CN103421566B - A kind of natural gas deviates from sulfur recovery technology and device - Google Patents
A kind of natural gas deviates from sulfur recovery technology and device Download PDFInfo
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- CN103421566B CN103421566B CN201310368393.7A CN201310368393A CN103421566B CN 103421566 B CN103421566 B CN 103421566B CN 201310368393 A CN201310368393 A CN 201310368393A CN 103421566 B CN103421566 B CN 103421566B
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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- Y02P20/50—Improvements relating to the production of bulk chemicals
- Y02P20/584—Recycling of catalysts
Abstract
The present invention relates to a kind of natural gas purification method, be specifically related to a kind ofly from natural gas, remove hydrogen sulfide and reclaim the method and apparatus of sulphur simple substance.Apparatus of the present invention, by hydrophobic membrane assembly, oxidation regeneration groove, absorb the formation such as flow container.The present invention is by selexol process, catalytic solution regeneration and the step reclaiming elementary sulfur, and utilize membrane-base absorption method to carry out selexol process, larger than conventional suction device 30 ~ 50 times of the loading density due to hollow fiber membrane contactors, hydrogen sulfide removal rate can reach more than 99%.Adopt arrange in pairs or groups different complexing agent and catalyst of iron ion to form catalytic oxidation system under air effect, the hydrogen sulfide of absorption is converted into sulphur simple substance effectively and is reclaimed, can be used as absorbing liquid after lean solution regeneration and recycle.Absorbing liquid involved in the present invention, regenerated catalyst is all cheap and easy to get and not containing heavy metal contaminants, in whole process except producing useful elemental sulfur, do not produce material environment being had to harm.
Description
Technical field
The present invention relates to a kind of Processes and apparatus removed hydrogen sulfide and reclaim sulphur simple substance from natural gas, belong to gas purification processing technology field.
Background technology
Natural gas is a kind of high-energy, free of contamination fossil energy, and the development and use strengthening natural gas not only can solve China's energy supply in short supply, also can realize changing to low-carbon (LC), environment-friendly type industrial model.China has abundant natural gas resource, but containing sulphur in the natural gas of about 30%.Hydrogen sulfide has severe toxicity and severe corrosive, is one of pollution sources causing acid rain, and understands corrosion pipeline and device, and harm environment and human health, belong to the atmosphere pollution that must control.Specify, by total sulfur content in a class natural gas from 100mg/m in the natural gas new standard GB17820 that China promulgates for 2012
3reduce to 60mg/m
3.On the other hand, sulfur-containing compound is important industrial chemicals, is the indispensable thing preparing the products such as sulphur, sulfuric acid, rubber, if can not these components of Appropriate application, will cause the loss of natural resources and the heavy damage to ecological environment.So, the content of control discharge sulfide in gas to realize that element sulphur reclaims be the focus that scholars pay close attention to always.
At present, there are many technologies at selexol process and sulfur recovery field both at home and abroad, combustion method, reducing absorping method and catalytic oxidation three kinds can be divided into generally.Combustion method is claus process the most typically, and this technique comprises combustion phases and catalytic reaction stages, and comprise the main equipments such as combustion furnace, condenser, catalytic reactor, whole set process flow process is comparatively complicated; And in final tail gas of discharging, the content of hydrogen sulfide or other sulfide fails to reach discharge standard, need process further.SCOT technique is the representative of reducing absorping method, usually comprises hydrogenating reduction, chilling and absorption and regeneration three parts.This technology degree of purification is high, but its technology investment and consumption indicators are also the highest.Arsyl technique is mainly contained, ADA method etc. in oxidizing process.Use absorbing liquid to contain heavy metal in arsyl technique, generation is polluted by its discharging of waste liquid; And ADA method oxidation rate is comparatively slow, accessory substance is too many.
Chinese patent CN1218421A discloses a kind of to the method for gas purification containing hydrogen sulfide and all the other sulfide, the sulfide that this method adopts biological oxidation technology to process in waste gas obtains elemental sulfur, cleaning solution after process is being looped back in gas scrubbing tower step, technique is comparatively complicated, and adaptability is not high.In patent CN102527202A, disclose a kind of sulphur-containing exhaust gas desulfurization and reclaim the technology of elemental sulfur, this technique adopts sulphite and acid solution to be combined to form absorbing liquid and removes sulfide, carry out separation again and obtain elemental sulfur, but this method does not relate to the regeneration issues of absorbing liquid, and resource recycling rate is not high.In sum, all take much count of the improvement of hydrogen sulfide both at home and abroad, but existing desulfurization and sulfur recovery technology all to there is cost high, the deficiency that secondary pollution is serious, economic benefit is low and by-product utilization rate is low.Therefore, the selexol process designing and developing out a kind of brief and practical can realize again the technique of Sulphur ressource recovery simultaneously, will produce huge benefit in economy and environmental protection.
Summary of the invention
The object of the present invention is to provide a kind of natural gas purification and the technique reclaimed sulphur simple substance, employing membrane-base absorption method removes the hydrogen sulfide in natural gas, and because the loading density of hollow fiber membrane contactors is large, the contact area of unit volume reaches 3000 ~ 5000m
2/ m
3, larger than traditional absorber 30 ~ 50 times, so the desulfurization degree of more than 99% can be realized.Overall cost of investment is low, and purification efficiency is high, realizes easy to operate easy to control and reach the effect reclaiming utility under mild conditions.The absorbing liquid that the present invention is used and actified solution, catalyst are all cheap and easy to get, and can recycle, and effectively reduce the secondary pollution to environment.Its operation principle is as follows:
Alkaline solution absorption H
2s:Na
2cO
3+ H
2s → NaHCO
3+ NaHS
Analyse sulphur process: 2Fe
3+(complex state)+HS
-→ 2Fe
2+(complex state)+S ↓+H
+
Regenerative response: 2Fe
2+(complex state)+1/2O
2+ H
2o → 2Fe
3+(complex state)+OH
-
For achieving the above object, the present invention adopts a kind of selexol process and reclaims the method for elemental sulfur, comprises the following steps:
(1) selexol process: the basic salt absorbing liquid absorbed in flow container is sent into the shell side of hydrophobic membrane assembly by immersible pump, be passed into the tube side of membrane module after unstripped gas supercharging, hydrogen sulfide penetrates fenestra and absorbing liquid generation chemical reaction, generates HS
-thus be removed; The purified gas obtained is discharged from membrane module, and carry out collection and detect, and a rich solution part enters absorption flow container, a part enters oxidation regeneration groove;
(2) catalytic solution regeneration: in oxidation regeneration groove, by ferric ion solution, slaine complexing agent, regenerated catalyst, and HS-is oxidized to elemental sulfur by the catalytic oxidation agent solution of the sulfur modifier composition of trace, and Fe
3+be reduced into Fe
2+; Be passed into the inner air of oxidation trough regeneration by Fe simultaneously
2+be oxidized to Fe
3+, make regeneration of waste liquor;
(3) recovery elementary sulfur: the elemental sulfur that oxidation generates coexists with hygrometric state and washing state in the solution, and sulfur granules becomes greatly gradually, because Action of Gravity Field is deposited to bottom the funnel type of oxidation regeneration groove; Be sent in cyclone separator by sulphur stock pump by oxidation regeneration groove bottom solution, carry out Separation of Solid and Liquid, the sulphur simple substance separated is sent to sulfur recovery process, and liquid input absorption flow container after circulating pump pressurization can utilize again.
Described in step (1), membrane module is preferably multistage, and assembling mode is serial or parallel connection; Described absorbing liquid is alkaline solution, such as Na
2cO
3solution, alcamines solvent or the ammoniacal liquor etc. such as APA, DEA, preferably Na
2cO
3with NaHCO
3cushioning liquid, pH value is about 9.
Described in step (2), ferric ion solution is iron chloride, Fe
3+concentration is at 200 ~ 250mg/L; Slaine complexing agent selects NTA (NTA) or sulfosalicylic acid (FD) its content to be 1 ~ 10 gram, and it can be combined with molysite, thus prevents Fe (OH)
2with the generation of FeS precipitation; Regenerated catalyst selects hydroquinones, 2-ethyl grace quinhydrones or oxidation state tannin extract, and this type of material can play the effect promoting that elemental sulfur generates; Sulfur modifier is preferred certain herbaceous plants with big flowers alcohol then, can increase sulphur particle size diameter, convenient recovery.
Described in step (3), oxidation trough inside is provided with resistive heater, and temperature controls at about 310K; There is bubble distributer air intake duct lower end, to improve regenerative response speed; Air flow control is at 3m
3/ h is upper and lower; Solution pH value, no more than 9, can reduce the generation of the accessory substance such as polysulfide and thiosulfate.
Reclaim the equipment of elemental sulfur method for above-mentioned selexol process, comprise one and absorb flow container, at least one hydrophobic membrane assembly, an oxidation regeneration groove; Unstripped gas pipeline is connected to hydrophobic membrane tube side upper end, absorbs in flow container and is provided with immersible pump, absorbs flow container and is connected with outlet with the import of hydrophobic membrane shell side respectively, form circulation line; Hydrophobic membrane assembly shell-side outlet is also connected with oxidation regeneration groove, oxidation regeneration groove lower part outlet is communicated with cyclone separator import by sulphur stock pump, two outlets of cyclone separator, one connects sulfur recovery treating apparatus, another connects filtrate receiver, and filtrate receiver is connected with absorption flow container by vavuum pump; Oxidation regeneration groove also connects an air compressor.
Exhaust outlet is arranged at oxidation regeneration groove top, and there is heater inside, and the breather line bottom be connected with air compressor is provided with bubble distributer, and sidewall has catalyst inlet, and bottom it is conical design.
In the present invention, sulfur removing pregnant solution is discharged rear portion from membrane module and is entered absorption flow container, and another part enters oxidation regeneration groove.Oxidation trough bottom sulphur slurry is after Separation of Solid and Liquid, and liquid enters absorbing liquid tank and recycles after vavuum pump supercharging.
The degree of purification of the present invention to natural gas is high, energy consumption is low, easy to operate.The absorption of hydrogen sulfide and regeneration of waste liquor and sulfur recovery once complete, and there is not any pollutant emission.This method had both eliminated this toxic gas of hydrogen sulfide, was turned waste into wealth by this material again, reclaimed, kill two birds with one stone.Its investment is lower, pollution-free, is the new technology of a kind of purified natural gas and sulfur recovery, meets current advocated energy-saving and emission-reduction, the requirement of low-altitude discharged.
Compared to existing technology, advantage of the present invention is: selexol process of the present invention and sulfur recovery technology do not need the main equipment such as combustion furnace, condenser, and operating cost is cheap, can carry out under mild conditions, easy to operate; Absorbing liquid used, catalyst are all cheap and easy to get, and all not containing heavy metal pollutants, regenerability is good, can reduce process costs further; Hydrogen sulfide stripping efficiency of the present invention is high, and single stage membrane assembly desulfurization degree reaches more than 95%, and maximum desulfurization degrees of Using Multistage Membranes assembly can reach 99.5%; Absorbing liquid and catalyst all can be recycled, and resource utilization is high; Metal chelating agent and sulfur modifier, have very strong catalytic activity, the generation accelerating elemental sulfur be separated, improve whole flow process required time, avoid the problems such as Corrosion blockage simultaneously.
Accompanying drawing explanation
Below in conjunction with accompanying drawing, the present invention will be further described:
Fig. 1 is selexol process of the present invention and the device schematic diagram reclaiming elemental sulfur
In figure: 1, Pressure gauge; 2, control valve; 3, one-level membrane module (hollow fiber hydrophobic membrane assembly); 4, flowmeter; 5, flow container is absorbed; 6, immersible pump; 7, oxidation regeneration groove; 8, resistive heater; 9, bubble distributer; 10, sulphur stock pump; 11, sulfur recovery treating apparatus; 12, cyclone separator; 13, filtrate receiver; 14, vavuum pump; 15, air compressor.
Detailed description of the invention
Unstripped gas is through Pressure gauge 1, and control valve 2 is adjusted to the tube side upper end that suitable pressure (0.1 ~ 2MPa) enters membrane module 3.Simultaneously stability liquid from tank 5 through immersible pump 6 supercharging, flowmeter 4 enters the shell side side of membrane module after measuring, with the hydrogen sulfide gas generation chemical reaction permeated in tube side, removed, purified gas flows out and collects detection on the downside of tube side, rich solution then flows out from the outlet of shell side opposite side, and a part enters and absorbs flow container 5, and a part enters oxidation regeneration groove 7.
Ferric ion solution is had, slaine complexing agent, regenerated catalyst in oxidation trough, and the sulfur modifier of trace, control fluid temperature at about 310K by resistive heater 8.HS
-catalyzedly be oxidized to elemental sulfur, the elemental sulfur that reaction generates coexists with hygrometric state and washing state in the solution, sulfur granules become gradually large after, because Action of Gravity Field is deposited to the bottom of funnel type.
When there being oligo-element sulphur to be suspended in liquid surface, the air produced by air compressor 15 is delivered in oxidation trough through control valve and pipeline, pipeline bottom is provided with bubble distributer 9, oxygen solubility in the solution can be increased, accelerate solution oxide regeneration rate, the exhaust outlet on oxidation trough top can carry out pressure in regulating tank.Mixed liquor is sent in cyclone separator 12 and is carried out Separation of Solid and Liquid by sulphur stock pump 10, isolated sulphur simple substance enters sulfur recovery treating apparatus 11, and liquid enters filtrate receiver 13, under the effect of vavuum pump 14, lean solution is sent to and absorbs in flow container 5, again can be used for purified natural gas.
Embodiment 1
Configuration concentration is the Na of 0.5mol/L
2cO
3with NaHCO3 cushioning liquid, measuring its pH value is about 9, and temperature is 30 DEG C, and flow-control, at 100L/h, is input to the tube side side of membrane module.Containing 10%(volume ratio) raw natural gas of hydrogen sulfide, keep flow velocity at 1500L/h, be passed into membrane module shell side and absorbing liquid adverse current is run.A rich solution part is back to and absorbs in flow container, and a part enters oxidation trough.Ferric chloride solution is contained, Fe in oxidation trough inside
3+concentration is 200mg/L, and slaine complexing agent selects NTA (NTA) content to be 5 grams, and solution temperature controls at 30 DEG C.After plant running a period of time, gas component after utilizing chromatographic to purify, result shows: in purified gas, hydrogen sulfide proportion is 0.48%, desulfurization degree is more than 95%, yellow drusen is had to produce in oxidation trough, elemental sulfur enters sulfur recovery process after cyclone separator is separated, and obtains bright sulfur product by operations such as washing, dehydrations.
Embodiment 2
Configuration concentration is the pure Na of 1mol/L
2cO
3solution, temperature is normal temperature 25 DEG C, and flow-control, at 150L/h, is input to the tube side side of membrane module.Containing 10%(volume ratio) raw natural gas of hydrogen sulfide, keep flow velocity at 2000L/h, be passed into membrane module shell side and absorbing liquid adverse current is run.A rich solution part is back to and absorbs in flow container, and a part enters oxidation trough.Ferric chloride solution is contained, Fe in oxidation trough inside
3+concentration is 250mg/L, and slaine complexing agent selects sulfosalicylic acid (FD) content to be 5 grams, and adds micro-sulfur modifier certain herbaceous plants with big flowers alcohol, and solution temperature controls at 30 DEG C.After plant running a period of time, gas component after utilizing chromatographic to purify, result shows: in purified gas, hydrogen sulfide proportion is 0.39%, desulfurization degree is more than 95%, in oxidation trough, yellow drusen generation time shortens, elemental sulfur enters sulfur recovery process after cyclone separator is separated, and obtains bright sulfur product by operations such as washing, dehydrations.
Embodiment 3
Configuration concentration is the pure Na of 1.5mol/L
2cO
3solution, temperature is normal temperature 30 DEG C, and flow-control is at 200L/h, and be input to the tube side side of membrane module, two-stage series connection mode selected by membrane module, and namely the shell side of first order membrane module exports with tube side and is connected with the entrance of next stage respectively.Containing 15%(volume ratio) raw natural gas of hydrogen sulfide, keep flow velocity at 2000L/h, be passed into membrane module shell side and absorbing liquid adverse current is run.A rich solution part is back to and absorbs in flow container, and a part enters oxidation trough.Ferric chloride solution is contained, Fe in oxidation trough inside
3+concentration is 300mg/L, and slaine complexing agent selects triethanolamine (TEA) content to be 5 grams, hydroquinones 5 grams, micro-sulfur modifier certain herbaceous plants with big flowers alcohol, and solution temperature controls at 30 DEG C, and pH value is 8.5.After plant running a period of time, gas component after utilizing chromatographic to purify, result shows: in purified gas, hydrogen sulfide proportion is less than 0.1%, desulfurization degree is more than 99%, yellow drusen generation time is had to shorten than in embodiment 2 in oxidation trough, elemental sulfur enters sulfur recovery process after cyclone separator is separated, and obtains bright sulfur product by operations such as washing, dehydrations.
Claims (7)
1. selexol process reclaim the method for elemental sulfur, is characterized in that comprising the steps:
(1) selexol process: the basic salt absorbing liquid absorbed in flow container is sent into the shell side of hydrophobic membrane assembly by immersible pump, be passed into the tube side of membrane module after unstripped gas supercharging, hydrogen sulfide penetrates fenestra and absorbing liquid generation chemical reaction, generates HS
-thus be removed; The purified gas obtained is discharged from membrane module, and carry out collection and detect, and a rich solution part enters absorption flow container, a part enters oxidation regeneration groove; Described basic salt absorbing liquid is Na
2cO
3with NaHCO
3cushioning liquid or single Na
2cO
3solution;
(2) catalytic solution regeneration: in oxidation regeneration groove, by ferric ion solution, slaine complexing agent, regenerated catalyst, and the catalytic oxidation agent solution of the sulfur modifier composition of trace is by HS
-be oxidized to elemental sulfur, and Fe
3+be reduced into Fe
2+; Be passed into the air of oxidation regeneration groove inside by Fe simultaneously
2+be oxidized to Fe
3+, make regeneration of waste liquor; Described regenerated catalyst is polyphenols or oxidation state tannin extract;
(3) recovery elementary sulfur: the elemental sulfur that oxidation generates coexists with hygrometric state and washing state in the solution, and sulfur granules becomes greatly gradually, because Action of Gravity Field is deposited to bottom the funnel type of oxidation regeneration groove; Be sent in cyclone separator by sulphur stock pump by oxidation regeneration groove bottom solution, carry out Separation of Solid and Liquid, the sulphur simple substance separated is sent to sulfur recovery process, and liquid input absorption flow container after circulating pump pressurization can utilize again.
2. a kind of selexol process according to claim 1 reclaim the method for elemental sulfur, it is characterized in that: described hydrophobic membrane assembly is polyvinylidene fluoride hollow fiber hydrophobic membrane, membrane module is at least one-level, and when for time multistage, combination is that serial or parallel connection is installed.
3. a kind of selexol process according to claim 1 reclaim the method for elemental sulfur, is characterized in that: described polyphenols is hydroquinones or 2-ethyl anthracene quinhydrones.
4. a kind of selexol process according to claim 1 reclaim the method for elemental sulfur, it is characterized in that: described sulfur modifier, is certain herbaceous plants with big flowers alcohol or other polyol agent.
5. a kind of selexol process according to claim 1 reclaim the method for elemental sulfur, is characterized in that: in oxidation regeneration groove, solution temperature controls at 25 ~ 50 DEG C, and pH value is below 9.5.
6. selexol process reclaim the device of elemental sulfur, comprises one and absorbs flow container, at least one hydrophobic membrane assembly, an oxidation regeneration groove; Unstripped gas pipeline is connected to hydrophobic membrane tube side upper end, absorbs in flow container and is provided with immersible pump, absorbs flow container and is connected with outlet with the import of hydrophobic membrane shell side respectively, form circulation line; Hydrophobic membrane assembly shell-side outlet is also connected with oxidation regeneration groove, oxidation regeneration groove lower part outlet is communicated with cyclone separator import by sulphur stock pump, two outlets of cyclone separator, one connects sulfur recovery treating apparatus, another connects filtrate receiver, and filtrate receiver is connected with absorption flow container by vavuum pump; Oxidation regeneration groove also connects an air compressor.
7. selexol process according to claim 6 reclaim the device of elemental sulfur, it is characterized in that: exhaust outlet is arranged at oxidation regeneration groove top, there is heater inside, the breather line bottom be connected with air compressor is provided with bubble distributer, sidewall has catalyst inlet, and bottom it is conical design.
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Families Citing this family (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103894063A (en) * | 2014-03-26 | 2014-07-02 | 南通正拓气体有限公司 | Recycling method and device for desulfurization waste liquid |
| CN106552476A (en) * | 2015-09-24 | 2017-04-05 | 中国石油化工股份有限公司 | A kind of method of removing hydrogen sulfide in natural gas |
| CN106554834A (en) * | 2015-09-24 | 2017-04-05 | 中国石油化工股份有限公司 | A kind of removal methods of hydrogen sulfide in natural gas |
| CN106554836A (en) * | 2015-09-24 | 2017-04-05 | 中国石油化工股份有限公司 | A kind of processing method of hydrogen sulfide in natural gas |
| CN108624370B (en) * | 2017-03-20 | 2021-04-06 | 中国石油化工股份有限公司 | Method for preparing biological methane by separating and purifying methane membrane |
| CN108970380B (en) * | 2018-09-07 | 2023-07-21 | 宜宾丝丽雅股份有限公司 | Method and device for removing hydrogen sulfide in waste gas by continuous oxidation |
| CN114591769B (en) * | 2020-12-04 | 2023-11-10 | 中国石油化工股份有限公司 | Membrane system structure for removing hydrogen sulfide from natural gas |
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| CN1785480A (en) * | 2005-11-17 | 2006-06-14 | 江苏工业学院 | Membrane adsorption natural gas desulfur method |
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| CN1785480A (en) * | 2005-11-17 | 2006-06-14 | 江苏工业学院 | Membrane adsorption natural gas desulfur method |
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