CN114835118A - Method for removing hydrogen sulfide from carbon disulfide - Google Patents
Method for removing hydrogen sulfide from carbon disulfide Download PDFInfo
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- CN114835118A CN114835118A CN202210491679.3A CN202210491679A CN114835118A CN 114835118 A CN114835118 A CN 114835118A CN 202210491679 A CN202210491679 A CN 202210491679A CN 114835118 A CN114835118 A CN 114835118A
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- carbon disulfide
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/70—Compounds containing carbon and sulfur, e.g. thiophosgene
- C01B32/72—Carbon disulfide
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B17/00—Sulfur; Compounds thereof
- C01B17/02—Preparation of sulfur; Purification
- C01B17/021—Separation of sulfur from gases
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B17/00—Sulfur; Compounds thereof
- C01B17/16—Hydrogen sulfides
- C01B17/167—Separation
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Abstract
The invention relates to the technical field of hydrogen sulfide production, in particular to a method for removing hydrogen sulfide by carbon disulfide, which comprises the following steps: s1, separating to obtain carbon disulfide; s2, introducing the separated carbon disulfide into absorption liquid to neutralize hydrogen sulfide, standing the mixed liquid, distilling and condensing the lower organic phase to obtain condensate; s3, regenerating the absorption liquid to obtain regenerated liquid, and returning the regenerated liquid to the step S2 to be used as the absorption liquid. The method is simple to operate, and can efficiently obtain the carbon disulfide finished product with the hydrogen sulfide content lower than 0.1 wt%.
Description
Technical Field
The invention relates to the technical field of hydrogen sulfide production, in particular to a method for removing hydrogen sulfide by carbon disulfide.
Background
Hydrogen sulfide belongs to a highly toxic substance, and researchers research various treatment methods of hydrogen sulfide, such as preparation of sulfide and hydrosulfide by strong alkali absorption, preparation of sulfur dioxide, sulfite or sulfur by oxidation, methanol absorption and the like. Because of the problems of the components, the concentration and the amount of the mixed gas, the methods are limited in use, the hydrogen sulfide can be oxidized and absorbed only when the rest components of the hydrogen sulfide are discarded, and the selectable treatment methods are limited when the rest components of the hydrogen sulfide are treated and also need to be recovered, and the methods mainly adopt a physical method.
Carbon disulfide is an important chemical intermediate used for preparing xanthic acid, xanthate, carbamic acid, carbamate and the like. The preparation of carbon disulfide from methane and sulfur is an industrialized method, excessive liquid sulfur is firstly condensed by condensation of reaction gas of methane and sulfur, then carbon disulfide is condensed and refined, hydrogen sulfide is easily dissolved in carbon disulfide and is difficult to remove in the refining process of carbon disulfide, the content of hydrogen sulfide in carbon disulfide has to be controlled by increasing the rectification reflux ratio or rectifying for many times, and great energy consumption is needed.
Patent CN109502587A discloses the use of a highly integrated rectification apparatus comprising a divided wall column for the separation of a mixture of hydrogen sulphide, carbon disulphide and sulphur, with a saving in energy consumption of approximately 50%. Although rectification is a conventional and theoretically mature separation means, in actual operation, the adjustment of the parameters of components to be separated, pressure and temperature in a highly integrated rectification tower is complicated and even difficult to realize.
Patent CN105129799A discloses a rectification method for removing sulfur from the reaction gas of methane and sulfur, then liquefying crude carbon disulfide to remove most hydrogen sulfide, and then condensing carbon disulfide to obtain pure carbon disulfide.
Patent CN1935645A discloses a method of three-tower continuous rectification to refine the reaction gas of methane and sulfur, a rough stripping tower to separate sulfur and most of hydrogen sulfide, a fine stripping tower to further separate sulfur, a finished product tower to further separate hydrogen sulfide, and hydrogen sulfide with a content of more than 99% and carbon disulfide far superior to national top-grade products are obtained.
The separation of carbon disulfide and hydrogen sulfide generally uses a rectification method, and the energy consumption for preparing high-concentration carbon disulfide by rectification is very high, which is the repeated mass transfer between gasification and liquefaction caused by the physical property that hydrogen sulfide is easily dissolved in carbon disulfide during rectification.
Disclosure of Invention
The invention aims to provide a method for removing hydrogen sulfide from carbon disulfide, and aims to produce high-quality carbon disulfide under the condition of reducing rectification.
In order to solve the technical problems, the invention adopts the following technical scheme:
a process for removing hydrogen sulfide from carbon disulfide comprising the steps of:
s1, separating to obtain carbon disulfide;
s2, introducing the separated carbon disulfide into absorption liquid to neutralize hydrogen sulfide, standing the mixed liquid, distilling and condensing the lower organic phase to obtain condensate;
s3, regenerating the absorption liquid to obtain regenerated liquid, and returning the regenerated liquid to the step S2 to be used as the absorption liquid.
Preferably, the specific processing method of carbon disulfide in step S2 is as follows: and (3) evaporating and gasifying the carbon disulfide separated in the S1, introducing a gas phase into an absorption liquid, mixing and standing at the normal pressure and the temperature of 20-40 ℃, and condensing the gas to obtain the carbon disulfide with the hydrogen sulfide content of less than 0.1 wt%.
Preferably, the specific processing method of carbon disulfide in step S2 is as follows: evaporating and gasifying the carbon disulfide separated in the S1 at the temperature of 50-60 ℃ and under the condition of higher than normal pressure, introducing a gas phase into a tower plate type absorption tower, injecting the gas phase from a tower plate at the lowest layer, transferring absorption liquid from a tower kettle to the tower top for circulation, and merging regenerated liquid into circulating absorption liquid; and the gas discharged from the top of the tower is further subjected to gas-liquid separation and then condensed to obtain a carbon disulfide finished product.
Preferably, the absorption liquid comprises 20-60 wt% of organic base, 5-10 wt% of auxiliary agent and solvent.
Preferably, the organic base is: triethanolamine, N-methyldiethanolamine, N-dimethylethanolamine or mixtures, preferably N-methyldiethanolamine; the auxiliary agent is: water-soluble organic matter which is difficult to decompose at the temperature of higher than 120 ℃, preferably glycol or diglycol which is difficult to decompose at the temperature of higher than 150 ℃; the solvent is water.
Preferably, the specific treatment method of the regeneration liquid in step S3 is as follows: when the exhausted gas contains more than 0.1 wt% of hydrogen sulfide, transferring the absorption liquid to a regeneration tower for regeneration at 110-150 ℃, preferably at 120-130 ℃, wherein the component evaporated by regeneration is the hydrogen sulfide; the regeneration pressure is 0-3 bar, the temperature of the top of the regeneration tower is controlled below 50 ℃, and more preferably, the pressure is higher than the atmospheric pressure, and the temperature of the top of the regeneration tower is below 30 ℃.
Preferably, the sources of carbon disulfide in step S1 include, but are not limited to: the reaction gas of the sulfur and the natural gas comprises hydrogen sulfide, carbon disulfide, sulfur, natural gas and the like, and the sulfur, the carbon disulfide and the hydrogen sulfide are respectively obtained through condensation and separation.
The invention has the beneficial effects that:
the method is simple to operate, effectively reduces the rectification steps, and can efficiently obtain the carbon disulfide finished product with the hydrogen sulfide content lower than 0.1 wt%.
Drawings
FIG. 1 is a schematic overall flow diagram of the present invention.
Reference numerals
1-an absorption column; 2-a regeneration tower; 3-a gas-liquid separator; 4-a condenser.
Detailed Description
In order to facilitate understanding of those skilled in the art, the present invention will be further described with reference to the following examples and drawings, which are not intended to limit the present invention.
Example 1
The invention provides the following technical scheme: gasifying carbon disulfide liquid containing hydrogen sulfide and transferring the gasified carbon disulfide liquid into absorption liquid, and carrying out gas-liquid separation and condensation on the discharged gas to obtain carbon disulfide with the hydrogen sulfide content of less than 0.1 wt%; the absorption liquid is regenerated at high temperature and then used for absorbing the hydrogen sulfide again.
The invention is further illustrated with reference to fig. 1: the carbon disulfide liquid containing hydrogen sulfide is gasified and transferred to the lowest tower plate of the absorption tower 1 at normal pressure and 50-60 ℃, and the number of the tower plates of the absorption tower 1 varies according to factors such as ventilation capacity, hydrogen sulfide content, effective components of absorption liquid and the like. And (3) transferring the absorption liquid from the tower kettle to the tower top, controlling the temperature of the tower top to be 45-60 ℃, continuously transferring part of the absorption liquid to a regeneration tower 2, controlling the temperature of the regeneration tower to be 120-130 ℃, controlling the temperature of the regeneration tower top to be below 30 ℃, continuously transferring the tower bottom liquid of the regeneration tower 2 to a circulating absorption liquid, and directly condensing the gas discharged from the tower top of the absorption tower 1 after passing through a gas-liquid separator 3 to obtain a carbon disulfide finished product with the hydrogen sulfide content of less than 0.1 wt%.
Example 2
The apparatus shown in figure 1 was used for the removal of hydrogen sulphide from carbon disulphide, wherein the absorption column 1 had a diameter of 1000mm, 8 trays and a weir height of 200 mm.
The specific content of the absorption liquid is as follows: 50 wt% of triethanolamine, 5 wt% of ethylene glycol and the balance of water.
The temperature is 60 ℃ and the sulfur content is 05 v/v% carbon disulfide gas at a flow rate of 1000m 3 Introducing the hydrogen sulfide into an absorption tower 1 for hours, circulating the tower bottom liquid of the absorption tower 1 to the top of the tower at a rate of 100 kg/hour, introducing the regenerated liquid into the circulation at a rate of 67 kg/hour, introducing the gas discharged from the top of the absorption tower into a gas-liquid separator 3, automatically transferring the liquid phase part into the absorption tower 1 by virtue of gravity, condensing the gas phase part at 30 ℃ to obtain carbon disulfide liquid, and not detecting the hydrogen sulfide. Transferring the tower bottom liquid of the absorption tower 1 to a regeneration tower 2 to maintain the liquid level stable, wherein the tower bottom temperature of the regeneration tower is 125 ℃, the tower top temperature is 15 ℃, and the regeneration time is 10 min.
Example 3
The apparatus shown in figure 1 was used for the removal of hydrogen sulphide from carbon disulphide, wherein the absorption column 1 had a diameter of 1000mm, 8 trays and a weir height of 200 mm.
The specific content of the absorption liquid is as follows: 30 wt% of N-methyldiethanolamine, 5 wt% of diethylene glycol and the balance of water.
A temperature of 55 ℃ and a carbon disulfide gas containing 0.5 v/v% hydrogen sulfide at a flow rate of 1000m 3 And/h, introducing the absorption tower 1, circulating the tower bottom liquid of the absorption tower 1 to the tower top at a rate of 200kg/h, introducing the regenerated liquid into the circulation at a rate of 110kg/h, introducing the discharged gas at the tower top of the absorption tower into a gas-liquid separator, automatically transferring the liquid phase part into the absorption tower by means of gravity, and condensing the gas phase part at 30 ℃ to obtain carbon disulfide liquid, wherein the content of hydrogen sulfide is 0.04 wt%. Transferring the tower bottom liquid of the absorption tower 1 to a regeneration tower 2 to maintain the liquid level stable, wherein the tower bottom temperature of the regeneration tower is 120 ℃, the tower top temperature is 25 ℃, and the regeneration time is 15 min.
Finally, it should be noted that the above-mentioned description is only a preferred embodiment of the present invention, and that those skilled in the art can make various similar representations without departing from the spirit and scope of the present invention.
Claims (7)
1. The method for removing hydrogen sulfide by using carbon disulfide is characterized by comprising the following steps: the method comprises the following steps:
s1, separating to obtain carbon disulfide;
s2, introducing the separated carbon disulfide into absorption liquid to neutralize hydrogen sulfide, standing the mixed liquid, distilling and condensing the lower organic phase to obtain condensate;
s3, regenerating the absorption liquid to obtain regenerated liquid, and returning the regenerated liquid to the step S2 to be used as the absorption liquid.
2. A process for the removal of hydrogen sulfide from carbon disulfide according to claim 1, wherein: the specific treatment method of carbon disulfide in step S2 is as follows: and (3) evaporating and gasifying the carbon disulfide separated in the S1, introducing a gas phase into an absorption liquid, mixing and standing at the normal pressure and the temperature of 20-40 ℃, and condensing the gas to obtain the carbon disulfide with the hydrogen sulfide content of less than 0.1 wt%.
3. A process for the removal of hydrogen sulfide from carbon disulfide according to claim 1, wherein: the specific treatment method of carbon disulfide in step S2 is as follows: evaporating and gasifying the carbon disulfide separated in the S1 at the temperature of 50-60 ℃ and under the condition of higher than normal pressure, introducing a gas phase into a tower plate type absorption tower, injecting the gas phase from a tower plate at the lowest layer, transferring absorption liquid from a tower kettle to the tower top for circulation, and merging regenerated liquid into circulating absorption liquid; and the gas discharged from the top of the tower is further subjected to gas-liquid separation and then condensed to obtain a carbon disulfide finished product.
4. A process for the removal of hydrogen sulfide from carbon disulfide according to claim 1, wherein: the absorption liquid comprises 20-60 wt% of organic alkali, 5-10 wt% of auxiliary agent and solvent.
5. The process for removing hydrogen sulfide from carbon disulfide according to claim 4, wherein: the organic base is: triethanolamine, N-methyldiethanolamine, N-dimethylethanolamine or mixtures, preferably N-methyldiethanolamine; the auxiliary agent is: water-soluble organic matter which is difficult to decompose at the temperature of higher than 120 ℃, preferably glycol or diglycol which is difficult to decompose at the temperature of higher than 150 ℃; the solvent is water.
6. A process for the removal of hydrogen sulfide from carbon disulfide according to claim 1, wherein: the specific treatment method of the regeneration liquid in step S3 is as follows: when the exhausted gas contains more than 0.1 wt% of hydrogen sulfide, transferring the absorption liquid to a regeneration tower for regeneration at 110-150 ℃, preferably at 120-130 ℃, wherein the component evaporated by regeneration is the hydrogen sulfide; the regeneration pressure is 0-3 bar, the temperature of the top of the regeneration tower is controlled below 50 ℃, and more preferably, the pressure is higher than the atmospheric pressure, and the temperature of the top of the regeneration tower is below 30 ℃.
7. A process for the removal of hydrogen sulfide from carbon disulfide according to claim 1, wherein: sources of carbon disulfide in step S1 include, but are not limited to: the reaction gas of the sulfur and the natural gas comprises hydrogen sulfide, carbon disulfide, sulfur, natural gas and the like, and the sulfur, the carbon disulfide and the hydrogen sulfide are respectively obtained through condensation and separation.
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| Application Number | Priority Date | Filing Date | Title |
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| CN202210491679.3A CN114835118A (en) | 2022-05-07 | 2022-05-07 | Method for removing hydrogen sulfide from carbon disulfide |
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| CN202210491679.3A CN114835118A (en) | 2022-05-07 | 2022-05-07 | Method for removing hydrogen sulfide from carbon disulfide |
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Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1169335A (en) * | 1996-07-02 | 1998-01-07 | 四川川化集团公司 | Method for taking off hydrogen sulfide from mixed gas |
| CN101062460A (en) * | 2007-06-07 | 2007-10-31 | 华东理工大学 | Method and device for removing hydrogen sulphide from mixture gas containing low-concentration hydrogen sulphide |
| CN101721883A (en) * | 2008-10-23 | 2010-06-09 | 株式会社日立制作所 | Method and device for removing CO2 and H2S |
| JP2011068751A (en) * | 2009-09-25 | 2011-04-07 | Hitachi Ltd | Method and apparatus for decarboxylating and desulfurizing raw material gas |
| CN106890545A (en) * | 2017-04-05 | 2017-06-27 | 安徽宣城金宏化工有限公司 | The separating technology and equipment of hydrogen sulfide in a kind of carbon disulphide production tail gas |
| CN114249676A (en) * | 2021-12-10 | 2022-03-29 | 宁夏紫光天化蛋氨酸有限责任公司 | Method and device for purifying and separating methyl mercaptan |
-
2022
- 2022-05-07 CN CN202210491679.3A patent/CN114835118A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1169335A (en) * | 1996-07-02 | 1998-01-07 | 四川川化集团公司 | Method for taking off hydrogen sulfide from mixed gas |
| CN101062460A (en) * | 2007-06-07 | 2007-10-31 | 华东理工大学 | Method and device for removing hydrogen sulphide from mixture gas containing low-concentration hydrogen sulphide |
| CN101721883A (en) * | 2008-10-23 | 2010-06-09 | 株式会社日立制作所 | Method and device for removing CO2 and H2S |
| JP2011068751A (en) * | 2009-09-25 | 2011-04-07 | Hitachi Ltd | Method and apparatus for decarboxylating and desulfurizing raw material gas |
| CN106890545A (en) * | 2017-04-05 | 2017-06-27 | 安徽宣城金宏化工有限公司 | The separating technology and equipment of hydrogen sulfide in a kind of carbon disulphide production tail gas |
| CN114249676A (en) * | 2021-12-10 | 2022-03-29 | 宁夏紫光天化蛋氨酸有限责任公司 | Method and device for purifying and separating methyl mercaptan |
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