Link |
|---|---|
| CN (1) | CN1016599B (en) |
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102153053A (en) * | 2010-11-20 | 2011-08-17 | 辽宁瑞兴化工集团有限公司 | Methods for purifying and comprehensively utilizing hydrogen sulfide byproduct during production of carbon disulfide by methane method |
| CN104003389A (en) * | 2014-06-16 | 2014-08-27 | 成都丽雅纤维股份有限公司 | Method for separating liquid sulfur in carbon disulfide preparation technology |
| CN104016344A (en) * | 2013-03-01 | 2014-09-03 | 辽宁瑞兴化工集团有限公司 | Method for avoiding forming hydrogen sulfide hydrate in carbon bisulfide production process |
| CN108483446A (en) * | 2018-04-10 | 2018-09-04 | 上海东庚设备工程技术有限公司 | The separation method and system of excessive sulphur during a kind of carbon disulphide production |
| CN108529627A (en) * | 2018-04-10 | 2018-09-14 | 上海东庚设备工程技术有限公司 | A kind of knockout tower for during carbon disulphide production |
| CN111265969A (en) * | 2020-03-20 | 2020-06-12 | 鹤壁市恒力橡塑股份有限公司 | Method for efficiently recovering carbon disulfide from tail gas |
| CN113428861A (en) * | 2021-07-19 | 2021-09-24 | 华东理工大学 | Methane and hydrogen sulfide reforming hydrogen production process |
| CN114906849A (en) * | 2022-06-23 | 2022-08-16 | 上海德迈世欧科技有限公司 | Process for the preparation of hydrogen sulphide and carbon disulphide |
-
1989
- 1989-10-17 CN CN 89104115 patent/CN1016599B/en not_active Expired
Cited By (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102153053A (en) * | 2010-11-20 | 2011-08-17 | 辽宁瑞兴化工集团有限公司 | Methods for purifying and comprehensively utilizing hydrogen sulfide byproduct during production of carbon disulfide by methane method |
| CN102153053B (en) * | 2010-11-20 | 2013-04-10 | 辽宁瑞兴化工集团有限公司 | Methods for purifying and comprehensively utilizing hydrogen sulfide byproduct during production of carbon disulfide by methane method |
| CN104016344A (en) * | 2013-03-01 | 2014-09-03 | 辽宁瑞兴化工集团有限公司 | Method for avoiding forming hydrogen sulfide hydrate in carbon bisulfide production process |
| CN104016344B (en) * | 2013-03-01 | 2016-02-10 | 辽宁瑞兴化工集团有限公司 | The method of hydrogen sulfide hydrate is avoided the formation of in a kind of carbon disulphide production process |
| CN104003389A (en) * | 2014-06-16 | 2014-08-27 | 成都丽雅纤维股份有限公司 | Method for separating liquid sulfur in carbon disulfide preparation technology |
| CN108529627A (en) * | 2018-04-10 | 2018-09-14 | 上海东庚设备工程技术有限公司 | A kind of knockout tower for during carbon disulphide production |
| CN108483446A (en) * | 2018-04-10 | 2018-09-04 | 上海东庚设备工程技术有限公司 | The separation method and system of excessive sulphur during a kind of carbon disulphide production |
| CN108483446B (en) * | 2018-04-10 | 2021-12-10 | 上海东庚化工技术有限公司 | Method and system for separating excessive sulfur in carbon disulfide production process |
| CN108529627B (en) * | 2018-04-10 | 2023-08-29 | 上海东庚化工技术有限公司 | Separation tower used in carbon disulfide production process |
| CN111265969A (en) * | 2020-03-20 | 2020-06-12 | 鹤壁市恒力橡塑股份有限公司 | Method for efficiently recovering carbon disulfide from tail gas |
| CN113428861A (en) * | 2021-07-19 | 2021-09-24 | 华东理工大学 | Methane and hydrogen sulfide reforming hydrogen production process |
| CN113428861B (en) * | 2021-07-19 | 2024-01-02 | 华东理工大学 | Methane and hydrogen sulfide reforming hydrogen production process |
| CN114906849A (en) * | 2022-06-23 | 2022-08-16 | 上海德迈世欧科技有限公司 | Process for the preparation of hydrogen sulphide and carbon disulphide |
Also Published As
| Publication number | Publication date |
|---|---|
| CN1016599B (en) | 1992-05-13 |
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Granted publication date: 19930303 |