CN106540512A - The absorbent of sulfide in a kind of selectively removing natural gas - Google Patents
The absorbent of sulfide in a kind of selectively removing natural gas Download PDFInfo
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- CN106540512A CN106540512A CN201510596761.2A CN201510596761A CN106540512A CN 106540512 A CN106540512 A CN 106540512A CN 201510596761 A CN201510596761 A CN 201510596761A CN 106540512 A CN106540512 A CN 106540512A
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Abstract
The invention belongs to natural gas purification technical field, the method that the aqueous solution that a kind of employing polyamide-amide class compound of proposition is formed after being mixed with hydramine makees the selectively removing sulfide of absorbent.Under conventional desulfurization technological process and each unit appointed condition, the absorbent can be from containing CO2And H2S、COS、CS2, selectively removing sulfide in the mixed airflow of one or more sulfide such as RSH, select removing ability with than the more preferable sulfide of conventional alcohol amine solvent, the more conventional solvent of solvent absorption ability is strong, and the circulating load of absorbing liquid can be greatly reduced.
Description
Technical field
The invention belongs to natural gas purification technical field, and in particular to a kind of from containing CO2And H2The absorbent of selectively removing sulfide in the natural gas of one or more sulfide such as S, COS, RSH.
Background technology
Natural gas is a kind of high-quality, the efficient, low-carbon energy of cleaning and industrial chemicals, and its resource status becomes increasingly conspicuous.In order to reduce CO2, the pollutant such as dust discharge capacity, the consumption figure continued smooth of global natural gas increases, it is Chinese then in rapid growth.However, having the natural gas of nearly 40% reserves to be containing H in whole world residue gas field according to statistics2S and CO2Acidity poor quality natural gas, partially acidic natural gas also cos-containing（COS）, mercaptan（RSH）Deng organic sulfur.China contains H2S natural gas explorations have a high potential, H2Gas reserves of the S volume fractions content more than 1% accounts for a quarter of national gas reserves, is mainly distributed on the Sichuan Basin, Ordos Basin, Tarim Basin and Bohai gulf basin, and first three producing region is the main force producing region of China's natural gas.These acid gas fields are projected the most with the Sichuan Basin again, and sulfur-containing gas yield accounts for 80%, H of China's total output2S mean volume fractions up to 10%, be in recent years Gas Fields especially super-huge self-contained gas field finds the more and larger block of Productivity Construction, the main force for being listed in China " 12 " conventional gas builds block.Continuing to increase for domestic and international Natural Gas Consumption Using, will promote gas extraction inferior.At the same time, both at home and abroad to SO in the quality index and waste gas of gas product2Emission control is increasingly severe.Therefore, in order that natural gas is smoothly exploited, natural gas purification technical requirements are using higher levels of technology.
At present, hydramine method is the leading technology technology for removing acid impurities in natural gas both at home and abroad, has been developed for range of solvents, to the requirement for meeting different material gas composition and purified gas product specification.At present, hydramine method removing H2S and CO2Technology be mainly based upon alcohol amine solvent（Monoethanolamine, diethanolamine, diethyl Propanolamine and N methyldiethanol amine）Technology, especially with N methyldiethanol amine（MDEA）And its Technology based on Formula type solvent.MDEA has the advantages that certain desulfuration selectivity and regeneration energy consumption are low, sour gas load is big, equipment corrosion is weak.Thus, MDEA solution is widely used in various removing H2S、CO2Industrial cleaning facility.
Using hydramine solvent removal H2S and CO2When, the organic sulfur such as weakly acidic COS, RSH, the concrete composition depending on its content height and removing solution also will obtain different degrees of removing.Substantial amounts of commercial Application and result of study show, brothers hydramine（Monoethanolamine, diethanolamine, diethyl Propanolamine）Generation reversible products of metamorphism or irreversible products of metamorphism can be reacted with COS, short chain RSH, so as to show higher removal efficiency to COS, but existed or regeneration energy consumption is high, or amine loss is big, or the defect such as equipment corrosion is serious.Tertiary alkanolamine（Such as MDEA）Alkalescence is weak, and reversible or irreversible metamorphic reaction does not occur with COS, RSH, and wherein COS can be removed by partial hydrolysiss mode, and RSH can only be removed on a small quantity by physical dissolution.In addition, its response speed compares CO when COS is hydrolyzed by hydramine solvent2With at least slow two orders of magnitude of the response speed of hydramine, only in H2S and CO2When removing degree is very low, certain removal efficiency is just can guarantee that.Therefore, the removing degree of COS is caused to depend critically upon H2S and CO2Sour gas load.Carbon bisulfide（CS2）Generally occur in unstripped gas with COS, CS2Removing principle and process it is identical with COS.Meanwhile, all hydramine for using are all relatively low to the removing degree of RSH at present.Therefore, the natural gas _ raw material gas higher for organic sulfur content, the industrial Relative economy for considering process, generally using hydramine solvent content or whole removing H2S and CO2Afterwards, hydrolysis reactor is set by hydrolyzing removing COS and CS2, mol sieve unit adsorbing and removing RSH is set, or organic sulfur is removed using other group technologies, ultimately caused that long flow path, equipment is more, investment is big and unit product consumption indicators height.
In order to sulfide being removed on conventional equipment and technological process, not being removed or appropriateness removing CO2, the research and development of substantial amounts of technique and solvent are had been carried out both at home and abroad.But more than 80 years of natural gas are applied to from hydramine method, process aspect does not have big change, and what progress was maximum is then solvent exploitation, defines the purification techniques development mode based on solvent exploitation.And solvent can remove H2S can remove the organic sulfurs such as COS, RSH an effective solvent developing way be exactly hydramine, physical solvent and water physical chemistry Physical Absorption solvent and hindered amine absorbers.US3989811 proposes to use diisopropanolamine (DIPA)（DIPA）With the aqueous solution selectively removing COS of sulfolane, in this process COS be first hydrolyzed into H2S and CO2Then absorbed.Although realizing Selective Separation H on the whole2S and COS, but the CO in acid gas2Also major part is absorbed, while rich solution regeneration temperature is also higher.US60456354 and CN100411710C proposes that the mixture using piperazine, MDEA and sulfolane or methoxy triglycol, alkyl ether or pyrrolidinone derivatives N- N-formyl morpholine Ns and N- acetyl morphine derivants, dialkylethers/N- N-formyl morpholine Ns or N- acetyl morphines and derivant process the H in natural gas2S and COS, RSH sulfides.US4749555 is similarly proposed with end of the bridge amine, tertiary alkanolamine（Such as MDEA）The aqueous solution formed with a kind of physical solvent in sulfolane, Allyl carbonate, N-Methyl pyrrolidone is processed containing H2S, COS and major part CO2Process gas, realization optionally remove H2S and COS.CA2498427-A1 proposes to use the mixture combined by several polyamine substances in hydramine, morpholine, piperazine, triazine and its derivant, can effectively remove H2S and RSH.FR0600448 and CN101374588B is proposed using one of industrial conventional component of thiodiglycol hydramine formula solvent, is removed the RSH in natural gas, and achieve preferable effect.The mixed solution that alkanolamine solution is formed with physical solvent, although have good H2S removes selectivity and higher organic sulfur removal rate, but haves the shortcomings that formula solvent is higher to C2 and above hydrocarbon dissolubility and cause higher hydrocarbon loss.There is a class reduce hydrocarbon loss using the solvent of bulky amine, while there is higher removing degree to organic sulfur.US4405585 proposes with sterically hindered amine aqueous solution to realize selectively removing H2S.US4892674 is proposed to non-space steric hindrance amine aqueous solution（Such as MDEA）The sterically hindered amine salt of middle addition and（Or）Sterically hindered aminoacid is improving the H of solution2S removes selectivity.US4895670 proposes to carry out selectively removing H using the mixed liquor of sterically hindered amines and sterically hindered aminoacid2S。
Polyamide-amide（PAMAM）It is the unique dendrimer of a class, the molecular weight and molecular structure of the PAMAM of different algebraically is different.When the molecular weight of PAMAM reaches to a certain degree, in its aqueous solution, space can be formed in PAMAM molecular surfaces, cavity is formed in intramolecule, and these cavitys can be used to wrap up the micromolecular compound for entering molecule content cavity from solution by gap, while them can be made to discharge again under certain condition again.Result of study shows that PAMAM dendrimers have obvious solubilization to weakly acidic nicotinic acid, salicylic acid and ibuprofen etc., and the organic sulfur such as COS and RSH is also Acidic Compounds.Therefore, PAMAM can be used as the component of removing COS and RSH formula solvents.In existing gas purification separation field, not yet have and polyamide-amide is used as into the report that natural gas removes sulfide solvent formula.
The content of the invention
The purpose of the present invention is to propose to one kind is from containing CO2And sulfide（H2S and COS, CS2、RSH）Natural gas in, under the conditions of conventional desulfurization technological process and unit, the absorbent of selectively removing sulfide relative to traditional absorbent, improves the absorbability of solvent, so as to reduce the circulating load and regeneration heat consumption of absorbing liquid.
The main technical schemes of the present invention：The absorbent of sulfide in a kind of selectively removing natural gas, it is characterized in that it makees absorbent using the aqueous solution formed after polyamide-amide class compound and hydramine mixing, wherein the mass fraction of polyamide-amide class compound is 3% ~ 15%, the mass fraction of hydramine is 50% ~ 10%, the mass fraction preferably 50% ~ 30% of hydramine.
Hydramine of the present invention is N methyldiethanol amine（MDEA）, -2 methyl isophthalic acid propanol of 2- amidos, one or two in hydroxyethyl piperazine, or the secondary alcohol amine that other use in the art or tertiary alkanolamine, secondary alcohol amine is in addition to DEA.
The polyamide-amide class compound be with ethylenediamine as core, the compound for preparing as branch of acrylic acid methyl ester..
The polyamide-amide class compound using when be not limited to the mixture of pure each PAMAM or different algebraically polyamide-amide.
The terminal groups of the polyamide-amide class compound can be amido, or modified terminal groups for the polyamide-amide class modified compound of hydroxyl.
It is any at the same include CO2And H2S、COS、CS2, RSH sulfides industrial gas can use the present invention absorbent be processed.What source of the gas was not critical to the invention, including such as natural gas, synthesis gas and various refinery gas.Typically, contain CO in these air-flows2And H2S, wherein, H2The content of S is about 0.01%～20%（mol）, CO2Content about 1%～50%（mol）.
The absorbent of the present invention can be from containing CO2And H2S、COS、CS2, selectively removing sulfide in the mixed airflow of one or more sulfide such as RSH, select removing ability with than the more preferable sulfide of conventional alcohol amine solvent, the more conventional solvent of solvent absorption ability is strong, and the circulating load of absorbing liquid can be greatly reduced.
Description of the drawings
Typical process flows of the Fig. 1 for the selectively removing sulphur compound absorbent application of the embodiment of the present invention, and the conventional flowsheet in natural gas purification field.
In figure, V01- purge gas separators, T01- absorption towers, V02- flash tanks, E02- lean solution coolers, P01- lean pumps, E01- poor rich liquid heat exchangers, T02- regenerators, E03- regeneration Gas Coolers, P02- reflux pumps, E04- boiling devices, V03- regeneration gas separating devices.
Specific embodiment
By following embodiment, the invention will be further described, but which is not intended to limit protection scope of the present invention.
The absorption of following examples and regenerative process flow process as shown in Figure 1.
Technological process is described as follows.Unstripped gas is entered from absorption tower T01 bottoms, with the desulfuration solution counter current contacting under the pouring of absorption tower top spray, the H in gas2S、COS、CS2, RSH sulfides and fraction CO2Absorbed, wet purification gas is sent to V01 purge gas separators and is separated the drop carried under one's arms by tower top extraction is absorbed, and is then drawn and is sent to down operation.
Absorb the desulfuration solution of acid gas（Rich solution）, rich solution flash tank V02 is sent under pressure itself effect, here flashes off the available gas of dissolving.According to specific processed material system and raw material its composition, flash tank flexibly can be set.Rich solution after flash distillation is exchanged heat with lean solution in poor rich liquid heat exchanger E01, after recovery section heat, enter from the top of regenerator T02, the stripping vapor counter current contacting produced with tower bottom steam boiling device E04 from bottom to top desorbs sulfide therein and CO2。
From the regeneration tower bottom solution for having regenerated out（Lean solution）, exchange heat with rich solution into poor rich liquid heat exchanger E01, then Jing after the cooling of lean solution cooler E02 is sent in lean pump P01 pressurizations, finally enter the recycling of absorption tower top.
Regeneration gas Jing regeneration Gas Cooler E03 coolings from the top of regenerator out, then operation after going Jing after moisture trap reclaims condensed fluid.
From regeneration gas, detached condensed fluid is by the pumped back regenerator that flows back, to maintain the solution concentration of system.
Embodiment 1
Raw natural gas（Pressure is 1.5MPaG, room temperature, H2S 1.0%, CO2 5.8%, COS 200mg/m3）, using the present invention absorbent, the solution after being stirred with the polyamide-amide compound of the MDEA of 45%w and 3% as absorbent, purified gas H2S ＜ 4ppmv and COS ＜ 60mg/m3, reach national class natural gas quality index（GB17820-2012）H in regeneration acid gas2S contents ＞ 25%.
Embodiment 2
Raw natural gas（Pressure be 4.6 MPaG, room temperature, H2S 4.8%, CO2 10.2%, COS 200mg/m3, MeSH 400mg/m3）, using the present invention absorbent, the solution after being stirred with the MDEA of 35%w, 5% -2 methyl isophthalic acid propanol of 2- amidos and 10% polyamide-amide as absorbent, purified gas H2The summation ﹤ 60mg/m of S ＜ 4ppmv and COS and MeSH organic sulfurs3, H in regeneration acid gas2S contents ＞ 50%.Under same materials gas composition and technological parameter, during using MDEA as absorbing liquid, when 1.5 times in its solution circulating load about the present embodiment, purified gas H2The summation ﹥ 60mg/m of S ＜ 4ppmv and COS and MeSH organic sulfurs3, not yet reach national class natural gas quality index（GB17820-2012）.
Embodiment 3
Raw natural gas（Pressure is 8.0MPaG, room temperature, H2S 10.1%, CO2 21.2%, COS 300mg/m3, MeSH 500mg/m3）, using the absorbent of the present invention, the solution stirred with the MDEA of 25%w, 10% hydroxyethyl piperazine and 15% polyamide-amide as absorbent, purified gas H2The summation ﹥ 60mg/m of the organic sulfur such as S ＜ 4ppmv and COS and MeSH3, H in regeneration acid gas2S contents ＞ 40%.Under same materials gas composition and technological parameter, during using MDEA as absorbing liquid, when 1.5 times in its solution circulating load about the present embodiment, purified gas H2The total and about 200g/m of S ＜ 4ppmv and COS and MeSH organic sulfurs3, can only achieve national two class natural gas quality index（GB17820-2012）.
Claims (8)
1. in a kind of selectively removing natural gas sulfide absorbent, it is characterized in that the aqueous solution formed using polyamide-amide class compound and hydramine makees absorbent, the wherein mass fraction of polyamide-amide class compound is 3% ~ 15%, and the mass fraction of hydramine is 50% ~ 10%.
2. absorbent according to claim 1, it is characterised in that the mass fraction of hydramine selects 50% ~ 30%.
3. absorbent according to claim 1, it is characterised in that the polyamide-amide class compound be with ethylenediamine as core, the compound for preparing as branch of acrylic acid methyl ester..
4. the absorbent according to claim 1 or 3, it is characterised in that the polyamide-amide class compound using when be not limited to the polyamide-amide mixture of pure each algebraically polyamide-amide or different algebraically.
5. absorbent according to claim 1 and 2, it is characterised in that the hydramine is N methyldiethanol amine, -2 methyl isophthalic acid propanol of 2- amidos, one or two in hydroxyethyl piperazine.
6. absorbent according to claim 1 and 2, it is characterised in that the hydramine is secondary alcohol amine or tertiary alkanolamine, secondary alcohol amine does not include DEA.
7. the absorbent according to claim 1 or 3, it is characterised in that the terminal groups of the polyamide-amide class compound are amido.
8. the absorbent according to claim 1 or 3, it is characterised in that modified compound of the terminal groups of the polyamide-amide class compound for hydroxyl.
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107398148A (en) * | 2017-09-20 | 2017-11-28 | 珠海蓝天环保科技有限公司 | Industrial waste gas inorganic agent and preparation method thereof |
| CN109504477A (en) * | 2018-12-18 | 2019-03-22 | 西安长庆科技工程有限责任公司 | A kind of gas field individual well liquid desulfurizer and process based on non-renewable solution |
| CN110385022A (en) * | 2018-04-19 | 2019-10-29 | 中国石油化工股份有限公司 | The method of desulfurizing agent and its application and lighter hydrocarbons desulfurization processing |
| CN110624390A (en) * | 2019-08-16 | 2019-12-31 | 内蒙古工业大学 | Rapid synthesis method of carbonyl sulfide storage material |
| CN110964492A (en) * | 2018-09-29 | 2020-04-07 | 中国石油化工股份有限公司 | Sulfur dissolving agent and preparation method and application thereof |
| CN113181743A (en) * | 2021-05-21 | 2021-07-30 | 中国纺织科学研究院有限公司 | Method for treating carbon disulfide in waste gas generated in viscose fiber production |
| CN114471127A (en) * | 2022-01-07 | 2022-05-13 | 骆驼集团(安徽)再生资源有限公司 | Secondary lead tail gas absorbent and preparation method thereof |
| WO2022257197A1 (en) * | 2021-06-09 | 2022-12-15 | 华东理工大学 | Application of amine compound in removing organic sulfides |
| WO2024099095A1 (en) * | 2022-11-07 | 2024-05-16 | 中国石油天然气股份有限公司 | Desulfurizer for absorbing hydrogen sulfide and organic sulfur under atmospheric pressure and preparation method for and use of desulfurizer |
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Cited By (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107398148A (en) * | 2017-09-20 | 2017-11-28 | 珠海蓝天环保科技有限公司 | Industrial waste gas inorganic agent and preparation method thereof |
| CN110385022B (en) * | 2018-04-19 | 2022-07-15 | 中国石油化工股份有限公司 | Desulfurizing agent and application thereof, and method for light hydrocarbon desulfurization processing |
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| CN110964492A (en) * | 2018-09-29 | 2020-04-07 | 中国石油化工股份有限公司 | Sulfur dissolving agent and preparation method and application thereof |
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| CN109504477A (en) * | 2018-12-18 | 2019-03-22 | 西安长庆科技工程有限责任公司 | A kind of gas field individual well liquid desulfurizer and process based on non-renewable solution |
| CN109504477B (en) * | 2018-12-18 | 2024-04-30 | 西安长庆科技工程有限责任公司 | Gas field single well liquid desulfurization device and process method based on non-regenerated solution |
| CN110624390A (en) * | 2019-08-16 | 2019-12-31 | 内蒙古工业大学 | Rapid synthesis method of carbonyl sulfide storage material |
| CN113181743A (en) * | 2021-05-21 | 2021-07-30 | 中国纺织科学研究院有限公司 | Method for treating carbon disulfide in waste gas generated in viscose fiber production |
| WO2022257197A1 (en) * | 2021-06-09 | 2022-12-15 | 华东理工大学 | Application of amine compound in removing organic sulfides |
| CN114471127A (en) * | 2022-01-07 | 2022-05-13 | 骆驼集团(安徽)再生资源有限公司 | Secondary lead tail gas absorbent and preparation method thereof |
| CN114471127B (en) * | 2022-01-07 | 2023-02-03 | 骆驼集团(安徽)再生资源有限公司 | Secondary lead tail gas absorbent and preparation method thereof |
| WO2024099095A1 (en) * | 2022-11-07 | 2024-05-16 | 中国石油天然气股份有限公司 | Desulfurizer for absorbing hydrogen sulfide and organic sulfur under atmospheric pressure and preparation method for and use of desulfurizer |
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Application publication date: 20170329 |