CN114044755B - Decolorization and purification method for ionic liquid - Google Patents
Decolorization and purification method for ionic liquid Download PDFInfo
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- CN114044755B CN114044755B CN202111245968.7A CN202111245968A CN114044755B CN 114044755 B CN114044755 B CN 114044755B CN 202111245968 A CN202111245968 A CN 202111245968A CN 114044755 B CN114044755 B CN 114044755B
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- 239000002608 ionic liquid Substances 0.000 title claims abstract description 147
- 238000000034 method Methods 0.000 title claims abstract description 50
- 238000000746 purification Methods 0.000 title claims abstract description 22
- 238000004042 decolorization Methods 0.000 title claims abstract description 19
- 239000002904 solvent Substances 0.000 claims abstract description 106
- 239000007787 solid Substances 0.000 claims abstract description 50
- 239000012535 impurity Substances 0.000 claims abstract description 34
- 239000012528 membrane Substances 0.000 claims abstract description 32
- 238000001914 filtration Methods 0.000 claims abstract description 20
- 239000000126 substance Substances 0.000 claims abstract description 17
- 238000002156 mixing Methods 0.000 claims abstract description 14
- 238000001704 evaporation Methods 0.000 claims abstract description 10
- 239000000047 product Substances 0.000 claims abstract description 5
- 238000000926 separation method Methods 0.000 claims abstract description 5
- 230000008020 evaporation Effects 0.000 claims abstract description 4
- 239000002245 particle Substances 0.000 claims description 30
- 238000004064 recycling Methods 0.000 claims description 13
- 150000001875 compounds Chemical class 0.000 claims description 11
- 238000005119 centrifugation Methods 0.000 claims description 7
- RAXXELZNTBOGNW-UHFFFAOYSA-N imidazole Natural products C1=CNC=N1 RAXXELZNTBOGNW-UHFFFAOYSA-N 0.000 claims description 6
- 150000001298 alcohols Chemical class 0.000 claims description 2
- 150000002148 esters Chemical class 0.000 claims description 2
- 150000002576 ketones Chemical class 0.000 claims description 2
- 239000011148 porous material Substances 0.000 claims 1
- 239000002994 raw material Substances 0.000 abstract description 2
- 230000000704 physical effect Effects 0.000 abstract 1
- 230000036314 physical performance Effects 0.000 abstract 1
- 239000000243 solution Substances 0.000 description 20
- 239000007788 liquid Substances 0.000 description 16
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 12
- 238000011084 recovery Methods 0.000 description 11
- 239000000203 mixture Substances 0.000 description 8
- 238000005303 weighing Methods 0.000 description 8
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 6
- 238000005086 pumping Methods 0.000 description 6
- 239000003463 adsorbent Substances 0.000 description 4
- 230000001276 controlling effect Effects 0.000 description 4
- 125000004122 cyclic group Chemical group 0.000 description 4
- 238000004321 preservation Methods 0.000 description 4
- 230000001105 regulatory effect Effects 0.000 description 4
- 238000007790 scraping Methods 0.000 description 4
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 description 3
- 238000005374 membrane filtration Methods 0.000 description 3
- 238000010926 purge Methods 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- JUJWROOIHBZHMG-UHFFFAOYSA-N Pyridine Chemical compound C1=CC=NC=C1 JUJWROOIHBZHMG-UHFFFAOYSA-N 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 230000008929 regeneration Effects 0.000 description 2
- 238000011069 regeneration method Methods 0.000 description 2
- 150000003839 salts Chemical class 0.000 description 2
- 239000002910 solid waste Substances 0.000 description 2
- 238000000638 solvent extraction Methods 0.000 description 2
- 238000001179 sorption measurement Methods 0.000 description 2
- RSEBUVRVKCANEP-UHFFFAOYSA-N 2-pyrroline Chemical compound C1CC=CN1 RSEBUVRVKCANEP-UHFFFAOYSA-N 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- FZWLAAWBMGSTSO-UHFFFAOYSA-N Thiazole Chemical compound C1=CSC=N1 FZWLAAWBMGSTSO-UHFFFAOYSA-N 0.000 description 1
- -1 alcohol amine Chemical class 0.000 description 1
- 238000005349 anion exchange Methods 0.000 description 1
- 239000012736 aqueous medium Substances 0.000 description 1
- 239000008346 aqueous phase Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- QRUDEWIWKLJBPS-UHFFFAOYSA-N benzotriazole Chemical compound C1=CC=C2N[N][N]C2=C1 QRUDEWIWKLJBPS-UHFFFAOYSA-N 0.000 description 1
- 239000012964 benzotriazole Substances 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 150000002357 guanidines Chemical class 0.000 description 1
- 150000008282 halocarbons Chemical class 0.000 description 1
- 229930195733 hydrocarbon Natural products 0.000 description 1
- 150000002430 hydrocarbons Chemical class 0.000 description 1
- 239000011261 inert gas Substances 0.000 description 1
- 239000011259 mixed solution Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 150000002825 nitriles Chemical class 0.000 description 1
- 239000012074 organic phase Substances 0.000 description 1
- XYFCBTPGUUZFHI-UHFFFAOYSA-N phosphine group Chemical group P XYFCBTPGUUZFHI-UHFFFAOYSA-N 0.000 description 1
- 229920000768 polyamine Polymers 0.000 description 1
- 230000002035 prolonged effect Effects 0.000 description 1
- UMJSCPRVCHMLSP-UHFFFAOYSA-N pyridine Natural products COC1=CC=CN=C1 UMJSCPRVCHMLSP-UHFFFAOYSA-N 0.000 description 1
- ZVJHJDDKYZXRJI-UHFFFAOYSA-N pyrroline Natural products C1CC=NC1 ZVJHJDDKYZXRJI-UHFFFAOYSA-N 0.000 description 1
- 150000003242 quaternary ammonium salts Chemical class 0.000 description 1
- 230000001172 regenerating effect Effects 0.000 description 1
- 238000007086 side reaction Methods 0.000 description 1
- CBDKQYKMCICBOF-UHFFFAOYSA-N thiazoline Chemical compound C1CN=CS1 CBDKQYKMCICBOF-UHFFFAOYSA-N 0.000 description 1
- 150000003852 triazoles Chemical class 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
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
- 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
- C07F9/11—Esters of phosphoric acids with hydroxyalkyl compounds without further substituents on alkyl
-
- 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
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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)
- Separation Using Semi-Permeable Membranes (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention relates to a high-efficiency decolorization and purification method of ionic liquid, in particular to a novel method for obtaining decolorized and purified ionic liquid by utilizing an added solvent to reduce the viscosity of the ionic liquid and dissolving the ionic liquid into the solvent so that solid impurities and colored substances are easy to centrifugally remove. The method comprises the following steps: firstly preparing a required solvent, mixing the prepared solvent and the ionic liquid at normal pressure and room temperature in a certain mass ratio, separating by adopting a centrifugal separator after mixing, centrifugally separating solid impurities at a certain rotating speed and time, finely filtering the centrifuged solution by a membrane filtering device, conveying the filtered solution into an evaporator, evaporating and separating the solvent at a certain temperature and pressure, and obtaining a decolorized and purified ionic liquid product, wherein the solvent obtained by evaporation and separation can be collected and recycled by a condenser. The ionic liquid decolorization and purification method has the advantages that the raw materials are cheap and easy to obtain, the solvent can be recycled, and the comprehensive cost is effectively reduced. The process is simple and easy to control, the purity and the yield of the ionic liquid are high, and the industrial application is easy. The method can efficiently separate solid impurities and colored substances from the ionic liquid, and the ionic liquid has stable structure, physical properties and performance, realizes decolorization and purification of the ionic liquid, and has wide application prospects in the fields of energy environment, chemistry and chemical industry and pharmacy.
Description
Technical Field
The invention relates to a high-efficiency ionic liquid decoloring and purifying method, in particular to a novel method which can utilize an added solvent to reduce the viscosity of the ionic liquid and dissolve the ionic liquid into the solvent, and can easily centrifugally remove solid impurities and colored substances through centrifugation and fine filtration, thereby obtaining the decoloring and purifying ionic liquid, and the method is particularly suitable for removing the solid impurities and the colored substances in the high-viscosity ionic liquid and has wide application prospects in the fields of energy environment, chemistry and chemical industry and pharmacy.
Background
The ionic liquid has the advantages of stable property, low vapor pressure, difficult volatilization, adjustable structure, functional design, wide range of liquid range, good solubility and good electrochemical performance, and has wide application prospect in the fields of biocatalysis, chemistry and chemical industry, energy environment and the like.
The ionic liquid can be oxidized, carbonized, decomposed or subjected to side reactions and other processes in the long-period industrial use process, so that solid impurities and colored substances can be generated, meanwhile, industrial raw materials in the industrial use process can also introduce impurities, the impurities in the ionic liquid can be increased due to long-period operation, the color deepening purity of the ionic liquid is reduced, the performance of the ionic liquid is directly influenced by the purity of the ionic liquid, particularly, the viscosity of the ionic liquid is increased when the solid content reaches a certain amount, the fluidity of the ionic liquid is influenced, the pressure drop of an industrial pipeline is increased, and the pipeline is easily blocked if the purification treatment is not performed for a long time, so that the decolorization and purification of the ionic liquid are particularly important. Compared with the traditional solvent, the ionic liquid has higher cost, the ionic liquid can be regenerated through the decolorization and purification process, the service life of the ionic liquid is prolonged, the recycling rate of the ionic liquid is improved, and the running cost is greatly reduced.
The current methods for decoloring and purifying ionic liquid mainly comprise an adsorption method (CN 201310100513.5), a purging method (CN 201010299353.8) and a solvent extraction method (CN 201610774246.3). The adsorption method adopts adsorbents such as diatomite, active carbon and the like to filter impurities in the ionic liquid and adsorb colored substances, the adsorbents in the method generally have a porous structure, so that not only can the impurities be adsorbed, but also a small amount of ionic liquid can be adsorbed, thereby causing the loss of the ionic liquid, and the used adsorbents become solid wastes if the used adsorbents cannot be recycled, so that the solid wastes are more difficult to treat than waste liquid, and secondary pollution is easy to cause. The purging method mainly utilizes inert gas to purge the ionic liquid so as to remove volatile impurities in the ionic liquid, and the method can only remove the volatile impurities contained in the ionic liquid and cannot be used for removing solid impurities and colored impurities in the ionic liquid. The extraction method is to extract the ionic liquid into the solvent by utilizing the principle of similar compatibility, finally separating the ionic liquid from insoluble impurity particles, the application number is CN201610774246.3, purifying the ionic liquid by adopting the solvent extraction method, firstly carrying out anion exchange reaction in an aqueous medium, then adding an organic extractant, standing for layering after mixing uniformly, discharging a lower aqueous phase, adding pure water and salt into an upper organic phase, and repeatedly adding the pure water and the salt for 2-3 times until the impurities are completely removed to obtain the product. The ionic liquid has the advantages that the solid impurities and the colored substances in the ionic liquid are removed with extremely low efficiency by directly adopting a filtering method due to the fact that the viscosity of the ionic liquid is high, and the novel method for decoloring and purifying the ionic liquid is provided, and particularly the decoloring and purifying method for removing the solid impurities and the colored substances in the ionic liquid is provided.
Disclosure of Invention
Aiming at the technical requirements of decolorization and purification of ionic liquid, the invention aims to provide a decolorization and purification method which has the advantages of simple process, high ionic liquid purity and yield, low comprehensive cost, rapidness and high efficiency and recyclable solvent.
The method adopts cheap and easily available solvents to separate solid impurities and colored substances in the ionic liquid, can not only highly purify the ionic liquid, but also has good decolorization effect, and can realize industrial application of decolorization and purification of the ionic liquid at low cost.
Specifically, the invention is realized by the following technical scheme:
the method is a new method for reducing the viscosity of the ionic liquid by using an added solvent and dissolving the ionic liquid into the solvent, and the solid impurities and the colored substances are easy to centrifugally remove by centrifugation and fine filtration, so that the decolorized and purified ionic liquid is obtained.
The invention comprises the following steps: firstly preparing a required solvent, mixing the prepared solvent and the ionic liquid at normal pressure and room temperature in a certain mass ratio, separating by adopting a centrifugal separator after mixing, centrifugally separating solid impurities at a certain rotating speed and time, finely filtering the centrifuged solution by a membrane filtering device, conveying the filtered solution into an evaporator, evaporating and separating the solvent at a certain temperature and pressure, and obtaining a decolorized and purified ionic liquid product, wherein the solvent obtained by evaporation and separation can be collected and recycled by a condenser.
The ionic liquid provided by the invention comprises guanidine salt ionic liquid, alcohol amine ionic liquid, imidazole ionic liquid, quaternary ammonium salt ionic liquid, pyridine ionic liquid, thiazole ionic liquid, polyamine ionic liquid, quaternary phosphine salt ionic liquid, triazole ionic liquid, pyrroline ionic liquid, thiazoline ionic liquid and benzotriazole ionic liquid.
The solvent is one or more of water, esters, ketones, alcohols, halogenated hydrocarbons, hydrocarbons and nitrile solvents.
After the solid impurities, the colored impurities and the solvent in the ionic liquid are mixed, solid particles or flocculent solid matters are formed, and the size of the solid particles or flocculent solid matters is 10 nm-1.0 mm.
The mass ratio of the solvent to the ionic liquid is in the range of 1:10 to 50:1, and the optimal range is 1:5 to 20:1..
The centrifugal rotational speed of the centrifugal separator is 1000-10000 rad/min.
The aperture of the filter membrane of the membrane filter device is 5 nm-10 mu m.
The evaporator is a direct contact heat transfer evaporator, a once-through evaporator and a circulating evaporator, the evaporation temperature is 20-150 ℃, and the pressure is-0.1 MPa.
The condenser of the invention is as follows: water-cooled, air-cooled and evaporative, the condensing temperature is-20-40 ℃.
The beneficial effects of the invention are as follows:
(1) Compared with the prior art and method, the ionic liquid recovered by the decolorization and purification method of the ionic liquid has high purity and yield, the purity of the ionic liquid after centrifugation can reach more than 99.5%, the purity of the ionic liquid after centrifugation can reach more than 99.8% after the micro-impurity is removed by fine filtration, the recovery rate of the ionic liquid can reach more than 99.6%, and the decolorization and purification can be performed especially for the ionic liquid with higher viscosity, so that the decolorization and purification method of the ionic liquid has wide application prospect in the fields of chemical industry, petrochemical industry and pharmacy.
(2) Compared with the prior art and the method, the decolorization and purification method of the ionic liquid has the characteristics that the used solvent is low in cost and easy to obtain, the solvent can be recycled, and the comprehensive cost is low.
(3) Compared with the prior art and the method, the decolorization and purification method of the ionic liquid has the advantages of simple process, high speed and high efficiency, shortened purification time and easy industrial application.
Therefore, the method for decoloring and purifying the ionic liquid can solve the industrial application problem that solid impurities and colored substances in the ionic liquid with larger viscosity are difficult to remove, can improve the purity of the ionic liquid, can decolor the ionic liquid, can recycle and reutilize both the solvent and the ionic liquid, and realizes resource utilization.
Drawings
FIG. 1 is a schematic view of the process flow of the present invention
The drawings of the drawings are described as follows:
wherein: 1-a centrifugal separator; 2-a liquid storage tank with a jacket; 3-gear pump; 4-primary membrane filtration; 5-second-stage membrane filtration; 6-three-stage membrane filtration; 7, a heat preservation liquid storage tank; 8-a metering pump; 9-an evaporator; 10-high and low temperature control equipment; 11-a first stage condenser; a 12-second stage condenser; 13-a solvent collection tank; 14-a dry vacuum pump; 15-solvent tank
The decoloring and purifying process of the ionic liquid mainly comprises three parts of a centrifugal separation unit, a membrane filtering and purifying unit and a solvent regenerating unit. The specific operation flow is that firstly, the ionic liquid and the solvent are pumped into a jacketed liquid storage tank 2 according to a certain proportion and are mixed, the mixture is conveyed into a centrifugal separator 1 through a gear pump 3, more than 99.5% of solid impurity particles in the ionic liquid are separated through centrifugation, the primarily separated ionic liquid and solvent are sequentially conveyed into a primary membrane filter 4, a secondary membrane filter 5 and a tertiary membrane filter 6 through the gear pump 3 to filter out trace solid particles, the filtered solution is conveyed into a heat preservation liquid storage tank 7 through a pipeline and is conveyed into an evaporator 9 through a metering pump 8, the system operation pressure is regulated and controlled by a dry vacuum pump 14, the temperature is controlled by a high-low temperature control device 10, the solvent is evaporated under a certain temperature and pressure, and the obtained product is the decolorized and purified ionic liquid which can be pumped into an industrial device again. The evaporated solvent is condensed by a first-stage condenser 11 and a second-stage condenser 12 in sequence, the solvent recovered by two-stage condensation is pumped into a jacketed solvent tank 2 from a solvent tank 15 and a solvent collecting tank 13 for cyclic utilization, and the solvent is continuously purified and regenerated by the ionic liquid after being compounded with the ionic liquid to be treated in the next batch, so that the cyclic utilization of the solvent is realized.
Detailed Description
The present invention will be further described with reference to the following examples, but the present invention is not limited to the following examples, and various modifications are possible within the technical scope of the present invention without departing from the spirit and scope of the present invention.
Example 1:
respectively weighing 5kg of methanol and 5kg of ethanol, mixing to prepare a compound solvent, and weighing BmimNO 3 2kg of ionic liquid and 10kg of prepared compound solvent are mixed and pumped into the beltIn a jacketed liquid storage tank 2, the mixed solution is conveyed into a centrifugal separator 1 through a gear pump 3 to be centrifugally separated for 15min at the rotating speed of 6000rad/min, 99.6% of solid impurity particles in the ionic liquid are separated through centrifugation, the primarily separated ionic liquid and solvent are conveyed into a primary membrane filter 4 through the gear pump 3 to filter out solid particles with the size of more than 0.45 mu m, the primarily separated ionic liquid and solvent are filtered out of the solid particles with the size of more than 0.22 mu m through a secondary membrane filter 5, the solid particles with the size of more than 0.1 mu m are filtered out through a tertiary membrane filter 6, the filtered solution is conveyed into a heat-preserving liquid storage tank 7 through a pipeline, and then conveyed into a scraping membrane evaporator 9 through a metering pump 8, the system operation pressure is regulated and controlled by a dry vacuum pump 14, the temperature is controlled by a high-low temperature control device 10, the temperature is 50 ℃, the pressure is-1.0 MPa, the solution is evaporated for 20min, the remained solution is the decolorized and purified ionic liquid, the evaporated solution is pumped into an industrial device again, the solvent is condensed out through a primary tube condenser 11 with the temperature of 10 ℃ and a secondary solvent condenser with the temperature of 5 ℃ and is further conveyed into a secondary solvent evaporator with a circulating tank 12 with the aid of the secondary solvent tank 13, and the circulating pump is recycled from the circulating solvent tank 13, and the circulating solvent is recycled through the circulating tank is further purified by the circulating pump 13. The recovery rate of the obtained ionic liquid is 99.6%, the purity of the ionic liquid is 99.9%, and the recovery rate of the solvent is 99.5%.
Example 2:
respectively weighing 12kg of isopropanol and 2kg of EmimDEP ionic liquid, pumping the isopropanol and the EmimDEP ionic liquid into a jacketed liquid storage tank 2, conveying the mixture into a centrifugal separator 1 through a gear pump 3, centrifugally separating the mixture for 12min at a rotating speed of 7000rad/min, centrifugally separating 99.5% of solid impurity particles in the ionic liquid, conveying the primarily separated ionic liquid and solvent into a first-stage membrane filter 4 through the gear pump 3 to filter out solid particles with the size of more than 0.45 mu m, filtering the solid particles with a second-stage membrane filter 5 to filter out solid particles with the size of more than 0.22 mu m, conveying the filtered solution into a heat-preserving liquid storage tank 7 through a three-stage membrane filter 6 to filter out solid particles with the size of more than 0.1 mu m, conveying the filtered solution into a scraping membrane evaporator 9 through a metering pump 8, controlling the system operating pressure by a dry vacuum pump 14, controlling the temperature by a high-low temperature control device 10, heating the solvent at the temperature of 55 ℃ for 20min under the pressure of-1.0 MPa, evaporating the solvent to obtain the remained solution, and re-pumping the solution into an industrial device, recycling the industrial device, conveying the solution into a first-stage solvent storage tank 11 through a condensing tube with the temperature of the solvent storage tank 11 and a circulating pump 11 at the temperature of the solvent storage tank 13, recycling the solvent storage tank to be recycled by the solvent storage tank 11, and recycling the solvent storage tank is realized. The recovery rate of the obtained ionic liquid is 99.7%, the purity of the ionic liquid is 99.9%, and the recovery rate of the solvent is 99.6%.
Example 3:
respectively weighing 5kg of methanol and isopropanol, mixing to prepare a compound solvent, weighing 2kg of BmimSCN ionic liquid and 10kg of prepared compound solvent, pumping into a jacketed liquid storage tank 2, mixing, conveying the mixture into a centrifugal separator 1 through a gear pump 3, centrifugally separating for 15min at a rotating speed of 5500rad/min, centrifugally separating 99.6% of solid impurity particles in the ionic liquid, conveying the ionic liquid and the solvent after preliminary separation into a primary membrane filter 4 through the gear pump 3, filtering solid particles with a size of more than 0.45 mu m, filtering solid particles with a size of more than 0.22 mu m through a secondary membrane filter 5, filtering solid particles with a size of more than 0.1 mu m through a tertiary membrane filter 6, conveying the filtered solution into a heat preservation liquid storage tank 7 through a pipeline, and then the solution is conveyed into a wiped film evaporator 9 through a metering pump 8, the system operation pressure is regulated and controlled by a dry vacuum pump 14, the temperature is controlled by a high-low temperature control device 10, the temperature is 45 ℃, the pressure is minus 0.08MPa, the compound solvent is evaporated, the remained solution is decolorized and purified ionic liquid, the decolorized and purified ionic liquid can be pumped into an industrial device again, the evaporated solvent is condensed by a primary tubular condenser 11 with the temperature of 5 ℃ and condensed by a secondary tubular condenser 12 with the temperature of 2 ℃, the solvent is pumped into a jacketed solvent tank 2 from a solvent tank 15 and a solvent collecting tank 13 for cyclic utilization, and the purification and regeneration of the ionic liquid are continuously carried out after the compound solvent is compounded with the next batch of ionic liquid to be treated, so that the cyclic utilization of the solvent is realized. The recovery rate of the obtained ionic liquid is 99.8%, the purity of the ionic liquid is 99.8%, and the recovery rate of the solvent is 99.6%.
Example 4:
the method comprises the steps of weighing 10kg of methanol and 1kg of BmimDCA ionic liquid, pumping the methanol and the BmimDCA ionic liquid into a jacketed liquid storage tank 2, mixing, conveying the mixture into a centrifugal separator 1 through a gear pump 3, centrifugally separating the mixture at a rotating speed of 6000rad/min for 18min, centrifugally separating 99.5% of solid impurity particles in the ionic liquid, conveying the primarily separated ionic liquid and solvent into a primary membrane filter 4 through the gear pump 3 to filter out solid particles with the size of more than 0.45 mu m, filtering the primarily separated ionic liquid and solvent by a secondary membrane filter 5 to filter out solid particles with the size of more than 0.22 mu m, filtering the primarily separated solid particles by a tertiary membrane filter 6 to filter out solid particles with the size of more than 0.1 mu m, conveying the filtered solution into a heat-preserving liquid storage tank 7 through a pipeline, conveying the solution into a scraping membrane evaporator 9 through a metering pump 8, controlling the system operating pressure by a dry vacuum pump 14, controlling the temperature by a high-low temperature control device 10, heating the solvent at 30 ℃ under the pressure of-0.08 MPa for 20min, evaporating the remained solution to obtain decolorized ionic liquid, pumping the decolorized ionic liquid into an industrial device again, recycling the solvent into a secondary membrane filter 2 through a condenser with the temperature of 6 ℃ and a circulating pipe of the secondary solvent collector 11, recycling the solvent from the secondary membrane filter 2, and a circulating the solvent through a circulating pipe 11, and a circulating pipe to a circulating pipe for a recycling the solvent tank for the solvent from the secondary solvent 2 to a recycling tank 13, and a recycling the solvent to a solvent 2, and a recycling tank is realized. The recovery rate of the obtained ionic liquid is 99.7%, the purity of the ionic liquid is 99.8%, and the recovery rate of the solvent is 99.4%.
Example 5:
respectively weighing ethyl acetate and acetone, mixing 6kg each, preparing into compound solvent, and weighing BmimPF 6 Pumping 2kg of ionic liquid and 12kg of prepared compound solvent into a jacketed liquid storage tank 2, mixing, conveying the mixture into a centrifugal separator 1 through a gear pump 3, centrifugally separating the mixture at a rotating speed of 6500rad/min for 20min, centrifugally separating 99.6% of solid impurity particles in the ionic liquid, conveying the primarily separated ionic liquid and solvent into a primary membrane filter 4 through the gear pump 3, filtering out solid particles with a diameter of more than 0.45 mu m, and filtering out solid particles with a diameter of more than 0.22 mu m through a secondary membrane filter 5The solid particles with the particle size of more than 0.1 mu m are filtered out by a three-stage membrane filter 6, the filtered solution is conveyed into a heat preservation liquid storage tank 7 through a pipeline, and then conveyed into a scraping membrane evaporator 9 through a metering pump 8, the system operation pressure is regulated and controlled by a dry vacuum pump 14, the temperature is controlled by a high-low temperature control device 10, the temperature is 60 ℃ and the pressure is minus 1.0MPa, the compound solvent is evaporated, the remained solution is decolorized and purified ionic liquid, the decolorized and purified ionic liquid can be pumped into an industrial device again, the evaporated solvent is condensed by a primary-stage tubular condenser 11 with the temperature of 15 ℃ and a secondary-stage tubular condenser 12 with the temperature of 12 ℃, the solvent is pumped into a jacketed solvent tank 2 from a solvent tank 15 and a solvent collecting tank 13 for recycling, and the purification and regeneration of the ionic liquid are continuously carried out after the compound ionic liquid is compounded with the next batch of ionic liquid to be treated, so that the solvent recycling is realized. The recovery rate of the obtained ionic liquid is 99.6%, the purity of the ionic liquid is 99.8%, and the recovery rate of the solvent is 99.6%.
Claims (4)
1. The decoloring and purifying method for the ionic liquid is characterized by comprising the following steps of: the method is a method for obtaining decolorized and purified ionic liquid by utilizing an added solvent to reduce the viscosity of the ionic liquid and dissolving the ionic liquid into the solvent, and removing solid impurities and colored substances through centrifugation and fine filtration;
the method comprises the following steps: firstly preparing a required solvent, mixing the prepared solvent and the ionic liquid at normal pressure and room temperature in a certain mass ratio, separating by adopting a centrifugal separator after mixing, centrifugally separating solid impurities at a certain rotating speed and time, finely filtering the centrifuged solution by a membrane filtering device, conveying the filtered solution to an evaporator, evaporating and separating the solvent at a certain temperature and pressure to obtain a decolorized and purified ionic liquid product, and collecting, recycling and reusing the solvent obtained by evaporation and separation by a condenser;
the ionic liquid is imidazole ionic liquid, and the solvent is a compound solvent prepared from one or more of esters, ketones or alcohols;
the mass ratio of the solvent to the ionic liquid ranges from 1:5 to 20:1;
after mixing solid impurities, colored substances and solvents in the ionic liquid, forming solid particles or flocculent solid matters, wherein the size of the solid particles or flocculent solid matters is 10 nm-1.0 mm;
the pore diameter of the filter membrane of the membrane filter device is 5 nm-10 mu m.
2. The method for decolorization and purification of an ionic liquid according to claim 1, wherein the centrifugal rotational speed of the centrifugal separator is 1000 to 10000rad/min.
3. The method for decolorization and purification of an ionic liquid according to claim 1, wherein the evaporator is: the evaporator with direct contact heat transfer, the once-through evaporator and the circulating evaporator have the evaporating temperature of 20-150 ℃ and the pressure of-0.1 MPa.
4. The method for decolorization and purification of an ionic liquid according to claim 1, wherein the condenser is: water-cooled, air-cooled and evaporative, the condensing temperature is-20-40 ℃.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102371078A (en) * | 2010-08-10 | 2012-03-14 | 中国科学院过程工程研究所 | Recovery method for ionic liquid solvent generated from homogeneous acylation reaction of cellulose |
| CN108997596A (en) * | 2018-07-09 | 2018-12-14 | 南京林业大学 | A method of from preparing reuse ionic liquid in cellulose nano-fibrous waste liquid |
| CN110387279A (en) * | 2019-07-03 | 2019-10-29 | 北方民族大学 | For removing the recovery method of the hydrophilic ionic liquid of sulphur content in coal |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102371078A (en) * | 2010-08-10 | 2012-03-14 | 中国科学院过程工程研究所 | Recovery method for ionic liquid solvent generated from homogeneous acylation reaction of cellulose |
| CN108997596A (en) * | 2018-07-09 | 2018-12-14 | 南京林业大学 | A method of from preparing reuse ionic liquid in cellulose nano-fibrous waste liquid |
| CN110387279A (en) * | 2019-07-03 | 2019-10-29 | 北方民族大学 | For removing the recovery method of the hydrophilic ionic liquid of sulphur content in coal |
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