CN105084319B - A kind of release agent that sulphur is separated from sulfur system is contained and the method for separating sulphur - Google Patents
A kind of release agent that sulphur is separated from sulfur system is contained and the method for separating sulphur Download PDFInfo
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- CN105084319B CN105084319B CN201410178019.5A CN201410178019A CN105084319B CN 105084319 B CN105084319 B CN 105084319B CN 201410178019 A CN201410178019 A CN 201410178019A CN 105084319 B CN105084319 B CN 105084319B
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- Prior art keywords
- sulphur
- release agent
- ionic liquid
- iron
- sulfur system
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- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 title claims abstract description 219
- 239000005864 Sulphur Substances 0.000 title claims abstract description 160
- 239000011593 sulfur Substances 0.000 title claims abstract description 59
- 229910052717 sulfur Inorganic materials 0.000 title claims abstract description 59
- 238000000034 method Methods 0.000 title claims abstract description 37
- 239000003795 chemical substances by application Substances 0.000 title claims description 78
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims abstract description 113
- 239000002608 ionic liquid Substances 0.000 claims abstract description 70
- 229910052742 iron Inorganic materials 0.000 claims abstract description 56
- 239000004094 surface-active agent Substances 0.000 claims abstract description 31
- 239000002904 solvent Substances 0.000 claims abstract description 25
- 239000000203 mixture Substances 0.000 claims abstract description 11
- 150000001875 compounds Chemical class 0.000 claims description 20
- 229910021578 Iron(III) chloride Inorganic materials 0.000 claims description 10
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 claims description 6
- 125000000217 alkyl group Chemical group 0.000 claims description 3
- 239000002245 particle Substances 0.000 abstract description 51
- 239000000126 substance Substances 0.000 abstract description 40
- 238000005516 engineering process Methods 0.000 abstract description 2
- 230000000903 blocking effect Effects 0.000 abstract 1
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 description 43
- 238000006477 desulfuration reaction Methods 0.000 description 23
- 230000023556 desulfurization Effects 0.000 description 22
- 238000001953 recrystallisation Methods 0.000 description 22
- 238000009826 distribution Methods 0.000 description 17
- 239000000243 solution Substances 0.000 description 17
- 238000000926 separation method Methods 0.000 description 16
- 238000001556 precipitation Methods 0.000 description 14
- 239000007788 liquid Substances 0.000 description 11
- 239000013078 crystal Substances 0.000 description 9
- 239000000047 product Substances 0.000 description 9
- 230000000052 comparative effect Effects 0.000 description 8
- 238000002425 crystallisation Methods 0.000 description 8
- 230000008025 crystallization Effects 0.000 description 8
- 239000007789 gas Substances 0.000 description 8
- 230000003009 desulfurizing effect Effects 0.000 description 7
- 230000000694 effects Effects 0.000 description 7
- FBAFATDZDUQKNH-UHFFFAOYSA-M iron chloride Chemical compound [Cl-].[Fe] FBAFATDZDUQKNH-UHFFFAOYSA-M 0.000 description 7
- 238000004062 sedimentation Methods 0.000 description 7
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 description 6
- 238000001914 filtration Methods 0.000 description 6
- 230000001965 increasing effect Effects 0.000 description 6
- -1 result in blockage Substances 0.000 description 6
- 239000012047 saturated solution Substances 0.000 description 6
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 description 5
- 238000005119 centrifugation Methods 0.000 description 5
- 230000008859 change Effects 0.000 description 5
- 238000006243 chemical reaction Methods 0.000 description 5
- 239000002798 polar solvent Substances 0.000 description 5
- 238000011084 recovery Methods 0.000 description 5
- 229910052938 sodium sulfate Inorganic materials 0.000 description 5
- 235000011152 sodium sulphate Nutrition 0.000 description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 5
- 230000009102 absorption Effects 0.000 description 4
- 238000010521 absorption reaction Methods 0.000 description 4
- 230000015572 biosynthetic process Effects 0.000 description 4
- QGBSISYHAICWAH-UHFFFAOYSA-N dicyandiamide Chemical compound NC(N)=NC#N QGBSISYHAICWAH-UHFFFAOYSA-N 0.000 description 4
- RAXXELZNTBOGNW-UHFFFAOYSA-N imidazole Natural products C1=CNC=N1 RAXXELZNTBOGNW-UHFFFAOYSA-N 0.000 description 4
- 230000003647 oxidation Effects 0.000 description 4
- 238000007254 oxidation reaction Methods 0.000 description 4
- 238000002360 preparation method Methods 0.000 description 4
- 230000008569 process Effects 0.000 description 4
- 238000004458 analytical method Methods 0.000 description 3
- 125000002091 cationic group Chemical group 0.000 description 3
- 238000001035 drying Methods 0.000 description 3
- 230000007613 environmental effect Effects 0.000 description 3
- 150000002500 ions Chemical class 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 238000012546 transfer Methods 0.000 description 3
- FHDQNOXQSTVAIC-UHFFFAOYSA-M 1-butyl-3-methylimidazol-3-ium;chloride Chemical compound [Cl-].CCCCN1C=C[N+](C)=C1 FHDQNOXQSTVAIC-UHFFFAOYSA-M 0.000 description 2
- VFWCMGCRMGJXDK-UHFFFAOYSA-N 1-chlorobutane Chemical compound CCCCCl VFWCMGCRMGJXDK-UHFFFAOYSA-N 0.000 description 2
- VVJKKWFAADXIJK-UHFFFAOYSA-N Allylamine Chemical compound NCC=C VVJKKWFAADXIJK-UHFFFAOYSA-N 0.000 description 2
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 2
- RWSOTUBLDIXVET-UHFFFAOYSA-N Dihydrogen sulfide Chemical compound S RWSOTUBLDIXVET-UHFFFAOYSA-N 0.000 description 2
- QYKIQEUNHZKYBP-UHFFFAOYSA-N Vinyl ether Chemical compound C=COC=C QYKIQEUNHZKYBP-UHFFFAOYSA-N 0.000 description 2
- XAQHXGSHRMHVMU-UHFFFAOYSA-N [S].[S] Chemical compound [S].[S] XAQHXGSHRMHVMU-UHFFFAOYSA-N 0.000 description 2
- 239000000010 aprotic solvent Substances 0.000 description 2
- 238000005660 chlorination reaction Methods 0.000 description 2
- 238000001816 cooling Methods 0.000 description 2
- 238000004090 dissolution Methods 0.000 description 2
- 239000000945 filler Substances 0.000 description 2
- 239000012467 final product Substances 0.000 description 2
- 229910000037 hydrogen sulfide Inorganic materials 0.000 description 2
- 239000002563 ionic surfactant Substances 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 238000010899 nucleation Methods 0.000 description 2
- 230000006911 nucleation Effects 0.000 description 2
- 230000001590 oxidative effect Effects 0.000 description 2
- 230000009467 reduction Effects 0.000 description 2
- 230000006641 stabilisation Effects 0.000 description 2
- 238000011105 stabilization Methods 0.000 description 2
- 239000002699 waste material Substances 0.000 description 2
- MCTWTZJPVLRJOU-UHFFFAOYSA-N 1-methyl-1H-imidazole Chemical class CN1C=CN=C1 MCTWTZJPVLRJOU-UHFFFAOYSA-N 0.000 description 1
- LXBGSDVWAMZHDD-UHFFFAOYSA-N 2-methyl-1h-imidazole Chemical compound CC1=NC=CN1 LXBGSDVWAMZHDD-UHFFFAOYSA-N 0.000 description 1
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- 241001272567 Hominoidea Species 0.000 description 1
- RCEAADKTGXTDOA-UHFFFAOYSA-N OS(O)(=O)=O.CCCCCCCCCCCC[Na] Chemical compound OS(O)(=O)=O.CCCCCCCCCCCC[Na] RCEAADKTGXTDOA-UHFFFAOYSA-N 0.000 description 1
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 description 1
- 229920003171 Poly (ethylene oxide) Polymers 0.000 description 1
- NWGKJDSIEKMTRX-AAZCQSIUSA-N Sorbitan monooleate Chemical compound CCCCCCCC\C=C/CCCCCCCC(=O)OC[C@@H](O)[C@H]1OC[C@H](O)[C@H]1O NWGKJDSIEKMTRX-AAZCQSIUSA-N 0.000 description 1
- IYFATESGLOUGBX-YVNJGZBMSA-N Sorbitan monopalmitate Chemical compound CCCCCCCCCCCCCCCC(=O)OC[C@@H](O)[C@H]1OC[C@H](O)[C@H]1O IYFATESGLOUGBX-YVNJGZBMSA-N 0.000 description 1
- HVUMOYIDDBPOLL-XWVZOOPGSA-N Sorbitan monostearate Chemical compound CCCCCCCCCCCCCCCCCC(=O)OC[C@@H](O)[C@H]1OC[C@H](O)[C@H]1O HVUMOYIDDBPOLL-XWVZOOPGSA-N 0.000 description 1
- 229930006000 Sucrose Natural products 0.000 description 1
- 230000003213 activating effect Effects 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 150000001450 anions Chemical class 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 125000000484 butyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 239000003093 cationic surfactant Substances 0.000 description 1
- 150000001768 cations Chemical class 0.000 description 1
- 238000002144 chemical decomposition reaction Methods 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000000460 chlorine Substances 0.000 description 1
- 229910052801 chlorine Inorganic materials 0.000 description 1
- 238000005345 coagulation Methods 0.000 description 1
- 230000015271 coagulation Effects 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 239000008367 deionised water Substances 0.000 description 1
- 229910021641 deionized water Inorganic materials 0.000 description 1
- 230000006866 deterioration Effects 0.000 description 1
- ZBCBWPMODOFKDW-UHFFFAOYSA-N diethanolamine Chemical compound OCCNCCO ZBCBWPMODOFKDW-UHFFFAOYSA-N 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 230000003292 diminished effect Effects 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 150000002148 esters Chemical class 0.000 description 1
- 150000002191 fatty alcohols Chemical class 0.000 description 1
- 229940044631 ferric chloride hexahydrate Drugs 0.000 description 1
- 229930182478 glucoside Natural products 0.000 description 1
- 125000005456 glyceride group Chemical group 0.000 description 1
- 230000036571 hydration Effects 0.000 description 1
- 238000006703 hydration reaction Methods 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 150000002460 imidazoles Chemical class 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- NQXWGWZJXJUMQB-UHFFFAOYSA-K iron trichloride hexahydrate Chemical compound O.O.O.O.O.O.[Cl-].Cl[Fe+]Cl NQXWGWZJXJUMQB-UHFFFAOYSA-K 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 1
- XLSZMDLNRCVEIJ-UHFFFAOYSA-N methylimidazole Natural products CC1=CNC=N1 XLSZMDLNRCVEIJ-UHFFFAOYSA-N 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 239000002736 nonionic surfactant Substances 0.000 description 1
- 239000007800 oxidant agent Substances 0.000 description 1
- 230000033116 oxidation-reduction process Effects 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 229940051841 polyoxyethylene ether Drugs 0.000 description 1
- 229920000056 polyoxyethylene ether Polymers 0.000 description 1
- 229920002503 polyoxyethylene-polyoxypropylene Polymers 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 230000006798 recombination Effects 0.000 description 1
- 238000005215 recombination Methods 0.000 description 1
- 230000008929 regeneration Effects 0.000 description 1
- 238000011069 regeneration method Methods 0.000 description 1
- 230000000284 resting effect Effects 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
- 238000002390 rotary evaporation Methods 0.000 description 1
- 229920006395 saturated elastomer Polymers 0.000 description 1
- 238000004904 shortening Methods 0.000 description 1
- 241000894007 species Species 0.000 description 1
- 230000002269 spontaneous effect Effects 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 239000005720 sucrose Substances 0.000 description 1
- 150000005846 sugar alcohols Chemical class 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 238000010792 warming Methods 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
- 238000009279 wet oxidation reaction Methods 0.000 description 1
Classifications
-
- 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
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/50—Improvements relating to the production of bulk chemicals
- Y02P20/54—Improvements relating to the production of bulk chemicals using solvents, e.g. supercritical solvents or ionic liquids
Landscapes
- Production Of Liquid Hydrocarbon Mixture For Refining Petroleum (AREA)
Abstract
The invention discloses a kind of from the method containing sulphur is separated in sulfur system, the method uses the composition comprising iron-based ionic liquid, solvent and surfactant, promote to reunite containing the sulphur simple substance generated in sulfur system, so that can fast-growth be at a lower temperature the larger drusen of particle diameter containing the little particle sulphur generated in sulfur system, so that the sulphur product produced in sulfur removal technology is easy to settle and reclaims, avoid its fouling or blocking pipeline on the reactor wall, resource reutilization is realized simultaneously, increases economic benefit.
Description
Technical field
It is more particularly to a kind of from the method containing sulphur is separated in sulfur system the present invention relates to Chemical Decomposition field.
Background technology
At present, the technique for being removed to sulfur-containing compound mainly has two kinds of dry desulfurization and wet desulphurization, wherein with wet
Method desulfurization is most widely used.
In the prior art, in order to remove sulfur-containing compound, there is the method for using nonaqueous phase ionic liquid as desulfurizing agent,
Sulfur-containing compound can be converted into sulphur simple substance by it, then accessory substance sulphur can be obtained by separating.Such as Chinese patent
A kind of sulfur method of high temperature wet oxidation hydrogen sulfide is disclosed in CN102559292A, needed after desulfurization by centrifugation or
The method of sedimentation is reclaimed to product sulphur, wherein, centrifugally operated is complicated, it is necessary to professional equipment, and sedimentation method need it is big
The amount time, sulphur is easily adsorbed on precipitation apparatus wall in infall process, additionally, desulfurization temperature needed for the method 70~
In the range of 240 DEG C, temperature is high, and consumed energy is big.And for example Chinese patent CN102020248B, discloses a kind of nonaqueous phase wet method oxygen
The method for changing hydrogen sulfide, the particle diameter of the desulfurization product sulphur simple substance of the method is small, needs also exist for being separated using the method for centrifugation
Sulphur simple substance.
In a word, prior art uses merely ionic liquid as desulfurizing agent, and the sulphur simple substance particle of generation is tiny, is difficult to sink
Drop, separate when be readily adsorbed on reactor wall or filler, result in blockage, and sulphur waste.
It would therefore be highly desirable to develop a kind of easy to operate, sulphur simple substance is difficult absorption on reactor wall or filler, it is easy to reclaim
The method of sulphur.
The content of the invention
In order to solve the above problems, present inventor has performed studying with keen determination, as a result find：By in iron-based ionic liquid
Addition solvent and surfactant, the composition for being formed can promote the sulphur simple substance that sulfur-containing compound is generated to reunite,
So as to increase the particle diameter of sulphur simple substance so that it is easy to sedimentation, and reactor plugs are not easily caused during separation, returning for sulphur is improve
Yield, will/contain sulfur system to being added in said composition, or to containing being separately added into each component in composition in sulfur system, you can it is real
The growth of existing drusen, so as to complete the present invention.
Therefore, an object of the present invention is to provide a kind of from containing the release agent that sulphur is separated in sulfur system, and its feature exists
In composition of the release agent comprising volumes below part：
100 parts of iron-based ionic liquid,
5~60 parts of solvent,
0.5~3 part of surfactant.
Another object of the present invention is to provide a kind of from the method containing sulphur is separated in sulfur system, and the method includes following step
Suddenly：
(1-1) prepares above-mentioned release agent；
(1-2) by/to adding containing sulfur system the release agent prepared in step 1-1；
(1-3) separates sulphur after standing.
Or, the method is comprised the following steps：
(2-1) is according to above-mentioned release agent to containing each component that release agent is separately added into sulfur system；
Stood after (2-2) is well mixed, separate sulphur.
According to present invention offer from the release agent and separation method that sulphur is separated containing sulfur system, have the advantages that：
First, the release agent preparation method is simple, it is not necessary to complex operations, and agents useful for same environmental protection does not cause environment
Pollution；
Second, the release agent agents useful for same volatility is small, and operating condition is gentle；
3rd, using the release agent after, rapid containing drusen growth in sulfur system, particle diameter is big, it is easy to sedimentation separation, sulphur
The sulphur rate of recovery is high；
4th, the release agent can effectively reduce the attachment containing the sulphur little particle generated in sulfur system on the reactor wall,
Reactor plugs are reduced to occur；
5th, the separation method is easy to operate, flexible, easy, can be specific to separate according to the physical condition of reactor
Process is adjusted, with very strong industrial applicibility.
Brief description of the drawings
Fig. 1 shows solubility curve of the sulphur in different DMI concentration systems；
Fig. 2 shows solubility curve of the sulphur in different DMF concentration systems；
Fig. 3 shows precipitation time graph of the sulphur at different temperatures in iron-based ionic liquid；
Fig. 4 shows the drusen grain size distribution obtained in embodiment 3；
Fig. 5 shows the drusen grain size distribution obtained in comparative example 1；
Fig. 6 a show the sulphur recrystallization grain size distribution in pure iron-based ionic liquid；
Fig. 6 b show the sulphur recrystallization grain size distribution in 5%DMI systems；
Fig. 6 c show the sulphur recrystallization grain size distribution in 10%DMI systems；
Fig. 6 d show the sulphur recrystallization grain size distribution in 33%DMI systems；
Fig. 6 e show the sulphur recrystallization grain size distribution in 10%DMF systems；
Fig. 6 f show the sulphur recrystallization grain size distribution in 33%DMF systems；
Fig. 7 shows solubility curve of the sulphur in variety classes surfactant system；
Fig. 8 a show the sulphur recrystallization grain size distribution under nonionic surface active agent TX-100 existence conditions；
Fig. 8 b show the sulphur recrystallization grain size distribution under cationic surface active agent SDS existence conditions；
Fig. 9 shows the time-consuming curve that sulphur is separated out in different solvents iron-based ionic liquid.
Specific embodiment
Below by the present invention is described in detail, the features and advantages of the invention will become more with these explanations
For clear, clear and definite.
According to the first aspect of the invention, there is provided a kind of from containing the release agent that sulphur is separated in sulfur system, it is characterised in that should
Composition of the release agent comprising volumes below part：
100 parts of iron-based ionic liquid,
5~60 parts of solvent,
0.5~3 part of surfactant.
The iron-based ionic liquid used in the release agent that the present invention is provided is a kind of ionic liquid and iron chloride or six hydrations
Iron chloride formed compound, the ionic liquid be glyoxaline ion liquid, its structural formula as shown in following formula I,
Wherein, R1And R2Base can be replaced for identical, or different substitution bases, wherein R1And/or R2It is alkyl,
Preferably C1~C12Alkyl, more preferably C1~C8Alkyl, such as methyl and butyl.The present invention is using abovementioned alkyl in imidazoles
Ionic liquid is modified on N- of class material, its hydrophobicity can be increased, so that it is mutual with surfactant to increase it
Dissolubility, makes stable homogeneous containing sulfur system, while crowding-out effect of the release agent to sulphur can be strengthened.
The ionic liquid used in release agent that the present invention is provided, is in a liquid state simultaneously at a temperature of room temperature or near room temperature
The material being all made up of cation and anion, it has larger polarity Modulatory character, and viscosity is low, and density is big, itself and chlorine
Change iron or ferric chloride hexahydrate it is compound after remain to keep the physical property constant, therefore, to being passed through gas in iron-based ionic liquid
Only needing the residual gas after smaller pressure, and removing sulfur-containing compound can form continuous during ionic liquid is discharged
The bubble of stabilization, so as to ensure that the production safety of sweetening process.
Additionally, iron-based ionic liquid is liquid at normal temperatures, corrosivity is weaker, and the deterioration effect to production equipment is small；
And iron-based ionic liquid has stronger Coulomb attraction almost without vapour pressure between its negative ions, therefore it is hardly waved
Hair, though at temperature and vacuum higher, the liquid of stabilization can be also kept, therefore, it will not be converted into steam and be diffused into
In air, using and storage in be lost it is small, hardly pollute environment, and can be recycled, meet green
The requirement of environmental protection.
Additionally, iron-based ionic liquid has liquid state range very wide, using iron-based ionic liquid as reaction dissolvent and catalysis
Agent, makes reaction condition easily controllable；Furthermore, ionic liquid stable chemical nature is not easily decomposed or burns, and is separating the process of sulphur
Employed in influence of the separation condition to iron-based ionic liquid property less, therefore iron-based ionic liquid be suitable as sulphur content from
Agent or the solvent of sulphur release agent.
Additionally, the present invention is by Fe3+It is dissolved in glyoxaline ion liquid by recombination reaction, forms iron-based ionic liquid, by
In Fe3+With strong oxidizing property, therefore, it can be used as oxidant in containing sulfur system, by sulfur-containing compound-divalent element sulphur
Sulphur simple substance is oxidized to, so as to improve the desulfurized effect containing sulfur system, increases the rate of recovery of sulphur.
In the present invention, iron chloride directly affects release agent to the close and distant characteristic of water and oxidation with the mol ratio of ionic liquid
Ability, when the mol ratio of iron chloride and ionic liquid is less than 0.5:When 1, release agent is dissolved in water, when iron chloride and ionic liquid
Mol ratio is not less than 0.5:When 1, release agent is water insoluble, and oxidation-reduction potential is high, shows strong oxidation characteristic, therefore,
Selective chlorination iron of the present invention is not less than 0.5 with the mol ratio of ionic liquid:1, and due to molten in ionic liquid by iron chloride
The restriction of Xie Du, selective chlorination iron of the present invention is not more than 3 with the mol ratio of ionic liquid:1, preferably 1:1~2.5:1, for example
2:1。
Solvent of the present invention selects non-protonic polar solvent, such as DMI (DMI), diformazan
Base allyl amine (DMAA) or N,N-dimethylformamide (DMF) etc..
Why the present invention selects non-protonic polar solvent to be combined with iron-based ionic liquid, because aprotic
Polar solvent can increase the polarity of desulfurizing agent, and desulfurization product sulphur simple substance belongs to apolar substance, therefore, the addition of solvent can
To reduce solubility of the desulfurization product sulphur simple substance in desulfurization system, make the sulphur of generation to greatest extent from desulfurization system
Separate out, improve the rate of recovery of sulphur simple substance, while promoting sulphur simple substance to form the particle of greater particle size.Therefore, present invention selection
Above-mentioned aprotic polar solvent, preferably DMI (DMI) and DMF (DMF), it is optimal
Elect 1,3- dimethyl-2-imidazolinones (DMI) as.
Additionally, the aprotic solvents of present invention selection can also reduce the viscosity and heat transfer coefficient of iron-based ionic liquid, make
Sulphur simple substance can be separated out quickly from desulfurization system, so as to improve crystalline growth velocity, shorten the precipitation time.
In release agent of the invention, when the volume ratio of solvent and iron-based ionic liquid is more than 60:When 100, in release agent
Ionic liquid content is too low, then maximum with the ratio of solvent in release agent, and the aprotic solvents of present invention selection have
Certain volatility, therefore, when ionic liquid ratio is too small, the limitation that separation condition may be caused to use release agent；And
When the volume ratio of solvent and iron-based ionic liquid is less than 5:When 100, solvent is too low in release agent, its rush separated out to sulphur
Enter to act on not significantly, particle diameter increase is not obvious (referring specifically to experimental example 1), therefore, the present invention selects solvent with ionic liquid
Volume ratio is (5~60):100, preferably (20~55):100, most preferably 50:100.
Because sulphur simple substance causes the change of solubility in containing sulfur system with the difference of the solvent species and consumption that add
Change (referring specifically to experimental example 2 and experimental example 3), as depicted in figs. 1 and 2, add 5%DMI to be carried for the solubility of sulphur simple substance
High more substantially and 10%, 33% DMI then substantially reduces solubility of the sulphur in system, based on above-mentioned experimental result, no
It is bound by any theory, inventors believe that a small amount of DMI can be combined with iron-based ionic liquid so as to promote the molten of sulphur simple substance
Solution, but DMI belongs to intensive polar solvent, it is little with the dissolving of nonpolar sulphur simple substance, therefore, increasing DMI consumptions can reduce sulphur list
Solubility of the matter in containing sulfur system, based on the reason for identical, as shown in Fig. 2 DMF is molten in containing sulfur system to sulphur simple substance
The influence of Xie Du is also first to increase to reduce afterwards.
Because in the industrial production, desulfurization system judges the desulfurization according to the measurement result of sulfur-containing compound content in tail gas
Whether system can continue to absorb sulfur-containing compound gas, i.e., judge the desulfurization when sulfur-containing compound content increases in tail gas
System reaches absorption saturation, and now sulphur simple substance may simultaneously be not up to saturation in desulfurization system, therefore, selection is at high temperature
The low amount of solvent of solubility can make sulphur simple substance that saturation state is rapidly achieved in containing sulfur system.
Surfactant is also included in release agent of the invention, the surfactant is that have fixed hydrophilic and oleophilic base
Group, can align on the surface of solution, and can make the material that surface tension is remarkably decreased, and surfactant is according to it in solution
In whether can ionize and be divided into ionic surfactant and nonionic surface active agent.
Inventors have surprisingly found that, by surfactant is added in release agent of the invention, especially nonionic
Type surfactant, can make the sulphur simple substance surface characteristic of generation change, and promote the reunion of sulphur simple substance, so as to promote sulphur
The increase of the particle diameter of sulphur simple substance.
Without being bound by any theory, inventors believe that ionic surfactant is changing sulphur simple substance surface characteristic
While can cause that the zeta potential on sulphur surface is raised, its possibility for being agglomerated into larger particles, Er Feili is reduced to a certain extent
Subtype surfactant, because it can not ionize out charged ion, the characteristic that it changes sulphur surface without changing zeta potential,
The facilitation reunited to sulphur simple substance is significantly (referring specifically to experimental example 4).
Therefore, the present invention adds nonionic surface active agent in release agent, such as AEO (AEO),
APES, aliphatic amine polyoxyethylene ether, alkylolamides polyethylene oxide, Block polyoxyethylene-polyoxypropylene
Ether, alkylolamides, alkyl poly glucoside, polyalcohol esters, sucrose ester, fatty glyceride series, Span series are told
Warm series etc., preferred fat alcohol APEO (3) (AEO-3), AEO (5) (AEO-5), fatty alcohol polyoxy
Vinethene (7) (AEO-7), AEO (9) (AEO-9), AEO (10) (AEO-10), TX-
10th, OP-10, O Π -10, ocytlphenol ethoxylate (TX-100), Arlacel-40, Arlacel-60 or Arlacel-80, more preferably pungent
Base phenol elhoxylate (TX-100).
When the volume ratio of surfactant and iron-based ionic liquid is more than 3:When 100, its promotion reunited to sulphur simple substance
Effect is not dramatically increased, and micella may be formed in separation process, causes the waste of surfactant；Work as surface-active
Agent is less than 0.5 with the volume ratio of iron-based ionic liquid:When 100, surface-active contents are too low in release agent, to sulphur simple substance
Agglomeration is not obvious (referring specifically to experimental example 5), therefore, the body with iron-based ionic liquid of present invention selection surfactant
Product is than being (0.5~3):100, preferably (0.8~2):100, most preferably 1:100.
The solvent and surfactant added in release agent have promotion to desulfurization product sulphur simple substance, and it is reunited, and forms sulphur
The effect of sulphur bulky grain, therefore, when sulphur is separated in containing sulfur system, with desulfuration efficiency higher, and enable the separation of sulphur
Carried out under conditions of more gently；Meanwhile, the addition of solvent and surfactant can make to be processed in iron-based ionic liquid
The Fe of " resting state "3+It is activated, it is de- that the sulfur-containing compound not being removed in making it to being dissolved in containing sulfur system carries out oxidation
Remove, so as to improve the desulphurizing ability of desulfurizing agent.
According to a second aspect of the present invention, there is provided a kind of from the method containing sulphur is separated in sulfur system, comprise the following steps：
Step 1-1, prepares above-mentioned release agent；
Step 1-2, by/to containing the release agent prepared in sulfur system addition step 1-1；
Step 1-3, separates sulphur after standing.
Or, the method is comprised the following steps：
Step 2-1, according to above-mentioned release agent to containing each component that release agent is separately added into sulfur system；
Step 2-2, stands after being well mixed, and separates sulphur.
In the present invention, described can be any system containing sulphur simple substance or the body containing sulfur-containing compound containing sulfur system
System, its may be from desulfurization system or other any sources containing sulfur system.
In the present invention, the feed postition of release agent is not particularly limited, i.e. both release agent can be added into sulfur-bearing body
In system, it is also possible to will contain sulfur system and be added in release agent, release agent is used after both each composition can be mixed, it is also possible to will be each
Composition is added separately to containing in sulfur system, and the addition sequence of each component is also not particularly limited.
After drusen grows into required particle diameter in containing sulfur system, you can sulphur therein is separated, the present invention
Mode to separation is not specially limited, and such as can carry out dividing for sulphur using sedimentation, filtering, centrifugation or filtration under diminished pressure mode
From.
Because at a temperature of different absorptions, precipitation time of the product sulphur in containing sulfur system is different, with temperature
Raise, the precipitation time first shortens increases (referring specifically to experimental example 6) afterwards, as shown in figure 3, when it is 70 DEG C to absorb temperature, sulphur
The precipitation time be about 1200~3700 seconds, total time-consuming is more than 1 hour；When it is 80 DEG C to absorb temperature, during the precipitation of sulphur
Between about 200~1000 seconds, total time-consuming be no more than 20 minutes；When temperature is absorbed more than 90 DEG C, the precipitation time of sulphur is about
100~1000 seconds, total time-consuming was no more than 20 minutes；And separating out that the time is shorter, drusen is more regular, and particle diameter is bigger, is consumed always
When substantially it is increased in the case of, selection temperature be 70~110 DEG C, preferably 75~100 DEG C, more preferably 80~90 DEG C.
Under these conditions, containing H2H in S gases2S gases are desulfurized the iron-based ionic liquid oxidation in agent, form simple substance
Sulphur, so as to obtain containing sulfur system.
Sulphur is the important raw material of industry, meanwhile, remaining desulfurization system may continue as through regeneration after sulphur is separated
Desulfurizing agent is used, therefore present invention selection separates accessory substance sulphur with desulfurization system, wherein, do not done for separation method especially
Limitation, such as sedimentation separation, centrifugation or is separated by filtration, due to method therefor of the present invention cause the particle diameter of accessory substance sulphur compared with
Greatly, sinking speed is fast, and is difficult to cause filter plant sulphur to block up, it is therefore preferable that separated by way of filtering, so as to carry
The reproduction speed of high separating efficiency and desulfurization system.
According to provided by the present invention for removing H2The desulfurizing agent and use desulfurizing agent removing H of S2The method of S has following
Beneficial effect：
(1) the release agent preparation method is simple, it is not necessary to complex operations, agents useful for same environmental protection, does not cause environment dirty
Dye；
(2) the release agent agents useful for same volatility is small, and operating condition is gentle；
(3) using after the release agent, rapid containing drusen growth in sulfur system, particle diameter is big, it is easy to sedimentation separation, reduces
In the absorption in reactor wall, reduce the possibility that filtering separation device is blocked, sulfur recovery rate is high；
(4) release agent can effectively reduce the attachment containing the sulphur little particle generated in sulfur system on the reactor wall, subtract
Few reactor plugs occur；
(5) separation method is easy to operate, flexible, easy, can according to the physical condition of reactor to separate specific mistake
Journey is adjusted, with very strong industrial applicibility.
(6) desulphurization reaction is quick, and the crystallization of sulphur simple substance is rapid, and total time-consuming is short；
(7) accessory substance drusen is pure, and impurity bag is miscellaneous few.
Embodiment
Information is as follows commercially available from agents useful for same in the present embodiment：
N- methylimidazoles (Mim), the micro- Industrial Co., Ltd. in Shanghai three, purity >=99%；
Chlorobutane (BuCl), Beijing Yili Fine Chemicals Co., Ltd. analyzes pure；
Ethyl acetate, Beijing North fine chemicals Co., Ltd analyzes pure；
Iron chloride (FeCl3·6H2O), Tianjin good fortune morning chemical reagent factory, analyzes pure；
Sulphur, Xilong Chemical Co., Ltd analyzes pure；
DMF (DMF), Beijing Chemical Plant analyzes pure；
DMI (DMI), Beijing Victor Chemical Co., Ltd. analyzes pure；
Lauryl sodium sulfate (SDS), Xilong Chemical Co., Ltd analyzes pure；
Ocytlphenol ethoxylate (TX-100), Beijing Victor Chemical Co., Ltd. analyzes pure.
(1) preparation of iron-based ionic liquid
It is 1.05 according to mol ratio:1 weighs chlorobutane 218g respectively mixes at room temperature with methylimidazole 200g, in 70 DEG C
Isothermal reaction 72h, product washs 5 removing unreacted reactants with ethyl acetate, and Fen Ye get lower floors liquid, 70 DEG C of rotary evaporations are remained
Excess is ionic liquid [Bmim] Cl, by ionic liquid [Bmim] Cl and FeCl3·6H2O is 1 according to mol ratio:2 in opening
Environment in mix, be thoroughly mixed rear centrifugation and obtain upper strata iron-based ionic liquid (ILs) product.
Embodiment 1
(1) 60mL iron-based ionic liquids as obtained in () are taken, 30mL DMI, 0.6mL TX-100 is added thereto to, is mixed
Close uniform, obtain final product release agent；
(2) obtained release agent in step 1 is warming up to 80 DEG C, is added thereto to remove H2After S containing sulfur system；
(3) system that will be obtained in step 2 naturally cools to room temperature, containing having crystal to separate out in sulfur system after 20min, will analyse
The crystal separation and recovery for going out.
The average grain diameter that microscopical eyepiece micrometer measures gained drusen is 3.1mm.
Embodiment 2
(1) 50mL iron-based ionic liquids as obtained in () are taken, 25mL DMI, 0.5mL TX-100 is added thereto to, is mixed
Close uniform, obtain final product release agent；
(2) to being passed through and contain 1%H in the release agent prepared in step 12The admixture of gas of S, standing separation sulphur.
The average grain diameter that microscopical eyepiece micrometer measures gained drusen is 3.2mm, its particle diameter distribution such as Fig. 4 institutes
Show.
Comparative example
Comparative example 1
This comparative example operates identical with embodiment 1, to differ only in and be added without DMI in release agent, is also added without TX-100.
The average grain diameter that microscopical eyepiece micrometer measures gained drusen is 0.9mm, its particle diameter distribution such as Fig. 5 institutes
Show.
Comparative example 2
This comparative example method therefor is same as Example 1, differs only in and is added without TX-100.
The average grain diameter that microscopical eyepiece micrometer measures gained drusen is 0.9mm.
Comparative example 3
This comparative example method therefor is same as Example 1, differs only in and is added without DMI.
The average grain diameter that microscopical eyepiece micrometer measures gained drusen is 0.9mm.
Experimental example
(2) sulphur solubility test method：
(1) take in the dicyandiamide solution that excessive sulphur adds 20mL, be stirred at room temperature until dissolution equilibrium, is then leaked with G4 cores
Bucket is filtrated to get undissolved sulphur, and deionized water is washed three times, is put into drying baker drying to constant weight, the addition of sulphur and not
The difference of meltage is solubility x of the room temperature sulphur in dicyandiamide solution0；
(2) take in the dicyandiamide solution that excessive sulphur adds 30mL, stir and be heated to t DEG C, until dissolution equilibrium, stand 1h
So that undissolved sulphur is layered in solution bottom, takes 20mL upper stratas saturated solvent system and be placed in small beaker, be cooled to normal temperature, until
All crystallization is separated out sulphur, filtering water washing three times, and drying to constant weight can obtain sulphur amount of precipitation for xt, so that sulphur exists at t DEG C
The solubility of dicyandiamide solution is x0+xt。
The sulphur of experimental example 1 particle size determination in different solvents system
Iron-based ionic liquid used by this experimental example is preparation in embodiment ().
At 80 DEG C, sulphur is dissolved separately in pure iron-based ionic liquid, 5%DMI systems, 10%DMI systems, 33%DMI
In system, 10%DMF systems and 33%DMF systems, room temperature is naturally cooling to, determines the particle diameter distribution of drusen, as a result such as
Shown in Fig. 6 a~Fig. 6 f.
From Fig. 6 a, sulphur recrystallization average grain diameter is 1.101mm in pure iron-based ionic liquid, and particle diameter distribution more collects
In it is uniform, but particle diameter is smaller；
From Fig. 6 b, sulphur recrystallization average grain diameter is 3.214mm in 5%DMI systems, and particle diameter distribution is more concentrated
Even, particle diameter substantially increases；
From Fig. 6 c, sulphur recrystallization average grain diameter is 4.841mm in 10%DMI systems, and particle diameter distribution is not enough concentrated,
Particle diameter substantially increases；
From Fig. 6 d, sulphur recrystallization average grain diameter is 4.862mm, centralized particle diameter, particle diameter in 33%DMI systems
Substantially increase；
From Fig. 6 e, sulphur recrystallization average grain diameter is 2.852mm, centralized particle diameter, particle diameter in 10%DMF systems
Increased；
From Fig. 6 f, sulphur recrystallization average grain diameter is 3.032mm, centralized particle diameter, particle diameter in 33%DMF systems
Increase obvious；
In from Fig. 6 d and Fig. 6 f, in iron-based ionic liquid add 33% DMI than add 33% DMF for sulphur
Sulphur recrystallization grain diameter influence is bigger, and sulphur particle diameter is more concentrated, and is more uniformly spread.
Solubility of the sulphur of experimental example 2 in different DMI concentration systems
Iron-based ionic liquid used by this experimental example is prepared for embodiment ().
This experimental example method of (two), determine sulphur DMI concentration be respectively 0,5%, 10% and 33% iron-based from
Solubility in sub- liquid, is designated as curve a, curve b, curve c and curve d, as a result as shown in Figure 1 respectively.
As shown in Figure 1,5%DMI is added in the desulfurization system of iron-based ionic liquid, sulphur solubility can be made substantially to carry
Height, and the DMI of addition 10% or 33% then can substantially reduce the solubility of sulphur, without being bound by any theory, the present inventor
Think that a small amount of DMI can be combined with iron-based ionic liquid so as to promote the dissolving of sulphur, but DMI belongs to polarity compared with strong solvent, therefore
When increasing its consumption, nonpolar sulphur in desulfurization system solubility reduction, further increase DMI consumptions, sulphur it is molten
Solution degree is further reduced.
Solubility of the sulphur of experimental example 3 in different DMF concentration systems
Iron-based ionic liquid used by this experimental example is prepared for embodiment ().
This experimental example method of (two), determines the iron-based ionic liquid that sulphur is respectively 0,10% and 33% in DMF concentration
Solubility in body, is designated as curve a, curve b and curve c, as a result as shown in Figure 2 respectively.
As shown in Figure 2, solubility behavior of the sulphur in different DMF concentration systems from different DMI concentration systems
Solubility behavior is similar, inventors believe that the reason for causing the solubility behavior is also similar.
Solubility of the sulphur of experimental example 4 in variety classes surfactant system
Iron-based ionic liquid used by this experimental example is prepared for embodiment ().
This experimental example method of (two), determine sulphur saturation SDS (cationic surfactant) ion liquid system,
Solubility in desulfurization system and simple iron-based ionic liquid containing 1% TX-100 (nonionic surface active agent), point
Curve a, curve b and curve c are not designated as, as a result as shown in Figure 7.
As shown in Figure 7, two kinds of surfactants make solubility reduction of the sulphur in iron-based ionic liquid, wherein TX-
100 effect is more notable, without being bound by any theory, inventors believe that sulphur is acted in nonionic surfactant
Under, zeta potential does not change, and phase inter coagulation can form hydrated sheath between sulphur little particle so that prevent sulphur and iron-based from
Sub- liquid is further contacted, and then reduces its solubility in iron-based ionic liquid.
The sulphur of experimental example 5 particle size determination in different surfaces surfactant system
At 80 DEG C, by sulphur be dissolved separately in containing volume content be 1%TX-100 or dissolving saturation SDS iron-based from
In sub- liquid, room temperature is naturally cooled to, determine the particle diameter distribution of drusen, as a result as figures 8 a and 8 b show.
Knowable to Fig. 8 a and Fig. 8 b, under nonionic surface active agent TX-100 existence conditions, sulphur recrystallization particle diameter
More than the particle diameter that the sulphur in the presence of cationic surface active agent SDS is recrystallized, inventors believe that being due to nonionic table
Face activating agent TX-100 can soak the drusen surface of precipitation, so that cohesion enhancing between sulphur little particle,
The final particle diameter for causing drusen reaches 3.041mm, and cationic surface active agent can make the zeta potential between sulphur little particle
Increase, hinders it to reunite, and causes the particle diameter only 2.073mm of drusen.
Precipitation time of the sulphur of experimental example 6 in iron-based ionic liquid
Sulphur simple substance is dissolved at 40 DEG C, 50 DEG C, 60 DEG C, 70 DEG C, 80 DEG C, 90 DEG C, 100 DEG C and 110 DEG C respectively
(1) in the ionic liquid for preparing, saturated solution is formed, then is naturally cooling to room temperature, sulphur recorded respectively and starts crystallization time point
And whole crystallization time points, curve is drawn as shown in figure 3, wherein, curve a represents beginning crystallization time, curve b represents crystallization knot
The beam time.
From the figure 3, it may be seen that in iron-based ionic liquid, the sulphur recrystallization time of the saturated solution of formation is under different temperatures
Different：
The 40 DEG C and 50 DEG C saturated solutions of formation, do not there is obvious crystalline polamer still during more than a hour, recrystallize
Time is more long, and discovery recrystallizes sulphur for molecule, it is necessary to 5h is staticly settled after standing one day, and it is tight to inhale wall phenomenon
Weight, therefore should not select.Particle diameter is about between 100 μm~300 μm.
Inventors believe that, the condition be in the first Metastable zone, solution will not spontaneous nucleation, but add crystal seed after, crystal
Will be grown on crystal seed, now the degree of supersaturation very little of solution, comparatively, the growth tendency of crystal is generated more than new nucleus
Tendency.The precipitation of solute declines concentration in solution, and solution state can return to the first Metastable zone again, thus in this temperature province
Although sulphur particle diameter is maximum, the time is separated out very long.
60 DEG C of saturated solutions of formation, sulphur is presented rhabdolith in recrystallization.Sulphur weight at a temperature of 60~80 DEG C
Crystallization particle diameter is larger, particle is uniform, be easily isolated, but 60~70 DEG C to separate out the times relatively long, it is necessary to time-consuming about 1 hour.
The saturated solution formed at 80 DEG C, sulphur particle diameter is larger and the precipitation time is shorter, can be separated out in 10min or so,
Particle diameter is big, particle is uniform, be easily isolated.Inventors believe that, with this understanding, between solution is in first, second Metastable zone, into
Core needs the certain intervals time, and crystal growth and nucleation are vied each other so as to obtain medium-grained particle.
90 DEG C~110 DEG C saturated solutions of formation, the sulphur recrystallization time is very short, very fast recrystallization point occur, all analysis
Go out the time also in 1000s, but recrystallization is in range of instability, and grain crystalline speed is more than growth rate, and degree of supersaturation is excessive,
Crystal cannot fully grow and become core, so produce a large amount of fine crystals to be suspended in solution, not free settling.
The sulphur of experimental example 7 separates out time-consuming measure in different solvents system
It is 1%, 5%, 10% and the iron-based ionic liquid of 33%DMF or DMI that sulphur is dissolved separately in into concentration at 80 DEG C
In body, crystallization total time-consuming is determined, as a result as shown in figure 9, wherein curve a represents DMI system curves, curve b represents that DMF systems are bent
Line.
As shown in Figure 9, at 80 DEG C, with the rising of solvent strength, the precipitation time needed for sulphur recrystallization shortens, this
Inventor is considered because DMI, DMF viscosity are low so that diffusion rate and rate of heat transfer increase, so that sulphur analysis wherein
Go out time shortening, when the concentration of solvent reaches 33%, heat-transfer effect is good in solution, and degree of supersaturation is larger, separate out the time short.
The present invention has been described in detail above in association with specific embodiment and exemplary example, but these explanations are simultaneously
It is not considered as limiting the invention.It will be appreciated by those skilled in the art that without departing from the spirit and scope of the invention,
Various equivalencings, modification can be carried out to technical solution of the present invention and embodiments thereof or is improved, these each fall within the present invention
In the range of.Protection scope of the present invention is determined by the appended claims.
Claims (7)
1. it is a kind of from containing the release agent that sulphur is separated in sulfur system, it is characterised in that composition of the release agent comprising volumes below part：
100 parts of iron-based ionic liquid,
20~55 parts of solvent,
0.8~2 part of surfactant,
The solvent is DMI,
The surfactant is ocytlphenol ethoxylate, and the iron-based ionic liquid is compound (a) and FeCl3Or
FeCl3·6H2The compound that O is formed, wherein,
The compound (a) and FeCl3Or FeCl3·6H2The mol ratio of O is 1:(0.5~3)
The compound (a) as shown in following formula I,
Wherein, R1And/or R2It is alkyl.
2. release agent according to claim 1, it is characterised in that R1And/or R2It is C1~C12Alkyl.
3. release agent according to claim 2, it is characterised in that R1And/or R2It is C1~C8Alkyl.
4. release agent according to claim 1, it is characterised in that the release agent includes the composition of volumes below part：
100 parts of iron-based ionic liquid,
50 parts of DMI,
1 part of ocytlphenol ethoxylate.
5. release agent according to claim 1, it is characterised in that
The iron-based ionic liquid is compound (b) and FeCl3Or FeCl3·6H2The compound that O is formed, wherein,
The compound (b) and FeCl3Or FeCl3·6H2The mol ratio of O is 1:2,
The compound (b) as shown in Formula Il,
6. usage right one of 1~5 described release agent of requirement is from the method containing sulphur is separated in sulfur system, it is characterised in that should
Method is comprised the following steps：
(1-1) prepares one of Claims 1 to 5 described release agent；
(1-2) by/to adding containing sulfur system the release agent prepared in step 1-1；
(1-3) separates sulphur after standing.
7. usage right one of 1~5 described release agent of requirement is from the method containing sulphur is separated in sulfur system, it is characterised in that should
Method is comprised the following steps：
(2-1) is according to one of Claims 1 to 5 release agent to containing each component that release agent is separately added into sulfur system；
Stood after (2-2) is well mixed, separate sulphur.
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