CN103691289A - Processing method of liquid sulfur pool tail gas in claus process - Google Patents

Processing method of liquid sulfur pool tail gas in claus process Download PDF

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Publication number
CN103691289A
CN103691289A CN201410026037.1A CN201410026037A CN103691289A CN 103691289 A CN103691289 A CN 103691289A CN 201410026037 A CN201410026037 A CN 201410026037A CN 103691289 A CN103691289 A CN 103691289A
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tail gas
claus
subsider
processing
molten sulfur
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CN201410026037.1A
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Chinese (zh)
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CN103691289B (en
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曾翔鹏
朱元彪
曹玉虎
候怡帆
姜艾汝
吕明方
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烟台新瑞环保科技有限公司
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Abstract

The invention discloses a processing method of liquid sulfur pool tail gas in a claus process. The processing method comprises the following steps: air blows a liquid sulfur pool of a claus device, the liquid sulfur pool tail gas is mixed with the air, then the mixture enters an absorption supergravity reactor to be in contact with a desulfurizer of a subsider, and gas after removal of sulfuretted hydrogen is evacuated; a sulfur-containing reduction-state desulfurizer realizes desulfurizer regeneration under the action of blowing air; the regenerated desulfurizer is pumped back to the subsider, and sulfur is quickly settled to the bottom of the subsider to form sulfur plasma; the sulfur plasma forms solid sulfur, filter liquid is pumped back to the subsider, and regenerated desulfurizing liquid in the subsider is pumped into the absorption supergravity reactor to enter the next circulation. By utilizing the processing method, the emission of tail gas is up to the standard, claus tail gas with any volume can be processed, a tail gas incinerator is omitted so that discharge of smoke dust in the air is reduced, the processing rate is high, the mass transfer intensity is high, the size of the device is small, floor space is less, sulfur loss is reduced, the safety performance is high, the processing method is environmentally friendly, waste gas, waste water and industrial residue are not produced, operation is stable, and running is reliable.

Description

The processing method of molten sulfur pond tail gas in a kind of claus process
 
Technical field:
The present invention relates to a kind of processing method of tail gas, relate in particular to the processing method of molten sulfur pond tail gas in a kind of claus process.
Background technology:
Current domestic recovery technology of sulfur, the overwhelming majority adopts the low-temperature catalyzed conversion claus process of thermal transition+secondary, and the advantage technique of claus process is simple, is applicable to maximize and the device of realizing high automation production, and device efficiency is high.But owing to being subject to the restriction of chemical balance and reversible reaction under reaction temperature, sulfur recovery rate is the highest also can only reach 96-97%, still has the sulphur of 3-4% with SO 2form enter atmosphere, after increasing tail gas hydrogenation treating apparatus, sulfur recovery rate can reach 99.7%.Still be difficult to guarantee to meet new discharging standards.In addition in actual production process, owing to producing load, do not reach initial designs ability, cause the flow fluctuation variation larger with composition of tail gas, not only cause the rising of cost, also caused exceeding standard of tail gas sulfur content.
The H comprising in molten sulfur pond in claus process 2s gas progressively discharges in Molten sulphur cooling procedure, is discharged in atmosphere, is to have caused one of reason that Claus tail gases sulfur content exceeds standard.The feature that Claus tail gases has is large-minded, hydrogen sulfide content is little, conventional treatment process is difficult for the discharging standards that reaches new.
Goal of the invention:
The object of the invention is to overcome the deficiency of prior art and molten sulfur pond exhaust gas treating method in a kind of claus process is provided, making tail gas qualified discharge.Vent gas treatment rate of the present invention is high, and mass transfer intensity is high, and equipment volume is little, and floor space is few; Reduced sulphur loss; Security performance is high, and environmental friendliness does not have the three wastes to produce; Stable operation, reliable.
Object of the present invention can reach by following measure: the processing method of molten sulfur pond tail gas in a kind of claus process, it is characterized in that it is under super gravity field, the method of using novel chelated iron liquid phase oxidation to process the molten sulfur pond tail gas of claus process device, comprises the steps:
, desulfurizing agent is pumped in subsider;
, air purge Cross unit molten sulfur pond, molten sulfur pond tail gas mixing air enters absorption supergravity reactor, contacts at the wire packing of rotor with the desulfurizing agent coming from subsider, hydrogen sulfide is oxidized to elemental sulfur, Fe in desulfurizing agent 3+become Fe 2+, the gas that removes hydrogen sulfide is emptying through supergravity reactor built-in filter;
, reduction-state desulfurizing agent Fe under the effect at purging air in absorbing supergravity reactor of containing sulphur 2+become Fe 3+, realize desulfurizer regeneration; Desulfurizing agent blowback subsider after regeneration, sulphur is deposited to rapidly subsider bottom and forms sulphur slurry;
, sulphur slurry is pumped into and vacuum filter, forms solid sulfur, filtrate blowback subsider from subsider outlet at bottom;
, the regenerative sulfur binding liquid pump in subsider enters to absorb supergravity reactor, enters next circulation.
In order further to realize object of the present invention, the described desulfurizing agent that contains chelated iron ion contains following component: chelated iron catalyst, chelating agent, surfactant, chelating agent protective agent, bactericide, alkali lye, water, chelated iron catalyst concn scope: 350 ~ 10000ppm in desulfurizing agent; Chelating agent concentration range: 400 ~ 15000ppm; Surfactant concentration ranges: 1 ~ 1000ppm; Concentration of sterilant scope: 1 ~ 1000ppm; Chelating agent protective agent concentration range: 10 ~ 100000ppm; Alkali concn scope: 0.1 ~ 1mol/L; The volume ratio of chelating agent/chelated iron catalyst is 1 ~ 5; PH value of solution is 8 ~ 10.
In order further to realize object of the present invention, described chelated iron catalyst is the mixture of chelated iron, alcohol and water, and the mol ratio of alcohol/chelating Fe is 0.1 ~ 5, and in solution, the content of iron is 350 ~ 10000ppm.
In order further to realize object of the present invention, described chelated iron is HEDP, EDTMPS, DTPMPA, EDDHA, STPP, NTA, Na 3nTA, EDTA, HEDTA, Na 3hEDTA, Na 4at least one in EDTA, gluconic acid sodium salt, sodium metasilicate, potassium tartrate, natrium citricum and soluble ferric iron salt FeCl 3, Fe 2(SO 4) 3, Fe (NO 3) 3, FeNH 4(SO 4) at least one chelate, the mol ratio of chelate part/Fe is 1 ~ 10; Alcohol is at least one in micromolecular secondary alcohol, the tertiary alcohol, reproducibility alcohol, as the tert-butyl alcohol, isopropyl alcohol, isoamyl alcohol, glucitol, sorbierite, sweet mellow wine etc.;
In order further to realize object of the present invention, described chelating agent is HEDP, EDTMPS, DTPMPA, EDDHA, STPP, NTA, Na 3nTA, EDTA, HEDTA, Na 3hEDTA, Na 4at least one in EDTA, gluconic acid sodium salt, sodium metasilicate, potassium tartrate, natrium citricum.
In order further to realize object of the present invention, described surfactant be carbon number be 5 ~ 20 straight chain alcohol or polyalcohol at least one.Mainly C 5h 11oH, C 5h 12o 2, C 6h 13oH, C 6h 14o 2, C 6h 12o 2, C 8h 11oH, C 12h 25one or more mixtures of OH;
In order further to realize object of the present invention, described bactericide is at least one in wide-spectrum bactericide zephiran, as docosyl dimethyl benzyl ammonium chloride, myristyl dimethyl benzyl ammonium chloride, two dodecyl dimethyl ammonium chlorides etc.;
In order further to realize object of the present invention, described chelating agent protective agent is at least one of KI, KCl, KBr; In hydrogen sulfide stripping process, can produce hydroxyl radical free radical, destroy the stable of chelating agent, the protectant effect of chelating agent is the hydroxyl radical free radical producing in Absorption Desulfurization process, makes chelating agent all the time in stable state.
In order further to realize object of the present invention, described alkali lye is KOH, NaOH; In doctor solution, add alkali lye, make doctor solution system keep pH to be stabilized between 8 ~ 10.
For molten sulfur pond tail gas, adopt air bubbling purging process, utilize the bleed mode of pressurization of roots blower to enter absorption supergravity reactor.In the gas treatment equipment of molten sulfur pond, owing to using air purge to make to enter the air capacity absorbing in supergravity reactor enough large, do not need separately to establish regeneration reactor, absorb and regeneration is all carried out in absorption reactor thermally, subsider is set.
The present invention can produce following good effect compared with the prior art: the present invention is under a kind of super gravity field, uses novel chelated iron liquid phase oxidation to process the method for claus process molten sulfur pond tail gas, and it is by following advantage:
, any tolerance tail gas can process, there is no tail gas incinerator, reduced the discharge of flue dust in air;
, vent gas treatment rate is high, after processing, in tail gas, hydrogen sulfide content is less than 1ppm, reaches national requirements for environmental protection;
, mass transfer intensity is high, equipment volume is little, floor space is few;
, doctor solution time of staying in reactor is short, reduced sulphur loss;
, security performance is high, do not use any poisonous chemical substance, there is no hydrogen sulfide gas in sulfur product, avoided the poisoning danger of operating personnel;
, environmental friendliness, do not have the three wastes to produce;
, open, stop easily, can within a few minutes, reach steady state operation;
, reliable, device do not stop up, can long-term operation.
Accompanying drawing explanation:
Fig. 1 is process chart of the present invention;
The specific embodiment: the specific embodiment of the present invention is elaborated below in conjunction with accompanying drawing:
The preparation of desulfurizing agent:
1, by FeCl 3, NTA, potassium tartrate, the tert-butyl alcohol be 1:2.5:1:1.5 according to mol ratio ratio is mixed, making total concentration of iron is the chelated iron catalyst concentrates of 14g/L.Get chelated iron catalyst concentrates 37.5mL, NTA chelating agent concentrate 56.25mL is diluted to 1500mL, in dilution, total concentration of iron is 350ppm, in dilution, adds C 5h 12o 20.15g, KCl 0.15g, KOH8.5g makes desulfurizing agent;
2, by Fe 2(SO 4) 3, EDTA, HEDTA, natrium citricum, isoamyl alcohol be 1:2:1.5:1:1:1.5 according to mol ratio ratio is mixed, making total concentration of iron is the chelated iron catalyst concentrates of 56g/L.Get chelated iron catalyst concentrates 267mL, EDTA and HEDTA chelating agent concentrate 321mL is diluted to 1500mL, in dilution, total concentration of iron is 10000ppm, in dilution, adds C 5h 12o 20.9g, KCl 0.6g, KOH8.5g makes desulfurizing agent;
3, by Fe (NO 3) 3, HEDP, NTA, gluconic acid sodium salt, glucitol be 1:1:1:1:1 according to mol ratio ratio is mixed, making total concentration of iron is the chelated iron catalyst concentrates of 35g/L, gets chelated iron catalyst concentrates 21.5mL, Na 4eDTA chelating agent concentrate 33mL is diluted to 1500mL, and in dilution, total concentration of iron is 500ppm, in dilution, adds C 5h 12o 20.3g, KCl 0.3g, KOH8.5g makes desulfurizing agent;
4, by Fe (NO 3) 3, HEDP, DTPMPA, sorbierite, the tert-butyl alcohol be 1:2:1:0.5:0.5 according to mol ratio ratio is mixed, making total concentration of iron is the chelated iron catalyst concentrates of 56g/L, get chelated iron catalyst concentrates 27mL, HEDTA chelating agent concentrate 32mL is diluted to 1500mL, in dilution, total concentration of iron is 1000ppm, in dilution, adds C 5h 12o 20.3g, C 12h 25oH0.15g, KBr 0.3g, KI 0.15g, KOH8.5g makes desulfurizing agent;
5, by FeCl 3, Fe 2(SO 4) 3, Fe (NO 3) 3, EDTMPS, DTPMPA, sorbierite be 1:1:0.5:2:1:1 according to mol ratio ratio is mixed, making total concentration of iron is the chelated iron catalyst concentrates of 56g/L.Get chelated iron catalyst concentrates 107mL, Na 3hEDTA chelating agent concentrate 210mL is diluted to 1500mL, and in dilution, total concentration of iron is 4000ppm, in dilution, adds C 5h 12o 20.5g, C 6h 12o 20.3g, KI 0.5g, KOH8.5g makes desulfurizing agent;
6, by FeCl 3, Fe (NO 3) 3, STPP, HEDTA, sweet mellow wine, the tert-butyl alcohol be 1:1:2:1:1:1 according to mol ratio ratio is mixed, making total concentration of iron is the chelated iron catalyst concentrates of 56g/L.Get chelated iron catalyst concentrates 227mL, EDTA, HEDTA chelating agent concentrate 280mL is diluted to 1500mL, in dilution, total concentration of iron is 8500ppm, in dilution, adds C 5h 12o 20.5g, C 6h 12o 20.3g, C 8h 11oH 0.3g, KCl 0.3g, KBr 0.3g, KI 0.15g, KOH8.5g makes desulfurizing agent.
Embodiment: the processing method of a kind of molten sulfur pond vent gas treatment, it comprises the steps:
, the desulfurizing agent of above-mentioned preparation is pumped in subsider;
, with air purge molten sulfur pond, in molten sulfur pond, gas mixing air enters absorption supergravity reactor through booster fan, contact at the wire packing of rotor with the desulfurizing agent coming from subsider, the chelated iron ionic oxide formation that hydrogen sulfide is desulfurized in agent is sulphur, ferric ion is reduced to ferrous ion, and the gas that removes hydrogen sulfide is emptying through supergravity reactor built-in filter; ;
, the reduction-state desulfurizing agent that contains sulphur contacts with the air that air inlet comes in absorbing supergravity reactor, ferrous ion is oxidized to ferric ion, realizes desulfurizer regeneration; The recycling desulfurizer that contains sulphur enters subsider by regeneration liquid pump, and sulphur is deposited to rapidly subsider bottom and forms sulphur slurry;
, sulphur slurry enters vacuum filter by sulphur stock pump and forms solid sulfur, in filtrate blowback subsider;
, the regenerative sulfur binding liquid in subsider enters and absorbed supergravity reactor and carry out next one and circulate by recycle liquid pump.
 
Adopt above-mentioned desulfurizing agent, process the claus process molten sulfur pond tail gas of variable concentrations by the method for embodiment 1, result is as shown in table 1:
Table 1 result
Numbering Molten sulfur pond concentration of hydrogen sulfide % Fluid flow m 3/h Desulfurization/regeneration temperature ℃ Purified gas hydrogen sulfide content ppm
1 0.015 3 45/45 0.0
2 0.032 3 45/45 0.1
3 0.067 3 45/45 0.1
4 0.138 3 45/45 0.0
5 0.179 3 45/45 0.1
6 0.230 3 45/45 0.0
Theoretically, tannin extract method, modified ADA method, PDS method, OR-GREEN method, FD method, LO-CAT method are all applicable to the present invention, but tannin extract method, modified ADA method, PDS method, equipment needed thereby are many, alkali consumption is large in complex operation, course of reaction, investment is large; FD method sulfosalicylic acid Complexing Iron used is catalyst, and recovery time length and catalyst are easily degraded, and technology investment is large; PDS method have the danger of hydrogen cyanide poisoning and alkali consumption large; Although OR-GREEN method and the technological process of LO-CAT method are simple, the catalyst using is unstable, and easily degraded, increases investment cost.
Below for process that concentration of hydrogen sulfide is 0.032% molten sulfur pond tail gas time, respectively under super gravity field by tannin extract method, modified ADA method, FD method, PDS method, LO-CAT method, OR-GREEN method and the inventive method processing, result is as shown in table 2.
Table 2 comparing result
Numbering Technique title Main catalyst Purified gas hydrogen sulfide content ppm
1 Tannin extract method Tannin extract catalyst 26
2 Modified ADA method Improvement anthraquinone disulphonate 32
3 FD method Sulfosalicylic acid Complexing Iron 49
4 PDS method PDS catalyst 58
5 LO-CAT method Complexing Iron 5
6 OR-GREEN method Complexing Iron 17
7 Novel chelating iron processes Novel chelated iron 0.1
Desulfurizing agent in above-described embodiment can also adopt other existing desulfurizing agents that contains chelated iron ion; above embodiment is described the preferred embodiment of the present invention; not scope of the present invention is limited; design under the prerequisite of spirit not departing from the present invention; various distortion and improvement that the common engineers and technicians in this area make technical scheme of the present invention, all should fall in the definite protection domain of claims of the present invention.

Claims (8)

1. a processing method for molten sulfur pond tail gas in claus process, is characterized in that it is under super gravity field, and the method for using novel chelated iron liquid phase oxidation to process the molten sulfur pond tail gas of claus process device, comprises the steps:
, desulfurizing agent is pumped in subsider;
, air purge Cross unit molten sulfur pond, molten sulfur pond tail gas mixing air enters absorption supergravity reactor, contacts at the wire packing of rotor with the desulfurizing agent coming from subsider, hydrogen sulfide is oxidized to elemental sulfur, Fe in desulfurizing agent 3+become Fe 2+, the gas that removes hydrogen sulfide is emptying through supergravity reactor built-in filter;
, reduction-state desulfurizing agent Fe under the effect at purging air in absorbing supergravity reactor of containing sulphur 2+become Fe 3+, realize desulfurizer regeneration; Desulfurizing agent blowback subsider after regeneration, sulphur is deposited to rapidly subsider regeneration reactor bottom and forms sulphur slurry;
, sulphur slurry is pumped into and vacuum filter, forms solid sulfur, filtrate blowback subsider regeneration reactor from subsider regeneration reactor outlet at bottom;
, the regenerative sulfur binding liquid pump in subsider regeneration reactor enters to absorb supergravity reactor, enters next circulation.
2. the processing method of molten sulfur pond tail gas in a kind of claus process according to claim 1, it is characterized in that described desulfurizing agent is the desulfurizing agent that contains chelated iron ion, it contains following component: chelated iron catalyst, chelating agent, surfactant, chelating agent protective agent, bactericide, alkali lye, water, chelated iron catalyst concn scope: 350 ~ 10000ppm in desulfurizing agent; Chelating agent concentration range: 400 ~ 15000ppm; Surfactant concentration ranges: 1 ~ 1000ppm; Concentration of sterilant scope: 1 ~ 1000ppm; Chelating agent protective agent concentration range: 10 ~ 100000ppm; Alkali concn scope: 0.1 ~ 1mol/L; The volume ratio of chelating agent/chelated iron catalyst is 1:1 ~ 5:1; PH value of solution is 8 ~ 10.
3. the processing method of molten sulfur pond tail gas in a kind of claus process according to claim 2, it is characterized in that described chelated iron catalyst is the mixture of chelated iron, alcohol and water, the mol ratio of alcohol/chelating Fe is 0.1 ~ 5, and in solution, the content of iron is 350 ~ 10000ppm.
4. the processing method of molten sulfur pond tail gas in a kind of claus process according to claim 3, is characterized in that described described chelated iron is HEDP, EDTMPS, DTPMPA, EDDHA, STPP, NTA, Na 3nTA, EDTA, HEDTA, Na 3hEDTA, Na 4at least one in EDTA, gluconic acid sodium salt, sodium metasilicate, potassium tartrate, natrium citricum and soluble ferric iron salt FeCl 3, Fe 2(SO 4) 3, Fe (NO 3) 3, FeNH 4(SO 4) at least one chelate, the mol ratio of chelate part/Fe is 1 ~ 10; Alcohol is at least one in micromolecular secondary alcohol, the tertiary alcohol, reproducibility alcohol.
5. the processing method of molten sulfur pond tail gas in a kind of claus process according to claim 2, is characterized in that described chelating agent is HEDP, EDTMPS, DTPMPA, EDDHA, STPP, NTA, Na 3nTA, EDTA, HEDTA, Na 3hEDTA, Na 4at least one in EDTA, gluconic acid sodium salt, sodium metasilicate, potassium tartrate, natrium citricum.
6. the processing method of molten sulfur pond tail gas in a kind of claus process according to claim 2, it is characterized in that described surfactant be carbon number be 5 ~ 20 straight chain alcohol or polyalcohol at least one.
7. the processing method of molten sulfur pond tail gas in a kind of claus process according to claim 2, is characterized in that described bactericide is at least one in spectrum bactericide zephiran.
8. the processing method of molten sulfur pond tail gas in a kind of claus process according to claim 2, is characterized in that described chelating agent protective agent is at least one of KI, KCl, KBr.
CN201410026037.1A 2014-01-21 2014-01-21 The processing method of molten sulfur pond tail gas in a kind of claus process CN103691289B (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104043326A (en) * 2014-06-04 2014-09-17 北京化工大学 Apparatus for high gravity removal of hydrogen sulfide of novel industrial gas, and technology thereof

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US6610264B1 (en) * 1992-04-15 2003-08-26 Exxonmobil Oil Corporation Process and system for desulfurizing a gas stream
JP4847949B2 (en) * 2004-03-03 2011-12-28 シエル・インターナシヨネイル・リサーチ・マーチヤツピイ・ベー・ウイShell Internationale Research Maatschappij Besloten Vennootshap A highly efficient method for the recovery of sulfur from acid gas streams.
CN101874968B (en) * 2009-12-31 2013-01-02 中北大学 Iron complex desulfurizer suitable for super-gravity desulfurization
CN102151476B (en) * 2011-03-29 2013-06-05 武汉国力通化工环保科技有限公司 Method for removing hydrogen sulfide in gas phase through oxidization under high gravity field

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104043326A (en) * 2014-06-04 2014-09-17 北京化工大学 Apparatus for high gravity removal of hydrogen sulfide of novel industrial gas, and technology thereof
CN104043326B (en) * 2014-06-04 2016-08-17 北京化工大学 The device of a kind of industrial gases hypergravity removing hydrogen sulfide and technique

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