CN109865313A - A kind of method of trace water in removal ionic liquid - Google Patents
A kind of method of trace water in removal ionic liquid Download PDFInfo
- Publication number
- CN109865313A CN109865313A CN201711259342.5A CN201711259342A CN109865313A CN 109865313 A CN109865313 A CN 109865313A CN 201711259342 A CN201711259342 A CN 201711259342A CN 109865313 A CN109865313 A CN 109865313A
- Authority
- CN
- China
- Prior art keywords
- molecular sieve
- ionic liquid
- water
- removal
- trace water
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 title claims abstract description 45
- 239000002608 ionic liquid Substances 0.000 title claims abstract description 36
- 238000000034 method Methods 0.000 title claims abstract description 21
- 239000002808 molecular sieve Substances 0.000 claims abstract description 40
- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 claims abstract description 40
- 238000001914 filtration Methods 0.000 claims abstract description 12
- 239000007788 liquid Substances 0.000 claims abstract description 5
- 230000003068 static effect Effects 0.000 abstract description 5
- 239000008236 heating water Substances 0.000 abstract description 3
- 239000012299 nitrogen atmosphere Substances 0.000 abstract description 3
- 238000001035 drying Methods 0.000 abstract 1
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 6
- 239000003792 electrolyte Substances 0.000 description 6
- 229910001416 lithium ion Inorganic materials 0.000 description 6
- 238000010438 heat treatment Methods 0.000 description 4
- 150000003839 salts Chemical class 0.000 description 3
- 239000002904 solvent Substances 0.000 description 3
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 2
- 239000000654 additive Substances 0.000 description 2
- 229910000323 aluminium silicate Inorganic materials 0.000 description 2
- 229910052593 corundum Inorganic materials 0.000 description 2
- 239000010431 corundum Substances 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 description 2
- 238000004146 energy storage Methods 0.000 description 2
- 238000001704 evaporation Methods 0.000 description 2
- 230000008020 evaporation Effects 0.000 description 2
- 238000001179 sorption measurement Methods 0.000 description 2
- QGHDLJAZIIFENW-UHFFFAOYSA-N 4-[1,1,1,3,3,3-hexafluoro-2-(4-hydroxy-3-prop-2-enylphenyl)propan-2-yl]-2-prop-2-enylphenol Chemical group C1=C(CC=C)C(O)=CC=C1C(C(F)(F)F)(C(F)(F)F)C1=CC=C(O)C(CC=C)=C1 QGHDLJAZIIFENW-UHFFFAOYSA-N 0.000 description 1
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 description 1
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 1
- 229910019142 PO4 Inorganic materials 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 125000004122 cyclic group Chemical group 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 238000002242 deionisation method Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 150000002148 esters Chemical class 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 229910052744 lithium Inorganic materials 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000011259 mixed solution Substances 0.000 description 1
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 description 1
- 239000010452 phosphate Substances 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
Abstract
The present invention relates to the methods of trace water in water removal techniques field, especially removal ionic liquid.Successively the following steps are included: (1) is by molecular sieve, drying removes water this method at high temperature；(2) molecular sieve is sent into the ionic liquid prepared in glove box；(3) after molecular sieve being stood filtering, lower clear liquid is the ionic liquid for removing trace water.The invention is by putting into after molecular sieve high-temperature heating water removal in the ionic liquid protected under nitrogen atmosphere after static water removal, filtering can remove trace water in ionic liquid.
Description
Technical field
The present invention relates to the methods of trace water in water removal techniques field, especially removal ionic liquid.
Background technique
Demand with people to energy storage is increasingly strong, and lithium ion battery is by environmental protection, efficient, safety, specific energy density
The advantages such as high, easy to carry, become the optimal selection of current energy storage technology, however, electrolyte used in current lithium ion battery
Main Salts are that lithium hexafluoro phosphate has the defect for meeting water decomposition, and this requires the carbonate solvents in lithium-ion battery electrolytes
And in other additives water ratio not above 20ppm.At present the primary solvent of lithium-ion battery electrolytes be it is cyclic annular or
The mixed solution of the carbonic ester of chain, however, the defects of carbonats compound tool is inflammable, and electrochemical window is narrow, ionic liquid
Because its is non-ignitable, the advantages such as electrochemical window mouth width are expected to add as the substitution ingredient of electrolyte solvent or as additive
Into lithium-ion battery electrolytes.Though ionic liquid is as low temperature molten salt, not soluble in water, in the process for preparing and cleaning
In, the water content in ionic liquid is far beyond limit needed for lithium-ion battery electrolytes.Therefore, it is necessary to in ionic liquid
Trace water is removed, however, being unable to reach the purpose of removal trace water by the methods of heating evaporation at present.
Summary of the invention
In order to overcome the shortcomings of that the methods of existing heating evaporation can not eliminate trace water, the present invention provides remove deionization
The method of trace water in liquid.
The technical solution adopted by the present invention to solve the technical problems is: a kind of side removing trace water in ionic liquid
Method, this method successively the following steps are included:
(1) by molecular sieve dry water removal at high temperature；
(2) molecular sieve is sent into the ionic liquid prepared in glove box；
(3) after molecular sieve being stood filtering, lower clear liquid is the ionic liquid for removing trace water.
It according to another embodiment of the invention, further comprise that the molecular sieve divides for 3A molecular sieve, 4A molecular sieve, 5A
Son sieve, 13X molecular sieve are one such or several.
It according to another embodiment of the invention, further comprise the dry temperature for removing water of the molecular sieve is 400~600 DEG C
Between.
It according to another embodiment of the invention, further comprise the molecular sieve dry water removal time is 1~24 hour.
It according to another embodiment of the invention, further comprise that stand filtration time be 1~48 hour for the molecular sieve.
The invention has the advantages that the invention is by putting into after molecular sieve high-temperature heating water removal in nitrogen atmosphere
It encloses in the ionic liquid of lower protection after static water removal, filtering can remove trace water in ionic liquid.
Specific embodiment
A kind of method of trace water in removal ionic liquid, this method successively the following steps are included:
(1) by molecular sieve dry water removal at high temperature；
(2) molecular sieve is sent into the ionic liquid prepared in glove box；
(3) after molecular sieve being stood filtering, lower clear liquid is the ionic liquid for removing trace water.
The molecular sieve is that 3A molecular sieve, 4A molecular sieve, 5A molecular sieve, 13X molecular sieve are one such or several.It is described
The dry temperature for removing water of molecular sieve is between 400~600 DEG C.The molecular sieve dry water removal time is 1~24 hour.The molecule
It is 1~48 hour that sieve, which stands filtration time,.
There are very strong polarity and Coulombian field inside molecular sieve crystal hole, to polar molecule (such as water) and unsaturated molecule table
Reveal strong adsorption capacity.The pore-size distribution of molecular sieve is very uniform, and only molecular diameter is less than the substance of hole diameter
Inside the bug hole of molecular sieve, the molecular diameter of water is about in 0.4nm or so, and ionic liquid is as fuse salt,
The diameter of zwitterion is far longer than the diameter of hydrone, therefore, if the diameter of molecular sieve is greater than the diameter of hydrone, is less than
The diameter of ionic liquid zwitterion can be by hydrone by the high specific surface area of molecular sieve and extremely strong adsorption capacity
It is fully imbibed into inside molecular sieve bore diameter, meanwhile, ionic liquid is unaffected.
Embodiment 1
Each 40 grams of alumino-silicate of 4A and 5A are weighed, are contained in corundum crucible, it is small to be put into the interior heating 11 at 570 DEG C of Muffle furnace
When, it is then transferred into glove box, puts into the 400ml ionic liquid being placed in glove box, static 30 hours, filtering, i.e.,
It can get the ionic liquid without trace water.
Embodiment 2
Each 60 grams of alumino-silicate of 4A and 5A are weighed, are contained in corundum crucible, it is small to be put into the interior heating 13 at 580 DEG C of Muffle furnace
When, it is then transferred into glove box, puts into the 600ml ionic liquid being placed in glove box, static 32 hours, filtering, i.e.,
It can get the ionic liquid without trace water.
The invention is by putting into after molecular sieve high-temperature heating water removal in the ionic liquid protected under nitrogen atmosphere
After static water removal, filtering can remove trace water in ionic liquid.
Claims (5)
1. it is a kind of removal ionic liquid in trace water method, characterized in that this method successively the following steps are included:
(1) by molecular sieve dry water removal at high temperature；
(2) molecular sieve is sent into the ionic liquid prepared in glove box；
(3) after molecular sieve being stood filtering, lower clear liquid is the ionic liquid for removing trace water.
2. the method for trace water in removal ionic liquid according to claim 1, characterized in that the molecular sieve is 3A points
Sub- sieve, 4A molecular sieve, 5A molecular sieve, 13X molecular sieve are one such or several.
3. the method for trace water in removal ionic liquid according to claim 1 or 2, characterized in that the molecular sieve is dry
Dry temperature for removing water is between 400~600 DEG C.
4. the method for trace water in removal ionic liquid according to claim 1 or 2, characterized in that the molecular sieve is dry
The dry water removal time is 1~24 hour.
5. the method for trace water in removal ionic liquid according to claim 1, characterized in that the molecular sieve was stood
Filtering the time is 1~48 hour.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201711259342.5A CN109865313A (en) | 2017-12-04 | 2017-12-04 | A kind of method of trace water in removal ionic liquid |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201711259342.5A CN109865313A (en) | 2017-12-04 | 2017-12-04 | A kind of method of trace water in removal ionic liquid |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN109865313A true CN109865313A (en) | 2019-06-11 |
Family
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201711259342.5A Pending CN109865313A (en) | 2017-12-04 | 2017-12-04 | A kind of method of trace water in removal ionic liquid |
Country Status (1)
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112707866A (en) * | 2019-10-25 | 2021-04-27 | 中国石油化工股份有限公司 | Dewatering method for ionic liquid alcohol solution |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4528281A (en) * | 1983-03-16 | 1985-07-09 | Calgon Carbon Corporation | Carbon molecular sieves and a process for their preparation and use |
| RU2176155C2 (en) * | 1998-06-09 | 2001-11-27 | Юоп | Method of removing ions of contaminating metals from flows of liquids |
| CN102180456A (en) * | 2011-03-08 | 2011-09-14 | 江苏九九久科技股份有限公司 | Method for purifying lithium hexafluorophosphate and special device thereof |
| CN104436752A (en) * | 2014-11-26 | 2015-03-25 | 林州市科能材料科技有限公司 | Dehydration process for mixed ionic liquid |
| CN106384841A (en) * | 2016-11-17 | 2017-02-08 | 上海应用技术大学 | Method for enhancing utilization ratio of electrolyte in lithium ion battery |
-
2017
- 2017-12-04 CN CN201711259342.5A patent/CN109865313A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4528281A (en) * | 1983-03-16 | 1985-07-09 | Calgon Carbon Corporation | Carbon molecular sieves and a process for their preparation and use |
| RU2176155C2 (en) * | 1998-06-09 | 2001-11-27 | Юоп | Method of removing ions of contaminating metals from flows of liquids |
| CN102180456A (en) * | 2011-03-08 | 2011-09-14 | 江苏九九久科技股份有限公司 | Method for purifying lithium hexafluorophosphate and special device thereof |
| CN104436752A (en) * | 2014-11-26 | 2015-03-25 | 林州市科能材料科技有限公司 | Dehydration process for mixed ionic liquid |
| CN106384841A (en) * | 2016-11-17 | 2017-02-08 | 上海应用技术大学 | Method for enhancing utilization ratio of electrolyte in lithium ion battery |
Non-Patent Citations (3)
| Title |
|---|
| 邢淑建;臧甲忠;刘伟;刘冠锋;孙春晖;于海斌;: "分子筛吸附剂的工业应用研究进展" * |
| 马光耀等: "电解液纯化对锂离子电池负极电化学性能影响" * |
| 黄文煌,严玉顺,万春荣,王建武: "锂化分子筛的制备和应用研究" * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112707866A (en) * | 2019-10-25 | 2021-04-27 | 中国石油化工股份有限公司 | Dewatering method for ionic liquid alcohol solution |
| 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 |
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Application publication date: 20190611 |