CN109078490A - A method of promoting iron-based ionic liquid desulfurization effect - Google Patents
A method of promoting iron-based ionic liquid desulfurization effect Download PDFInfo
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- CN109078490A CN109078490A CN201811092129.4A CN201811092129A CN109078490A CN 109078490 A CN109078490 A CN 109078490A CN 201811092129 A CN201811092129 A CN 201811092129A CN 109078490 A CN109078490 A CN 109078490A
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- ionic liquid
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- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 title claims abstract description 102
- 239000002608 ionic liquid Substances 0.000 title claims abstract description 74
- 238000006477 desulfuration reaction Methods 0.000 title claims abstract description 64
- 229910052742 iron Inorganic materials 0.000 title claims abstract description 51
- 230000023556 desulfurization Effects 0.000 title claims abstract description 50
- 230000000694 effects Effects 0.000 title claims abstract description 24
- 238000000034 method Methods 0.000 title claims abstract description 22
- 230000001737 promoting effect Effects 0.000 title claims abstract description 13
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 45
- 239000003960 organic solvent Substances 0.000 claims abstract description 14
- 239000003513 alkali Substances 0.000 claims abstract description 13
- 238000013329 compounding Methods 0.000 claims description 22
- 239000007788 liquid Substances 0.000 claims description 21
- SECXISVLQFMRJM-UHFFFAOYSA-N N-Methylpyrrolidone Chemical compound CN1CCCC1=O SECXISVLQFMRJM-UHFFFAOYSA-N 0.000 claims description 17
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 claims description 12
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims description 11
- 238000006243 chemical reaction Methods 0.000 claims description 10
- 238000002156 mixing Methods 0.000 claims description 8
- FHDQNOXQSTVAIC-UHFFFAOYSA-M 1-butyl-3-methylimidazol-3-ium;chloride Chemical compound [Cl-].CCCCN1C=C[N+](C)=C1 FHDQNOXQSTVAIC-UHFFFAOYSA-M 0.000 claims description 6
- 239000013067 intermediate product Substances 0.000 claims description 6
- 239000005864 Sulphur Substances 0.000 claims description 4
- VFWCMGCRMGJXDK-UHFFFAOYSA-N 1-chlorobutane Chemical compound CCCCCl VFWCMGCRMGJXDK-UHFFFAOYSA-N 0.000 claims description 3
- MCTWTZJPVLRJOU-UHFFFAOYSA-N 1-methyl-1H-imidazole Chemical compound CN1C=CN=C1 MCTWTZJPVLRJOU-UHFFFAOYSA-N 0.000 claims description 3
- 239000012535 impurity Substances 0.000 claims description 3
- NQXWGWZJXJUMQB-UHFFFAOYSA-K iron trichloride hexahydrate Chemical compound O.O.O.O.O.O.[Cl-].Cl[Fe+]Cl NQXWGWZJXJUMQB-UHFFFAOYSA-K 0.000 claims description 3
- 238000000926 separation method Methods 0.000 claims description 3
- 238000003756 stirring Methods 0.000 claims description 3
- 239000006228 supernatant Substances 0.000 claims description 3
- 238000005292 vacuum distillation Methods 0.000 claims description 3
- 230000015572 biosynthetic process Effects 0.000 claims description 2
- 238000004821 distillation Methods 0.000 claims description 2
- 238000001914 filtration Methods 0.000 claims description 2
- 239000003643 water by type Substances 0.000 claims 1
- 230000008929 regeneration Effects 0.000 abstract description 4
- 238000011069 regeneration method Methods 0.000 abstract description 4
- 238000012360 testing method Methods 0.000 description 23
- 238000012795 verification Methods 0.000 description 22
- 239000007789 gas Substances 0.000 description 21
- RWSOTUBLDIXVET-UHFFFAOYSA-N Dihydrogen sulfide Chemical compound S RWSOTUBLDIXVET-UHFFFAOYSA-N 0.000 description 19
- 229910000037 hydrogen sulfide Inorganic materials 0.000 description 19
- 229910052717 sulfur Inorganic materials 0.000 description 8
- 239000011593 sulfur Substances 0.000 description 8
- 239000012071 phase Substances 0.000 description 6
- 239000003795 chemical substances by application Substances 0.000 description 5
- 230000003009 desulfurizing effect Effects 0.000 description 5
- 238000001514 detection method Methods 0.000 description 5
- 238000010586 diagram Methods 0.000 description 5
- 230000003647 oxidation Effects 0.000 description 5
- 238000007254 oxidation reaction Methods 0.000 description 5
- 150000001875 compounds Chemical class 0.000 description 4
- 239000002253 acid Substances 0.000 description 3
- 238000006555 catalytic reaction Methods 0.000 description 3
- 230000008676 import Effects 0.000 description 3
- 150000002500 ions Chemical class 0.000 description 3
- 230000008569 process Effects 0.000 description 3
- VTLYFUHAOXGGBS-UHFFFAOYSA-N Fe3+ Chemical compound [Fe+3] VTLYFUHAOXGGBS-UHFFFAOYSA-N 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 2
- XYIBRDXRRQCHLP-UHFFFAOYSA-N ethyl acetoacetate Chemical compound CCOC(=O)CC(C)=O XYIBRDXRRQCHLP-UHFFFAOYSA-N 0.000 description 2
- 229910001447 ferric ion Inorganic materials 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000012546 transfer Methods 0.000 description 2
- 230000002745 absorbent Effects 0.000 description 1
- 239000002250 absorbent Substances 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 150000001768 cations Chemical class 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 239000000839 emulsion Substances 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 150000002576 ketones Chemical group 0.000 description 1
- 238000003475 lamination Methods 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 238000011068 loading method Methods 0.000 description 1
- 150000007530 organic bases Chemical class 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 238000007614 solvation Methods 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
Classifications
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/34—Chemical or biological purification of waste gases
- B01D53/74—General processes for purification of waste gases; Apparatus or devices specially adapted therefor
- B01D53/86—Catalytic processes
- B01D53/8603—Removing sulfur compounds
- B01D53/8612—Hydrogen sulfide
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J31/00—Catalysts comprising hydrides, coordination complexes or organic compounds
- B01J31/02—Catalysts comprising hydrides, coordination complexes or organic compounds containing organic compounds or metal hydrides
- B01J31/0277—Catalysts comprising hydrides, coordination complexes or organic compounds containing organic compounds or metal hydrides comprising ionic liquids, as components in catalyst systems or catalysts per se, the ionic liquid compounds being used in the molten state at the respective reaction temperature
- B01J31/0278—Catalysts comprising hydrides, coordination complexes or organic compounds containing organic compounds or metal hydrides comprising ionic liquids, as components in catalyst systems or catalysts per se, the ionic liquid compounds being used in the molten state at the respective reaction temperature containing nitrogen as cationic centre
- B01J31/0281—Catalysts comprising hydrides, coordination complexes or organic compounds containing organic compounds or metal hydrides comprising ionic liquids, as components in catalyst systems or catalysts per se, the ionic liquid compounds being used in the molten state at the respective reaction temperature containing nitrogen as cationic centre the nitrogen being a ring member
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Environmental & Geological Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Health & Medical Sciences (AREA)
- Biomedical Technology (AREA)
- Analytical Chemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Gas Separation By Absorption (AREA)
Abstract
The present invention discloses a kind of method for promoting iron-based ionic liquid desulfurization effect, comprising the following steps: sequentially adds alkali organic solvent and water into iron-based ionic liquid, forms doctor solution, then by H2S gas is passed through the doctor solution and carries out desulfurization.It is that water is introduced into " Fe-IL+NMP " desulfurization system by active, promotes desulfurization effect and desulfuration efficiency, can be recycled after regeneration, no pollution to the environment using remarkable result of the invention.
Description
Technical field
The present invention relates to liquid phase catalytic oxidation hydrogen sulfide field, a method of promoting iron-based ionic liquid desulfurization effect.
Background technique
Sulfur-containing gas cleaning and desulfurization technology generally uses two kinds of dry and wet.Dry desulfurizing process process is relatively simple
Single, steady, desulfurization precision is higher, its right sulfur capacity is small, is only applicable to low concentration H2S processing, and desulfurizing agent is vulnerable to desulfurization condition
It influences and is sintered, regeneration is also more difficult, need to regularly replace desulfurizing agent；Wet desulphurization can not only be compared with peracidity gas loading condiction
Lower desulfurization, and it is applied widely, and operation stability is not influenced vulnerable to desulfurization condition, but wet desulfurizing process needs heat-exchanger rig
And regeneration energy consumption is higher, and it is serious there are secondary pollution the problems such as.
Desulfurization is carried out using iron-based ionic liquid (Fe-IL), compares and has a clear superiority compared with Regular Desulfurization Methods: as one kind
The nonaqueous phase wet oxidation-desulfurizing agent of green, has environmentally protective, and thermal stability, chemical stability are high, and sulfur capacity is high, are not easy to drop
Solution does not generate secondary pollution, and the sulphur of removing is easy to realize the advantages that separating with solvent have extremely strong application potential.
Because the product that iron-based ionic liquid (Fe-IL) carries out catalysis oxidation to hydrogen sulfide is sulphur and water, the prior art
Generally for desulfuration efficiency is guaranteed, the initial aqueous rate of iron-based ionic liquid is reduced, as far as possible often to reduce iron-based ion
Degradation (such as Chinese patent CN201510811159.6) of cation during catalysis oxidation hydrogen sulfide in liquid.This
Outside, Fe-IL is in acidity, and viscosity is higher, leads to its Fe3+Activity it is not high, so that so that practical Sulfur capacity is much smaller than theoretical
Sulfur capacity weakens the acidity of Fe-IL so being all made of the mode for introducing the organic solvent of faintly acid or alkalinity in the prior art.
Summary of the invention
The present invention provides one kind by introducing suitable quantity of water and organic base into iron-based ionic liquid, to weaken iron-based ionic liquid
The acidity of body improves its Sulfur capacity, and then a kind of method for promoting iron-based ionic liquid desulfurization effect.
Technical solution is as follows:
A method of iron-based ionic liquid desulfurization effect being promoted, key is the following steps are included: to iron-based ion
It sequentially adds alkali organic solvent and water in liquid, forms doctor solution, then by H2S gas is passed through the doctor solution and carries out desulfurization.
Preferably, it is above-mentioned it is a kind of promoted iron-based ionic liquid desulfurization effect method the following steps are included:
Step (1), configuration iron-based ionic liquid；
Alkali organic solvent is added into the iron-based ionic liquid in step (2), and the two is stood after evenly mixing to be formed
Compound ionic liquid；
Step (3), into the compounding ionic liquid, addition water forms the doctor solution；
Step (4) is passed through H to the doctor solution2S gas carries out desulfurization.
Preferably, the alkali organic solvent in the step (2) is N-Methyl pyrrolidone (NMP), institute
The mass ratio for stating iron-based ionic liquid and N-Methyl pyrrolidone is 1:1.
Preferably, it is 5%-70%'s that volume ratio is added into the compounding ionic liquid of the step (3)
Water forms the doctor solution after shaking up.
Preferably, the water that volume ratio is 5%-30% is added into the compounding ionic liquid of step (3) to shake
The doctor solution is formed after even.
Preferably, H is passed through with the flow of 20ml/min into the doctor solution of step (4)2S gas is kept
H2The concentration of S gas feed is 5%.
Preferably, when step (4) carries out, the real-time aqueous of doctor solution is kept using distillation or by the way of filtering
It measures consistent with initial water content.
Preferably, the iron-based ionic liquid is made by following steps:
Step (1.1): 1- methylimidazole and chloro-normal butane are fitted into there-necked flask according to mass ratio 1:2, in 70 DEG C of perseverances
48h is stirred in tepidarium, obtains reaction solution；
Step (1.2): the reaction solution being poured into separatory funnel and is separated, and takes lower layer's yellow liquid, the bodies such as addition
Long-pending ethyl acetate washs 3 times, removes reaction solution impurity；
Step (1.3): liquid separation is carried out again and obtains lower liquid, then removes second through the 90 DEG C of vacuum distillations of Rotary Evaporators constant temperature
Acetoacetic ester, obtained weak yellow liquid, as intermediate product [Bmim] Cl；
Step (1.4): the intermediate product [Bmim] Cl is mixed with Iron(III) chloride hexahydrate with mass ratio 1:3, normal
Stir 36h under normal temperature and pressure, be then allowed to stand one day and be layered, separated and supernatant liquid and filtered 2-3 time with separatory funnel, obtain described in
Iron-based ionic liquid.
Detailed description of the invention
Fig. 1 is the state diagram that pure Fe-IL is mixed with water and do not shaken up；
Fig. 2 is that the state diagram after standing is shaken up after pure Fe-IL is mixed with water；
Compounding ionic liquid and the mixed state diagram of water that Fig. 3 is NMP:Fe-IL=5:5；
The water that different proportion is added in the compounding ionic liquid that Fig. 4 is NMP:Fe-IL=5:5 carries out its absorption tower when desulfurization
Sulfur content-time diagram in tail gas；
Specific embodiment
Below with reference to embodiment and attached drawing, the invention will be further described.
Embodiment:
A method of promoting iron-based ionic liquid desulfurization effect, comprising the following steps:
Step (1) configures iron-based ionic liquid using following steps:
Step (1.1): 1- methylimidazole and chloro-normal butane are fitted into there-necked flask according to mass ratio 1:2, in 70 DEG C of perseverances
48h is stirred in tepidarium, obtains reaction solution；
Step (1.2): the reaction solution being poured into separatory funnel and is separated, and takes lower layer's yellow liquid, the bodies such as addition
Long-pending ethyl acetate washs 3 times, removes reaction solution impurity；
Step (1.3): liquid separation is carried out again and obtains lower liquid, then removes second through the 90 DEG C of vacuum distillations of Rotary Evaporators constant temperature
Acetoacetic ester, obtained weak yellow liquid, as intermediate product [Bmim] Cl；
Step (1.4): the intermediate product [Bmim] Cl is mixed with Iron(III) chloride hexahydrate with mass ratio 1:3, normal
Stir 36h under normal temperature and pressure, be then allowed to stand one day and be layered, separated and supernatant liquid and filtered 2-3 time with separatory funnel, obtain described in
Iron-based ionic liquid.
Alkali organic solvent is added into the iron-based ionic liquid in step (2), and the two is stood after evenly mixing to be formed
N- crassitude can be added by 1:1 in mass ratio into iron-based ionic liquid when compounding ionic liquid, then be embodied
Ketone forms the compounding ionic liquid of iron-based ionic liquid and N-Methyl pyrrolidone；
Organic solvent NMP inherently H2A certain amount of H can be absorbed in the physical absorbent of S2S, and NMP is in alkalinity, it can
To weaken iron-based ionic liquid acidity, strengthen to its H2The capturing ability of S, to promote to H2S catalysis oxidation ability；It is another
Aspect is to form solvation with iron-based ionic liquid, reduces the viscosity of iron-based ionic liquid, improves gas-liquid mass transfer rate, from
And iron-based ionic liquid is made to aoxidize more H2S gas, also makes it to H2S oxidation is more abundant, and mass ratio can guarantee iron-based for 1:1
Ionic liquid and NMP's is sufficiently mixed.
The water formation doctor solution that volume ratio is 30% is added into above-mentioned compounding ionic liquid for step (3)；
Step (4) is passed through H to above-mentioned doctor solution with the flow of 20ml/min2S gas carries out desulfurization, and keeps H2S gas
The concentration of body import is 5%.
Formed after iron-based ionic liquid and alkali organic solvent mixing it is homogeneous compound ionic liquid, add water with compound
Ionic liquid is mixed to form doctor solution, can make doctor solution homogeneous liquid, is not in the situation of layering, while water can dilute
The solution of Fe-IL weakens the acid Sulfur capacity for improving doctor solution, promotes the desulfuration efficiency of doctor solution.
The application is described further below with reference to verification test:
(1), intersolubility comparative test
A, the H of different proportion as shown in Fig. 1, is added in pure Fe-IL2O, water content is from left to right successively are as follows: 0,
5%, 10%, 30%, 40%, 50%, 60%, 70%, 80%, 90%, when without shaking up, observe it can be seen that pure Fe-IL
With water at two-phase, lower layer is blackish green iron-based ion, and upper layer is the water phase of pale yellow transparent, and immiscible, only micro water can
To exist in Fe-IL in the form of an emulsion or micro Fe-IL is soluble in water.
B, the H of different proportion as shown in Fig. 2, is added in pure Fe-IL2O, water content is from left to right successively are as follows: 0,
5%, 10%, 30%, 40%, 50%, 60%, 70%, 80%, 90%, after shaking up, observe the amount it can be seen that aqueous
When for 5%-70%, pure Fe-IL and water are divided into two-phase again, and lower layer is blackish green iron-based ionic liquid, and upper layer is brown color
Water phase, not at homogeneous, immiscible；And when water content is greater than 80%, it is that homogeneous, a small amount of Fe-IL is dissolved in a large amount of water phases.
C, it as shown in Fig. 3, is formed in Fe-IL by 1:1 addition alkali organic solvent-NMP and compounds ionic liquid, then to
The H of different proportion is wherein added2O, water content is followed successively by 0 from left to right, 5%, 10%, 30%, 40%, 50%, 60%,
70%, 80%, 90%.It can be seen that water does not occur lamination with compounding ionic liquid and dissolve each other completely from attached drawing 3.
(2), desulfurization effect verification test:
Verification test 1: it first takes step in above embodiments (2) to configure obtained compounding ionic liquid 100g, places it in
In closed container, which is equipped with gas feed and outlet, then with the flow of 20ml/min to the compounding ionic liquid
In be passed through H2S gas (inlet concentration 5%) carries out desulfurization, measures inlet and outlet H by Hydrothion concentration detection device2S concentration.
Verification test 2: the compounding ionic liquid for first taking step in above embodiments (2) configuration to obtain is appropriate, after mixing again
Water is added into the compounding ionic liquid, doctor solution is made 1., makes the quality 100g of doctor solution 1., water content 5%, then incite somebody to action
1. doctor solution is placed in closed container, which is equipped with gas feed and outlet, is then passed through with the flow of 20ml/min
H2S gas (inlet concentration 5%) carries out desulfurization, measures inlet and outlet H by Hydrothion concentration detection device2S concentration.
Verification test 3: the compounding ionic liquid for first taking step in above embodiments (2) configuration to obtain is appropriate, after mixing again
Water is added into the compounding ionic liquid, doctor solution is made 2., makes the quality 100g of doctor solution 2., water content 30%, then
2. doctor solution is placed in closed container, which is equipped with gas feed and outlet, then logical with the flow of 20ml/min
Enter H2S gas (inlet concentration 5%) carries out desulfurization, measures inlet and outlet H by Hydrothion concentration detection device2S concentration.
Verification test 4: the compounding ionic liquid for first taking step in above embodiments (2) configuration to obtain is appropriate, after mixing again
Water is added into the compounding ionic liquid, doctor solution is made 3., makes the quality 100g of doctor solution 3., water content 50%, then
3. doctor solution is placed in closed container, which is equipped with gas feed and outlet, then logical with the flow of 20ml/min
Enter H2S gas (inlet concentration 5%) carries out desulfurization, measures inlet and outlet H by Hydrothion concentration detection device2S concentration.
Verification test 5: the compounding ionic liquid for first taking step in above embodiments (2) configuration to obtain is appropriate, after mixing again
Water is added into the compounding ionic liquid, doctor solution is made 4., makes the quality 100g of doctor solution 4., water content 70%, then
4. doctor solution is placed in closed container, which is equipped with gas feed and outlet, then logical with the flow of 20ml/min
Enter H2S gas (inlet concentration 5%) carries out desulfurization, measures inlet and outlet H by Hydrothion concentration detection device2S concentration.
The exit H that above each verification test is obtained2S concentration data carries out finishing analysis, according to inlet and outlet H2S concentration
Value calculates desulfuration efficiency (desulfuration efficiency=(import H2S concentration-outlet H2S concentration)/import H2S concentration * 100%), as a result such as
Shown in Fig. 4:
Attached drawing 4 is desulfuration efficiency-time diagram of verification test 1,2,3,4,5, in 20min, verification test 2,3,4,5
Desulfuration efficiency is superior to verification test 1；After 20min, the desulfuration efficiency of verification test 5 starts to significantly reduce, and gradually bad
In verification test 1；In 20-60min time range, the desulfuration efficiency of verification test 2,4 is persistently better than verification test 1；It is connecing
When nearly 60min, the desulfuration efficiency of verification test 3 begins lower than verification test 1；In 35min, the desulfuration efficiency of verification test 3
It is significantly higher than verification test 1,2,4,5.
Illustrate: within a certain period of time, the desulfuration efficiency of verification test 2,3,4,5 is superior to verification test 1,
Conclusion:
It is analyzed according to the result to above each desulfurization effect verification test:
1, iron-based ionic liquid and N-Methyl pyrrolidone can make desulfurizing agent, but the high-efficiency desulfurization duration is not grown.Its
Reason is mainly:
(1) iron-based ionic liquid is in acid, viscosity is larger, and serves not only as during desulfurization solvent and as urging
Agent, hydrogen sulfide is ingeniously small in solubility wherein, and ferric ion concentration is lower, and gas-liquid mass transfer is slow, influences desulfurization effect；
(2) N-Methyl pyrrolidone is only used as Physical Absorption, can not achieve chemical conversion, can not keep for a long time efficient
Desulfurization is adsorbed, and its tail gas generated also needs to carry out secondary treatment.
2, water is introduced in traditional " Fe-IL+ alkali organic solvent (NMP) " desulfurization system, it can model in different times
Interior its desulfuration efficiency of raising is enclosed, desulfurization effect is reinforced；In 35min, "+30% water of Fe-IL+ alkali organic solvent (NMP) " is de-
Sulphur efficiency highest；In 60min, "+5% water of Fe-IL+ alkali organic solvent (NMP) " desulfurization duration is higher, is able to maintain longer
The desulfurization high efficiency of time.
The utility model has the advantages that using a kind of method of promotion iron-based ionic liquid desulfurization effect of the invention, by active to
Introduce water in " Fe-IL+NMP " desulfurization system, promote desulfurization effect and desulfuration efficiency, can be recycled after regeneration, to environment without
Pollution.
Finally, it should be noted that foregoing description is only the preferred embodiment of the present invention, the ordinary skill people of this field
Member under the inspiration of the present invention, without prejudice to the purpose of the present invention and the claims, can make multiple similar tables
Show, such transformation each falls within protection scope of the present invention.
Claims (8)
1. a kind of method for promoting iron-based ionic liquid desulfurization effect, it is characterised in that the following steps are included: to iron-based ionic liquid
It sequentially adds alkali organic solvent and water in body, forms doctor solution, then by H2S gas is passed through the doctor solution and carries out desulfurization.
2. it is according to claim 1 it is a kind of promoted iron-based ionic liquid desulfurization effect method, it is characterised in that including with
Lower step:
Step (1), configuration iron-based ionic liquid；
Alkali organic solvent is added into the iron-based ionic liquid in step (2), and the two is stood to formation compounding after evenly mixing
Ionic liquid；
Step (3), into the compounding ionic liquid, addition water forms the doctor solution；
Step (4) is passed through H to the doctor solution2S gas carries out desulfurization.
3. a kind of method for promoting iron-based ionic liquid desulfurization effect according to claim 2, it is characterised in that: the step
Suddenly the alkali organic solvent in (2) is N-Methyl pyrrolidone, the iron-based ionic liquid and N-Methyl pyrrolidone
Mass ratio is 1:1.
4. a kind of method for promoting iron-based ionic liquid desulfurization effect according to claim 2, it is characterised in that: to described
Water is added in the compounding ionic liquid of step (3), forms the doctor solution after shaking up, the volumetric(al) moisture content of the doctor solution is
5%-70%.
5. a kind of method for promoting iron-based ionic liquid desulfurization effect according to claim 4, it is characterised in that: described de-
The volumetric(al) moisture content of sulphur liquid is 5%-30%.
6. a kind of method for promoting iron-based ionic liquid desulfurization effect according to claim 2, it is characterised in that: to step
(4) H is passed through with the flow of 20ml/min in the doctor solution2S gas keeps H2The concentration of S gas feed is 5%.
7. a kind of method for promoting iron-based ionic liquid desulfurization effect according to claim 1, it is characterised in that: step
(4) when carrying out, keep the real-time water content of doctor solution consistent with initial water content using distillation or by the way of filtering.
8. a kind of method for promoting iron-based ionic liquid desulfurization effect according to claim 1 or 2, it is characterised in that described
Iron-based ionic liquid is made by following steps:
Step (1.1): 1- methylimidazole and chloro-normal butane are fitted into there-necked flask according to mass ratio 1:2, in 70 DEG C of thermostatted waters
48h is stirred in bath, obtains reaction solution；
Step (1.2): the reaction solution being poured into separatory funnel and is separated, and takes lower layer's yellow liquid, is added isometric
Ethyl acetate washs 3 times, removes reaction solution impurity, carries out liquid separation again and obtains lower liquid；
Step (1.3): again through 90 DEG C of vacuum distillations removal ethyl acetate of Rotary Evaporators constant temperature, obtained weak yellow liquid, i.e.,
For intermediate product [Bmim] Cl；
Step (1.4): the intermediate product [Bmim] Cl is mixed with Iron(III) chloride hexahydrate with mass ratio 1:3, normal in room temperature
Pressure stirring 36h, be then allowed to stand one day be layered, with the isolated supernatant liquid of separatory funnel and filter 2-3 time, obtain described in
Iron-based ionic liquid.
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111592474A (en) * | 2020-05-29 | 2020-08-28 | 河北品臣环保科技有限公司 | Preparation method of complex iron catalyst for wet desulphurization |
| CN113041791A (en) * | 2021-03-18 | 2021-06-29 | 重庆科技学院 | Iron-copper ionic liquid desulfurizing agent, preparation method and desulfurization method |
Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20110215052A1 (en) * | 2010-03-05 | 2011-09-08 | Instituto Mexicano Del Petroleo | Process of recovery of exhausted ionic liquids used in the extractive desulfurization of naphthas |
| CN102553436A (en) * | 2010-12-13 | 2012-07-11 | 北京化工大学 | Method for removing sulfur dioxide from iron-based ionic liquid |
| CN105084319A (en) * | 2014-04-29 | 2015-11-25 | 北京化工大学 | Separating agent for separating sulfur from sulfur-containing system and method for separating sulfur |
| CN105080316A (en) * | 2014-04-29 | 2015-11-25 | 北京化工大学 | Desulfurizer used for removing H2S and method for removing H2S |
| CN105198815A (en) * | 2015-08-24 | 2015-12-30 | 四川大学 | Iron-based imidazole ion liquid for removing SO2 from smoke and preparation method of iron-based imidazole ion liquid |
| CN107088349A (en) * | 2017-06-28 | 2017-08-25 | 重庆科技学院 | One kind compounding ion liquid reclaiming agent and preparation method |
| CN107812450A (en) * | 2017-12-07 | 2018-03-20 | 北京石油化工学院 | A kind of method of alkaline nonaqueous phase wet method catalysis oxidation hydrogen sulfide |
-
2018
- 2018-09-19 CN CN201811092129.4A patent/CN109078490A/en active Pending
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20110215052A1 (en) * | 2010-03-05 | 2011-09-08 | Instituto Mexicano Del Petroleo | Process of recovery of exhausted ionic liquids used in the extractive desulfurization of naphthas |
| CN102553436A (en) * | 2010-12-13 | 2012-07-11 | 北京化工大学 | Method for removing sulfur dioxide from iron-based ionic liquid |
| CN105084319A (en) * | 2014-04-29 | 2015-11-25 | 北京化工大学 | Separating agent for separating sulfur from sulfur-containing system and method for separating sulfur |
| CN105080316A (en) * | 2014-04-29 | 2015-11-25 | 北京化工大学 | Desulfurizer used for removing H2S and method for removing H2S |
| CN105198815A (en) * | 2015-08-24 | 2015-12-30 | 四川大学 | Iron-based imidazole ion liquid for removing SO2 from smoke and preparation method of iron-based imidazole ion liquid |
| CN107088349A (en) * | 2017-06-28 | 2017-08-25 | 重庆科技学院 | One kind compounding ion liquid reclaiming agent and preparation method |
| CN107812450A (en) * | 2017-12-07 | 2018-03-20 | 北京石油化工学院 | A kind of method of alkaline nonaqueous phase wet method catalysis oxidation hydrogen sulfide |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111592474A (en) * | 2020-05-29 | 2020-08-28 | 河北品臣环保科技有限公司 | Preparation method of complex iron catalyst for wet desulphurization |
| CN113041791A (en) * | 2021-03-18 | 2021-06-29 | 重庆科技学院 | Iron-copper ionic liquid desulfurizing agent, preparation method and desulfurization method |
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