CN101947422A - Alkaline solution gel and preparation method as well as application thereof - Google Patents
Alkaline solution gel and preparation method as well as application thereof Download PDFInfo
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- CN101947422A CN101947422A CN201010261425XA CN201010261425A CN101947422A CN 101947422 A CN101947422 A CN 101947422A CN 201010261425X A CN201010261425X A CN 201010261425XA CN 201010261425 A CN201010261425 A CN 201010261425A CN 101947422 A CN101947422 A CN 101947422A
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- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
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- Y02E60/10—Energy storage using batteries
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Abstract
The invention discloses alkaline solution gel and a preparation method as well as applications thereof. The alkaline solution gel is prepared by the following steps: taking a polyol mono-acetal compound to be added into an alkaline aqueous solution with the concentration of 0.1-12mol/L, so that the mass fraction of the polyol mono-acetal compound is 0.5%-10%; and heating until the polyol mono-acetal compound is fully dissolved. The polyol mono-acetal compound is generated by condensation reaction of polyol compounds containing 4-6 hydroxyl groups and aromatic aldehyde compounds. Experiments prove that the alkaline solution gel is stable in an alkaline environment, and can be used for avoiding the leakage of electrolyte and solving the problem of low conductivity of solid electrolyte in an alkaline battery.
Description
Technical field
The present invention relates to a kind of aqueous slkali gel and preparation method thereof and purposes.
Background technology
From the seventies 1,3; 2, since the synthetic patent of 4-dibenzal sorbitol was come out, the production of this type of sorbitol acetal compounds and development had obtained bigger progress.They are generally obtained through acetalation by an one's share of expenses for a joint undertaking sorbierite and two molecule aromatic aldehydes.Because it has the characteristic that can make the nucleus moulding and make the organic solvent gelation, is used as additive in industries such as plastics, coating, binding agent, printing ink, daily use chemicals and medical articles for use.Sorbierite bisacetal compounds is used as the gel factor in recent years always and studies, and Kobayashi etc. (Journal of Japan Rheology Society, 1989,17:104) be mainly used to gel organic solvent and polymer.(Bull.Chem.Soc.Jpn. such as Yamasaki, 1995,68:146-151) to DBS (1,3:2,4-(two benzals)-D-sorbierite) carries out discovering of gelling performance, the gelling performance of DBS mainly is the intermolecular hydrogen bond action between the acetal oxygen of 6-position hydroxyl and another one's share of expenses for a joint undertaking in the DBS molecule, and the hydroxyl of 5-position mainly is to form intramolecular hydrogen bond with acetal oxygen with molecule; Behind the HM of 6-position, lose the gel activity, and 5-position hydroxylating is little to the gelatification influence.Holt is harvested, and bright (CN11011389C) prepares and synthesized polyalcohol monoacetal compounds, by at water, contain and add components such as the gel factor and dispersant in the aqueous solution of inorganic salts or polymer and make its gel.At present, do not see the report for preparing the aqueous slkali gel with the polyalcohol aldehyde compound.
Electrolyte is an important component part of DSSC, lithium ion battery, ultracapacitor and electrochromic display device (ECD).The electrical conductivity of aqueous electrolyte is higher, but operating voltage is low, and electrochemical window is young, and H takes place easily
2And O
2The side reaction of separating out, poor performance at low temperatures.The organic solvent electrolyte has higher decomposition voltage (general 2～4 volts), helps obtaining higher energy density, and the wider range of work, but electrical conductivity is low than aqueous electrolyte, has that electrolyte is volatile, the problem of easy leakage.Solid electrolyte has good reliability, no electrolyte leakage, high-energy-density and can realize advantages such as ultra-thin shape, but the most solid electrolyte exists electrical conductivity lower, the shortcoming that the contact condition between electrode and the electrolyte is very poor.
Compare with above-mentioned electrolyte, gel electrolyte is being caught luminous energy, electric conductivity and at aspects such as stability and workabilities special advantages is being arranged.There is the lower problem of electrolytic salt solubility in polymeric matrix in the gel electrolyte that is made of polymeric matrix, causes near the crystallization of the electrolytic salt of polarizing electrode during charging.And by using the little molecule organogel factor, will contain the gel electrolyte that the organic solvent of supporting electrolyte is made, have stable performance, no electrolyte leakage, electrode and electrolyte contact condition better, can make advantage such as arbitrary shape.But make the aqueous slkali gel as the little molecular gel factor and the application in the alkaline cell electrolyte still is not reported with polyalcohol monoacetal compound.
Summary of the invention
The purpose of this invention is to provide a kind of aqueous slkali gel.
Another object of the present invention provides a kind of preparation method of aqueous slkali gel.
The 3rd purpose of the present invention provides a kind of purposes of aqueous slkali gel.
Technical scheme of the present invention is summarized as follows:
A kind of aqueous slkali gel, make with following method:
Getting polyalcohol monoacetal compound joins in the aqueous alkali that concentration is 0.1～12mol/L, the mass fraction that makes polyalcohol monoacetal compound is 0.5%～10%, be heated to it and dissolve fully, described polyalcohol monoacetal compound is that the multicomponent alcoholics compound and the aromatic aldehyde compound condensation reaction that contain 4-6 hydroxyl generate.
Described alkali is preferably potassium hydroxide or NaOH.
Described multicomponent alcoholics compound is preferably sorbierite, xylitol, sweet mellow wine or pentaerythrite.
Described aromatic aldehyde compounds is benzaldehyde, 2-tolyl aldehyde, 3-tolyl aldehyde, 4-tolyl aldehyde, 3,4-dimethylbenzaldehyde, 4-ethylo benzene formaldehyde, 4-cumene formaldehyde, 4-tert-butyl benzene formaldehyde, 2-chlorobenzaldehyde, 4-chlorobenzaldehyde, 2,3-dichlorobenzaldehyde, 2,4-dichlorobenzaldehyde, 3,4-dichlorobenzaldehyde, 4-fluorobenzaldehyde or 4-cyanobenzaldehyde.
A kind of preparation method of aqueous slkali gel may further comprise the steps:
Getting polyalcohol monoacetal compound joins in the aqueous alkali that concentration is 0.1～12mol/L, the mass fraction that makes polyalcohol monoacetal compound is 0.5%～10%, be heated to it and dissolve fully, described polyalcohol monoacetal compound is that the multicomponent alcoholics compound and the aromatic aldehyde compound condensation reaction that contain 4-6 hydroxyl generate.
Described alkali is preferably potassium hydroxide or NaOH.
Described multicomponent alcoholics compound is preferably sorbierite, xylitol, sweet mellow wine or pentaerythrite.
Described aromatic aldehyde compounds is preferably benzaldehyde, 2-tolyl aldehyde, 3-tolyl aldehyde, 4-tolyl aldehyde, 3,4-dimethylbenzaldehyde, 4-ethylo benzene formaldehyde, 4-cumene formaldehyde, 4-tert-butyl benzene formaldehyde, 2-chlorobenzaldehyde, 4-chlorobenzaldehyde, 2,3-dichlorobenzaldehyde, 2,4-dichlorobenzaldehyde, 3,4-dichlorobenzaldehyde, 4-fluorobenzaldehyde or 4-cyanobenzaldehyde.
A kind of aqueous slkali gel is as the purposes of battery electrolyte.
Experimental results show that: aqueous slkali of the present invention coagulates very stable in alkaline environment, is used for the leakage that alkaline battery can be avoided electrolyte, can solve problems such as the electrical conductivity of solid electrolyte is low simultaneously again.
The specific embodiment
The phase transition temperature method of testing of aqueous slkali gel:
At φ=12mm, in the teat glass of L=120mm, add polyalcohol monoacetal compound and aqueous alkali, be heated to sample with alcolhol burner and be uniform solution.After treating the abundant cooled and solidified of sample, be 0.88g with quality, diameter is that the little firm ball of 0.57cm is put into this small test tube, places on the testing sample, forms temperature with separating of gel of fusing point instrument test.Adopt the heating rate of 1.0 ℃/min, observe the sample in the test tube, when liquid object was oozed out, the small ball liquid level that just submerges was the gel initial solution and forms temperature (Td
i); When sample all turned to liquid, little firm ball fell into the test tube bottom, and the temperature of this moment is whole the separating of gel and forms temperature (Td
f).
Embodiment 1
The potassium hydroxide aqueous solution of getting concentration and be 6mol/L joins φ=12mm, in the teat glass of L=120mm, add the sorbierite list 3-tolyl aldehyde that contracts, making the contract mass fraction of 3-tolyl aldehyde of sorbierite list is 1%, heating is dissolved it fully, make it naturally cool to room temperature behind the thing clear to be mixed, make a kind of aqueous slkali gel.
The phase transition temperature of the aqueous slkali gel of present embodiment preparation is 68.2～70.1 ℃.
Embodiment 2
The potassium hydroxide aqueous solution of getting concentration and be 6mol/L joins φ=12mm, in the teat glass of L=120mm, add the sorbierite list 3-tolyl aldehyde that contracts, making the contract mass fraction of 3-tolyl aldehyde of sorbierite list is 2%, heating is dissolved it fully, make it naturally cool to room temperature behind the thing clear to be mixed, make a kind of aqueous slkali gel.
The phase transition temperature of the aqueous slkali gel of present embodiment preparation is 72.7～74.2 ℃.
Embodiment 3
The potassium hydroxide aqueous solution of getting concentration and be 6mol/L joins φ=12mm, in the teat glass of L=120mm, add the sorbierite list 3-tolyl aldehyde that contracts, making the contract mass fraction of 3-tolyl aldehyde of sorbierite list is 5%, heating is dissolved it fully, make it naturally cool to room temperature behind the thing clear to be mixed, make a kind of aqueous slkali gel.
The phase transition temperature of the aqueous slkali gel of present embodiment preparation is 73.7～75.2 ℃.
Embodiment 4
The potassium hydroxide aqueous solution of getting concentration and be 6mol/L joins φ=12mm, in the teat glass of L=120mm, add the sorbierite list and contract 3, the 4-dimethylbenzaldehyde, make the sorbierite list contract 3, the mass fraction of 4-dimethylbenzaldehyde is 0.5%, and heating is dissolved it fully, make it naturally cool to room temperature behind the thing clear to be mixed, make a kind of aqueous slkali gel.
The phase transition temperature of a kind of aqueous slkali gel of present embodiment preparation is 41.7～102.3 ℃.
Embodiment 5
The potassium hydroxide aqueous solution of getting concentration and be 6mol/L joins φ=12mm, in the teat glass of L=120mm, add the sorbierite list and contract 3, the 4-dimethylbenzaldehyde, make the sorbierite list contract 3, the mass fraction of 4-dimethylbenzaldehyde is 1%, and heating is dissolved it fully, make it naturally cool to room temperature behind the thing clear to be mixed, make a kind of aqueous slkali gel.
The phase transition temperature of a kind of aqueous slkali gel of present embodiment preparation is 65.0～104.6 ℃.
Embodiment 6
The potassium hydroxide aqueous solution of getting concentration and be 6mol/L joins φ=12mm, in the teat glass of L=120mm, add the sorbierite list and contract 3, the 4-dimethylbenzaldehyde, make the sorbierite list contract 3, the mass fraction of 4-dimethylbenzaldehyde is 2%, and heating is dissolved it fully, make it naturally cool to room temperature behind the thing clear to be mixed, make a kind of aqueous slkali gel.
The phase transition temperature of a kind of aqueous slkali gel of present embodiment preparation is 104.3～109.2 ℃.
Embodiment 7
The potassium hydroxide aqueous solution of getting concentration and be 6mol/L joins φ=12mm, in the teat glass of L=120mm, add the sorbierite list and contract 3, the 4-dimethylbenzaldehyde, make the sorbierite list contract 3, the mass fraction of 4-dimethylbenzaldehyde is 5%, and heating is dissolved it fully, make it naturally cool to room temperature behind the thing clear to be mixed, make a kind of aqueous slkali gel.
The phase transition temperature of a kind of aqueous slkali gel of present embodiment preparation is 109.4～110.2 ℃.
Embodiment 8
The potassium hydroxide aqueous solution of getting concentration and be 1mol/L joins φ=12mm, in the teat glass of L=120mm, add the sorbierite list and contract 3, the 4-dimethylbenzaldehyde, make the sorbierite list contract 3, the mass fraction of 4-dimethylbenzaldehyde is 2%, and heating is dissolved it fully, make it naturally cool to room temperature behind the thing clear to be mixed, make a kind of aqueous slkali gel.
The phase transition temperature of a kind of aqueous slkali gel of present embodiment preparation is 71.1～76.9 ℃.
Embodiment 9
The potassium hydroxide aqueous solution of getting concentration and be 3mol/L joins φ=12mm, in the teat glass of L=120mm, add the sorbierite list and contract 3, the 4-dimethylbenzaldehyde, make the sorbierite list contract 3, the mass fraction of 4-dimethylbenzaldehyde is 2%, and heating is dissolved it fully, make it naturally cool to room temperature behind the thing clear to be mixed, make a kind of aqueous slkali gel.
The phase transition temperature of a kind of aqueous slkali gel of present embodiment preparation is 68.7～72.7 ℃.
Embodiment 10
The potassium hydroxide aqueous solution of getting concentration and be 9mol/L joins φ=12mm, in the teat glass of L=120mm, add the sorbierite list and contract 3, the 4-dimethylbenzaldehyde, make the sorbierite list contract 3, the mass fraction of 4-dimethylbenzaldehyde is 2%, and heating is dissolved it fully, make it naturally cool to room temperature behind the thing clear to be mixed, make a kind of aqueous slkali gel.
The phase transition temperature of a kind of aqueous slkali gel of present embodiment preparation is 104.4～110.0 ℃.
Embodiment 11
The sodium hydrate aqueous solution of getting concentration and be 9mol/L joins φ=12mm, in the teat glass of L=120mm, add the xylitol list 2-tolyl aldehyde that contracts, making the contract mass fraction of 2-tolyl aldehyde of xylitol list is 10%, heating is dissolved it fully, make it naturally cool to room temperature behind the thing clear to be mixed, make a kind of aqueous slkali gel.
The phase transition temperature of a kind of aqueous slkali gel of present embodiment preparation is 78.4～103.2 ℃.
Embodiment 12
The sodium hydrate aqueous solution of getting concentration and be 9mol/L joins φ=12mm, in the teat glass of L=120mm, add the sweet mellow wine list 4-fluorobenzaldehyde that contracts, making the contract mass fraction of 4-fluorobenzaldehyde of sweet mellow wine list is 5%, heating is dissolved it fully, make it naturally cool to room temperature behind the thing clear to be mixed, make a kind of aqueous slkali gel.
The phase transition temperature of a kind of aqueous slkali gel of present embodiment preparation is 69.3～110.2 ℃.
Embodiment 13
The sodium hydrate aqueous solution of getting concentration and be 12mol/L joins φ=12mm, in the teat glass of L=120mm, add the pentaerythrite list 4-cyanobenzaldehyde that contracts, making the contract mass fraction of 4-cyanobenzaldehyde of pentaerythrite list is 6%, heating is dissolved it fully, make it naturally cool to room temperature behind the thing clear to be mixed, make a kind of aqueous slkali gel.
The phase transition temperature of a kind of aqueous slkali gel of present embodiment preparation is 81.2～109.6 ℃.
Embodiment 14
The sodium hydrate aqueous solution of getting concentration and be 9mol/L joins φ=12mm, in the teat glass of L=120mm, add sweet mellow wine list condensing benzaldehyde, the mass fraction that makes sweet mellow wine list condensing benzaldehyde is 8%, heating is dissolved it fully, make it naturally cool to room temperature behind the thing clear to be mixed, make a kind of aqueous slkali gel.
The phase transition temperature of a kind of aqueous slkali gel of present embodiment preparation is 67.6～101.4 ℃.
Embodiment 15
The sodium hydrate aqueous solution of getting concentration and be 0.1mol/L joins φ=12mm, in the teat glass of L=120mm, add the sweet mellow wine list 2-chlorobenzaldehyde that contracts, the mass fraction that makes sweet mellow wine list condensing benzaldehyde is 8%, heating is dissolved it fully, make it naturally cool to room temperature behind the thing clear to be mixed, make a kind of aqueous slkali gel.
The phase transition temperature of a kind of aqueous slkali gel of present embodiment preparation is 71.3～102.4 ℃.
Can also use 4-tolyl aldehyde, 4-ethylo benzene formaldehyde, 4-cumene formaldehyde, 4-tert-butyl benzene formaldehyde, 4-chlorobenzaldehyde, 2,3-dichlorobenzaldehyde, 2,4-dichlorobenzaldehyde or 3, the 4-dichlorobenzaldehyde substitutes the 2-chlorobenzaldehyde in the present embodiment, make the corresponding alkali solution gel, after testing, its phase transition temperature is between 60～110 ℃.
Claims (9)
1. aqueous slkali gel is characterized in that making with following method:
Getting polyalcohol monoacetal compound joins in the aqueous alkali that concentration is 0.1～12mol/L, the mass fraction that makes polyalcohol monoacetal compound is 0.5%～10%, be heated to it and dissolve fully, described polyalcohol monoacetal compound is that the multicomponent alcoholics compound and the aromatic aldehyde compound condensation reaction that contain 4-6 hydroxyl generate.
2. a kind of aqueous slkali gel according to claim 1 is characterized in that described alkali is potassium hydroxide or NaOH.
3. a kind of aqueous slkali gel according to claim 1 is characterized in that described multicomponent alcoholics compound is sorbierite, xylitol, sweet mellow wine or pentaerythrite.
4. a kind of aqueous slkali gel according to claim 1, it is characterized in that described aromatic aldehyde compounds is benzaldehyde, 2-tolyl aldehyde, 3-tolyl aldehyde, 4-tolyl aldehyde, 3,4-dimethylbenzaldehyde, 4-ethylo benzene formaldehyde, 4-cumene formaldehyde, 4-tert-butyl benzene formaldehyde, 2-chlorobenzaldehyde, 4-chlorobenzaldehyde, 2,3-dichlorobenzaldehyde, 2,4-dichlorobenzaldehyde, 3,4-dichlorobenzaldehyde, 4-fluorobenzaldehyde or 4-cyanobenzaldehyde.
5. the preparation method of an aqueous slkali gel, its feature may further comprise the steps:
Getting polyalcohol monoacetal compound joins in the aqueous alkali that concentration is 0.1～12mol/L, the mass fraction that makes polyalcohol monoacetal compound is 0.5%～10%, be heated to it and dissolve fully, described polyalcohol monoacetal compound is that the multicomponent alcoholics compound and the aromatic aldehyde compound condensation reaction that contain 4-6 hydroxyl generate.
6. the preparation method of a kind of aqueous slkali gel according to claim 5 is characterized in that described alkali is potassium hydroxide or NaOH.
7. the preparation method of a kind of aqueous slkali gel according to claim 5 is characterized in that described multicomponent alcoholics compound is sorbierite, xylitol, sweet mellow wine or pentaerythrite.
8. the preparation method of a kind of aqueous slkali gel according to claim 5, it is characterized in that described aromatic aldehyde compounds is benzaldehyde, 2-tolyl aldehyde, 3-tolyl aldehyde, 4-tolyl aldehyde, 3,4-dimethylbenzaldehyde, 4-ethylo benzene formaldehyde, 4-cumene formaldehyde, 4-tert-butyl benzene formaldehyde, 2-chlorobenzaldehyde, 4-chlorobenzaldehyde, 2,3-dichlorobenzaldehyde, 2,4-dichlorobenzaldehyde, 3,4-dichlorobenzaldehyde, 4-fluorobenzaldehyde or 4-cyanobenzaldehyde.
9. a kind of aqueous slkali gel of claim 1 is as the purposes of battery electrolyte.
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| CN201010261425XA CN101947422B (en) | 2010-08-24 | 2010-08-24 | Alkaline solution gel and preparation method as well as application thereof |
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| CN201010261425XA CN101947422B (en) | 2010-08-24 | 2010-08-24 | Alkaline solution gel and preparation method as well as application thereof |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106898843A (en) * | 2015-12-17 | 2017-06-27 | 中国科学院大连化学物理研究所 | A kind of metal-air batteries electrolyte and its preparation and application |
| CN108250459A (en) * | 2018-01-17 | 2018-07-06 | 泰山医学院 | A kind of hydrogel with multiple stimulation response and its preparation method and application |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH05314968A (en) * | 1992-05-12 | 1993-11-26 | Fuji Elelctrochem Co Ltd | Alkaline battery |
| CN101531358A (en) * | 2009-04-28 | 2009-09-16 | 湖南理工学院 | Method for preparing porous carbon electrode material used for super capacitor |
-
2010
- 2010-08-24 CN CN201010261425XA patent/CN101947422B/en not_active Expired - Fee Related
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH05314968A (en) * | 1992-05-12 | 1993-11-26 | Fuji Elelctrochem Co Ltd | Alkaline battery |
| CN101531358A (en) * | 2009-04-28 | 2009-09-16 | 湖南理工学院 | Method for preparing porous carbon electrode material used for super capacitor |
Non-Patent Citations (2)
| Title |
|---|
| 《Journal of Materials Chemistry》 20040518 Nils Mohmeyer etal Quasi-solid-state dye sensitized solar cells with 1,3:2,4-di-O-benzylidene-D-sorbitol derivatives as low molecular weight organic gelators 1905-1909 1-9 , 第14期 2 * |
| 《化学通报》 20051231 侯仲轲 等 有机低分子凝胶因子 643-649 1-9 , 第9期 2 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106898843A (en) * | 2015-12-17 | 2017-06-27 | 中国科学院大连化学物理研究所 | A kind of metal-air batteries electrolyte and its preparation and application |
| CN108250459A (en) * | 2018-01-17 | 2018-07-06 | 泰山医学院 | A kind of hydrogel with multiple stimulation response and its preparation method and application |
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