CN114394938A - Method for effectively removing metal ions in ionic liquid water system - Google Patents
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- CN114394938A CN114394938A CN202210088272.6A CN202210088272A CN114394938A CN 114394938 A CN114394938 A CN 114394938A CN 202210088272 A CN202210088272 A CN 202210088272A CN 114394938 A CN114394938 A CN 114394938A
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- 239000002608 ionic liquid Substances 0.000 title claims abstract description 98
- 229910021645 metal ion Inorganic materials 0.000 title claims abstract description 42
- 238000000034 method Methods 0.000 title claims abstract description 42
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 title claims abstract description 32
- 238000001179 sorption measurement Methods 0.000 claims abstract description 25
- 239000012535 impurity Substances 0.000 claims abstract description 20
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 15
- 238000003795 desorption Methods 0.000 claims abstract description 9
- 239000007788 liquid Substances 0.000 claims abstract description 9
- 238000004821 distillation Methods 0.000 claims abstract description 7
- 239000003463 adsorbent Substances 0.000 claims abstract description 6
- 239000002808 molecular sieve Substances 0.000 claims description 18
- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 claims description 18
- 239000000243 solution Substances 0.000 claims description 18
- 239000007864 aqueous solution Substances 0.000 claims description 13
- 239000011734 sodium Substances 0.000 claims description 7
- -1 alkyl imidazole salt Chemical class 0.000 claims description 6
- 125000000217 alkyl group Chemical group 0.000 claims description 4
- 238000004064 recycling Methods 0.000 claims description 4
- 230000008929 regeneration Effects 0.000 claims description 4
- 238000011069 regeneration method Methods 0.000 claims description 4
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims description 3
- 229910052708 sodium Inorganic materials 0.000 claims description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 2
- 229910021536 Zeolite Inorganic materials 0.000 claims description 2
- 229910052799 carbon Inorganic materials 0.000 claims description 2
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 claims description 2
- 150000004714 phosphonium salts Chemical group 0.000 claims description 2
- 239000010457 zeolite Substances 0.000 claims description 2
- 230000018044 dehydration Effects 0.000 claims 1
- 238000006297 dehydration reaction Methods 0.000 claims 1
- 238000011084 recovery Methods 0.000 abstract description 14
- 150000002500 ions Chemical class 0.000 description 13
- 239000002904 solvent Substances 0.000 description 5
- 229910052784 alkaline earth metal Inorganic materials 0.000 description 3
- 150000001768 cations Chemical class 0.000 description 3
- 229920002678 cellulose Polymers 0.000 description 3
- 239000001913 cellulose Substances 0.000 description 3
- HQWOEDCLDNFWEV-UHFFFAOYSA-M diethyl phosphate;1-ethyl-3-methylimidazol-3-ium Chemical compound CC[N+]=1C=CN(C)C=1.CCOP([O-])(=O)OCC HQWOEDCLDNFWEV-UHFFFAOYSA-M 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
- BMQZYMYBQZGEEY-UHFFFAOYSA-M 1-ethyl-3-methylimidazolium chloride Chemical compound [Cl-].CCN1C=C[N+](C)=C1 BMQZYMYBQZGEEY-UHFFFAOYSA-M 0.000 description 2
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 description 2
- 150000001342 alkaline earth metals Chemical class 0.000 description 2
- 239000000835 fiber Substances 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000000746 purification Methods 0.000 description 2
- 235000000346 sugar Nutrition 0.000 description 2
- XOAAWQZATWQOTB-UHFFFAOYSA-N taurine Chemical compound NCCS(O)(=O)=O XOAAWQZATWQOTB-UHFFFAOYSA-N 0.000 description 2
- 238000005406 washing Methods 0.000 description 2
- 229920003043 Cellulose fiber Polymers 0.000 description 1
- 229920001661 Chitosan Polymers 0.000 description 1
- 229910019142 PO4 Inorganic materials 0.000 description 1
- 238000009825 accumulation Methods 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 229910001413 alkali metal ion Inorganic materials 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 230000001112 coagulating effect Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- UCQFCFPECQILOL-UHFFFAOYSA-N diethyl hydrogen phosphate Chemical compound CCOP(O)(=O)OCC UCQFCFPECQILOL-UHFFFAOYSA-N 0.000 description 1
- ZDIRKWICVFDSNX-UHFFFAOYSA-N diethyl phosphate 1-ethyl-3-methyl-1,2-dihydroimidazol-1-ium Chemical compound P(=O)(OCC)(OCC)O.C(C)N1CN(C=C1)C ZDIRKWICVFDSNX-UHFFFAOYSA-N 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 229910001385 heavy metal Inorganic materials 0.000 description 1
- 238000005342 ion exchange Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 239000004005 microsphere Substances 0.000 description 1
- 238000005191 phase separation Methods 0.000 description 1
- 239000010452 phosphate Substances 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000004627 regenerated cellulose Substances 0.000 description 1
- 238000001223 reverse osmosis Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 238000009987 spinning Methods 0.000 description 1
- 150000008163 sugars Chemical class 0.000 description 1
- 229960003080 taurine Drugs 0.000 description 1
- 238000005292 vacuum distillation Methods 0.000 description 1
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Classifications
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D233/00—Heterocyclic compounds containing 1,3-diazole or hydrogenated 1,3-diazole rings, not condensed with other rings
- C07D233/54—Heterocyclic compounds containing 1,3-diazole or hydrogenated 1,3-diazole rings, not condensed with other rings having two double bonds between ring members or between ring members and non-ring members
- C07D233/56—Heterocyclic compounds containing 1,3-diazole or hydrogenated 1,3-diazole rings, not condensed with other rings having two double bonds between ring members or between ring members and non-ring members with only hydrogen atoms or radicals containing only hydrogen and carbon atoms, attached to ring carbon atoms
- C07D233/58—Heterocyclic compounds containing 1,3-diazole or hydrogenated 1,3-diazole rings, not condensed with other rings having two double bonds between ring members or between ring members and non-ring members with only hydrogen atoms or radicals containing only hydrogen and carbon atoms, attached to ring carbon atoms with only hydrogen atoms or radicals containing only hydrogen and carbon atoms, attached to ring nitrogen atoms
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D213/00—Heterocyclic compounds containing six-membered rings, not condensed with other rings, with one nitrogen atom as the only ring hetero atom and three or more double bonds between ring members or between ring members and non-ring members
- C07D213/02—Heterocyclic compounds containing six-membered rings, not condensed with other rings, with one nitrogen atom as the only ring hetero atom and three or more double bonds between ring members or between ring members and non-ring members having three double bonds between ring members or between ring members and non-ring members
- C07D213/04—Heterocyclic compounds containing six-membered rings, not condensed with other rings, with one nitrogen atom as the only ring hetero atom and three or more double bonds between ring members or between ring members and non-ring members having three double bonds between ring members or between ring members and non-ring members having no bond between the ring nitrogen atom and a non-ring member or having only hydrogen or carbon atoms directly attached to the ring nitrogen atom
- C07D213/06—Heterocyclic compounds containing six-membered rings, not condensed with other rings, with one nitrogen atom as the only ring hetero atom and three or more double bonds between ring members or between ring members and non-ring members having three double bonds between ring members or between ring members and non-ring members having no bond between the ring nitrogen atom and a non-ring member or having only hydrogen or carbon atoms directly attached to the ring nitrogen atom containing only hydrogen and carbon atoms in addition to the ring nitrogen atom
- C07D213/16—Heterocyclic compounds containing six-membered rings, not condensed with other rings, with one nitrogen atom as the only ring hetero atom and three or more double bonds between ring members or between ring members and non-ring members having three double bonds between ring members or between ring members and non-ring members having no bond between the ring nitrogen atom and a non-ring member or having only hydrogen or carbon atoms directly attached to the ring nitrogen atom containing only hydrogen and carbon atoms in addition to the ring nitrogen atom containing only one pyridine ring
- C07D213/20—Quaternary compounds thereof
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07F—ACYCLIC, CARBOCYCLIC OR HETEROCYCLIC COMPOUNDS CONTAINING ELEMENTS OTHER THAN CARBON, HYDROGEN, HALOGEN, OXYGEN, NITROGEN, SULFUR, SELENIUM OR TELLURIUM
- C07F9/00—Compounds containing elements of Groups 5 or 15 of the Periodic Table
- C07F9/02—Phosphorus compounds
- C07F9/06—Phosphorus compounds without P—C bonds
- C07F9/08—Esters of oxyacids of phosphorus
- C07F9/09—Esters of phosphoric acids
- C07F9/091—Esters of phosphoric acids with hydroxyalkyl compounds with further substituents on alkyl
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- Molecular Biology (AREA)
- Treatment Of Water By Ion Exchange (AREA)
Abstract
The invention discloses a method for effectively removing metal ions in an ionic liquid water system, which comprises the following steps: introducing an ionic liquid water solution containing metal ion impurities into an adsorption tower filled with an adsorbent to remove metal ions, dehydrating the ionic liquid until the water content is qualified by high-temperature reduced pressure distillation of effluent liquid, introducing desorption liquid dilute hydrochloric acid into the adsorption tower after adsorption saturation to regenerate and recycle, and separating the metal ions and recovering the ionic liquid. The method for separating inorganic metal ions in the ionic liquid water system provided by the invention avoids the loss of the ionic liquid in the system, has high recovery efficiency, is suitable for different ionic liquid water systems, and has stronger universality and industrial application prospect.
Description
Technical Field
The invention relates to the technical field of ionic liquid recovery treatment, in particular to a method for separating impurity metal ions in an ionic liquid water system.
Background
In recent years, ionic liquids have attracted much attention due to their excellent physicochemical properties, such as strong polarity, non-volatility, designability of structure, etc., and are widely used in industry as green solvents, catalysts, etc., including extraction separation of alkali/alkaline earth metals, recovery of n-butanol, purification of taurine, etc., as solvents. In addition, the ionic liquid is also well applied to the dissolving process of cellulose as a solvent, but the phenomenon of trace cellulose degradation is accompanied in the dissolving process of the ionic liquid, and impurity ions (Na) are inevitably introduced into an ionic liquid aqueous solution obtained in the drawing and washing processes of the ionic liquid dissolving spinning process due to the fact that the cellulose contains a plurality of impurity ions+、K+、Ca2+、Mg2+、Fe3+、Cu2+、Zn2+Etc.). Due to the continuous accumulation of impurity ions in the coagulating bath and the water washing bath and partial entry into the regenerated fibers, the performance of the regenerated fibers and the recycling of the ionic liquid are seriously influenced. Therefore, the removal of impurity ions in the ionic liquid aqueous solution and the recycling of the ionic liquid are engineering problems to be solved urgently, and have very important significance for the comprehensive utilization of resources.
There are patents relating to the recovery of ionic liquids from the materials presently disclosed, and several of the reported patents are listed below for details: CN202011324962.4 provides a method for removing impurity ions in an ionic liquid system, which is to use a purification device filled with cellulose-chitosan microspheres to adsorb heavy metal ions Fe in an ionic liquid aqueous solution3+And Cu2+But does not involve the alkali metal ion Na+、K+And alkaline earth metal Ca2+、Mg2+And subsequent ionic liquid recovery. CN101503866 provides a method for recovering a solvent in the preparation of regenerated cellulose fibers by taking an ionic liquid as the solvent, wherein the ionic liquid solution is subjected to filtration, reverse osmosis and reduced pressure distillation to obtain the ionic liquid with the water content of less than 2%. CN101664612 discloses a method for purifying and separating ionic liquid and water, which takes sugar as additive to realize phase separation of ionic liquid and water, and then separates ions by gradient crystallizationLiquids and sugars.
In summary, in the existing ionic liquid recovery treatment process, Na in the ionic liquid is not generally considered comprehensively+、K+、Ca2+、Mg2+、Fe3+、Cu2+、Zn2+The removal of the metal ions and the subsequent recovery of the ionic liquid are realized, so that a process method for recovering the ionic liquid in an ionic liquid water system, which has the advantages of high efficiency, low energy consumption and easy operation, is developed, the recovery and utilization of the ionic liquid are realized, and the method has important economic value and research significance.
Disclosure of Invention
Aiming at the defects of the prior art, the invention aims to provide a method for effectively removing metal ions in an ionic liquid water system, which can effectively remove Na in the ionic liquid water system+、K+、Ca2+、Mg2+、Fe3+、Cu2+、Zn2+And the impurity metal ions are equal, the loss of the ionic liquid in the system is avoided, and the method is suitable for different ionic liquid water systems and has stronger universality and industrial application prospect.
In order to achieve the purpose, the invention adopts the following technical scheme: introducing an ionic liquid water solution containing metal ion impurities into an adsorption tower filled with an ionic adsorbent to remove metal ions, dehydrating the ionic liquid until the water content is qualified by high-temperature reduced pressure distillation of effluent liquid, and introducing desorption liquid dilute hydrochloric acid into the adsorption tower after adsorption saturation to regenerate and recycle.
Preferably, the ionic liquid is one or more of alkyl imidazole salt, alkyl pyridine salt, alkyl quaternary ammonium salt and alkyl quaternary phosphonium salt, wherein the carbon number of the alkyl is 1-10.
Preferably, the mass concentration of the ionic liquid in the ionic liquid water system is 1-10%.
Preferably, the impurity metal ion species is Na+、K+、Ca2+、Mg2+、Fe3+、Cu2+、Zn2+One or more of the above-mentioned (B) are used, and the mass concentration is 10-200 mg/L.
Preferably, the metal ion adsorbent is one or more of an artificial zeolite, a 4A molecular sieve, a 5A molecular sieve and a sodium X molecular sieve.
Preferably, the temperature of the high-temperature reduced pressure distillation is 90-120 ℃, and the pressure is 10-1000 Pa.
Preferably, the concentration of the dilute hydrochloric acid is 0.1-0.5 mol/L.
The method for effectively removing the metal ions in the ionic liquid water system is simple to operate, avoids the loss of the ionic liquid in the system, and is an environment-friendly method for purifying and recycling the ionic liquid.
The technical advantages are as follows: the invention provides a method for effectively removing metal ions in an ionic liquid water system, which can effectively remove Na in the ionic liquid system+、K+、Ca2+、Mg2+、Fe3+、Cu2+、Zn2+And the impurity metal ions are equal, the loss of the ionic liquid in the system is avoided, and the method is suitable for different ionic liquid water systems and has stronger universality and industrial application prospect.
Drawings
Fig. 1 is a process flow diagram of a method for effectively removing metal ions in an ionic liquid water system according to the present invention.
The symbols in the figure have the following meanings:
V1-V3: raw material liquid tank, regeneration liquid tank and regeneration liquid recovery tank
T1-T2: adsorption column and vacuum distillation column
Detailed Description
The adsorbent used in the invention is a commercially available molecular sieve, and the mechanism of adsorbing metal ion impurities is that the molecular sieve has a pore structure with the similar radius to the hydrated ion of the impurity metal and can perform ion exchange with free cations in the molecular sieve. And cations of the ionic liquid exist in a cluster form, the space radius is large, and the cations are difficult to enter the molecular sieve, so that the adsorption of the molecular sieve on the ionic liquid is limited, and the loss of the ionic liquid in the adsorption process is avoided.
According to some embodiments of the invention, the removal of metal ions is performed using an adsorption column packed with molecular sieves, the flow rate of the ionic liquid aqueous solution into the adsorption column being 5 to 50BV per hour (bed volume), preferably 10 to 30BV per hour (bed volume).
The technical solution of the present invention is further explained by the following embodiments. It will be appreciated by those skilled in the art that the specific material ratios, process conditions and results described in the examples are merely provided to assist in understanding the present invention and should not be construed as specifically limiting the invention.
Example 1
This example provides a method for effectively removing metal ions from an ionic liquid water system, where the ionic liquid to be recovered in an ionic liquid aqueous solution is 1-ethyl-3 methylimidazolium chloride, the mass fraction of which is 2%, and the impurity ions are Ca2+、Mg2+、Fe3+And Cu2+The concentrations were all 100 mg/L. The method comprises the following specific steps: introducing the ionic liquid aqueous solution into an adsorption tower filled with a 4A molecular sieve at the flow rate of 15BV/h, and carrying out ICP and ultraviolet spectrophotometer analysis on the effluent to determine the removal efficiency of metal ions and the loss condition of the ionic liquid. And distilling the effluent for 3h under the conditions of 100 ℃ and 200Pa to finally obtain the 1-ethyl-3-methylimidazolium chloride with the water mass content of 1.2 percent, wherein the recovery rate of the ionic liquid is 98.5 percent. After saturation of the adsorption, the solution was regenerated with a 0.2mol/L hydrochloric acid solution, and the regenerated solution was subjected to ICP analysis to determine the desorption efficiency, and the results are shown in Table 1.
Example 2
This example provides a method for effectively removing metal ions from an ionic liquid aqueous system, where the ionic liquid to be recovered is 1-ethyl-3-methylimidazolium diethyl phosphate, the mass fraction is 5%, and the impurity ion is K+、Ca2 +、Mg2+、Fe3+And Zn2+The concentrations were all 50 mg/L. The method comprises the following specific steps: the ionic liquid aqueous solution is added at the flow rate of 10BV/hIntroducing into an adsorption tower filled with 4A molecular sieve, and performing ICP and ultraviolet spectrophotometer analysis on the effluent to determine the removal efficiency of metal ions and the loss condition of ionic liquid. And distilling the effluent for 3h under the conditions of 120 ℃ and 300Pa to finally obtain the 1-ethyl-3-methylimidazolium diethyl phosphate with the water mass content of 1.5 percent, wherein the recovery rate of the ionic liquid is 99.2 percent. After saturation of the adsorption, the solution was regenerated with a 0.2mol/L hydrochloric acid solution, and the regenerated solution was subjected to ICP analysis to determine the desorption efficiency, and the results are shown in Table 1.
Example 3
This example provides a method for effectively removing metal ions from an ionic liquid aqueous system, where the ionic liquid to be recovered is 1-allyl-3 methylpyridine diethyl phosphate, the mass fraction of the ionic liquid is 3%, and the impurity ions are Na+、Fe3+、Cu2+And Zn2+The concentrations were 150 mg/L. The method comprises the following specific steps: introducing the ionic liquid aqueous solution into an adsorption tower filled with a 4A and 5A molecular sieve mixture at the flow rate of 10BV/h, and carrying out ICP and ultraviolet spectrophotometer analysis on the effluent to determine the removal efficiency of metal ions and the loss condition of the ionic liquid. And distilling the effluent at 110 ℃ under 500Pa for 4h under reduced pressure to finally obtain the 1-allyl-3-methylpyridine diethyl phosphate with the water mass content of 1.1 percent, wherein the recovery rate of the ionic liquid is 97.8 percent. After saturation of adsorption, the solution was regenerated with a 0.5mol/L hydrochloric acid solution, and the regenerated solution was subjected to ICP analysis to determine the desorption efficiency, and the results are shown in Table 1.
Example 4
This example provides a method for effectively removing metal ions from an ionic liquid aqueous system, where the ionic liquid to be recovered is 1-ethyl-3-methylimidazolium diethyl phosphate, the mass fraction is 10%, and the impurity ion is K+、Ca2 +And Mg2+The concentrations were all 100 mg/L. The method comprises the following specific steps: introducing an ionic liquid aqueous solution into an adsorption tower filled with a mixture of a 4A molecular sieve and a 5A molecular sieve at the flow rate of 20BV/h, and carrying out ICP and ultraviolet spectrophotometer analysis on the effluent to determine the removal efficiency of metal ions and the loss condition of the ionic liquid. The effluent is at 12And carrying out reduced pressure distillation for 4h at the temperature of 0 ℃ and under the condition of 200Pa, and finally obtaining the 1-ethyl-3-methylimidazole diethyl phosphate with the water mass content of 0.8 percent, wherein the recovery rate of the ionic liquid is 99.4 percent. After adsorption saturation, regeneration is carried out by 0.3mol/L hydrochloric acid solution, ICP analysis is carried out on the regenerated solution, and desorption efficiency is determined.
Example 5
This example provides a method for effectively removing metal ions from an ionic liquid water system, where the ionic liquid to be recovered in an ionic liquid aqueous solution is 1-butyl-3 methylimidazolium chloride, the mass fraction of which is 10%, and the impurity ions are Ca2+And Mg2+The concentrations were all 100 mg/L. The method comprises the following specific steps: introducing the ionic liquid aqueous solution into an adsorption tower filled with a sodium X molecular sieve at the flow rate of 10BV/h, and carrying out ICP and ultraviolet spectrophotometer analysis on the effluent to determine the removal efficiency of metal ions and the loss condition of the ionic liquid. And distilling the effluent for 5 hours under the conditions of 120 ℃ and 300Pa to finally obtain the 1-butyl-3 methylimidazolium chloride with the water mass content of 1.0 percent, wherein the recovery rate of the ionic liquid is 99.4 percent. After saturation of the adsorption, the solution was regenerated with a 0.2mol/L hydrochloric acid solution, and the regenerated solution was subjected to ICP analysis to determine the desorption efficiency, and the results are shown in the following table.
| Adsorption rate | Example 1 | Example 2 | Example 3 | Example 4 | Example 5 |
| Na+ | - | - | 87.2％ | - | - |
| K+ | - | 98.8％ | - | 98.2％ | - |
| Ca2+ | 98.5％ | 97.5％ | 97.0％ | 98.3％ | 99.2％ |
| Mg2+ | 99.2％ | 99.4％ | 98.4％ | 98.7％ | 99.1％ |
| Fe3+ | 98.5％ | 99.2％ | 98.2％ | - | - |
| Cu2+ | 99.2％ | - | 98.6％ | - | - |
| Zn2+ | - | 99.4％ | 99.1％ | - | - |
| Ionic liquids | <0.05％ | <0.05％ | <0.05％ | <0.05％ | <0.05％ |
| Efficiency of desorption | Example 1 | Example 2 | Example 3 | Example 4 | Example 5 |
| Na+ | - | - | 95.7％ | - | - |
| K+ | - | 99.2％ | - | 98.7％ | - |
| Ca2+ | 98.7％ | 98.8％ | 99.1％ | 98.9％ | 97.8％ |
| Mg2+ | 98.2％ | 98.5％ | 98.8％ | 99.2％ | 98.3％ |
| Fe3+ | 97.5％ | 98.7％ | 98.5％ | - | - |
| Cu2+ | 98.5％ | - | 98.6％ | - | - |
| Zn2+ | - | 98.6％ | 99.2％ | - | - |
The embodiment of the invention shown and described above, or the technical scheme of the attached drawings, all represent the process for recovering ionic liquid in an ionic liquid aqueous solution system of the invention. It will be understood that modifications and variations are possible to those skilled in the art in light of the above teachings and all such modifications and variations are intended to be included within the scope of the appended claims.
Claims (7)
1. A method for effectively removing metal ions in an ionic liquid water system is characterized in that an ionic liquid water solution containing metal ion impurities is introduced into an adsorption tower filled with an adsorbent to remove inorganic metal ions, an effluent liquid is subjected to high-temperature reduced pressure distillation to realize dehydration of the ionic liquid until the moisture is qualified, and desorption liquid dilute hydrochloric acid is introduced into the adsorption tower after adsorption saturation for regeneration and recycling.
2. The method of claim 1 for the effective removal of metal ions from an aqueous ionic liquid system, wherein: the ionic liquid is one or more of alkyl imidazole salt, alkyl pyridinium salt, alkyl quaternary ammonium salt and alkyl quaternary phosphonium salt, wherein the carbon number of the alkyl is 1-10.
3. The method of claim 1 for the effective removal of metal ions from an aqueous ionic liquid system, wherein: the mass concentration of the ionic liquid in the ionic liquid aqueous solution is 1-10%.
4. The method of claim 1 for the effective removal of metal ions from an aqueous ionic liquid system, wherein: the inorganic impurity metal ion species is Na+、K+、Ca2+、Mg2+、Fe3+、Cu2+、Zn2+One or more of them, the mass concentration is 10-200 mg/L.
5. The method of claim 1 for the effective removal of metal ions from an aqueous ionic liquid system, wherein: the metal ion adsorbent is one or more of artificial zeolite, 4A molecular sieve, 5A molecular sieve and sodium X molecular sieve.
6. The method of claim 1 for the effective removal of metal ions from an aqueous ionic liquid system, wherein: the temperature of the high-temperature reduced pressure distillation is 90-120 ℃, and the pressure is 10-1000 Pa.
7. The method of claim 1 for the effective removal of metal ions from an aqueous ionic liquid system, wherein: the concentration of the dilute hydrochloric acid is 0.1-0.5 mol/L.
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Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101664608A (en) * | 2009-09-29 | 2010-03-10 | 东华大学 | Method for purifying hydrophilic ionic liquid |
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