CN101045830B - Preparation method of functional group linken on surface of polymer electrolyte nano SiO2 - Google Patents
Preparation method of functional group linken on surface of polymer electrolyte nano SiO2 Download PDFInfo
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- CN101045830B CN101045830B CN2007100738398A CN200710073839A CN101045830B CN 101045830 B CN101045830 B CN 101045830B CN 2007100738398 A CN2007100738398 A CN 2007100738398A CN 200710073839 A CN200710073839 A CN 200710073839A CN 101045830 B CN101045830 B CN 101045830B
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- 125000000524 functional group Chemical group 0.000 title claims abstract description 14
- 238000002360 preparation method Methods 0.000 title claims description 11
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 title abstract 6
- 229910052681 coesite Inorganic materials 0.000 title abstract 3
- 229910052906 cristobalite Inorganic materials 0.000 title abstract 3
- 239000000377 silicon dioxide Substances 0.000 title abstract 3
- 235000012239 silicon dioxide Nutrition 0.000 title abstract 3
- 229910052682 stishovite Inorganic materials 0.000 title abstract 3
- 229910052905 tridymite Inorganic materials 0.000 title abstract 3
- 239000005518 polymer electrolyte Substances 0.000 title description 14
- 229910004298 SiO 2 Inorganic materials 0.000 claims description 18
- 239000002904 solvent Substances 0.000 claims description 9
- 239000011261 inert gas Substances 0.000 claims description 8
- 239000000203 mixture Substances 0.000 claims description 8
- 238000012986 modification Methods 0.000 claims description 8
- 230000004048 modification Effects 0.000 claims description 8
- 238000003756 stirring Methods 0.000 claims description 8
- 238000001291 vacuum drying Methods 0.000 claims description 6
- 238000006243 chemical reaction Methods 0.000 claims description 5
- 238000005303 weighing Methods 0.000 claims description 5
- 238000010438 heat treatment Methods 0.000 claims description 4
- 206010013786 Dry skin Diseases 0.000 claims description 3
- 239000006087 Silane Coupling Agent Substances 0.000 claims description 3
- 238000001035 drying Methods 0.000 claims description 3
- 239000002245 particle Substances 0.000 claims description 3
- 238000005554 pickling Methods 0.000 claims description 3
- 238000005406 washing Methods 0.000 claims description 3
- 230000008859 change Effects 0.000 claims description 2
- 229920000642 polymer Polymers 0.000 abstract description 9
- WEVYAHXRMPXWCK-UHFFFAOYSA-N Acetonitrile Chemical compound CC#N WEVYAHXRMPXWCK-UHFFFAOYSA-N 0.000 description 12
- 239000002131 composite material Substances 0.000 description 10
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 6
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 6
- ZMANZCXQSJIPKH-UHFFFAOYSA-N Triethylamine Chemical compound CCN(CC)CC ZMANZCXQSJIPKH-UHFFFAOYSA-N 0.000 description 6
- 229910052744 lithium Inorganic materials 0.000 description 5
- YMWUJEATGCHHMB-UHFFFAOYSA-N Dichloromethane Chemical compound ClCCl YMWUJEATGCHHMB-UHFFFAOYSA-N 0.000 description 4
- ROSDSFDQCJNGOL-UHFFFAOYSA-N Dimethylamine Chemical compound CNC ROSDSFDQCJNGOL-UHFFFAOYSA-N 0.000 description 4
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 description 4
- NEHMKBQYUWJMIP-UHFFFAOYSA-N chloromethane Chemical compound ClC NEHMKBQYUWJMIP-UHFFFAOYSA-N 0.000 description 4
- 239000000945 filler Substances 0.000 description 4
- GETQZCLCWQTVFV-UHFFFAOYSA-N trimethylamine Chemical compound CN(C)C GETQZCLCWQTVFV-UHFFFAOYSA-N 0.000 description 4
- 229910013684 LiClO 4 Inorganic materials 0.000 description 3
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 3
- 230000008901 benefit Effects 0.000 description 3
- 238000002474 experimental method Methods 0.000 description 3
- 238000004128 high performance liquid chromatography Methods 0.000 description 3
- 239000002808 molecular sieve Substances 0.000 description 3
- 238000011160 research Methods 0.000 description 3
- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 description 3
- 239000007787 solid Substances 0.000 description 3
- 238000001179 sorption measurement Methods 0.000 description 3
- BFKJFAAPBSQJPD-UHFFFAOYSA-N tetrafluoroethene Chemical group FC(F)=C(F)F BFKJFAAPBSQJPD-UHFFFAOYSA-N 0.000 description 3
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 description 2
- 229960001701 chloroform Drugs 0.000 description 2
- 238000001816 cooling Methods 0.000 description 2
- HPNMFZURTQLUMO-UHFFFAOYSA-N diethylamine Chemical compound CCNCC HPNMFZURTQLUMO-UHFFFAOYSA-N 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000012528 membrane Substances 0.000 description 2
- 238000000034 method Methods 0.000 description 2
- 239000012764 mineral filler Substances 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 238000005245 sintering Methods 0.000 description 2
- 238000003860 storage Methods 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 1
- 239000000470 constituent Substances 0.000 description 1
- 239000007822 coupling agent Substances 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000005518 electrochemistry Effects 0.000 description 1
- 239000002001 electrolyte material Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 239000007770 graphite material Substances 0.000 description 1
- 238000002329 infrared spectrum Methods 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 229910001416 lithium ion Inorganic materials 0.000 description 1
- 229910003002 lithium salt Inorganic materials 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 238000013508 migration Methods 0.000 description 1
- 230000005012 migration Effects 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 238000002444 silanisation Methods 0.000 description 1
- 238000000967 suction filtration Methods 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
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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
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Abstract
This invention relates to a kind of polymer dielectric nanometer SiO2 linkage upper surface functional group. It is hydrophobicity functional group with Si - CH2CH2( CF2) 5CF3 topcoated; the particlesize of nanometer SiO2 is 7 to 20 nm, specific surface area is 150 to 300 sq m/g. Hydrophobicity quality of this invention is good for dispersing at PEO group polymer dielectric system, thereby couldreduce crystalline phase content og this system, advance conductivity.
Description
Technical field
The present invention relates to nanometer SiO
2The preparation method of functional group linken on surface.
Background technology
Metallic lithium with respect to existing graphite material, has the low (3.05Vv.s.Li of redox potential as secondary lithium battery cathode
+/ Li), the little (0.535g/cm of density
3), specific storage height plurality of advantages such as (3862mAh/g), thereby lithium metal battery will have higher specific energy and specific storage than present lithium ion battery, but because the specific conductivity of the polymer dielectric that matches is low, so there is not sophisticated product to occur at present yet.
About the used solid polymer electrolyte of lithium metal battery, report, the deficiency of its maximum have been arranged is that the order of magnitude of specific conductivity at room temperature only is 10 more
-7S/cm can't satisfy actual needs at all.In order to improve the specific conductivity of polymer dielectric, people have carried out research in many ways, particularly the research of the composite polymer electrolyte of the dopen Nano mineral filler of simple, the excellent property of preparation becomes focus especially, F.Croce etc. have delivered their achievement in research [F.Croce on " Nature ", G.B.Appetecchi, L.Persi et al.Nature[J], 1998,394 (6692): 456-458]: add nanometer SiO
2Deng the high molecular PEO base composite polymer electrolyte of mineral filler, its conductive capability, mechanical property all significantly improve than having had before mixing, and the specific conductivity under the room temperature reaches 10
-5S/cm.FAN has studied the SiO that has the different surfaces group
2To the influence [J.Fan, S.R.Raghavaan, X.Y.Yu.Solid StateIonics[J] of lower molecular weight PEO polymer dielectric specific conductivity, 1998,111 (1): 117-123], the conductive capability and the SiO of discovery composite polymer electrolyte
2Functional group's kind on surface is relevant.As long as above document shows at SiO
2Suitable functional group in the connection of particle surface will improve the conductivity of composite polymer electrolyte.Kim etc. have reported the SiO that adds in PEO-lithium salts system
2Have two kinds of surface functional groups [J.W.Kim, K.S.Ji, J.P.Lee, et al.J.Power Sources[J], 2003,119-121:415-421], ((CH
3)
3) and Si-O-[Si (CH
3)
2-O]
4-H, experimental result shows the preceding SiO of kind that mixes
2The composite polymer electrolyte specific conductivity higher, the author think this be because-CH
3Group can impel filler to be dispersed in more fully in the PEO matrix, and can not hinder ion migration.But in the literary composition to having Si-O-[Si (CH
3)
2-O]
4The SiO of-H group
2The preparation method do not elaborate.Liu is with (CH
3O)
3Si (CH
2)
3(CH
2O)
6-9CH
3For coupling agent to nanometer SiO
2Carried out modifying [Y.Liu, J.Y.Lee, L.Hong.J.Power Sources[J], 2002,109 (2): 507-514], on its surface bond-Si (CH
2)
3(CH
2O)
6-9CH
3Hydrophobic group, and the nanometer SiO after this modification
2Be incorporated into the PEO-LIBF4 polymer electrolyte system, the result has reduced the crystallization phases content of polymeric system, has improved conductivity of electrolyte materials.But this experiment is with CH
3CH
2OH is a solvent, and reaction conditions is difficult to reach complete anhydrous requirement, thereby has a strong impact on productive rate.Hou is once for SiO
2The Silanization reaction condition of the novel functional group of this surface bond carried out benefiting our pursuits [J.Hou.Ph.D thesis[D], Michigan State University, Michigan, 1997], a series of sign experiments prove that all this experiment has reached certain effect, and just productivity ratio is lower.These report demonstration, if rationally control reaction conditions, introduce suitable silane coupling agent, at SiO
2Target functional group on the surface bond also just might improve the conductive capability and the mechanical property of composite polymer electrolyte, thereby quickens the industrialization process of full solid state polymer lithium cell.
Summary of the invention
The purpose of this invention is to provide a kind of practical, nanometer SiO that the product production rate is higher
2The preparation method of functional group linken on surface.
One object of the present invention is achieved through the following technical solutions.
A kind of nanometer SiO
2The preparation method of functional group linken on surface is characterized in that: this preparation method's step is:
1) with original agglomerating nanometer SiO
2The vacuum high-temperature baking, temperature is 120～550 ℃, the time is 24～72 hours;
2) the HCl pickling nanometer SiO of employing 3～7M
2, not stopping therebetween to stir, rotating speed is 10～40 commentaries on classics/min, the time is 1～6 hour;
3) with nanometer SiO
2Suction filtration, washing, vacuum-drying, temperature is 80～250 ℃, the time is 12～36 hours;
4) with nanometer SiO
2Transfer in the encloses container under protection of inert gas, add benzene or toluene or dimethylbenzene or monochloro methane or methylene dichloride or trichloromethane and dimethylamine or diethylamine or Trimethylamine 99 or triethylamine simultaneously, each constituent mass is than being nanometer SiO
2: benzene or toluene or dimethylbenzene or monochloro methane or methylene dichloride or trichloromethane: dimethylamine or diethylamine or Trimethylamine 99 or triethylamine=100: (10-30): (0.5-30);
5) each component heated and stirred under protection of inert gas, temperature is 20～80 ℃, the time is 8～24 hours;
6) after the reaction times end, mixture is filtered in ventilated environment;
7) 120 ℃ of dryings of vacuum.
Described rare gas element is N
2Or Ar.
The present invention compared with prior art has the following advantages.
Practical, product production rate advantage of higher that the present invention has.
Description of drawings
Fig. 1 is nanometer SiO
2Diffuse reflectance IR before and after modification;
Fig. 2 is nanometer SiO
2Before and after the modification, be spiked in the polymer dielectric, be prepared into the electrolytical specific conductivity of mixture as filler, and with do not mix before straight polymer system specific conductivity-temperature curve relatively.
Embodiment
Below in conjunction with accompanying drawing Fig. 1 and Fig. 2 the present invention is described in further detail.
Embodiment 2. takes by weighing 0.7gPEO (weight-average molecular weight～600,000, down together), 0.2108gLiClO
4, put into the exsiccant round-bottomed flask then together, (CH3CN, HPLC) as solvent, under protection of inert gas, controlled temperature is 50 ℃, stirs 60 hours to add the 40ml acetonitrile.After thing to be mixed becomes colloidal sol, be cast on the tetrafluoroethylene template, use
The solvent that molecular sieve adsorption evaporates was transferred in the vacuum drying oven after 24 hours, and 60 ℃ were continued down dry 48 hours.So just made straight polymer electrolytic thin-membrane dry, even, self-supporting.
Embodiment 3. is with the original sintering nanometer SiO before the modification
2120 ℃ of bakings of vacuum 24 hours take by weighing 0.09108g, with 0.7gPEO, 0.2108g LiClO
4Put into the exsiccant round-bottomed flask together, (CH3CN, HPLC) as solvent, under protection of inert gas, controlled temperature is 50 ℃, stirs 60 hours to add the 40ml acetonitrile.After thing to be mixed becomes colloidal sol, be cast on the tetrafluoroethylene template, use
The solvent that molecular sieve adsorption evaporates was transferred in the vacuum drying oven after 24 hours, and 60 ℃ were continued down dry 48 hours.So just made composite polymer electrolyte film dry, even, self-supporting.
Embodiment 4. is with the nanometer SiO after the modification
2120 ℃ of bakings of vacuum 24 hours take by weighing 0.09108g, with 0.7gPEO, 0.2108g LiClO
4Put into the exsiccant round-bottomed flask together, (CH3CN, HPLC) as solvent, under protection of inert gas, controlled temperature is 50 ℃, stirs 60 hours to add the 40ml acetonitrile.After thing to be mixed becomes colloidal sol, be cast on the tetrafluoroethylene template, use
The solvent that molecular sieve adsorption evaporates was transferred in the vacuum drying oven after 24 hours, and 60 ℃ were continued down dry 48 hours.So just made composite polymer electrolyte film dry, even, self-supporting.
Claims (1)
1. nanometer SiO
2The preparation method of functional group linken on surface is characterized in that: this preparation method's step is: get the original agglomerating of 10g, particle diameter is that 7～20nm, specific surface area are 380m
2The nanometer SiO of/g
2, place 450 ℃ of pre-burnings of retort furnace 24 hours, change pickling in the HCl solution of the 5M that fills 30ml afterwards over to, stirring at normal temperature 3 hours; Will be through the SiO of overpickling
2Filter, wash 120 ℃ of dryings of vacuum 12 hours; Take by weighing the SiO that 5g handled
2, under protection of inert gas, insert in the encloses container, add 2g silane coupling agent Cl simultaneously
3Si-CH
2CH
2(CF
2)
5CF
3With 0.5g catalyzer HN (CH
3)
2, add 30ml CH at last
2Cl
2Solvent; Mixture was 45～55 ℃ of following stirring heating 10～12 hours; After reaction finishes, in stink cupboard, mixture is filtered, use CH successively
3CH
2OCH
2CH
3, anhydrous CH
3CH
2The OH washing; The nanometer SiO that surface modification is crossed then
2Put into 120 ℃ of bakings of vacuum drying oven.
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|---|---|---|---|
| CN2007100738398A CN101045830B (en) | 2007-04-16 | 2007-04-16 | Preparation method of functional group linken on surface of polymer electrolyte nano SiO2 |
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|---|---|---|---|
| CN2007100738398A CN101045830B (en) | 2007-04-16 | 2007-04-16 | Preparation method of functional group linken on surface of polymer electrolyte nano SiO2 |
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|---|---|
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| CN101045830B true CN101045830B (en) | 2010-06-09 |
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Families Citing this family (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101597437B (en) * | 2008-06-04 | 2012-07-25 | 中国科学院大连化学物理研究所 | Organic modified nanometer complex oxide material and preparation method thereof |
| CN104051692B (en) * | 2014-06-09 | 2016-01-06 | 常州大学 | A kind of lithium ion battery microporous polyolefin film and preparation method thereof |
| CN107134587B (en) * | 2017-04-26 | 2019-06-18 | 华中科技大学 | A kind of solid electrolyte inorganic nano particle filler and preparation method thereof |
| CN108530953A (en) * | 2018-04-24 | 2018-09-14 | 曹俊峰 | A kind of preparation method of water tight packing |
| CN109666455A (en) * | 2019-01-16 | 2019-04-23 | 中国海洋大学 | The preparation method of amphipathic silica solid particle base marine oil spill dispersing agent |
| CN110845765A (en) * | 2019-12-06 | 2020-02-28 | 扬州海吉科技有限公司 | Hydrophobic function coated particle material and preparation method thereof |
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Denomination of invention: Method for preparing surface functional group on nano SiO[sub]2[/sub] bonding Effective date of registration: 20121225 Granted publication date: 20100609 Pledgee: China Development Bank Co Pledgor: Du Hongyan|Shandong Runfeng group Amperex Technology Limited Registration number: 2012990000850 |
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