CN104548905B - A kind of emulsion oxidation sweetening and sulfur recovery method - Google Patents
A kind of emulsion oxidation sweetening and sulfur recovery method Download PDFInfo
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- CN104548905B CN104548905B CN201310495673.4A CN201310495673A CN104548905B CN 104548905 B CN104548905 B CN 104548905B CN 201310495673 A CN201310495673 A CN 201310495673A CN 104548905 B CN104548905 B CN 104548905B
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Abstract
The invention discloses a kind of emulsion oxidation sweetening and sulfur recovery method, the method includes following content: H 2 S-containing gas enters absorber and oil Complexing Iron emulsion contacts, hydrogen sulfide reaction generates sulfur, and sulfur is dissolved in oil phase, purifies gas and discharges from absorber overhead；Sulfureted oil Complexing Iron emulsion carries out breakdown of emulsion process, then oil-water separation, and Recovered sulphur from oil phase；Wherein oil Complexing Iron emulsion is water-in-oil emulsion.The method has the features such as infiltration rate is fast, desulfuration efficiency is high, simple to operate, has broad application prospects in petroleum refining, Coal Chemical Industry in terms of the removal of hydrogen sulfide gas and the recycling of sulfur.
Description
Technical field
The present invention relates to a kind of oxidation sweetening and sulfur recovery method, specifically a kind of oil-Complexing Iron emulsion oxidation
Desulfurization and sulfur recovery method.
Background technology
LO-CAT Complexing Iron desulfurization technology is the method for a kind of wet oxidation with ferrum as catalyst reduction removing sulfide,
Its feature be absorbent nontoxic, can a step by H2S is transformed into elementary sulfur, H2The removal efficiency of S is up to more than 99%.Complexing Iron desulfurization
Technology is applicable to H2S concentration is relatively low or H2S concentration is higher but occasion that gas flow is little.< during 20t/d, it is somebody's turn to do in elemental sulfur yield
Equipment investment and the operating cost of technique have clear superiority.Complexing Iron desulfurization generally uses alkali (Na2CO3Or K2CO3) water-soluble
Liquid absorbs sulfide, H2S gas and alkali react and generate HS-, become lower valency Fe ion by high-valence state Fe ion reduction, will
HS-Change into sulfur.In regenerative process, it is molten that Complexing Iron solution and the air contact of lower valency is oxidized to high-valence state Complexing Iron
Liquid, recovers oxidation susceptibility, solution cyclic absorption hydrogen sulfide gas.The reaction mechanism of complex iron oxidation sweetening is as follows: wherein g generation
Table gaseous state, l represents liquid；
H2S(g)→H2S (l) ；
H2S (l)+(OH-)→ (HS-)+H2O；
HS-+OH-→2S2-+H2O；
2Fe3++2S2-→2Fe2++S；
Net reaction is:
H2S+2Fe3+→2Fe2++S+2H+；
Regenerative response formula is:
O2(g)→O2(l)；
O2 (l)+4Fe2++2H2O→4Fe3++4OH-。
LO-CAT process route mainly has a two ways: (1) H2S absorbs the regeneration with catalyst respectively at two bubble towers
In carry out, doctor solution circulates between two towers；(2) H2S absorbs and catalyst regeneration is carried out in the zones of different of a bubble tower, as
Self-loopa LO-CAT flow process, absorbs and regenerates central authorities and annular space part at an interior circulation bubble tower respectively and carry out.But this
The drusen that two ways is required for generating reaction separates rapidly from desulfuration solution, otherwise will cause stifled tower and side reaction
Generation, affect device properly functioning.The particle diameter the least (hundreds of nanometer to several microns) of the drusen that reaction produces, has spy
Different surface nature, easily adsorbs, and not free settling.Prior art, by adding the methods such as dispersion, flocculant, improves sulfur
Settling ratio, make sulfur reactor bottom settle after, by sedimentation liquid discharge, be then peeled off sulfur, due to the sulfur in sedimentation liquid
Sulphur content is low, makes tank solution circulate between filter element and reactor, adds the loss of energy consumption and desulfurizing agent, and separate
Effect is the most undesirable.
CN1554467A discloses a kind of method of removing sulfide from CO 2 enriched gas by complex iron.The method is adopted
With Complexing Iron desulfurizing agent and efficient spray tower and fluid bed group technology, improve gas-liquid mass transfer efficiency, solve sulfur
Stifled tower problem, improves degree of purification.But the sulfide removing that the method is only applicable under lower pressure, complexation in regenerative process
Ferrum doctor solution separates not thorough with drusen, and following cycle process can be produced impact.
CN101870884A discloses a kind of Complexing Iron liquid phase oxidation and absorbs hydrogen sulfide gas and the method for sulphur recovery.Should
Method includes a kind of regeneration knockout tower being made up of blistering reaction section, gas-liquid separation section and foam collection section, in blistering reaction section,
Catalyst oxidation regeneration, drusen is enriched with at bubble interface, at gas-liquid separation section, regenerative sulfur binding solution and foam separation, takes off
Sulfur solution returns to absorption tower and recycles, and sulfur to foam collection section, is improve drusen separation rate and again by foamover
Raw reaction rate is high.But the method the most thoroughly solves stifled tower always and foaming problems.
Summary of the invention
For the deficiencies in the prior art, the present invention provides a kind of emulsion oxidation sweetening and sulfur recovery method, and the method has
Have that infiltration rate is fast, desulfuration efficiency is high and the feature such as simple to operate.
Emulsion oxidation sweetening of the present invention and sulfur recovery method, including following content: H 2 S-containing gas enters absorber
With oil-Complexing Iron emulsion contacts, hydrogen sulfide reaction generates sulfur, and sulfur is dissolved in oil phase, purifies gas and arranges from absorber overhead
Go out；Sulfureted oil-Complexing Iron emulsion carries out breakdown of emulsion process, then oil-water separation, and Recovered sulphur from oil phase.
In the inventive method, described oil-Complexing Iron emulsion is water-in-oil type (W/O), and the Sulfur capacity of oil-Complexing Iron emulsion is
3% ~ 9%(g/g).
In the inventive method, in the water-in-oil emulsion of oil-Complexing Iron emulsion, its oil phase is catalytic cracking diesel oil, aqueous phase
For Complexing Iron solution, wherein Complexing Iron solution is 1:10 ~ 2:3 with the mass ratio of catalytic cracking diesel oil.
In the inventive method, the boiling range scope of catalytic cracking diesel oil is any fraction in being 180 ~ 380 DEG C, and preferably 240 ~ 330
Any fraction in DEG C.
In the inventive method, in described catalytic cracking diesel oil, two ring aromatic content is 30wt% ~ 80wt%.
In the inventive method, in Complexing Iron solution, iron concentration is 0.05 ~ 0.1mol/L, and pH value is 8 ~ 10.
In the inventive method, the aqueous phase of Complexing Iron contains alkaline matter well known to those skilled in the art simultaneously, stablizes
The additive such as agent and corrosion inhibiter.
In the inventive method, the preparation method of oil-Complexing Iron emulsion is as follows: the emulsifying agent added at catalytic cracking diesel oil, mixed
Close uniformly, be subsequently adding Complexing Iron aqueous solution, carry out emulsion reaction, prepare water-in-oil type oil-Complexing Iron emulsion.
Wherein, emulsifying agent used be Span class, Tween class, fatty alcohol-polyoxyethylene ether, alkylphenol polyoxyethylene or
One or more in dodecyl benzene sulfonate, preferably Span60, Span80, Tween80, OP-10, MOA-3 or dodecane
One or more in base benzene sulfonic acid sodium salt compound, and on the basis of oil-Complexing Iron quality of the emulsion, the addition of emulsifying agent is 0.5% ~
4%；It is preferably added to the matter of the auxiliary agents such as oleic acid, methanol, ethanol, glycerol, ethylene glycol, n-butyl alcohol or ethanolamine, auxiliary agent and emulsifying agent
Amount ratio is 1:10 ~ 1:1.
Wherein, emulsifying temperature is 25 ~ 50 DEG C, and emulsification times is 15 ~ 60 minutes, and emulsion reaction is carried out under agitation,
Mixing speed is 100～600r/min.
In the inventive method, H 2 S-containing gas is various sulfide hydrogen waste gas, refinery gas, natural gas, Selexol tail gas
One or mixed gas with Claus tail gases etc..H in H 2 S-containing gas2The percent by volume of S is 0.01% ~ 20%.
In the inventive method, the volume ratio of H 2 S-containing gas volume flow per hour and oil-Complexing Iron emulsion be 1:3 ~
8:1.
In the inventive method, absorber interior reaction temperature is 35 ~ 80 DEG C, and reaction pressure is 0.1 ~ 2MPa.
In the inventive method, absorber can use this area conventional structure, as plate column, packed tower, bubble absorbing tower,
Spray column and rotary packed bed etc..
In the inventive method, described breakdown of emulsion process can be excellent to use transformation temperature, to be centrifuged, filter or the mode such as stirring
Select centrifugation.
In the inventive method, described oil water separation process is the method such as standing separation or cyclonic separation, is divided into profit two
Phase, the most sulfureted oil phase and the aqueous phase containing Complexing Iron.
In the inventive method, sulfureted oil phase enters cooling in solid-liquid separator and makes sulfur separate out and separate, and returns
Receiving sulfur, oil phase recycles as preparing oil-Complexing Iron emulsion materials with the aqueous phase containing Complexing Iron through regeneration.
In the inventive method, described solid-liquid separator is cooled down by outside condensed water or other coolants.Contain
The oil phase of sulfur refrigerated separation temperature in solid-liquid separator is generally 0 ~ 30 DEG C, preferably 10 ~ 25 DEG C.
In the inventive method, the regeneration of the aqueous phase containing Complexing Iron can use this area conventional method to carry out ex-situ regeneration,
Such as air oxidation process, electrolysis and bioanalysis etc..
In the inventive method, absorber a preparation and a use, when oil-Complexing Iron emulsion reaches saturated Sulfur capacity, carry out breakdown of emulsion, oil
Water separates, and simultaneity factor automatically switches to another absorber and continues reaction, it would however also be possible to employ accomplished continuously or intermittently discharge part oil-network
The mode closing ferrum emulsion maintains absorber to operate continuously.
The inventive method compared with prior art has the advantage that
(1) the inventive method uses the oil-Complexing Iron emulsion of water-in-oil type (W/O), and H 2 S-containing gas enters reactor
First contact with oil phase, to the harmful substance removal such as naphthalene, anthracene, quinone, benzene class, acids and thiophene present in gas, decrease pair
The generation of reaction, the beneficially holding of Complexing Iron Solution Active；
(2) in oil-Complexing Iron emulsion, it is dispersed in the middle of oil phase containing Complexing Iron aqueous phase with the form of droplet, sulfuration
Contacting between hydrogen with drop is more abundant, improves reaction efficiency；
(3) in oil-Complexing Iron emulsion, oil phase is preferably catalytic cracking diesel oil, and catalytic cracking diesel oil contains a certain amount of double
PAH so that catalytic cracking diesel oil has the strongest solvability to sulfur, the sulfur of generation is directly dissolved in oil phase, breaks
Chemical equilibrium, has further speeded up the speed of reaction, has avoided the stifled tower phenomenon of drusen simultaneously；
(4) oil-Complexing Iron emulsion has higher Sulfur capacity, catalytic cracking diesel oil wide material sources, the oil phase after separation and aqueous phase
Can recycle, there is not secondary pollution, reclaim elemental sulfur purity and reach more than 98%.
Accompanying drawing explanation
Fig. 1 is the emulsion oxidation sweetening that uses of the present invention and the flow chart of sulphur recovery.
Wherein, 1 contains H2S gas；2 absorbers；3 purify gas；4 breaking devices；5 regeneratoies；6 solid-liquid separators.
Detailed description of the invention
The present invention is further described with embodiment below in conjunction with the accompanying drawings, but is not so limited the present invention.The present invention is made
Catalytic cracking diesel oil each boiling range character be shown in Table 1.
The present invention is realized by such mode:
Containing H2S gas 1 enters absorber 2 and oil-Complexing Iron emulsion contacts, H2S is complexed ferrum and is oxidized to sulfur, and sulfur is molten
In solution oil phase around, deviate from H2The purification gas 3 of S is discharged from absorber 2 top, after oil-Complexing Iron emulsion absorption is saturated,
Oil-Complexing Iron emulsion carries out breakdown of emulsion, after breakdown of emulsion, profit standing separation in breaking device 4, and upper strata is sulfureted oil phase,
Lower floor is the aqueous phase containing Complexing Iron, and sulfureted oil phase enters solid-liquid separator 5, refrigerated separation, reclaims sulfur in withdrawer 6
Sulphur, the aqueous phase containing Complexing Iron enters regenerator 7 and regenerates, newborn as preparing oil-Complexing Iron with the oil phase after separating sulfur
The feedstock circulation of liquid uses.
Race's composition of table 1 catalytic cracking diesel oil difference boiling range.
| Ingredient names | 240 ~ 260 DEG C, wt% | 260 ~ 280 DEG C, wt% | 300 ~ 330 DEG C, wt% |
| Total cycloalkane | 7.5 | 6 | 8.8 |
| Total saturated hydrocarbons | 24.5 | 19.9 | 20.3 |
| Total mononuclear aromatics | 35.6 | 23.6 | 6.3 |
| Total double ring arene | 39.8 | 56.1 | 69.5 |
| Total aromatic hydrocarbons | 75.5 | 80.1 | 79.7 |
Embodiment 1
(1) preparation of water-in-oil type oil-Complexing Iron emulsion: on the basis of oil-Complexing Iron quality of the emulsion, add in the reactor
Entering the catalytic cracking diesel oil of 82.2wt%, add the emulsifying agent of 2wt%, wherein emulsifier is the compounding breast of Span80 and OP-10
Agent (mass ratio is 3:1), 30 DEG C of constant temperature 5 minutes, then stir, mixing speed is 300～500r/min, is simultaneously added dropwise
The n-butyl alcohol auxiliary agent of 0.8wt% and the Complexing Iron aqueous solution of 15wt%, 30 DEG C of constant temperature stir 30 minutes, prepare water-in-oil type oil-network
Close ferrum emulsion.
(2) removing H2Reaction condition during S is as follows: in absorber: temperature is 50 DEG C, and reaction pressure is 0.6MPa, containing H2S
Gas flow per hour is 6:1 with the volume ratio of oil-Complexing Iron emulsion；In solid-liquid separator: the temperature of refrigerated separation sulfur is
10℃.H 2 S-containing gas composition (volume): hydrogen sulfide content is 0.62%, SO2Being 0.01%, COS is 0.01%；Oil-Complexing Iron
Emulsion includes: boiling range is the catalytic diesel oil of 240 ~ 260 DEG C, and Fe ion concentration is 0.06mol/L.Through oil-Complexing Iron emulsion oxygen
Change desulfurization, purify H in gas2S concentration is 8mg/m3, Recovered sulphur purity is 98.9%, every oil-water separation in 1 hour, absorbs simultaneously
Device handover operation.
Embodiment 2
(1) with embodiment 1.
(2) removing H2Reaction condition during S is as follows: in absorber: temperature is 60 DEG C, and reaction pressure is 0.3MPa, containing H2S
Gas flow per hour is 3:1 with the volume ratio of oil-Complexing Iron emulsion；In solid-liquid separator: the temperature of refrigerated separation sulfur is 5
℃.H 2 S-containing gas composition (volume): hydrogen sulfide content is 0.18%, SO2Being 0.1%, COS is 0.03%；Oil-Complexing Iron breast
Liquid includes: boiling range is the catalytic diesel oil of 260 ~ 280 DEG C, and Fe ion concentration is 0.08 mol/L.Through doctor solution oxidation sweetening, only
H in activating QI2S concentration is 9mg/m3, Recovered sulphur purity was 99%, every 4 hours oil-water separation, simultaneously absorber handover operations.
Embodiment 3
(1) preparation of water-in-oil type oil-Complexing Iron emulsion: on the basis of oil-Complexing Iron quality of the emulsion, add in the reactor
Enter the catalytic cracking diesel oil of 74.5wt%, add the emulsifying agent of 3.5wt%, wherein emulsifier be Tween80, Span60 and
MOA-3 composite emulsifier (mass ratio is 2:1:1), 30 DEG C of constant temperature 5 minutes, then stir, mixing speed is 300～500r/
Min, is simultaneously added dropwise the glycerol auxiliary agent of 2wt% and the Complexing Iron aqueous solution of 20wt%, and 40 DEG C of constant temperature stir 25 minutes, prepare oil bag
Water type oil-Complexing Iron emulsion.
(2) removing H2Reaction condition during S is as follows: in absorber: temperature is 80 DEG C, and reaction pressure is 0.1MPa, containing H2S
Gas flow per hour is 1:2 with the volume ratio of oil-Complexing Iron emulsion；In solid-liquid separator: the temperature of refrigerated separation sulfur is
15℃.H 2 S-containing gas composition (volume): hydrogen sulfide content is 1.05%, SO2Being 0.36%, COS is 0.27%.Oil-Complexing Iron
Emulsion composition includes: boiling range is the catalytic diesel oil of 300 ~ 330 DEG C, and Fe ion concentration is 0.1 mol/L.De-through doctor solution oxidation
Sulfur, purifies H in gas2S concentration is 12mg/m3, Recovered sulphur purity is 98%, and every oil-water separation in 12 hours, absorber was cut simultaneously
Change operation.
Embodiment 4
(1) with embodiment 3.
(2) removing H2Reaction condition during S is as follows: in absorber: temperature is 50 DEG C, and reaction pressure is 0.1MPa, containing H2S
Gas flow per hour is 1:4 with the volume ratio of oil-Complexing Iron emulsion；In solid-liquid separator: the temperature of refrigerated separation sulfur is
15℃.H 2 S-containing gas composition (volume): hydrogen sulfide content is 8.4%, CO2Being 1.2%, CO is 0.3%；Oil-Complexing Iron emulsion
Composition includes: boiling range is the catalytic diesel oil of 260 ~ 280 DEG C, and Fe ion concentration is 0.1 mol/L.Through oil-Complexing Iron emulsion oxygen
Change desulfurization, purify H in gas2S concentration is 6mg/m3, Recovered sulphur purity is 98.9%, every oil-water separation in 2 hours, absorbs simultaneously
Device handover operation.
Claims (11)
1. an emulsion oxidation sweetening and sulfur recovery method, it is characterised in that include following content: H 2 S-containing gas enters
Absorber and oil-Complexing Iron emulsion contacts, hydrogen sulfide reaction generates sulfur, and sulfur is dissolved in oil phase, purifies gas from absorber
Top is discharged；Sulfureted oil-Complexing Iron emulsion carries out breakdown of emulsion process, then oil-water separation, and Recovered sulphur from oil phase；Institute
It is 3% ~ 9% that the Sulfur capacity of the oil stated-Complexing Iron emulsion is calculated in mass percent；Wherein oil-Complexing Iron emulsion is water-in-oil emulsion；
In the water-in-oil emulsion of described oil-Complexing Iron emulsion, its oil phase is catalytic cracking diesel oil, and aqueous phase is Complexing Iron solution, its
Middle complexation ferrous solution is 1:10 ~ 2:3 with the mass ratio of catalytic cracking diesel oil；The boiling range scope of catalytic cracking diesel oil is 180 ~ 380
Any fraction in DEG C；In catalytic cracking diesel oil, two ring aromatic content is 30wt% ~ 80wt%.
The most in accordance with the method for claim 1, it is characterised in that: in Complexing Iron solution, iron concentration is 0.05 ~ 0.1mol/
L, pH value is 8 ~ 10.
The most in accordance with the method for claim 1, it is characterised in that: the preparation method of oil-Complexing Iron emulsion is as follows: split in catalysis
Change diesel oil and add emulsifying agent, mix homogeneously, be subsequently adding Complexing Iron aqueous solution, carry out emulsion reaction, prepare water-in-oil type oil-network
Close ferrum emulsion.
The most in accordance with the method for claim 3, it is characterised in that: emulsifying agent used is Span class, Tween class, fatty alcohol
One or more in polyoxyethylene ether, alkylphenol polyoxyethylene or dodecyl benzene sulfonate；With oil-Complexing Iron emulsion matter
On the basis of amount, the addition of emulsifying agent is 0.5% ~ 4%.
The most in accordance with the method for claim 3, it is characterised in that: in emulsion process add oleic acid, methanol, ethanol, glycerol,
One or more auxiliary agents in ethylene glycol, n-butyl alcohol or ethanolamine, auxiliary agent is 1:10 ~ 1:1 with the mass ratio of emulsifying agent.
The most in accordance with the method for claim 3, it is characterised in that: emulsifying temperature is 25 ~ 50 DEG C, and emulsification times is 15 ~ 60 points
Clock, emulsion reaction is carried out under agitation, and mixing speed is 100～600r/min.
The most in accordance with the method for claim 1, it is characterised in that: H 2 S-containing gas is refinery gas, natural gas, Selexol
Tail gas and the one of Claus tail gases or mixed gas；H in H 2 S-containing gas2The percent by volume of S is 0.01% ~ 20%.
The most in accordance with the method for claim 1, it is characterised in that: H 2 S-containing gas volume flow per hour and oil-complexation
The volume ratio of ferrum emulsion is 1:3 ~ 8:1.
The most in accordance with the method for claim 1, it is characterised in that: absorber interior reaction temperature is 35 ~ 80 DEG C, and reaction pressure is
0.1~2MPa。
The most in accordance with the method for claim 1, it is characterised in that: described oil water separation process is standing separation or eddy flow
Separation method, is divided into water-oil phase, the most sulfureted oil phase and the aqueous phase containing Complexing Iron.
11. in accordance with the method for claim 1, it is characterised in that: absorber a preparation and a use, when oil-Complexing Iron emulsion reaches
During saturated Sulfur capacity, carrying out breakdown of emulsion, oil-water separation, simultaneity factor automatically switches to another absorber and continues reaction；Or use continuously
Or the mode of interval discharge part oil-Complexing Iron emulsion maintains absorber to operate continuously.
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| CN107814360A (en) * | 2016-09-14 | 2018-03-20 | 中国石油化工股份有限公司 | A kind of device and method that sulphur is separated from desulfuration solution |
| CN110841614B (en) * | 2019-10-08 | 2022-11-11 | 北京海新能源科技股份有限公司 | Sulfur suspension separating agent and preparation method and application thereof |
| CN113880056A (en) * | 2021-10-29 | 2022-01-04 | 雅邦绿色过程与新材料研究院南京有限公司 | Method for preparing hydrophilic sulfur microspheres by using chemical sulfur |
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| US4414194A (en) * | 1981-05-26 | 1983-11-08 | Shell Oil Company | Extraction process |
| CN102451612A (en) * | 2010-10-22 | 2012-05-16 | 中国石油化工集团公司 | Method for removing hydrogen sulfide in gas by non-aqueous solvent |
| CN103041679A (en) * | 2013-01-15 | 2013-04-17 | 美景（北京）环保科技有限公司 | Waste gas treatment system of acid gas containing ammonia |
| CN103111177A (en) * | 2013-02-26 | 2013-05-22 | 余国贤 | Method and device for removing hydrogen sulfide in gas phase through oxidation |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| WO2012164467A1 (en) * | 2011-05-27 | 2012-12-06 | Frames Biogas Processing B.V. | Method for regenerating absorption liquid |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4414194A (en) * | 1981-05-26 | 1983-11-08 | Shell Oil Company | Extraction process |
| CN102451612A (en) * | 2010-10-22 | 2012-05-16 | 中国石油化工集团公司 | Method for removing hydrogen sulfide in gas by non-aqueous solvent |
| CN103041679A (en) * | 2013-01-15 | 2013-04-17 | 美景（北京）环保科技有限公司 | Waste gas treatment system of acid gas containing ammonia |
| CN103111177A (en) * | 2013-02-26 | 2013-05-22 | 余国贤 | Method and device for removing hydrogen sulfide in gas phase through oxidation |
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