CN104436752B - A kind of mixed type ionic liquid dewatering process - Google Patents
A kind of mixed type ionic liquid dewatering process Download PDFInfo
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- CN104436752B CN104436752B CN201410688952.7A CN201410688952A CN104436752B CN 104436752 B CN104436752 B CN 104436752B CN 201410688952 A CN201410688952 A CN 201410688952A CN 104436752 B CN104436752 B CN 104436752B
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Abstract
A kind of mixed type ionic liquid dewatering process, take following steps: in rectifying column, 1. fill solid to dewater filler mixture, described solid dewater that filler mixture is aluminium oxide, active carbon and the sorbing material NSUL-1 mixture that forms of 3:0.5-1:0.5-1 in mass ratio; 2. under nitrogen protection the ionic liquid in raw material fluid reservoir is passed in rectifying column, keep Rectification column pressure 0.1-2.0MPa, temperature 80-100 DEG C; 3., after the water content≤20ppm of ionic liquid, dried ionic liquid is squeezed into dry products fluid reservoir.Relative to prior art, the present invention can remove the micro-moisture in ionic liquid fast, and in the ionic liquid obtained, water content can reach below 20ppm, meets the downstream higher to water content requirement and uses.
Description
Technical field
The present invention relates to a kind of industrial water-eliminating method, particularly a kind of mixed type ionic liquid dewatering process.
Background technology
Ionic liquid, is also called ionic liquid, ionic fluid or normal temperature molten salts, is the fused salt combined by cation and anion.The feature of ionic liquid is in liquid condition in the wide temperature range of-50 ~ 400 DEG C, and the existing multiple fused salt in liquid condition under room temperature (25 DEG C) is known.
Except being in the feature of liquid condition in wide temperature range, ionic liquid also have vapour pressure extremely low and present fixedness, there is good heat endurance and electrochemical stability, the low and ionic conductivity high of viscosity.Utilize these features, ionic liquid is applied to dissolving in the electronic device of electrolyte or electrolyte solution composition, DSSC, fuel cell, lithium rechargeable battery and double layer capacitor etc.
As mentioned above, ionic liquid is the fused salt that cation and anion combine, only to become perfect condition by cation and anionic group.But the trace impurity in practice, containing such as water etc. in ionic liquid.These impurity are mainly mixed into when the synthesis of ionic liquid, have a significant impact the ionic liquid prepared.Time such as, in ionic liquid containing moisture, moisture contained in ionic liquid can cause degradation under viscosity of il, has an impact to ionic liquid physical property.In addition, when using ionic liquid as electrolyte, easily producing accessory substance, is the reason causing product deterioration.Water in ionic liquid often makes transition-metal catalyst inactivation, and water may participate in reaction.In addition, minor amount of water can make some ionic liquid decompose in a heated condition.Therefore in ionic liquid, the control of water content is also an important indicator of ionic liquid purifying and quality control.
In order to remove the moisture in ionic liquid, known water-eliminating method carries out vacuum drying under the condition of high vacuum and high temperature, and carry out adsorption dewatering with phosphorus pentoxide, silica gel or aluminium oxide etc.But there is no a kind of ionic liquid dewatering process efficiently.
Summary of the invention
The invention provides a kind of mixed type ionic liquid dewatering process, traditional handicraft be solved the low problem of water rem oval is carried out to ionic liquid.
The object of the invention is to realize in the following manner:
A kind of mixed type ionic liquid dewatering process, take following steps: in rectifying column, 1. fill solid to dewater filler mixture, described solid dewater that filler mixture is aluminium oxide, active carbon and the sorbing material NSUL-1 mixture that forms of 3:0.5-1:0.5-1 in mass ratio; 2. under nitrogen protection the ionic liquid in raw material fluid reservoir is passed in rectifying column, keep Rectification column pressure 1.0-2.0MPa, temperature 80-100 DEG C; 3., after the water content≤20ppm of ionic liquid, dried ionic liquid is squeezed into dry products fluid reservoir.
Described ionic liquid enters at the bottom of rectifying tower, ejects from rectifying tower.
Described rectifying column outlet connects filter.
Described rectifying column has chuck layer.
Described rectifying column, raw material fluid reservoir and dry products fluid reservoir are 316 stainless steels.
Described ionic liquid is that any two kinds in imidazolium ionic liquid, trifluoromethyl sulfonyl ionic liquid, difluoro oxalate boronate ionic liquid and tetrafluoro boric acid base ionic liquid mix by weight 1:1.
Relative to prior art, the present invention can remove the micro-moisture in ionic liquid fast, and in the ionic liquid obtained, water content can reach below 20ppm, meets the downstream higher to water content requirement and uses.
Accompanying drawing explanation
Fig. 1 is process chart of the present invention.
Wherein, 1 is raw material fluid reservoir, and 2 is membrane pumps, and 3 is rectifying columns, and 4 is dry products fluid reservoirs.
Detailed description of the invention
Processing step of the present invention is as follows: in rectifying column 3,1. fill solid to dewater filler mixture, wherein solid dewater that filler mixture is aluminium oxide, active carbon and the sorbing material NSUL-1 mixture that forms of 3:0.5-1:0.5-1 in mass ratio; The dewater cumulative volume of filler mixture of above-mentioned solid is 2/3 of rectifying column 3 volume; 2. under nitrogen protection the ionic liquid in raw material fluid reservoir 1 is passed in rectifying column 3, keep rectifying column 3 pressure 1.0-2.0MPa, temperature 80-100 DEG C; 3., after the water content≤20ppm of ionic liquid, dried ionic liquid is squeezed into dry products fluid reservoir 4.Ionic liquid enters at the bottom of rectifying column 3 tower, goes out from rectifying column 3 tower top.Rectifying column 3 exports and connects filter.Described rectifying column has chuck layer, and installs thermometer, Pressure gauge.Rectifying column 3, raw material fluid reservoir 1 and dry products fluid reservoir 4 is 316 stainless steels.The all pipelines connected are 316 or 304 stainless steels.Ionic liquid is that any two kinds in imidazolium ionic liquid, trifluoromethyl sulfonyl ionic liquid, difluoro oxalate boronate ionic liquid and tetrafluoro boric acid base ionic liquid mix by weight 1:1.
Above-mentioned raw materials fluid reservoir 1, rectifying column 3, dry products fluid reservoir 4 can be many covers, are connected between each cover by control valve.
Embodiment 1:
As shown in Figure 1, the present invention uses rectifying column 3 dry mass than being the 1-methyl-2-pi-allyl-3-methylimidazole-bis trifluoromethyl sulfimide salt of 1:1 and the mixture of N-Methyl-N-propyl piperidines-bis trifluoromethyl sulfimide salt.Load solid in rectifying column 3 to dewater filler mixture, wherein solid dewater that filler mixture is aluminium oxide, active carbon and the sorbing material NSUL-1 mixture that forms of 3:1:1 in mass ratio.Ionic liquid in raw material fluid reservoir 1 is passed in rectifying column 3, makes the pressure of rectifying column 3 remain on 1.0MPa, pass into steam or conduction oil in rectifying column 3 chuck layer, make tower body temperature remain on 80 DEG C; Ionic liquid enters at the bottom of rectifying column, goes out from tower top, when ionic liquid water content≤20ppm being detected, dried ionic liquid is squeezed into dry products fluid reservoir 4.
Comparative example: use phosphorus pentoxide to carry out drying for the mixture of drier to the mass ratio 1-methyl-2-pi-allyl-3-methylimidazole-bis trifluoromethyl sulfimide salt that is 1:1 and N-Methyl-N-propyl piperidines-bis trifluoromethyl sulfimide salt.Compared with embodiment 1, each parameter such as table 2(vides infra) shown in:
As can be seen from the table, obtain the product of identical weight, the present invention is than traditional handicraft except water speed is fast, and drying effect is good.The present invention can remove the micro-moisture in ionic liquid fast, and in the ionic liquid obtained, water content can reach below 20ppm, and traditional handicraft can not reach this technic index.
Above-described is only the preferred embodiment of the present invention, it should be pointed out that for a person skilled in the art, and not departing under general idea prerequisite of the present invention, can also make some changes and improvements, these also should be considered as protection scope of the present invention.
Table 1 embodiment argument table
Table 2 implementation result contrasts
Claims (6)
1. a mixed type ionic liquid dewatering process, it is characterized in that having the following steps: in rectifying column, 1. fill solid to dewater filler mixture, described solid dewater that filler mixture is aluminium oxide, active carbon and the sorbing material NSUL-1 mixture that forms of 3:0.5-1:0.5-1 in mass ratio; 2. under nitrogen protection the ionic liquid in raw material fluid reservoir is passed in rectifying column, keep Rectification column pressure 1.0-2.0MPa, temperature 80-100 DEG C; 3., after the water content≤20ppm of ionic liquid, dried ionic liquid is squeezed into dry products fluid reservoir.
2. mixed type ionic liquid dewatering process according to claim 1, is characterized in that: described ionic liquid enters at the bottom of rectifying tower, ejects from rectifying tower.
3. mixed type ionic liquid dewatering process according to claim 1, is characterized in that: described rectifying column outlet connects filter.
4. mixed type ionic liquid dewatering process according to claim 1, is characterized in that: described rectifying column has chuck layer.
5. mixed type ionic liquid dewatering process according to claim 1, is characterized in that: described rectifying column, raw material fluid reservoir and dry products fluid reservoir are 316 stainless steels.
6. mixed type ionic liquid dewatering process according to claim 1, is characterized in that: described ionic liquid is that any two kinds in imidazolium ionic liquid, trifluoromethyl sulfonyl ionic liquid, difluoro oxalate boronate ionic liquid and tetrafluoro boric acid base ionic liquid mix by weight 1:1.
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| CN109865313A (en) * | 2017-12-04 | 2019-06-11 | 北京市合众创能光电技术有限公司 | A kind of method of trace water in removal ionic liquid |
| CN112707866B (en) * | 2019-10-25 | 2022-11-04 | 中国石油化工股份有限公司 | Dewatering method for ionic liquid alcohol solution |
| CN111675678B (en) * | 2020-06-29 | 2022-06-17 | 国联汽车动力电池研究院有限责任公司 | Deep drying and water removing method for ionic liquid |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1531988A (en) * | 2003-03-25 | 2004-09-29 | 巴斯福股份公司 | Method for purifying or treating ionic liquid by absorption separation |
| CN101679292A (en) * | 2007-06-12 | 2010-03-24 | 日宝化学株式会社 | Ionic liquid and method for producing the same |
| CN102516177A (en) * | 2011-11-24 | 2012-06-27 | 南京大学 | Preparation method for high-purity ionic liquid |
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| ZA200108461B (en) * | 2000-10-27 | 2002-06-06 | Celanese Chem Europe Gmbh | Process of telomerizing conjugated dienes. |
| PT102655B (en) * | 2001-08-06 | 2004-09-30 | Inst De Biolog Ex E Tecnologic | REMOVAL AND RECOVERY OF SOLUTIONS PRESENT IN IONIC LIQUIDS BY PERVAPORATION |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1531988A (en) * | 2003-03-25 | 2004-09-29 | 巴斯福股份公司 | Method for purifying or treating ionic liquid by absorption separation |
| CN101679292A (en) * | 2007-06-12 | 2010-03-24 | 日宝化学株式会社 | Ionic liquid and method for producing the same |
| CN102516177A (en) * | 2011-11-24 | 2012-06-27 | 南京大学 | Preparation method for high-purity ionic liquid |
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