CN101471153A - Production method for silica gel encapsulated ion liquid solid state electrolyte material - Google Patents
Production method for silica gel encapsulated ion liquid solid state electrolyte material Download PDFInfo
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- CN101471153A CN101471153A CN 200710307475 CN200710307475A CN101471153A CN 101471153 A CN101471153 A CN 101471153A CN 200710307475 CN200710307475 CN 200710307475 CN 200710307475 A CN200710307475 A CN 200710307475A CN 101471153 A CN101471153 A CN 101471153A
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Abstract
The invention discloses a method for preparing a silica gel embedding ion liquid solid electrolyte material, the method mixing one or more than one kinds of ion liquid to compound the silica gel embedding ion liquid solid electrolyte material in one step through the collosol-gel process. The method has simple operation and mild reaction, and has great potential application prospects in the fields of solar cells, fuel cells, secondary lithium ion cells, chemical capacitors and the like.
Description
Technical field
The present invention relates to a kind of preparation method of silica gel encapsulated ion liquid solid state electrolyte material.
Background technology
Along with clean energy resource is subjected to the great attention of countries in the world, secondary lithium battery, DSSC, ultracapacitor etc. are efficient, the clean energy resource device becomes the research focus.In the research process of these energy devices, particularly in the research process of secondary lithium battery, the positive and negative electrode material is by extensively and profoundly research, and relatively less obtains paying attention to as indispensable electrolyte.In fact, the effect of electrolyte in these energy devices is not the so simple of imagination, selects different electrolytes, and the battery performance that obtains may be different fully.Therefore, the development of lithium rechargeable battery, DSSC, ultracapacitor all is subjected to the restriction of electrolyte medium material.At present, be to be the main body electrolyte with the organic carbonate in the commercial secondary lithium battery.The loss of volatilizing easily of these organic baths also brings potential danger to the security performance of lithium ion battery, and lithium ion battery can catch fire or explode under hot conditions.Simultaneously, these organic baths also exist the low weakness of battery cathode stability, cause the unstable properties of battery, and the life-span is short.DSSC is the strong competitor of the silicon solar cell of phase plaid matching costliness.For DSSC electrolyte, liquid electrolyte mainly is that organic solvents such as acetonitrile, ethylene carbonate (EC), propene carbonate (PC), N-methyl oxazolidinedione (NMO) and EC/PC mixed solvent are formed, exist volatile, problems such as unstable properties, same problem also is present in the ultracapacitor.Therefore develop novel electrolyte, carrying out correlative study is the high performance secondary lithium battery of development, and the requisite link of DSSC has crucial meaning to the development clean energy resource.
Ionic liquid at room temperature be fully by certain cationic and anion constitute in room temperature or be bordering on the material that is in a liquid state under the room temperature.Ion liquid main feature is: non-volatile or " zero " vapour pressure (this should be the important evidence that ionic liquid is considered to green) low melting point (can hang down-90 ℃); Wide liquid journey (can reach 200 ℃); Strong electrostatic field (this should be the key character that is different from molecule-type medium and material); Wide electrochemical window (even can be greater than 6V, good electricity is (present ion liquid conductivity the highest can greater than 100mS/cm) electrically, thermal capacitance and thermal energy storage density; High thermal stability (decomposition temperature can be higher than 400 ℃); Selective dissolution power is so be called " liquid " molecular sieve (liquid zeolite); Designability
[1]
In recent years, except using in traditional catalytic field, ionic liquid at room temperature has obtained in fields such as lithium ion battery, DSSC, ultracapacitor and photoelectric materials using widely as a kind of electrolyte
[2]Liquid ionic liquid has many plurality of advantages that are better than conventional solvent as the electrolyte of energy battery, but ionic liquid is a liquid, and is unfavorable for the encapsulation of battery.Solid electrolyte is compared with liquid electrolyte, has many advantages, does not flow as solid electrolyte, therefore can not cause the leakage of electrolyte; Because of it is easy to make different shape, the fail safe of battery and stability are improved or the like.At present ionic liquid is prepared into solid electrolyte and mainly is with polymer and ionic liquid is coated or the method for " grafting " realizes electrolytical solid state, and polymer electrolytic confrontation energy battery can produce potential unsafe factor, as its combustibility.Therefore in this patent, we developed safer with silica gel bag borne ionic liquid as solid electrolyte material, ionic liquid exists with the form of liquid nano, and the liquid of nanomorphic can represent multiple nano effect, as make that silica gel material produces that electricity is led, phase behavior, spectrum etc. unusual.Up to now, do not find to use the patent report of silica gel bag borne ionic liquid solid electrolyte as yet.
Summary of the invention
The object of the present invention is to provide a kind of preparation method of silica gel encapsulated ion liquid solid state electrolyte material.
A kind of preparation method of silica gel encapsulated ion liquid solid state electrolyte material is characterized in that: use one or more ionic liquids to mix through one step of sol-gel process synthesized silicon rubber encapsulated ion liquid solid state electrolyte material;
Described ionic liquid, cationic structural be:
In a kind of, wherein m is the integer between 0 to 12, comprises 0 and 12, n is 0 to 12 integer, comprises 0 and 12; Anion is BF
4 -, PF
6 -, NTf
2 -, N (CN)
2 -, NO
3 -, Cl
-, Br
-, I
-, CH
3COO
-, CF
3COO
-, CF
3SO
3 -, HPO
4 2-, H
2PO
4 -, CH
3SO
3 -, HSO
4 -And ClO
4 -In a kind of.
Mol ratio between one or more ionic liquids of the present invention, two kinds of ionic liquids is that 0.1-10, three kinds of mol ratios between the ionic liquid are (1-10): (1-10): any ratio (1-10), ionic liquid mostly is three kinds most.
The precursor of the silica gel of bag borne ionic liquid of the present invention is positive silicic acid tetraalkyl ester.
Sol-gel process of the present invention, it is acid catalyzed sol-gal process that preparation silica gel wraps the ion liquid method of carrying, used catalyst is hydrochloric acid, CH
3COOH or HCOOH.
It is 10%-80% that silica gel that the present invention synthesizes wraps the ion liquid content that carries.
Silica gel encapsulated ion liquid solid state electrolyte material of the present invention is characterized in that, the organic acid catalysis silica gel bag borne ionic liquid electrolyte that self-catalysis obtains with the acid functionalization ionic liquid has relative higher conductivity.
Ionic liquid of the present invention, its preparation method and character can be referring to Deng Youquan. ionic liquid-character, preparation and application [M]. and Sinopec publishing house, 2006,7.
Characteristics of the present invention:
1. the present invention is simple to operate, reaction condition is gentle.
2. with respect to the ionic liquid electrolyte of liquid, silica gel bag borne ionic liquid solid electrolyte have shape adjustable, do not flow, be assembled into the advantage that electrolyte does not leak behind the battery.
3. silica gel bag borne ionic liquid solid electrolyte has than the high characteristics of the dipping ionic liquid solid electrolyte of the silica gel under the same amount.
4. organic acid catalysis and acidic ion liquid self-catalysis prepare the silica gel bag borne ionic liquid of gained, the higher relatively characteristics of conductivity.
The present invention can be fixed on ionic liquid in the silica gel by the method for colloidal sol-gel, and ionic liquid exists with the liquid nano form in silica gel.Silica gel bag borne ionic liquid solid electrolyte has than the high characteristics of the dipping ionic liquid solid electrolyte of the silica gel under the same amount, by organic acid catalysis and functionalized acidic ionic liquid self-catalysis colloidal sol-gel process, the silica gel bag borne ionic liquid conductivity of preparation gained can reach 1.0 * 10
-3MS/cm.With respect to the ionic liquid electrolyte of liquid, silica gel bag borne ionic liquid solid electrolyte have shape adjustable, do not flow, be assembled into the advantage that electrolyte does not leak behind the battery.The present invention prepares the method for modified electrode and solid electrolyte by silica gel bag borne ionic liquid, simple to operate, reaction temperature and, in fields such as solar cell, fuel cell, secondary lithium battery, chemical capacitors very big potential application foreground is arranged.
Embodiment
In order to further specify details of the present invention, enumerate some embodiment below, but should not be so limited.
Embodiment 1
Get 5ml TEOS and add in the 100ml conical flask, add the 2.5ml absolute ethyl alcohol then successively, 0.5ml water, 0.50g[EMIm] BF
4(1-ethyl-3-methyl imidazolium tetrafluoroborate) ionic liquid, adding the stirring magneton stirred 2 hours down at 40 ℃, then conical flask being put into ice bath continues to stir, the HCl solution that adds 2.5ml 38% with dropping funel, at room temperature continue then to stir, after 2 hours, just obtained water white ionic liquid silicon gel, behind the gel it is taken out with vacuum pump under 60 ℃ and took out with remaining ethanol with at the water that gel process produces in 5 hours, at last ionic liquid silicon gel is put in the baking oven at 60 ℃ and continues down agingly just to have obtained the silica gel bag and carry [BMIm] BF
4Solid electrolyte, its ionic liquid content are that to measure its conductivity be 0.94 * 10 to 27.8% usefulness electrochemical impedance
-3MS/cm.
Embodiment 2
Get 5ml TEOS and add in the 100ml conical flask, add the 2.5m absolute ethyl alcohol then successively, 0.5ml water, 0.50g[BMIm] NTf
2(1-butyl-3-methylimidazole fluoroform sulfonamide) ionic liquid, adding the stirring magneton stirred 2 hours down at 40 ℃, then conical flask being put into ice bath continues to stir, the HCl solution that adds 2.5ml38% with dropping funel, at room temperature continue then to stir, after 2 hours, just obtained water white ionic liquid silicon gel, behind the gel it is taken out with vacuum pump under 60 ℃ and took out with remaining ethanol with at the water that gel process produces in 5 hours, at last ionic liquid silicon gel is put in the baking oven at 60 ℃ and continues down agingly just to have obtained the silica gel bag and carry [BMIm] NTf
2Solid electrolyte, its ionic liquid content are that to measure its conductivity be 1.31 * 10 to 27.8% usefulness electrochemical impedance
-3MS/cm.
Embodiment 3
Get 5ml TEOS and add in the 100ml conical flask, add the 2.5ml absolute ethyl alcohol then successively, 0.5ml water, 1.41g[BMIm] BF
4(1-butyl-3-methyl imidazolium tetrafluoroborate) ionic liquid, adding the stirring magneton stirred 2 hours down at 40 ℃, then conical flask being put into ice bath continues to stir, the HCl solution that adds 2.5ml 38% with dropping funel, at room temperature continue then to stir, after 2 hours, just obtained water white ionic liquid silicon gel, behind the gel it is taken out with vacuum pump under 60 ℃ and took out with remaining ethanol with at the water that gel process produces in 5 hours, at last ionic liquid silicon gel is put in the baking oven at 60 ℃ and continues down agingly just to have obtained the silica gel bag and carry [BMIm] BF
4Solid electrolyte, its ionic liquid content is 52.0%, measuring its conductivity with electrochemical impedance is 5.56 * 10
-3MS/cm.
Embodiment 4
Get 5ml TEOS and add in the 100ml conical flask, add the 2.5ml absolute ethyl alcohol then successively, 0.5ml water, 0.43g[OMIm] BF
4(1-octyl group-3-methyl imidazolium tetrafluoroborate) ionic liquid, adding the stirring magneton stirred 2 hours down at 40 ℃, then conical flask being put into ice bath continues to stir, the HCl solution that adds 2.5ml 38% with dropping funel, at room temperature continue then to stir, after 2 hours, just obtained water white ionic liquid silicon gel, behind the gel it is taken out with vacuum pump under 60 ℃ and took out with remaining ethanol with at the water that gel process produces in 5 hours, at last ionic liquid silicon gel is put in the baking oven at 60 ℃ and continues down agingly just to have obtained the silica gel bag and carry [OMIm] BF
4Solid electrolyte, its ionic liquid content is 24.9%, measuring its conductivity with electrochemical impedance is 0.552 * 10
-4MS/cm.
Embodiment 5
Get 5ml TMOS and add in the 100ml conical flask, add the 2.5ml absolute ethyl alcohol then successively, 0.5ml water, 0.48g[BMIm] CF
3SO
3(1-butyl-3-methylimidazole four trifluoro-methanyl sulfonates) ionic liquid, adding the stirring magneton stirred 2 hours down at 40 ℃, then conical flask being put into ice bath continues to stir, the HCl solution that adds 2.5ml 38% with dropping funel, at room temperature continue then to stir, just obtained water white ionic liquid silicon gel after 2 hours, behind the gel it is taken out with vacuum pump under 60 ℃ and took out with remaining ethanol with at the water that gel process produces in 5 hours, at last ionic liquid silicon gel is put in the baking oven at 60 ℃ and continues down agingly just to have obtained the silica gel bag and carry [BMIm] CF
3SO
3Solid electrolyte, its ionic liquid content are that to measure its conductivity be 0.860 * 10 to 27.0% usefulness electrochemical impedance
-3MS/cm.
Embodiment 6
Get 5ml TMOS and add in the 100ml conical flask, add the 2.5ml absolute ethyl alcohol then successively, 0.5ml water, 0.52g[BMIm] BF
4(1-butyl-3-methyl imidazolium tetrafluoroborate) ionic liquid, adding the stirring magneton stirred 2 hours down at 40 ℃, then conical flask being put into ice bath continues to stir, the HCl solution that adds 2.5ml 38% with dropping funel, at room temperature continue then to stir, after 2 hours, just obtained water white ionic liquid silicon gel, behind the gel it is taken out with vacuum pump under 60 ℃ and took out with remaining ethanol with at the water that gel process produces in 5 hours, at last ionic liquid silicon gel is put in the baking oven at 60 ℃ and continues down agingly just to have obtained the silica gel bag and carry [BMIm] BF
4Solid electrolyte, its ionic liquid content is 28.6%, measuring its conductivity with electrochemical impedance is 1.60 * 10
-3MS/cm.
Embodiment 7
Getting 5ml TEOS adds in the 100ml conical flask, add the 2.5m absolute ethyl alcohol then successively, 0.5ml water, 0.48gPMII, 1-propyl group-3-methylimidazole iodine, adding the stirring magneton stirred 2 hours down at 40 ℃, then conical flask being put into ice bath continues to stir, the HCOOH that adds 0.5ml 98% with dropping funel, at room temperature continue then to stir, after 2 hours, just obtained filemot ionic liquid silicon gel, behind the gel it is taken out 5 hours with remaining ethanol with vacuum pump under 60 ℃, responseless HCOOH and take out at the water that gel process produces is put into ionic liquid silicon gel at last in the baking oven at 60 ℃ and continues down agingly just to have obtained the silica gel bag and carry the PMII solid electrolyte, and its ionic liquid content is that to measure its conductivity be 1.21 * mS/cm to 27.0% usefulness electrochemical impedance.
Embodiment 8
Getting 5ml TMOS adds in the 100ml conical flask, add the 2.5ml absolute ethyl alcohol then successively, 0.5ml water, 0.45g 1-fourth sulfonic group-3-methylimidazole four trifluoro-methanyl sulfonate ionic liquids, adding the stirring magneton stirred 2 hours down at 40 ℃, then conical flask being put into ice bath continues to stir, at room temperature continue then to stir, after 2 hours, just obtained faint yellow transparent ionic liquid silicon gel, behind the gel it is taken out with vacuum pump under 60 ℃ and took out with remaining ethanol with at the water that gel process produces in 5 hours, at last ionic liquid silicon gel is put in the baking oven at 60 ℃ and continues down agingly just to have obtained the silica gel bag and carry 1-fourth sulfonic group-3-methylimidazole four trifluoro-methanyl sulfonate solid electrolytes, its ionic liquid content is that to measure its conductivity be 2.05 * mS/cm to 25.7% usefulness electrochemical impedance.
Embodiment 9
Getting 5ml TEOS adds in the 100ml conical flask, add the 2.5ml absolute ethyl alcohol then successively, 0.5ml water, 0.43g 1-fourth carboxyl-3-methyl imidazolium tetrafluoroborate ionic liquid, adding the stirring magneton stirred 2 hours down at 40 ℃, then conical flask being put into ice bath continues to stir, the HCl solution that adds 2.5ml 38% with dropping funel, at room temperature continue then to stir, after 2 hours, just obtained water white ionic liquid silicon gel, behind the gel it is taken out with vacuum pump under 60 ℃ and took out with remaining ethanol with at the water that gel process produces in 5 hours, at last ionic liquid silicon gel is put in the baking oven at 60 ℃ and continues down agingly just to have obtained the silica gel bag and carry 1-fourth carboxyl-3-methyl imidazolium tetrafluoroborate solid electrolyte, its ionic liquid content is that to measure its conductivity be 0.860 * 10 to 24.9% usefulness electrochemical impedance
-3MS/cm.
Embodiment 10
Get 5ml TMOS and add in the 100ml conical flask, add the 2.5ml absolute ethyl alcohol then successively, 0.5ml water, 0.25g[BMIm] BF
4(1-butyl-3-methyl imidazolium tetrafluoroborate) and 0.25[BMIm] CF
3SO
3(1-butyl-3-methylimidazole four trifluoro-methanyl sulfonates), adding the stirring magneton stirred 2 hours down at 40 ℃, then conical flask being put into ice bath continues to stir, the HCl solution that adds 2.5ml 38% with dropping funel, at room temperature continue then to stir, after leaving standstill one day, just obtained water white ionic liquid silicon gel, behind the gel it is taken out with vacuum pump under 60 ℃ and took out with remaining ethanol with at the water that gel process produces in 5 hours, at last ionic liquid silicon gel is put in the baking oven at 60 ℃ and continues down agingly just to have obtained the silica gel bag and carry [BMIm] BF
4[BMIm] CF
3SO
3(ionic liquid is than being 1:1) solid electrolyte, its ionic liquid total content is 27.8%, measuring its conductivity with electrochemical impedance is 0.781 * 10
-3MS/cm.
Embodiment 11
Get 5ml TEOS and add in the 100ml conical flask, add the 2.5ml absolute ethyl alcohol then successively, 0.5ml water, 0.25g[BMIm] BF
4(1-butyl-3-methyl imidazolium tetrafluoroborate), 0.25[EMIm] BF
4(1-butyl-3-methylimidazole four trifluoro-methanyl sulfonates) and 0.1g 1-fourth sulfonic group-3-methylimidazole four trifluoro-methanyl sulfonate ionic liquids, adding the stirring magneton stirred 2 hours down at 40 ℃, at room temperature continue then to stir, after leaving standstill one day, just obtained water white ionic liquid silicon gel, behind the gel it is taken out with vacuum pump under 60 ℃ and took out with remaining ethanol with at the water that gel process produces in 5 hours, at last ionic liquid silicon gel is put in the baking oven at 60 ℃ and continues down agingly just to have obtained the silica gel bag and carry [BMIm] BF
4, [EMIm] BF
4With 1-butyl-3-methylimidazole four trifluoro-methanyl sulfonates (ionic liquid than for 5:5:2) solid electrolyte, its ionic liquid total content is that to measure its conductivity be 0.860 * mS/cm to 31.6% usefulness electrochemical impedance.
Claims (3)
1, a kind of preparation method of silica gel encapsulated ion liquid solid state electrolyte material is characterized in that: use one or more ionic liquids to mix through one step of sol-gel process synthesized silicon rubber encapsulated ion liquid solid state electrolyte material;
Described ionic liquid, cationic structural be:
In a kind of, wherein m is the integer between 0 to 12, comprises 0 and 12, n is 0 to 12 integer, comprises 0 and 12; Anion is BF
4 -, PF
6 -, NTf
2 -, N (CN)
2 -, NO
3 -, Cl
-, Br
-, I
-, CH
3COO
-, CF
3COO
-, CF
3SO
3 -, HPO
4 2-, H
2PO
4 -, CH
3SO
3 -, HSO
4 -And ClO
4 -In a kind of.
2, the method for claim 1, it is characterized in that described one or more ionic liquids, mol ratio between two kinds of ionic liquids is that 0.1-10, three kinds of mol ratios between the ionic liquid are (1-10): (1-10): any ratio (1-10), ionic liquid mostly is three kinds most.
3, the method for claim 1, the precursor that it is characterized in that the silica gel of described bag borne ionic liquid are positive silicic acid tetraalkyl esters.
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| CN 200710307475 CN101471153A (en) | 2007-12-28 | 2007-12-28 | Production method for silica gel encapsulated ion liquid solid state electrolyte material |
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|---|---|---|---|
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102473530A (en) * | 2009-08-03 | 2012-05-23 | 索尼公司 | Electrochemical capacitor |
| CN104466237A (en) * | 2014-12-09 | 2015-03-25 | 上海交通大学 | Composite mesoporous silica (IL/SiO2) for encapsulating ionic liquid and preparation and application thereof |
| CN104466243A (en) * | 2014-12-09 | 2015-03-25 | 上海交通大学 | Composite all-solid-state polymer electrolyte and preparation method thereof |
| CN106423075A (en) * | 2016-11-14 | 2017-02-22 | 齐鲁工业大学 | Silica gel immobilization functionalized ionic liquid adsorbing agent, preparation method and application |
| CN109585889A (en) * | 2018-11-29 | 2019-04-05 | 江苏师范大学 | A kind of preparation method of ionic gel matrix proton exchange |
| CN109585890A (en) * | 2018-11-29 | 2019-04-05 | 江苏师范大学 | High temperature proton exchange film fuel cell ionic gel base electrolyte and preparation method thereof |
-
2007
- 2007-12-28 CN CN 200710307475 patent/CN101471153A/en active Pending
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102473530A (en) * | 2009-08-03 | 2012-05-23 | 索尼公司 | Electrochemical capacitor |
| CN104466237A (en) * | 2014-12-09 | 2015-03-25 | 上海交通大学 | Composite mesoporous silica (IL/SiO2) for encapsulating ionic liquid and preparation and application thereof |
| CN104466243A (en) * | 2014-12-09 | 2015-03-25 | 上海交通大学 | Composite all-solid-state polymer electrolyte and preparation method thereof |
| CN106423075A (en) * | 2016-11-14 | 2017-02-22 | 齐鲁工业大学 | Silica gel immobilization functionalized ionic liquid adsorbing agent, preparation method and application |
| CN109585889A (en) * | 2018-11-29 | 2019-04-05 | 江苏师范大学 | A kind of preparation method of ionic gel matrix proton exchange |
| CN109585890A (en) * | 2018-11-29 | 2019-04-05 | 江苏师范大学 | High temperature proton exchange film fuel cell ionic gel base electrolyte and preparation method thereof |
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