CN1551791A - 酸的分离 - Google Patents
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- 150000002148 esters Chemical class 0.000 claims abstract description 13
- -1 phosphonate ester Chemical class 0.000 claims description 12
- 239000002904 solvent Substances 0.000 claims description 12
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- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 8
- 229910052731 fluorine Inorganic materials 0.000 claims description 6
- 125000001153 fluoro group Chemical group F* 0.000 claims description 5
- 239000002516 radical scavenger Substances 0.000 claims description 4
- 229910019142 PO4 Inorganic materials 0.000 claims description 3
- 230000005611 electricity Effects 0.000 claims description 3
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- 238000005868 electrolysis reaction Methods 0.000 claims 1
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- 230000002378 acidificating effect Effects 0.000 abstract 1
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- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 2
- RJUFJBKOKNCXHH-UHFFFAOYSA-N Methyl propionate Chemical compound CCC(=O)OC RJUFJBKOKNCXHH-UHFFFAOYSA-N 0.000 description 2
- 125000000217 alkyl group Chemical group 0.000 description 2
- 125000001118 alkylidene group Chemical group 0.000 description 2
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 2
- BVKZGUZCCUSVTD-UHFFFAOYSA-N carbonic acid Chemical compound OC(O)=O BVKZGUZCCUSVTD-UHFFFAOYSA-N 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 150000005690 diesters Chemical class 0.000 description 2
- 150000002367 halogens Chemical class 0.000 description 2
- 230000007062 hydrolysis Effects 0.000 description 2
- 238000006460 hydrolysis reaction Methods 0.000 description 2
- 229910052744 lithium Inorganic materials 0.000 description 2
- 229910003002 lithium salt Inorganic materials 0.000 description 2
- 159000000002 lithium salts Chemical class 0.000 description 2
- 229940017219 methyl propionate Drugs 0.000 description 2
- 150000007524 organic acids Chemical class 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
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- IUVKMZGDUIUOCP-BTNSXGMBSA-N quinbolone Chemical compound O([C@H]1CC[C@H]2[C@H]3[C@@H]([C@]4(C=CC(=O)C=C4CC3)C)CC[C@@]21C)C1=CCCC1 IUVKMZGDUIUOCP-BTNSXGMBSA-N 0.000 description 2
- 230000035945 sensitivity Effects 0.000 description 2
- DRVMZMGCPWFDBI-UHFFFAOYSA-N 2,2,2-trifluoroethyl dihydrogen phosphate Chemical class OP(O)(=O)OCC(F)(F)F DRVMZMGCPWFDBI-UHFFFAOYSA-N 0.000 description 1
- NOWKCMXCCJGMRR-UHFFFAOYSA-N Aziridine Chemical compound C1CN1 NOWKCMXCCJGMRR-UHFFFAOYSA-N 0.000 description 1
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 description 1
- OFOBLEOULBTSOW-UHFFFAOYSA-L Malonate Chemical compound [O-]C(=O)CC([O-])=O OFOBLEOULBTSOW-UHFFFAOYSA-L 0.000 description 1
- XBDQKXXYIPTUBI-UHFFFAOYSA-M Propionate Chemical compound CCC([O-])=O XBDQKXXYIPTUBI-UHFFFAOYSA-M 0.000 description 1
- 229910004298 SiO 2 Inorganic materials 0.000 description 1
- RHQDFWAXVIIEBN-UHFFFAOYSA-N Trifluoroethanol Chemical compound OCC(F)(F)F RHQDFWAXVIIEBN-UHFFFAOYSA-N 0.000 description 1
- 150000001335 aliphatic alkanes Chemical class 0.000 description 1
- 125000003545 alkoxy group Chemical group 0.000 description 1
- 150000001450 anions Chemical class 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 150000001733 carboxylic acid esters Chemical class 0.000 description 1
- 239000000969 carrier Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- IKDHALVKVCXQQI-UHFFFAOYSA-N difluoro propanedioate Chemical compound FOC(=O)CC(=O)OF IKDHALVKVCXQQI-UHFFFAOYSA-N 0.000 description 1
- BXNKCKFDLBMOTA-UHFFFAOYSA-N dioxol-3-one Chemical compound O=C1C=COO1 BXNKCKFDLBMOTA-UHFFFAOYSA-N 0.000 description 1
- 238000004520 electroporation Methods 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 239000011737 fluorine Substances 0.000 description 1
- 125000003709 fluoroalkyl group Chemical group 0.000 description 1
- 150000002466 imines Chemical class 0.000 description 1
- 150000007522 mineralic acids Chemical class 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- ITMCEJHCFYSIIV-UHFFFAOYSA-N triflic acid Chemical compound OS(=O)(=O)C(F)(F)F ITMCEJHCFYSIIV-UHFFFAOYSA-N 0.000 description 1
Classifications
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D15/00—Separating processes involving the treatment of liquids with solid sorbents; Apparatus therefor
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/30—Processes for preparing, regenerating, or reactivating
- B01J20/32—Impregnating or coating ; Solid sorbent compositions obtained from processes involving impregnating or coating
- B01J20/3231—Impregnating or coating ; Solid sorbent compositions obtained from processes involving impregnating or coating characterised by the coating or impregnating layer
- B01J20/3242—Layers with a functional group, e.g. an affinity material, a ligand, a reactant or a complexing group
- B01J20/3268—Macromolecular compounds
- B01J20/3272—Polymers obtained by reactions otherwise than involving only carbon to carbon unsaturated bonds
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/04—Hybrid capacitors
- H01G11/06—Hybrid capacitors with one of the electrodes allowing ions to be reversibly doped thereinto, e.g. lithium ion capacitors [LIC]
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/54—Electrolytes
- H01G11/58—Liquid electrolytes
- H01G11/62—Liquid electrolytes characterised by the solute, e.g. salts, anions or cations therein
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M6/00—Primary cells; Manufacture thereof
- H01M6/14—Cells with non-aqueous electrolyte
- H01M6/16—Cells with non-aqueous electrolyte with organic electrolyte
- H01M6/162—Cells with non-aqueous electrolyte with organic electrolyte characterised by the electrolyte
- H01M6/164—Cells with non-aqueous electrolyte with organic electrolyte characterised by the electrolyte by the solvent
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/052—Li-accumulators
- H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/056—Accumulators with non-aqueous electrolyte characterised by the materials used as electrolytes, e.g. mixed inorganic/organic electrolytes
- H01M10/0564—Accumulators with non-aqueous electrolyte characterised by the materials used as electrolytes, e.g. mixed inorganic/organic electrolytes the electrolyte being constituted of organic materials only
- H01M10/0566—Liquid materials
- H01M10/0569—Liquid materials characterised by the solvents
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M2300/00—Electrolytes
- H01M2300/0017—Non-aqueous electrolytes
- H01M2300/0025—Organic electrolyte
- H01M2300/0028—Organic electrolyte characterised by the solvent
- H01M2300/0034—Fluorinated solvents
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- 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
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
-
- 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
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/13—Energy storage using capacitors
Abstract
当非质子有机液体与附载载体上的聚亚烷基亚胺接触时，酸可以从这种液体中分离出来。特别适宜的是使用附载在非晶形二氧化硅上的聚亚乙基亚胺。例如可以将酸性成分从氟化的酯中去除。
Description
说明书
本发明涉及一种适用于从非质子有机液体中去除酸的新方法。
有机液体，例如溶剂，可以在制备中或出于其它理由含有酸。碳酸酯和羧酸酯、磷酸酯、膦酸酯或次膦酸酯可以例如被相应的游离酸、HF或HCl污染。通常进一步的无酸化是理想的。这例如是在电池的电解液或电容器使用的溶剂的情形下。
本发明的任务在于，提供一种用于在非质子有机溶剂中去除酸成分的方法，而不污染溶剂，并且是对于碱性水解敏感的物质可使用的。
此任务是通过本发明的方法解决的。根据本发明的方法用于分离被酸污染的非质子、有机液体中的酸，将酸清除剂聚亚烷基亚胺附载于载体上使用。
可使用的例如是聚亚丙基亚胺。优选使用聚亚乙基亚胺，借助这种优选的实施形式进一步阐明本发明。
聚亚乙基亚胺优选附载于氧化的无机载体上，特别优选的载体是非晶形二氧化硅，例如硅胶。
聚亚乙基亚胺的组合物被吸附于所使用的载体上可以用于从非质子有机液体中分离酸。在此可以涉及由制备条件或其它来源造成的有机或无机酸。
用根据本发明的方法制备液体，其具有极少含量(例如小于50ppm)的酸。根据本发明的方法可良好地应用于制备基本上无酸的非质子有机液体，所述有机液体例如在电学技术中作为电解液溶剂使用。优选为碳酸、醋酸、丙酸的酯，被含卤素的C1-C4-羧酸取代的或被卤素取代的或不被卤素取代的磷酸、膦酸或次膦酸的酯。特别适用于被1个氟原子取代的碳酸、醋酸、丙酸、磷酸、膦酸或次膦酸的酯。在此所述酯可以另外地被其它取代基如烷氧基或氟代烷氧基取代。特别优选净化被至少1个氟原子取代的二烷基羧酸酯、亚烷基羧酸酯、乙酸酯、丙酸酯和2-甲氧基-四氟丙酸烷酯。“烷”优选为C1-C4。其也适用于同样可以被至少1个氟原子取代的次膦酸的烷基，以及次膦酸相应的酯。
根据本发明的方法也可应用于其它物质类别，例如醚、丙二酸酯和一般用于亚烷基桥连的二酯，特别是当涉及到通过至少1个氟原子取代的化合物时。
很合适的可以例如是在EP-A 0 807 986中所描述的含氟的醚、EP-A 0806 804和0 887 874所述的部分氟化的碳酸酯、WO 01/38319的Dioxolone、德国专利申请101 13 902的氟化的烷基碳酸酯、德国专利申请100 37 627的二氟丙二酸酯和在WO 00/38264中公开的亚烷基桥连的二酯同样如此的磷酸酯或膦酸酯，特别是有三氟乙醇衍生的酯，例如在EP-A 696 077或0806 804中所述的三(三氟乙基)磷酸酯或在UA-A 6,210,840中所述的膦酸酯或次膦酸酯。
以下将给出简单的其上吸附有聚亚烷基亚胺(例如聚亚乙基亚胺)的载体制备方法，将所述载体(适宜的是有孔的材料，优选一种无机氧化材料，特别是二氧化硅)与聚亚乙基亚胺水性溶液接触。当选择这种制备方法时，只使用这样的聚亚乙基亚胺，即在制备过程中在即将转变为水不溶性的临界前中断聚合反应。相应的聚亚乙基亚胺是商购可得的，例如品牌Polynin。所述含有了吸收的聚亚基乙亚胺的载体，将被干燥并成为备用的成品。在SiO2-载体上含有聚亚乙基亚胺的成品组合物从Aldrich公司也能获取。
根据本发明的方法允许在非质子有机液体中无水去除酸含量。所述酸分离剂可以通过轻轻倒出或过滤而简单地去除。其可以用于宽阔的酸污染浓度范围。有机液体(例如为一种溶剂)不会被有机化合物污染。其也可应用于对于碱性水解敏感的物质和特别适用于用于电池的高纯度电解液溶剂方面，特别是锂离子-电池和电容器。可以将经净化的电解液溶剂与电导盐(如阴离子如六氟磷酸盐、四氟硼酸盐或三氟甲烷磺酸盐的锂盐或四烷基氨盐)制备电解液。理想的是可以首先用电导盐和电解液溶剂制备电解液并将其用根据本发明的酸分离处理。如此分离有机酸、HF和HCl。
下述实施例应该进一步阐明本发明，而非限制于其范围内。
实施例
实例例1：净化2-甲氧基四氟丙酸甲酯
具有含量为40ppm的游离酸的2-甲氧基四氟丙酸甲酯(10g；190g/mol；0.053mol)用1g聚亚乙基亚胺在硅胶(Aldrich公司)上吸附20分钟接触。所述游离酸的含量随即为16ppm。
实施例2：三氟乙基甲基碳酸酯
具有含量为48ppm的游离酸的三氟乙基甲基碳酸酯(10g；158g/mol；0.063mol)用1g聚亚乙基亚胺在硅胶上吸附20分钟接触。所述游离酸的含量随即为26ppm。
实施例3：乙酸三氟乙酯的净化
具有含量为0.244％(GC，面积％)的游离酸的乙酸三氟乙酯(10g；142g/mol；0.070mol)用1g聚亚乙基亚胺在硅胶上吸附20分钟接触。所述游离酸的含量随即为0.038％(GC，面积％)。
在实施例1-3中所述的溶剂可以无需进一步进化而作为锂盐或四烷基氨盐的电解液溶剂用于锂离子-电池和双层电容器。
Claims (9)
1.用酸清除剂从的非质子有机液体中去除酸的方法，其特征在于，作为酸清除剂使用附载于载体上的聚亚烷基亚胺。
2.根据权利要求1的方法，其特征在于，作为酸清除剂使用聚亚乙基亚胺。
3.根据权利要求1或2的方法，其特征在于，使用无机氧化载体。
4.根据权利要求3的方法，其特征在于，使用二氧化硅，优选使用非晶形二氧化硅作为载体。
5.根据权利要求1的方法，其特征在于，将酸从非质子、氟化的有机液体中去除。
6.根据权利要求5的方法，其特征在于，将酸从氟化的酯中去除，其中所述酯是被至少1个氟原子取代的。
7.根据权利要求6的方法，其特征在于，所述酯选自氟化的羧酸酯、乙酸酯、丙酸酯、磷酸酯、膦酸酯和次膦酸酯。
8.根据权利要求1的方法，其特征在于，净化电解液溶剂。
9.根据权利要求8的方法，其特征在于，净化含有电导盐和电解液溶剂的电解液。
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| DE10143171.6 | 2001-09-04 | ||
| DE10143171A DE10143171A1 (de) | 2001-09-04 | 2001-09-04 | Verfahren zur Säureabtrennung |
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| Publication Number | Publication Date |
|---|---|
| CN1551791A true CN1551791A (zh) | 2004-12-01 |
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNA028172353A Pending CN1551791A (zh) | 2001-09-04 | 2002-08-27 | 酸的分离 |
Country Status (7)
| Country | Link |
|---|---|
| US (1) | US7037431B2 (zh) |
| EP (1) | EP1427501A1 (zh) |
| JP (1) | JP2005501891A (zh) |
| KR (1) | KR20040044504A (zh) |
| CN (1) | CN1551791A (zh) |
| DE (1) | DE10143171A1 (zh) |
| WO (1) | WO2003020392A1 (zh) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101081337B (zh) * | 2006-06-01 | 2010-05-12 | 比亚迪股份有限公司 | 一种稳定非水电解液色泽的方法 |
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| FR2855075B1 (fr) | 2003-05-21 | 2007-04-20 | Centre Nat Rech Scient | Procede pour immobiliser des composes acides ou electrophiles presents dans une solution |
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|---|---|---|---|---|
| US4104160A (en) * | 1972-05-10 | 1978-08-01 | Ciba-Geigy Corporation | Process for the purification of industrial effluents |
| CH634283A5 (de) * | 1978-02-24 | 1983-01-31 | Ciba Geigy Ag | Verfahren zur entfernung von schwermetallionen aus waesserigen loesungen. |
| JPS62216641A (ja) * | 1986-03-19 | 1987-09-24 | Nippon Shokubai Kagaku Kogyo Co Ltd | 環境浄化用吸着剤 |
| JPS62225244A (ja) * | 1986-03-27 | 1987-10-03 | Nippon Shokubai Kagaku Kogyo Co Ltd | 吸着剤 |
| JP3618764B2 (ja) * | 1992-03-13 | 2005-02-09 | ダイキン工業株式会社 | 揮発性酸類の回収方法 |
| DE19827631A1 (de) * | 1998-06-20 | 1999-12-23 | Merck Patent Gmbh | Aufreinigung von Batterieelektrolyten mittels physikalischer Adsorption |
| DE19827630A1 (de) * | 1998-06-20 | 2000-04-27 | Merck Patent Gmbh | Aufreinigung von Batterieelektrolyten mittels chemischer Adsorption |
| US6780327B1 (en) * | 1999-02-25 | 2004-08-24 | Pall Corporation | Positively charged membrane |
| DE10049097B4 (de) * | 2000-09-27 | 2004-08-26 | Chemetall Gmbh | Verfahren zur Trocknung von organischen Flüssigelektrolyten |
-
2001
- 2001-09-04 DE DE10143171A patent/DE10143171A1/de not_active Withdrawn
-
2002
- 2002-08-27 WO PCT/EP2002/009545 patent/WO2003020392A1/de active Application Filing
- 2002-08-27 CN CNA028172353A patent/CN1551791A/zh active Pending
- 2002-08-27 KR KR10-2004-7002959A patent/KR20040044504A/ko not_active Application Discontinuation
- 2002-08-27 EP EP02758485A patent/EP1427501A1/de not_active Withdrawn
- 2002-08-27 JP JP2003524695A patent/JP2005501891A/ja active Pending
-
2004
- 2004-03-03 US US10/791,272 patent/US7037431B2/en not_active Expired - Fee Related
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101081337B (zh) * | 2006-06-01 | 2010-05-12 | 比亚迪股份有限公司 | 一种稳定非水电解液色泽的方法 |
Also Published As
| Publication number | Publication date |
|---|---|
| EP1427501A1 (de) | 2004-06-16 |
| DE10143171A1 (de) | 2003-03-20 |
| US7037431B2 (en) | 2006-05-02 |
| JP2005501891A (ja) | 2005-01-20 |
| WO2003020392A1 (de) | 2003-03-13 |
| US20040232081A1 (en) | 2004-11-25 |
| KR20040044504A (ko) | 2004-05-28 |
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