CN103421566A - Process and device for recycling sulfur removed from natural gas - Google Patents
Process and device for recycling sulfur removed from natural gas Download PDFInfo
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- CN103421566A CN103421566A CN2013103683937A CN201310368393A CN103421566A CN 103421566 A CN103421566 A CN 103421566A CN 2013103683937 A CN2013103683937 A CN 2013103683937A CN 201310368393 A CN201310368393 A CN 201310368393A CN 103421566 A CN103421566 A CN 103421566A
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Abstract
The invention relates to a natural gas purifying method, in particular to a method and equipment for removing hydrogen sulfide from natural gas and recycling elemental sulfur. The device is composed of a hydrophobic membrane component, an oxidation regeneration tank, an absorbing liquid tank and the like. Natural gas desulfuration is realized through steps of natural gas desulfuration, catalytic solution regeneration and elemental sulfur recycling and by utilizing a membrane-based absorption method. Filling density of a hollow fibrous membrane contactor is 30-50 times larger than that of a conventional absorber, and hydrogen sulfide removal rate can reach more than 99%. A catalytic oxidation system is formed by adopting an iron ion tower and different complexing agents and catalysts under the action of air, absorbed hydrogen sulfide is effectively converted into elemental sulfur to be recycled, and barren liquor after regeneration can serve as absorbing liquid for cyclic utilization. The absorbing liquid and the catalysts are all low in price, easy to obtain and free of heavy metal pollutants, so that useful elemental sulfur is generated in the whole process while no substance harmful to environment is generated.
Description
Technical field
The present invention relates to a kind of Processes and apparatus of removing hydrogen sulfide and reclaim sulphur simple substance from Sweet natural gas, belong to the gas sweetening processing technology field.
Background technology
Sweet natural gas is a kind of high-energy, free of contamination fossil energy, and the development and use that strengthens Sweet natural gas not only can solve China's power supply in short supply, also can realize changing to low-carbon (LC), environment-friendly type industrial model.China has abundant natural gas source, but approximately in 30% Sweet natural gas, contains sulphur.Hydrogen sulfide has severe toxicity and severe corrosive, is one of source of pollution that cause acid rain, and meeting corrosion pipeline and device, and harm environment and human health belong to the atmospheric polluting material that must control.In the Sweet natural gas new standard GB17820 that China 2012 promulgates, stipulate, by total sulfur content in a class natural gas from 100mg/m
3Reduce to 60mg/m
3.On the other hand, sulfocompound is important industrial chemicals, is the indispensable thing for preparing the products such as sulphur, sulfuric acid, rubber, if can not rationally utilize these components, will cause the loss of natural resources to reach the havoc to ecotope.So, control the content of emission gases medium sulphide content and realize that it is the focus that scholars pay close attention to that element sulphur reclaims always.
At present, at selexol process and sulfur recovery field, many Technologies are arranged both at home and abroad, can be divided into generally three kinds of combustion method, Reducing and absorption method and catalytic oxidations.Combustion method is typically claus process the most, and this technique comprises combustion phases and catalytic reaction stages, comprises the main equipments such as roasting kiln, condenser, catalyticreactor, and a whole set of technical process is comparatively complicated; And in final tail gas of discharging, the content of hydrogen sulfide or other sulfide fails to reach emission standard, need further process.SCOT technique is the representative of Reducing and absorption method, usually comprises hydrogenating reduction, chilling and three parts of absorption and regeneration.This technology degree of purification is high, but its technology investment and consumption indicators are also the highest.Mainly contain arsyl technique in oxidation style, ADA method etc.In arsyl technique, use absorption liquid to contain heavy metal, its discharging of waste liquid will produce pollution; And ADA method oxidation rate is slower, by product is too many.
Chinese patent CN1218421A discloses a kind of method for gas purification to containing hydrogen sulfide and all the other sulfide, the sulfide that this method adopts the bio-oxidation technology to process in waste gas obtains elemental sulfur, in the washings by after processing loops back the gas wash tower step, technique is comparatively complicated, and adaptability is not high.Disclose a kind of sulphur-containing exhaust gas desulfurization and reclaimed the Technology of elemental sulfur in patent CN102527202A, this process using sulphite and acid solution are combined to form absorption liquid and remove sulfide, separate again and obtain elemental sulfur, but this method does not relate to the regeneration problem of absorption liquid, and the 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 technique all exist cost high, the deficiency that secondary pollution is serious, economic benefit is low and the by-product utilization rate is low.Therefore, design and develop out a kind of selexol process of succinct practicality and can realize again the technique that the sulphur resource reclaims simultaneously, will produce huge benefit aspect economy and environmental protection.
Summary of the invention
The technique that the object of the present invention is to provide a kind of natural gas conditioning and sulphur simple substance is reclaimed, adopt film base absorption process to remove the hydrogen sulfide in Sweet natural gas, and because the packing density of hollow fiber membrane contactors is large, the contact area of unit volume reaches 3000～5000m
2/ m
3, large 30～50 times than traditional resorber, so can realize the desulfurization degree more than 99%.Whole cost of investment is low, and purification efficiency is high, under gentle condition, realizes easy to operate easy to control and reach the effect that reclaims useful matter.The absorption liquid that the present invention is used and regeneration soln, catalyzer are all cheap and easy to get, and can recycle, have effectively reduced the secondary pollution to environment.Its principle of work is as follows:
Basic solution absorbs 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 absorption liquid absorbed in flow container is sent into the shell side of hydrophobic membrane assembly by submersible pump, be passed into the tube side of membrane module after the unstripped gas supercharging, and hydrogen sulfide penetrates fenestra and absorption liquid generation chemical reaction, generates HS
-Thereby be removed; The purified gas obtained is discharged from membrane module, collect detection, and a rich solution part enters the absorption flow container, and a part enters the oxidation regeneration groove;
(2) catalytic solution regeneration: in the oxidation regeneration groove, by ferric ion solution, metal-salt complexing agent, regenerated catalyst, and the catalyzed oxidation agent solution that the sulfur modifier of trace forms is oxidized to elemental sulfur by HS-, and Fe
3+Be reduced into Fe
2+Be passed into oxidation trough simultaneously and regenerate inner air by Fe
2+Be oxidized to Fe
3+, make regeneration of waste liquor;
(3) reclaim elementary sulfur: the elemental sulfur that oxidation generates coexists with hygrometric state and washing state in solution, sulfur granules become gradually large after, because action of gravity is deposited to the funnel type bottom of oxidation regeneration groove; By the sulphur stock pump, oxidation regeneration groove bottom solution is sent in cyclone separator, carries out solid-liquid separation, the sulphur simple substance separated is sent to sulfur recovery and processes, and liquid input absorption flow container after the recycle pump pressurization can utilize again.
Membrane module described in step (1) is preferably multistage, and assembling mode is that serial or parallel connection all can; Described absorption liquid is basic solution, such as Na
2CO
3Solution, the alcamines solvent such as APA, DEA or ammoniacal liquor etc., preferably Na
2CO
3With NaHCO
3Buffered soln, pH value is in 9 left and right.
Described in step (2), ferric ion solution is iron(ic) chloride, Fe
3+Concentration is at 200～250mg/L; It is 1～10 gram that the metal-salt complexing agent is selected nitrilotriacetic acid(NTA) (NTA) or its content of sulphosalicylic acid (FD), and it can be combined with molysite, thereby prevents Fe (OH)
2Generation with the FeS precipitation; Regenerated catalyst is selected Resorcinol, 2-ethyl grace quinhydrones or oxidation state tannin extract, and this type of material can play the effect that promotes that elemental sulfur generates; Sulfur modifier is preferred certain herbaceous plants with big flowers alcohol, can increase the sulphur particle size diameter, the convenient recovery.
Described in step (3), oxidation trough inside is provided with resistive heater, and temperature is controlled at the 310K left and right; There is bubble distributer the air intake duct lower end, to improve regenerative response speed; Air flow control is at 3m
3/ h is upper and lower; The solution pH value should not surpass 9, can reduce the generation of the by products such as polysulfide and thiosulphate.
A kind of for above-mentioned selexol process and reclaim the equipment of elemental sulfur method, comprise that one absorbs flow container, at least one hydrophobic membrane assembly, an oxidation regeneration groove; The unstripped gas pipeline is connected in hydrophobic membrane tube side upper end, absorbs in flow container and is provided with submersible pump, absorbs flow container and is connected with the import of hydrophobic membrane shell side and outlet respectively, forms circulation line; The outlet of hydrophobic membrane assembly shell side also is connected with the oxidation regeneration groove, oxidation regeneration groove lower part outlet communicates with the cyclone separator import by the sulphur stock pump, two outlets of cyclone separator, one connects the sulfur recovery treatment unit, another connects filtrate receiver, and filtrate receiver is connected with the absorption flow container by vacuum pump; The oxidation regeneration groove also connects an air compressor.
Venting port is arranged at oxidation regeneration groove top, and there is heating unit inside, and the breather line bottom be connected with air compressor is provided with bubble distributer, and sidewall has the catalyzer fluid inlet, and its bottom is conical design.
In the present invention, sulfur removing pregnant solution is discharged rear portion from membrane module and is entered the absorption flow container, and another part enters the oxidation regeneration groove.Oxidation trough bottom sulphur slurry is after solid-liquid separation, and liquid enters the recycle of absorption liquid tank after the vacuum pump supercharging.
The present invention is high to the degree of purification of Sweet natural gas, energy consumption is low, easy to operate.The absorption of hydrogen sulfide and regeneration of waste liquor and sulfur recovery once complete, and do not have any pollutant emission.This method had both been removed this toxic gas of hydrogen sulfide, again this material was turned waste into wealth, and was reclaimed, and killed 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 technique do not need the main equipments such as roasting kiln, condenser, and running cost is cheap, can under gentle condition, carry out, easy to operate; Absorption liquid used, catalyzer are all cheap and easy to get, and all do not contain heavy metal pollutants, and regenerability is good, can further reduce process costs; 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%; Absorption liquid and catalyzer all can be recycled, and resource utilization is high; Metal chelating agent and sulfur modifier, have very strong catalytic activity, the generation of having accelerated elemental sulfur with separate, improved whole flow process required time, avoided the problems such as Corrosion blockage simultaneously.
The 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 that reclaims elemental sulfur
In figure: 1, tensimeter; 2, control valve; 3, one-level membrane module (hollow fiber hydrophobic membrane assembly); 4, under meter; 5, absorb flow container; 6, submersible pump; 7, oxidation regeneration groove; 8, resistive heater; 9, bubble distributer; 10, sulphur stock pump; 11, sulfur recovery treatment unit; 12, cyclone separator; 13, filtrate receiver; 14, vacuum pump; 15, air compressor.
Embodiment
Unstripped gas is through tensimeter 1, and control valve 2 is adjusted to the tube side upper end that suitable pressure (0.1～2MPa) enters membrane module 3.Simultaneously absorption liquid from tank 5 through submersible pump 6 superchargings, shell side one side that enters membrane module after under meter 4 meterings, with the infiltration hydrogen sulfide generation chemical reaction of coming in tube side, it is removed, purified gas flows out and collects detection from the tube side downside, rich solution 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 arranged in oxidation trough, the metal-salt complexing agent, regenerated catalyst, and the sulfur modifier of trace, control fluid temperature in the 310K left and right by resistive heater 8.HS
-The catalyzed elemental sulfur that is oxidized to, the elemental sulfur that reaction generates coexists with hygrometric state and washing state in solution, sulfur granules become gradually large after, because action of gravity is deposited to the bottom of funnel type.
When having oligo-element sulphur to be suspended in fluid surface, the air produced by air compressor 15 is delivered in oxidation trough through control valve and pipeline, the pipeline bottom is provided with bubble distributer 9, can increase the solubleness of oxygen in solution, accelerate the solution oxide regeneration rate, the venting port on oxidation trough top can carry out the regulating tank internal pressure.Sulphur stock pump 10 is sent into mixed solution in cyclone separator 12 and is carried out solid-liquid separation, isolated sulphur simple substance enters sulfur recovery treatment unit 11, and liquid enters filtrate receiver 13, under the effect of vacuum pump 14, lean solution is sent to and absorbs in flow container 5, can again be used for purified natural gas.
Embodiment 1
The Na that configuration concentration is 0.5mol/L
2CO
3With NaHCO3 buffered soln, measuring its pH value is 9 left and right, and temperature is 30 ℃, and flow control, at 100L/h, is input to tube side one side of membrane module.Contain the 10%(volume ratio) raw natural gas of hydrogen sulfide, keep flow velocity at 1500L/h, be passed into the membrane module shell side and move with the absorption liquid adverse current.A rich solution part is back to and absorbs in flow container, and a part enters oxidation trough.Ferric chloride Solution is contained in oxidation trough inside, Fe
3+Concentration is 200mg/L, and it is 5 grams that the metal-salt complexing agent is selected nitrilotriacetic acid(NTA) (NTA) content, and solution temperature is controlled at 30 ℃.Device is after operation for some time, utilize the gas component after the gas chromatograph analysis purifies, result shows: in purified gas, the hydrogen sulfide proportion is 0.48%, desulfurization degree is more than 95%, in oxidation trough, there is yellow sulfur granule to produce, elemental sulfur enters sulfur recovery and processes after cyclone separator separates, and can make the bright sulfur product by operations such as washing, dehydrations.
Embodiment 2
The pure Na that configuration concentration is 1mol/L
2CO
3Solution, temperature is 25 ℃ of normal temperature, flow control, at 150L/h, is input to tube side one side of membrane module.Contain the 10%(volume ratio) raw natural gas of hydrogen sulfide, keep flow velocity at 2000L/h, be passed into the membrane module shell side and move with the absorption liquid adverse current.A rich solution part is back to and absorbs in flow container, and a part enters oxidation trough.Ferric chloride Solution is contained in oxidation trough inside, Fe
3+Concentration is 250mg/L, and it is 5 grams that the metal-salt complexing agent is selected sulphosalicylic acid (FD) content, and adds micro-sulfur modifier certain herbaceous plants with big flowers alcohol, and solution temperature is controlled at 30 ℃.Device is after operation for some time, utilize the gas component after the gas chromatograph analysis purifies, result shows: in purified gas, the hydrogen sulfide proportion is 0.39%, desulfurization degree is more than 95%, in oxidation trough, yellow sulfur granule generation time shortens, elemental sulfur enters sulfur recovery and processes after cyclone separator separates, and can make the bright sulfur product by operations such as washing, dehydrations.
Embodiment 3
The pure Na that configuration concentration is 1.5mol/L
2CO
3Solution, temperature is 30 ℃ of normal temperature, and flow control, at 200L/h, is input to tube side one side of membrane module, and membrane module is selected the two-stage series connection mode, and the shell side of first step membrane module is connected with the entrance of next stage respectively with the tube side outlet.Contain the 15%(volume ratio) raw natural gas of hydrogen sulfide, keep flow velocity at 2000L/h, be passed into the membrane module shell side and move with the absorption liquid adverse current.A rich solution part is back to and absorbs in flow container, and a part enters oxidation trough.Ferric chloride Solution is contained in oxidation trough inside, Fe
3+Concentration is 300mg/L, and it is 5 grams that the metal-salt complexing agent is selected trolamine (TEA) content, Resorcinol 5 grams, and micro-sulfur modifier certain herbaceous plants with big flowers alcohol, solution temperature is controlled at 30 ℃, and pH value is 8.5.Device is after operation for some time, utilize the gas component after the gas chromatograph analysis purifies, result shows: hydrogen sulfide proportion less than 0.1% in purified gas, desulfurization degree is more than 99%, yellow sulfur granule generation time is arranged than shortening in embodiment 2 in oxidation trough, elemental sulfur enters sulfur recovery and processes after cyclone separator separates, and can make the bright sulfur product by operations such as washing, dehydrations.
Claims (9)
1. a selexol process reclaim the method for elemental sulfur, is characterized in that comprising the steps:
(1) selexol process: the basic salt absorption liquid absorbed in flow container is sent into the shell side of hydrophobic membrane assembly by submersible pump, be passed into the tube side of membrane module after the unstripped gas supercharging, and hydrogen sulfide penetrates fenestra and absorption liquid generation chemical reaction, generates HS
-Thereby be removed; The purified gas obtained is discharged from membrane module, collect detection, and a rich solution part enters the absorption flow container, and a part enters the oxidation regeneration groove;
(2) catalytic solution regeneration: in the oxidation regeneration groove, by ferric ion solution, metal-salt complexing agent, regenerated catalyst, and the catalyzed oxidation agent solution that the sulfur modifier of trace forms is by HS
-Be oxidized to elemental sulfur, and Fe
3+Be reduced into Fe
2+Be passed into oxidation trough simultaneously and regenerate inner air by Fe
2+Be oxidized to Fe
3+, make regeneration of waste liquor;
(3) reclaim elementary sulfur: the elemental sulfur that oxidation generates coexists with hygrometric state and washing state in solution, sulfur granules become gradually large after, because action of gravity is deposited to the funnel type bottom of oxidation regeneration groove; By the sulphur stock pump, oxidation regeneration groove bottom solution is sent in cyclone separator, carries out solid-liquid separation, the sulphur simple substance separated is sent to sulfur recovery and processes, and liquid input absorption flow container after the recycle 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 basic salt absorption liquid is metal salt solution, alcamines solvent, ammoniacal liquor or their the formulated solution of various components.
3. 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 the polyvinylidene fluoride hollow fiber hydrophobic membrane, membrane module is at least one-level, and when being multistage, array mode is that serial or parallel connection is installed.
4. a kind of selexol process according to claim 1 reclaim the method for elemental sulfur, it is characterized in that: the regenerated catalyst that the catalyzed oxidation agent solution is contained is polyphenols or oxidation state tannin extract.
5. a kind of selexol process according to claim 4 reclaim the method for elemental sulfur, it is characterized in that: described polyphenols is Resorcinol or 2-ethyl grace quinhydrones.
6. 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 polyvalent alcohol materials.
7. a kind of selexol process according to claim 1 reclaim the method for elemental sulfur, it is characterized in that: in the oxidation regeneration groove, solution temperature is controlled at 25 ~ 50 ℃, and pH value is below 9.5.
8. a selexol process reclaim the device of elemental sulfur, comprise that one absorbs flow container, at least one hydrophobic membrane assembly, an oxidation regeneration groove; The unstripped gas pipeline is connected in hydrophobic membrane tube side upper end, absorbs in flow container and is provided with submersible pump, absorbs flow container and is connected with the import of hydrophobic membrane shell side and outlet respectively, forms circulation line; The outlet of hydrophobic membrane assembly shell side also is connected with the oxidation regeneration groove, oxidation regeneration groove lower part outlet communicates with the cyclone separator import by the sulphur stock pump, two outlets of cyclone separator, one connects the sulfur recovery treatment unit, another connects filtrate receiver, and filtrate receiver is connected with the absorption flow container by vacuum pump; The oxidation regeneration groove also connects an air compressor.
9. selexol process according to claim 8 reclaim the device of elemental sulfur, it is characterized in that: venting port is arranged at oxidation regeneration groove top, there is heating unit inside, the breather line bottom be connected with air compressor is provided with bubble distributer, sidewall has the catalyzer fluid inlet, and its bottom is conical design.
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Cited By (9)
| 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 |
| 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 |
| 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 |
| CN108624370A (en) * | 2017-03-20 | 2018-10-09 | 中国石油化工股份有限公司 | The method that biogas UF membrane purifies biological methane processed |
| CN108970380A (en) * | 2018-09-07 | 2018-12-11 | 宜宾丝丽雅股份有限公司 | Method and device for removing hydrogen sulfide in waste gas by continuous oxidation |
| CN114591769A (en) * | 2020-12-04 | 2022-06-07 | 中国石油化工股份有限公司 | Membrane system structure for removing hydrogen sulfide from natural gas |
| CN118681394A (en) * | 2024-08-29 | 2024-09-24 | 山东禧龙石油装备有限公司 | Wet desulfurization device for gas treatment and wet desulfurization method thereof |
| CN118681394B (en) * | 2024-08-29 | 2024-10-29 | 山东禧龙石油装备有限公司 | Wet desulfurization device for gas treatment and wet desulfurization method thereof |
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Cited By (12)
| 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 |
| 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 |
| 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 |
| CN108624370A (en) * | 2017-03-20 | 2018-10-09 | 中国石油化工股份有限公司 | The method that biogas UF membrane purifies biological methane processed |
| 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 |
| CN108970380A (en) * | 2018-09-07 | 2018-12-11 | 宜宾丝丽雅股份有限公司 | Method and device for removing hydrogen sulfide in waste gas by continuous oxidation |
| 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 |
| CN114591769A (en) * | 2020-12-04 | 2022-06-07 | 中国石油化工股份有限公司 | Membrane system structure for removing hydrogen sulfide from natural gas |
| 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 |
| CN118681394A (en) * | 2024-08-29 | 2024-09-24 | 山东禧龙石油装备有限公司 | Wet desulfurization device for gas treatment and wet desulfurization method thereof |
| CN118681394B (en) * | 2024-08-29 | 2024-10-29 | 山东禧龙石油装备有限公司 | Wet desulfurization device for gas treatment and wet desulfurization method thereof |
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|---|---|
| CN103421566B (en) | 2016-01-27 |
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