CN112408336A - Method and equipment for purifying hydrogen sulfide - Google Patents
Method and equipment for purifying hydrogen sulfide Download PDFInfo
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- CN112408336A CN112408336A CN202011340997.7A CN202011340997A CN112408336A CN 112408336 A CN112408336 A CN 112408336A CN 202011340997 A CN202011340997 A CN 202011340997A CN 112408336 A CN112408336 A CN 112408336A
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- 229910000037 hydrogen sulfide Inorganic materials 0.000 title claims abstract description 108
- RWSOTUBLDIXVET-UHFFFAOYSA-N Dihydrogen sulfide Chemical compound S RWSOTUBLDIXVET-UHFFFAOYSA-N 0.000 title claims abstract description 106
- 238000000034 method Methods 0.000 title claims abstract description 28
- 239000002904 solvent Substances 0.000 claims abstract description 91
- 239000007789 gas Substances 0.000 claims abstract description 38
- 239000000047 product Substances 0.000 claims abstract description 33
- 239000012535 impurity Substances 0.000 claims abstract description 31
- 239000012043 crude product Substances 0.000 claims abstract description 13
- 239000002912 waste gas Substances 0.000 claims abstract description 11
- 238000001179 sorption measurement Methods 0.000 claims abstract description 8
- 238000010521 absorption reaction Methods 0.000 claims description 48
- 238000011084 recovery Methods 0.000 claims description 34
- 238000010992 reflux Methods 0.000 claims description 26
- 238000009833 condensation Methods 0.000 claims description 9
- 230000005494 condensation Effects 0.000 claims description 9
- IAZDPXIOMUYVGZ-UHFFFAOYSA-N Dimethylsulphoxide Chemical compound CS(C)=O IAZDPXIOMUYVGZ-UHFFFAOYSA-N 0.000 claims description 8
- 230000006835 compression Effects 0.000 claims description 8
- 238000007906 compression Methods 0.000 claims description 8
- 238000001816 cooling Methods 0.000 claims description 7
- UWHCKJMYHZGTIT-UHFFFAOYSA-N tetraethylene glycol Chemical compound OCCOCCOCCOCCO UWHCKJMYHZGTIT-UHFFFAOYSA-N 0.000 claims description 7
- 229920001223 polyethylene glycol Polymers 0.000 claims description 6
- HXJUTPCZVOIRIF-UHFFFAOYSA-N sulfolane Chemical compound O=S1(=O)CCCC1 HXJUTPCZVOIRIF-UHFFFAOYSA-N 0.000 claims description 5
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 4
- 229910052739 hydrogen Inorganic materials 0.000 claims description 4
- 239000001257 hydrogen Substances 0.000 claims description 4
- 238000004064 recycling Methods 0.000 claims description 3
- 238000004508 fractional distillation Methods 0.000 claims 2
- 239000006096 absorbing agent Substances 0.000 claims 1
- 238000000605 extraction Methods 0.000 abstract description 12
- 238000005265 energy consumption Methods 0.000 abstract description 4
- 238000010924 continuous production Methods 0.000 abstract description 3
- 239000012467 final product Substances 0.000 abstract 1
- 239000000463 material Substances 0.000 description 27
- 238000000746 purification Methods 0.000 description 17
- 239000007791 liquid phase Substances 0.000 description 15
- 239000012071 phase Substances 0.000 description 13
- 238000005194 fractionation Methods 0.000 description 11
- 239000002994 raw material Substances 0.000 description 9
- 229910052717 sulfur Inorganic materials 0.000 description 9
- 239000011593 sulfur Substances 0.000 description 9
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 8
- 238000003860 storage Methods 0.000 description 7
- 239000006227 byproduct Substances 0.000 description 6
- 239000000126 substance Substances 0.000 description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 5
- QGJOPFRUJISHPQ-UHFFFAOYSA-N Carbon disulfide Chemical compound S=C=S QGJOPFRUJISHPQ-UHFFFAOYSA-N 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 3
- 239000002351 wastewater Substances 0.000 description 3
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 2
- UIIMBOGNXHQVGW-UHFFFAOYSA-M Sodium bicarbonate Chemical compound [Na+].OC([O-])=O UIIMBOGNXHQVGW-UHFFFAOYSA-M 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- 230000002378 acidificating effect Effects 0.000 description 2
- 238000001311 chemical methods and process Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 229930195733 hydrocarbon Natural products 0.000 description 2
- 150000002430 hydrocarbons Chemical class 0.000 description 2
- 238000009776 industrial production Methods 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 239000002808 molecular sieve Substances 0.000 description 2
- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 description 2
- HYHCSLBZRBJJCH-UHFFFAOYSA-M sodium hydrosulfide Chemical compound [Na+].[SH-] HYHCSLBZRBJJCH-UHFFFAOYSA-M 0.000 description 2
- UIIMBOGNXHQVGW-DEQYMQKBSA-M Sodium bicarbonate-14C Chemical compound [Na+].O[14C]([O-])=O UIIMBOGNXHQVGW-DEQYMQKBSA-M 0.000 description 1
- 239000003463 adsorbent Substances 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 239000013064 chemical raw material Substances 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000018044 dehydration Effects 0.000 description 1
- 238000006297 dehydration reaction Methods 0.000 description 1
- 230000003009 desulfurizing effect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
- 231100000086 high toxicity Toxicity 0.000 description 1
- 230000002401 inhibitory effect Effects 0.000 description 1
- XDAHMMVFVQFOIY-UHFFFAOYSA-N methanedithione;sulfane Chemical compound S.S=C=S XDAHMMVFVQFOIY-UHFFFAOYSA-N 0.000 description 1
- 239000012046 mixed solvent Substances 0.000 description 1
- 238000011165 process development Methods 0.000 description 1
- 238000011403 purification operation Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 229910000030 sodium bicarbonate Inorganic materials 0.000 description 1
- 235000017557 sodium bicarbonate Nutrition 0.000 description 1
- 229910000029 sodium carbonate Inorganic materials 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 238000010977 unit operation Methods 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
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Classifications
-
- 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
- C01B17/168—Purification
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Gas Separation By Absorption (AREA)
Abstract
The invention discloses a method for purifying hydrogen sulfide, which comprises the steps of adsorbing part of impurity solvents of crude hydrogen sulfide and liquefying the impurities to obtain a first crude hydrogen sulfide; fractionating the first hydrogen sulfide crude product to obtain a second hydrogen sulfide crude product and light waste gas; the second hydrogen sulfide crude product is fractionated to obtain hydrogen sulfide gas and a heavy impurity product, and the hydrogen sulfide gas is liquefied to obtain a final product; meanwhile, the invention also provides hydrogen sulfide extraction equipment using the method, the equipment can be used for continuous production, the energy consumption of the whole equipment is low, the adsorption equipment and the rectification equipment are integrated into a whole, and the operation is stable.
Description
Technical Field
The invention relates to the technical field of sulfuric acid gas purification, in particular to a method and equipment for purifying hydrogen sulfide.
Background
In industrial production, hydrogen sulfide is often generated as a byproduct in a chemical process in which sulfur-containing and hydrogen-containing hydrocarbons are used as raw materials, and the byproduct has high toxicity, pollutes the environment and has high treatment cost. If the catalyst can be recycled and purified to be used as a chemical raw material, the waste can be changed into valuable, the hydrogen sulfide is changed into a product with high added value, and the subsequent treatment cost and the environmental pollution are reduced.
Chinese patent CN105731496B discloses a method for producing sodium bicarbonate from acidic gas and purifying hydrogen sulfide, which uses sodium carbonate as solution to absorb hydrogen sulfide in acidic gas to generate sodium hydrosulfide and sodium bicarbonate, and decomposes the sodium hydrosulfide by flash evaporation to obtain hydrogen sulfide with purity of more than 99%. Chinese patent CN102153053B discloses a method for preparing carbon disulfide byproduct hydrogen sulfide by a methane purification method, which mainly comprises the steps of desulfurizing and distilling to obtain a mixer containing hydrogen sulfide and carbon disulfide, and further compressing, cooling and rectifying to obtain hydrogen sulfide with the purity of more than 99%. Chinese patent CN108392948A discloses a method and apparatus for purifying hydrogen sulfide, which uses activated alumina as adsorbent to obtain hydrogen sulfide with purity greater than 92% by four-stage pressure swing adsorption. CN110342471A discloses a method for preparing high-purity hydrogen sulfide, which mainly utilizes first-stage compression, molecular sieve adsorption dehydration, second-stage compression liquefaction, hydrogen sulfide rectification to remove light components, and hydrogen sulfide rectification to remove heavy components, and then obtains a hydrogen sulfide product with the purity of over 99.99%. In the above-mentioned scheme for hydrogen sulfide purification research, the separation and extraction of the product are all extracted by conventional high-pressure liquefaction, cryogenic rectification and molecular sieve adsorption in the prior art, and the research on the extraction unit of the target product has certain limitations. However, in practical research, it is found that when the conventional plausible means is adopted to extract and purify a target product, the extraction rate of the product is always low, the purity of the extracted product is not ideal enough, and subsequent additional purification operation is required to meet the requirement, so that the problem of extraction rate cannot be broken through no matter how the parameters and conditions of the whole extraction unit operation process are optimized, and the extraction rate and the product extraction purity cannot be greatly improved; or the extraction rate is very high, but higher energy consumption and larger equipment investment are needed as the guarantee premise, and in the actual production, no matter how dramatic the efficiency of the former synthesis unit is, products meeting the needs cannot be obtained by effective means, which always becomes a difficult problem and bottleneck for inhibiting the process development and becomes urgent to be solved in the field.
Disclosure of Invention
Aiming at the defects existing in the prior background, the invention aims to provide a process method combining liquid phase absorption and rectification, which is used for continuously operating the purification process of hydrogen sulfide to obtain a hydrogen sulfide product with the content of 99.99 percent, and all byproducts can be recycled; meanwhile, the invention also provides hydrogen sulfide extraction equipment using the method, the equipment can be used for continuous production, the energy consumption of the whole equipment is low, the adsorption equipment and the rectification equipment are integrated into a whole, and the operation is stable.
In order to achieve the purpose, the invention is realized by the following technical scheme:
a method of purifying hydrogen sulfide comprising the steps of:
s1, adsorbing a part of impurity solvent of a crude hydrogen sulfide product, and liquefying to obtain a first crude hydrogen sulfide product;
s2, fractionating the first hydrogen sulfide crude product to obtain a second hydrogen sulfide crude product and light waste gas;
and S3, fractionating the second hydrogen sulfide crude product to obtain hydrogen sulfide gas and a heavy impurity product.
Optionally, the light waste gas is condensed and liquefied, or returned again for fractionation treatment, to obtain a hydrogen product.
Optionally, the hydrogen sulfide gas is condensed and liquefied, or returned again for fractionation treatment, to obtain a hydrogen sulfide product.
Optionally, the solvent is subjected to fractionation after adsorption and then is returned for recycling.
Optionally, the solvent used for solvent absorption is one or more of sulfolane, dimethyl sulfoxide and tetraethylene glycol.
The invention also includes an apparatus for purifying hydrogen sulfide, comprising:
the inlet of the side wall of the absorption tower is communicated with the feeding pipeline, and the inlet of the solvent recovery tower is communicated with the outlet at the bottom of the absorption tower;
the inlet of the compression cooling device is connected with the outlet at the top of the absorption tower;
the inlet of the side wall of the light component removal tower is connected with the outlet of the compression cooling device, and the outlet of the top of the light component removal tower is communicated with the light waste gas condensation circulating reflux assembly;
and the side wall inlet of the heavy component removal tower is connected with the bottom outlet of the light component removal tower, and the top outlet of the heavy component removal tower is communicated with the hydrogen sulfide condensation circulating reflux assembly.
The compressor is a screw compressor or a diaphragm compressor and is connected with a heat exchanger to cool and liquefy the compressed gas;
and the gas phase material flow at the top of the light component removal tower is sequentially connected with two condensers, the liquid phase material flow cooled by the first condenser and the second condenser enters a tower top reflux tank, the material flow of the reflux tank partially flows to the top of the light component removal tower according to the reflux ratio of 30-50, a light component removal storage tank is partially extracted, and the liquid phase material flow of the tower bottom of the light component removal tower enters the middle part of the heavy component removal tower.
The heavy-component removal tower top gas phase material flow is sequentially connected with two condensers, the liquid phase material flow cooled by the first condenser and the second condenser enters a tower top reflux tank, part of the material flow of the reflux tank reflows to the heavy-component removal tower top according to the reflux ratio of 0.1-2, part of the material flow is collected as a high-purity hydrogen sulfide product to be sent to a product storage tank, and the liquid phase material flow of the heavy-component removal tower kettle is collected to be sent to a heavy impurity storage tank.
Injecting solvent into the upper part of the solvent absorption tower, and injecting raw material gas into the lower part of the solvent absorption tower; the material flow in the tower kettle is removed to the middle part of a solvent recovery tower; the gas phase material flow at the top of the solvent recovery tower is sequentially connected with a condenser, the cooled liquid phase material flow enters a tower top reflux tank, part of the material flow in the reflux tank reflows to the top of the solvent absorption tower according to the reflux ratio of 10-20, and part of the material flow is collected as sulfur-containing water-containing impurities and sent to a sulfur-containing impurity storage tank; the tower bottom material flow returns to the upper part of the solvent absorption tower.
Optionally, the pressure of the solvent absorption tower is 0.1MPa to 0.2MPa, and the temperature is 20 ℃ to 40 ℃.
Optionally, the top pressure of the light component removal tower is 1.0-2.5 MPa, preferably 1.2-1.8 MPa; the operation temperature is-30 ℃ to 40 ℃, and preferably-20 ℃ to 5 ℃; the operation pressure of the tower kettle is 1.1-2.6 MPa, preferably 1.25-1.9 MPa; the operation temperature is 0-40 ℃, preferably 5-20 ℃.
Optionally, the tower top pressure of the de-heavy tower is 1.0-2.5 MPa, preferably 1.2-1.8 MPa; the operation temperature is 0-40 ℃, preferably 5-20 ℃; the operation pressure of the tower kettle is 1.1-2.6 MPa, preferably 1.25-1.9 MPa; the operating temperature is 10 ℃ to 200 ℃, preferably 30 ℃ to 150 ℃.
Optionally, the tower top pressure of the solvent recovery tower is 0.01-0.2 MPa, preferably 0.05-0.1 MPa; the operation temperature is 10-120 ℃, and preferably 20-90 ℃; the operation pressure of the tower kettle is 0.005-0.25 MPa, preferably 0.01-0.11 MPa; (ii) a The operating temperature is 180 ℃ to 350 ℃, preferably 195 ℃ to 300 ℃.
The technical scheme of the invention has the following advantages:
the embodiment of the invention provides a method for purifying hydrogen sulfide, which combines liquid phase absorption and rectification, and researchers find that although liquid phase absorption purification or rectification belongs to the conventional technical process, when the liquid phase absorption purification or the rectification is combined, the hydrogen sulfide purification process is continuously operated, and the extraction rate of the hydrogen sulfide can be greatly improved by correspondingly changing and adjusting pressure and temperature parameters in the rectification process, and the product purity can reach 99.995%.
In the process of purifying hydrogen sulfide, all the generated byproducts can be recycled and recycled until the hydrogen sulfide is completely purified and can be recycled, so that zero emission to the environment and no pollution are realized.
The embodiment of the invention also provides hydrogen sulfide extraction equipment using the method, the equipment can be used for continuous production, the energy consumption of the whole equipment is low, the adsorption equipment and the rectification equipment are integrated into a whole, and the operation is stable.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, and it is obvious that the drawings in the following description are some embodiments of the present invention, and other drawings can be obtained by those skilled in the art without creative efforts.
FIG. 1 is a schematic flow diagram of a process for purifying hydrogen sulfide in accordance with the present invention;
in the figure: 1-absorption tower, 2-gas compressor, 3-raw material heat exchanger, 4-lightness-removing tower, 5-lightness-removing tower reflux tank, 6-lightness-removing tower first condenser, 7-lightness-removing tower second condenser, 8-weight-removing tower, 9-weight-removing tower first condenser, 10-weight-removing tower second condenser, 11-weight-removing tower reflux tank, 12-solvent recovery tower, 13-solvent recovery tower condenser, 14-solvent recovery tower reflux tank, S1-raw material pipeline, S2-light impurity material flow pipeline, S3-light impurity noncondensable gas pipeline, S4-hydrogen sulfide product pipeline, S5-heavy impurity material flow pipeline, S6-hydrogen sulfide noncondensable gas pipeline and S7-sulfur-containing waste water pipeline.
Detailed Description
The technical solutions of the present invention will be described clearly and completely with reference to the accompanying drawings, and it should be understood that the described embodiments are some, but not all embodiments of the present invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
In the description of the present invention, it should be noted that the terms "center", "upper", "lower", "left", "right", "vertical", "horizontal", "inner", "outer", etc., indicate orientations or positional relationships based on the orientations or positional relationships shown in the drawings, and are only for convenience of description and simplicity of description, but do not indicate or imply that the device or element being referred to must have a particular orientation, be constructed and operated in a particular orientation, and thus, should not be construed as limiting the present invention.
In addition, the technical features involved in the different embodiments of the present invention described below may be combined with each other as long as they do not conflict with each other.
Example 1
The embodiment of the invention is mainly used for purifying hydrogen sulfide by-products generated in the chemical process in which sulfur-containing and hydrogen-containing hydrocarbons are used as raw materials in industrial production.
The hydrogen sulfide purification process provided by the embodiment comprises the following steps:
s1, adsorbing a part of impurity solvent of a crude hydrogen sulfide product, and liquefying to obtain a first crude hydrogen sulfide product;
s2, fractionating the first hydrogen sulfide crude product to obtain a second hydrogen sulfide crude product and light waste gas;
and S3, fractionating the second hydrogen sulfide crude product to obtain hydrogen sulfide gas and a heavy impurity product.
And condensing and liquefying the light waste gas or returning the light waste gas to perform fractionation treatment again, specifically, obtaining a light product which comprises a non-condensable gas light substance and a liquid light substance, wherein the non-condensable gas light substance is still a gaseous substance after condensation treatment and is discharged in a gaseous form, the condensed and liquefied substance is discharged in proportion or is recycled by fractionation again, the second hydrogen sulfide crude product, namely the heavy fraction, is subjected to fractionation treatment again, specifically, the heavy impurity liquid phase substance is discharged in a liquid form, and the hydrogen sulfide is subjected to fractionation and condensation to form a high-purity hydrogen sulfide product.
Preferably, the solvent can be recycled by using a re-fractionation treatment.
Example 2
Referring to fig. 1, the present embodiment is a process apparatus, comprising: an absorption column 1 having a side wall inlet communicating with a feed line S1 and a bottom outlet solvent recovery column 12 inlet communicating; the inlet of the compression cooling device is connected with the outlet at the top of the absorption tower 1; the inlet of the side wall of the light component removal tower 4 is connected with the outlet of the compression cooling device, and the outlet of the top of the light component removal tower is communicated with the light waste gas condensation circulating reflux assembly; and a heavy component removal tower 8, wherein the inlet of the side wall of the heavy component removal tower 8 is connected with the outlet at the bottom of the light component removal tower 4, the outlet at the top of the heavy component removal tower is communicated with the hydrogen sulfide condensation circulating reflux assembly, and the bottom of the heavy component removal tower is communicated with a heavy impurity discharge pipeline S5.
Wherein, the gas compressor 2 is a screw compressor or a diaphragm compressor and is connected with the heat exchanger 3 to cool and liquefy the compressed gas.
Further, the top gas phase material flow of the light component removing tower 4 is sequentially connected with two condensers, a first condenser 6 of the light component removing tower and a second condenser 7 of the light component removing tower, the second condenser 7 of the light component removing tower comprises two output ends, one output end is connected with a light impurity gas phase output end S3, the other output end is connected with a light component removing tower reflux tank 5, the output ends of the reflux tanks are respectively communicated with the top of the light component removing tower 4, the fractionation circulation is carried out again, and the other output end is communicated with a liquid phase light impurity discharge line S2.
The gas phase material flow at the top of the heavy component removing tower 8 is sequentially connected with two condensers, a heavy component removing tower first condenser 9 and a heavy component removing tower second condenser 10, the heavy component removing tower second condenser 10 comprises two output ends, one output end is connected with a hydrogen sulfide gas phase output end S6, the other output end is connected with a heavy component removing tower reflux tank 11, the output end of the reflux tank is respectively communicated with the top of the heavy component removing tower 8, the fractionation is performed again, and the other output end is communicated with a hydrogen sulfide product pipeline S4.
The bottom end of the solvent absorption tower 1 is communicated with a solvent recovery tower 12, the bottom of the solvent recovery tower 12 is communicated with a reusable solvent through a pipeline and a solvent input port of the absorption tower 1, the top of the solvent recovery tower 12 is communicated with a solvent recovery tower condenser 13, the solvent recovery tower condenser is communicated with the top of the solvent recovery tower 12 through one output end of a recovery tower condensation tank 14 and is subjected to fractionation and circulation again, and the other output end of the solvent recovery tower condenser is communicated with a sulfur-containing waste water discharge pipeline S7.
Example 3
The hydrogen sulfide purification process provided in this embodiment is shown in fig. 1, and specifically includes:
s1, hydrogen sulfide gas phase raw materials containing impurities enter the lower part of a solvent absorption tower 1 through a raw material pipeline S1, absorption solvents are injected into the upper part of the solvent absorption tower 1, and water and part of sulfur-containing impurities in a gas phase are absorbed;
s2, after water and part of sulfur-containing impurities of the raw materials are removed by an absorption tower 1, the raw materials enter a gas compressor 2 from the top in a gas phase, are further cooled and liquefied by a heat exchanger 3 and then enter a light component removal tower 4;
s3, gas phase material flow at the top of the light component removal tower 4 enters a first condenser 6 of the light component removal tower and a second condenser 7 of the light component removal tower, non-condensable gas enters a light impurity non-condensable gas pipeline S3 to serve as a light impurity to be sent to a storage tank or a pipeline, condensed liquid phase material flow enters a light component removal tower reflux tank 5, part of the condensed liquid phase material flow reflows, part of the condensed liquid phase material flow serves as a light impurity material flow pipeline S2 to be sent to a impurity removal storage tank or a pipeline, and heavy components at the bottom of the tower are sent to a;
s4, the gas phase material flow at the top of the heavy component removal tower 8 passes through a first condenser 9 of the heavy component removal tower and a second condenser 10 of the heavy component removal tower, the non-condensable gas enters a hydrogen sulfide non-condensable gas pipeline S6 and is a small amount of hydrogen sulfide gas, a hydrogen sulfide product pipeline S4 is a high-purity hydrogen sulfide product, a heavy impurity material flow pipeline S5 is heavy impurities, and the impurity removal storage tank is subjected to subsequent treatment. The solvent containing water and a small amount of impurities at the bottom of the solvent absorption tower 1 enters a solvent recovery tower 12, the gas phase at the top of the solvent recovery tower passes through a solvent recovery tower condenser 13 and is changed into a liquid phase to enter a solvent recovery tower reflux tank 14, the fluid of the solvent recovery tower reflux tank 14 partially refluxes and is partially extracted, the extracted material flow mainly contains water and a small amount of impurities and is discharged from a sulfur-containing waste water pipeline S7, and the pure solvent at the bottom of the solvent recovery tower returns to the upper part of the solvent absorption tower 1 for recycling.
In this example, the solvent used in the solvent absorption tower was sulfolane, the operating pressure of the solvent absorption tower was 0.1MPa, and the operating temperature was 20 ℃; the operation pressure at the top of the light component removal tower is 2.5MPa, and the operation temperature is 2 ℃; the operation pressure of the tower kettle is 2.6MPa, and the operation temperature is 40 ℃; the operation pressure at the top of the de-heavy tower is 2.5MPa, and the operation temperature is 34 ℃; the operation pressure of the tower kettle is 2.6MPa, and the operation temperature is 241 ℃; the operation pressure at the top of the solvent recovery tower is 0.01MPa, and the operation temperature is 24 ℃; the operation pressure of the tower bottom is 0.02MPa, and the operation temperature is 220 ℃.
The hydrogen sulfide purity of this example was 99.991%.
Example 4
The hydrogen sulfide purification process provided in this example is the same as that in example 3, except that in this example, the solvent used in the solvent absorption tower is tetraethylene glycol, wherein the operating pressure of the solvent absorption tower is 0.15MPa, and the operating temperature is 30 ℃.
The operation pressure at the top of the light component removal tower is 1.8 MPa; the operating temperature is-11 ℃; the operation pressure of the tower kettle is 1.9 MPa; the operating temperature was 23 ℃.
The operation pressure at the top of the heavy component removal tower is 1.8 MPa; the operating temperature is 20 ℃; the operation pressure of the tower kettle is 1.9 MPa; the operating temperature was 223 ℃.
The operation pressure at the top of the solvent recovery tower is 0.05 MPa; the operation temperature is 63 ℃; the operation pressure of the tower kettle is 0.06 MPa; the operating temperature was 308 ℃.
The hydrogen sulfide purity of this example was 99.992%.
Example 5
The hydrogen sulfide purification process provided in this example is the same as that in example 3, except that in this example, the solvent used in the solvent absorption tower is dimethyl sulfoxide, wherein the operating pressure of the solvent absorption tower is 0.1MPa, and the operating temperature is 20 ℃.
The operation pressure at the top of the light component removal tower is 1.2 MPa; the operation temperature is-26 ℃; the operation pressure of the tower bottom is 1.25 MPa; the operating temperature was 7 ℃.
The operation pressure at the top of the heavy component removal tower is 1.2 MPa; the operation temperature is 5 ℃; the operation pressure of the tower bottom is 1.25 MPa; the operating temperature was 196 ℃.
The operation pressure at the top of the solvent recovery tower is 0.005 MPa; the operating temperature is 10 ℃; the operation pressure of the tower kettle is 0.006 MPa; the operating temperature was 105 ℃.
The hydrogen sulfide purity of this example was 99.991%.
Example 6
The present example provides a hydrogen sulfide purification process, which is the same as example 3, except that in this example, the solvent used in the solvent absorption tower is a mixed solvent of sulfolane and dimethyl sulfoxide, wherein the operating pressure of the solvent absorption tower is 0.2MPa, and the operating temperature is 30 ℃.
The operation pressure at the top of the light component removal tower is 1.8 MPa; the operating temperature is-11 ℃; the operation pressure of the tower kettle is 1.9 MPa; the operating temperature was 23 ℃.
The operation pressure at the top of the heavy component removal tower is 1.5 MPa; the operating temperature is 13 ℃; the operation pressure of the tower kettle is 1.8 MPa; the operating temperature was 219 ℃.
The operation pressure at the top of the solvent recovery tower is 0.05 MPa; the operation temperature is 63 ℃; the operation pressure of the tower kettle is 0.06 MPa; the operating temperature was 198 ℃.
The purity of hydrogen sulfide in this example was 99.99%.
Example 7
In this example, the other processes of the hydrogen sulfide purification process are the same as those in example 3, except that in this example, the solvent used in the solvent absorption tower is sulfolane.
The operating pressure of the solvent absorption tower is 0.15MPa, and the operating temperature is 30 ℃.
The operation pressure at the top of the light component removal tower is 1.5MPa, and the operation temperature is-18 ℃; the operation pressure of the tower bottom is 1.6MPa, and the operation temperature is 16 ℃.
The operation pressure at the top of the heavy component removal tower is 1.5MPa, and the operation temperature is 13 ℃; the operation pressure of the tower bottom is 1.63MPa, and the operation temperature is 213 ℃.
The operation pressure at the top of the solvent recovery tower is 0.02MPa, and the operation temperature is 40 ℃; the operation pressure of the tower bottom is 0.025MPa, and the operation temperature is 230 ℃.
The hydrogen sulfide purity of this example was 99.995%.
Example 8
The hydrogen sulfide purification process provided in this example is the same as that in example 3 except that the solvent used in the solvent absorption tower is dimethyl sulfoxide.
The operating pressure of the solvent absorption tower is 0.15MPa, and the operating temperature is 30 ℃.
The operation pressure at the top of the light component removal tower is 1.5MPa, and the operation temperature is-18 ℃; the operation pressure of the tower bottom is 1.6MPa, and the operation temperature is 16 ℃.
The operation pressure at the top of the heavy component removal tower is 1.5MPa, and the operation temperature is 13 ℃; the operation pressure of the tower bottom is 1.63MPa, and the operation temperature is 213 ℃.
The operation pressure at the top of the solvent recovery tower is 0.03MPa, and the operation temperature is 50 ℃; the operation pressure of the tower bottom is 0.035MPa, and the operation temperature is 153 ℃.
The hydrogen sulfide purity of this example was 99.991%.
Example 9
The process for purifying hydrogen sulfide provided in this example is the same as that in example 3, except that in this example, the solvent used in the solvent absorption tower is tetraethylene glycol.
The operating pressure of the solvent absorption tower is 0.15MPa, and the operating temperature is 30 ℃.
The operation pressure at the top of the light component removal tower is 1.5MPa, and the operation temperature is-18 ℃; the operation pressure of the tower bottom is 1.6MPa, and the operation temperature is 16 ℃.
The operation pressure at the top of the heavy component removal tower is 1.5MPa, and the operation temperature is 13 ℃; the operation pressure of the tower bottom is 1.63MPa, and the operation temperature is 213 ℃.
The operation pressure at the top of the solvent recovery tower is 0.01MPa, and the operation temperature is 24 ℃; the operation pressure of the tower bottom is 0.015MPa, and the operation temperature is 260 ℃.
The hydrogen sulfide purity of this example was 99.992%.
Comparative example 1
The hydrogen sulfide purification process provided in this example is the same as that in this example except that the solvent used in the solvent absorption tower is tetraethylene glycol.
The operating pressure of the solvent absorption tower is 0.5MPa, and the operating temperature is 20 ℃.
The operation pressure at the top of the light component removal tower is 0.5MPa, and the operation temperature is-15 ℃; the operation pressure of the tower bottom is 0.6MPa, and the operation temperature is-18 ℃.
The operation pressure at the top of the de-heavy tower is 3.5MPa, and the operation temperature is 49 ℃; the operation pressure of the tower bottom is 3.63MPa, and the operation temperature is 270 ℃.
The operation pressure at the top of the solvent recovery tower is 0.01MPa, and the operation temperature is 24 ℃; the operation pressure of the tower bottom is 0.015MPa, and the operation temperature is 260 ℃.
The purity of hydrogen sulfide in this example was 97.2%.
Comparative example 2
The hydrogen sulfide purification process provided in this example is the same as that in this example except that the solvent used in the solvent absorption tower is tetraethylene glycol.
The operating pressure of the solvent absorption tower is 0.25MPa, and the operating temperature is 30 ℃.
The operation pressure at the top of the light component removal tower is 3.0MPa, and the operation temperature is 5 ℃; the operation pressure of the tower bottom is 3.2MPa, and the operation temperature is 46 ℃.
The operation pressure at the top of the heavy component removal tower is 0.8MPa, and the operation temperature is-10 ℃; the operation pressure of the tower bottom is 1.0MPa, and the operation temperature is 180 ℃.
The operation pressure at the top of the solvent recovery tower is 0.01MPa, and the operation temperature is 24 ℃; the operation pressure of the tower bottom is 0.015MPa, and the operation temperature is 260 ℃.
The purity of hydrogen sulfide in this example was 98.1%.
Comparative example 3
The hydrogen sulfide purification process provided in this example is the same as that in this example except that the solvent used in the solvent absorption tower is tetraethylene glycol.
The operating pressure of the solvent absorption tower is 0.15MPa, and the operating temperature is 30 ℃.
The operation pressure at the top of the light component removal tower is 0.9MPa, and the operation temperature is-30 ℃; the operation pressure of the tower bottom is 1.0MPa, and the operation temperature is-5 ℃.
The operation pressure at the top of the heavy component removal tower is 1.3MPa, and the operation temperature is 12 ℃; the operation pressure of the tower bottom is 1.63MPa, and the operation temperature is 213 ℃.
The operation pressure at the top of the solvent recovery tower is 0.01MPa, and the operation temperature is 24 ℃; the operation pressure of the tower bottom is 0.015MPa, and the operation temperature is 260 ℃.
The purity of hydrogen sulfide in this example was 97.2%.
In summary, under other conditions, the change of the operating pressure and temperature in each reaction column has a certain effect on the final hydrogen sulfide purity, but the effect range is limited, and the purity of the hydrogen sulfide can reach 99.995% within the parameter range of the examples of the present application.
It should be understood that the above examples are only for clarity of illustration and are not intended to limit the embodiments. Other variations and modifications will be apparent to persons skilled in the art in light of the above description. And are neither required nor exhaustive of all embodiments. And obvious variations or modifications therefrom are within the scope of the invention.
Claims (10)
1. A method for purifying hydrogen sulfide, comprising the steps of:
s1, adsorbing a part of impurity solvent of a crude hydrogen sulfide product, and liquefying to obtain a first crude hydrogen sulfide product;
s2, fractionating the first hydrogen sulfide crude product to obtain a second hydrogen sulfide crude product and light waste gas;
and S3, fractionating the second hydrogen sulfide crude product to obtain hydrogen sulfide gas and a heavy impurity product.
2. The method for purifying hydrogen sulfide as claimed in claim 1, wherein the light waste gas is condensed and liquefied, or returned to fractional distillation again to obtain hydrogen product.
3. The method for purifying hydrogen sulfide as claimed in claim 1 or 2, wherein the hydrogen sulfide gas is condensed and liquefied, or returned to the fractional distillation treatment again to obtain hydrogen sulfide product.
4. The method of claim 1, wherein the solvent is used by adsorption and then fractionated and returned for recycling.
5. The method for purifying hydrogen sulfide as claimed in claim 1, wherein the solvent used for solvent absorption is one or more of sulfolane, dimethyl sulfoxide and tetraethylene glycol.
6. An apparatus for purifying hydrogen sulfide, comprising:
the inlet of the side wall of the absorption tower is communicated with the feeding pipeline, and the inlet of the solvent recovery tower is communicated with the outlet at the bottom of the absorption tower;
the inlet of the compression cooling device is connected with the outlet at the top of the absorption tower;
the inlet of the side wall of the light component removal tower is connected with the outlet of the compression cooling device, and the outlet of the top of the light component removal tower is communicated with the light waste gas condensation circulating reflux assembly;
and the side wall inlet of the heavy component removal tower is connected with the bottom outlet of the light component removal tower, and the top outlet of the heavy component removal tower is communicated with the hydrogen sulfide condensation circulating reflux assembly.
7. The apparatus of claim 6, wherein the solvent absorber column has a pressure of 0.1MPa to 0.2MPa and a temperature of 20 ℃ to 40 ℃.
8. The apparatus for purifying hydrogen sulfide as claimed in claim 6, wherein the top pressure of the lightness-removing column is 1.0MPa to 2.5 MPa; the temperature is-30 ℃ to 40 ℃; the pressure of the tower kettle is 1.1MPa to 2.6 MPa; the temperature is 0-40 ℃.
9. The apparatus for purifying hydrogen sulfide of claim 6, wherein the overhead pressure of said de-weighting column is 1.0MPa to 2.5 MPa; the temperature is 0-40 ℃; the pressure of the tower kettle is 1.1MPa to 2.6 MPa; the temperature is 10-200 ℃.
10. The apparatus for purifying hydrogen sulfide as claimed in claim 6, wherein the pressure in the top of the solvent recovery column is 0.01MPa to 0.2 MPa; the temperature is 10-120 ℃; the pressure of the tower kettle is 0.005 MPa-0.25 MPa; the temperature is 180-350 ℃.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN113387333A (en) * | 2021-06-18 | 2021-09-14 | 山东新和成氨基酸有限公司 | Post-treatment method of hydrogen sulfide |
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| CN110342471A (en) * | 2019-08-14 | 2019-10-18 | 山东中天科技工程有限公司 | The purification system and purifying technique of hydrogen sulfide gas |
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| US3365374A (en) * | 1967-06-07 | 1968-01-23 | Chevron Res | H2s recovery by absorption and plural distillation |
| CN106310691A (en) * | 2016-10-11 | 2017-01-11 | 成都深冷液化设备股份有限公司 | Process and device for purifying H2S in chemical tail gas |
| CN106823691A (en) * | 2017-02-21 | 2017-06-13 | 西南化工研究设计院有限公司 | A kind of method of hydrogen sulfide gas concentrate |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN113387333A (en) * | 2021-06-18 | 2021-09-14 | 山东新和成氨基酸有限公司 | Post-treatment method of hydrogen sulfide |
| CN113387333B (en) * | 2021-06-18 | 2023-01-31 | 山东新和成氨基酸有限公司 | Post-treatment method of hydrogen sulfide |
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