CN106159352A - A kind of preparation method of accumulator sol-electrolyte - Google Patents
A kind of preparation method of accumulator sol-electrolyte Download PDFInfo
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- CN106159352A CN106159352A CN201610746869.XA CN201610746869A CN106159352A CN 106159352 A CN106159352 A CN 106159352A CN 201610746869 A CN201610746869 A CN 201610746869A CN 106159352 A CN106159352 A CN 106159352A
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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
- H01M10/06—Lead-acid accumulators
- H01M10/08—Selection of materials as electrolytes
- H01M10/10—Immobilising of electrolyte
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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
- H01M2300/0085—Immobilising or gelification of electrolyte
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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
The invention discloses the preparation method of a kind of accumulator sol-electrolyte, belong to battery material technical field.The present invention produces acid clear liquid first with distiller grains inoculation acetic acid bacteria fermentation, dropped in the mixed liquors such as Triton X-100, prepare microemulsion, again tetraethyl orthosilicate is dropped in microemulsion, hydrolyze, with acetone as demulsifier, by dried for precipitate washing calcining after filtration, obtain white-amorphous superfines, it is mixed homogeneously with sulphuric acid etc. and prepares accumulator sol-electrolyte.The present invention makes full use of the amorphous superfines that microemulsion prepares and forms network structure in the electrolyte, and its amorphous state makes electrolyte be difficult to aquation, and stability is greatly enhanced, and thixotropy is excellent, and service life, more conventional accumulator improved more than 2 times.
Description
Technical field
The invention discloses the preparation method of a kind of accumulator sol-electrolyte, belong to battery material technical field.
Background technology
At present the electric bicycle battery overwhelming majority uses the valve-control sealed lead battery of 12V/12Ah, often group two or
Three, its electrical property can meet requirement substantially, it is desirable to the cry continuing to improve is the service life for battery.Now
The valve-regulatcd lead-acid battery life-span of most manufacturer production was at about 1 year, and fluctuation range is bigger.Break through for improving cycle life
The behave of property almost gets one's back to the wall, and the most desirably uses colloidal electrolyte.Several years, for colloid electricity
Solve matter and carried out a lot of research, and make encouraging progress, reach really can expand the stage of use.
A kind of Silica hydrogel of colloidal electrolyte, it is by Ludox and certain density bright sulfur acid mixed configuration
Become.When Ludox produces polyreaction formation network structure, being wrapped up in therein by a large amount of sulfuric acid solutions and form gel, this is just
It it is colloidal electrolyte.
At present, the electrolyte of colloid plumbic storage battery is mainly dispersed in sulfur by a certain amount of Ludox or aerosil
The colloid formed in acid.The quality of colloidal electrolyte performance is the key factor affecting colloid storage battery capacity and cycle life.
So that colloidal electrolyte existence and stability prepared by Ludox is poor, thixotropy is the best, easy aquation, the shortcoming such as it is easily cracked.Gas phase dioxy
Colloidal electrolyte prepared by SiClx is relatively costly, and what the performance of electrolyte was heavily dependent on aerosil utilizes journey
Degree, and easily there are the problems such as battery capacity is low, internal resistance is big, the easy aquation of colloid in the accumulator irrigated with this colloid.
Summary of the invention
Present invention mainly solves technical problem is that: occur during preparation and use for traditional storage battery electrolyte
Poor stability, the easy aquation of colloid, and thixotropy is the best, causes the problem that service life is shorter, it is provided that a kind of accumulator is molten
Glue electrolyte preparation method, the present invention produces acid clear liquid first with distiller grains inoculation acetic acid bacteria fermentation, is dropped to gather
In the mixed liquors such as ethylene glycol octyl phenyl ether, prepare microemulsion, then tetraethyl orthosilicate dropped in microemulsion, hydrolyze,
With acetone as demulsifier, by dried for precipitate washing calcining after filtration, obtain white-amorphous superfines, by itself and sulphuric acid etc.
Mix homogeneously prepares accumulator sol-electrolyte.The present invention makes full use of amorphous superfines that microemulsion prepares at electricity
Xie Zhizhong forms network structure, and its amorphous state makes electrolyte be difficult to aquation, and stability is greatly enhanced, and thixotropy is excellent
Different, service life, more conventional accumulator improved more than 2 times.
In order to solve above-mentioned technical problem, the technical solution adopted in the present invention is:
(1) weigh distiller grains 2～3kg, add in the fermentation tank filling 3～5L deionized waters, with 300～500r/min rotating speed stirrings
Mixing 20～30min, is seeded to acetic acid bacteria in fermentation tank material by the 6～8% of inoculum concentration, standing for fermentation 5～7 days subsequently, from
The heart separates, and removes lower sediment, collects to obtain upper strata acidity clear liquid；
(2) 200～220mL Triton X-100s, 150～180mL hexanol, 600～650mL hexamethylenes are measured successively
Alkane, adds in beaker, then beaker is placed in digital display tests the speed in constant temperature blender with magnetic force, is 40～45 DEG C in temperature, and rotating speed is 400
～under the conditions of 500r/min, constant temperature stirring mixing 15～20min, under constant temperature stirring, be slowly added dropwise in beaker 50～
60mL above-mentioned gained upper strata acidity clear liquid, controls to drip off in 15～20min；
(3) waiting to drip complete, continue stirring mixing 8～12min, obtain microemulsion, then raise temperature to 50～55 DEG C, regulation rotating speed is extremely
600～800r/min, under constant temperature stirring, in microemulsion, drip 80～100mL tetraethyl orthosilicates, control 10～
Drip off in 15min, wait to drip complete, continue constant temperature stirring reaction 3～5h；
(4) question response terminates, and under stirring, adds 50～70mL acetone, stir with 350～400r/min rotating speeds in beaker
Mix mixing 3～5min, stand 45～60min, sucking filtration, remove filtrate, with absolute ethanol washing filter cake 3～5 times, then filter cake is turned
Enter in baking oven, be dried to constant weight under the conditions of 105～110 DEG C, subsequently dried filter cake is proceeded to Muffle furnace, in 680～750
Under the conditions of DEG C, calcine 60～90min, cool to room temperature with the furnace, obtain white-amorphous superfines；
(5) counting by weight, in batch mixer, being sequentially added into 85～100 parts of mass fractions is 58～60% sulphuric acid, 6～8 parts
Above-mentioned gained white-amorphous superfines, 1～3 part of polyacrylamide, 0.6～0.8 part of glycerol, with 1600～1800r/min
Rotating speed high-speed stirred mixing 8～10h, obtains accumulator sol-electrolyte.
The application process of the present invention: gained accumulator sol-electrolyte of the present invention is poured in accumulator electrolyzer, until
Colloid liquid level exceedes pole plate group 2～4cm, adds sol-electrolyte quality 0.2～the phosphoric acid (mass fraction is 85%) of 0.4%, quiet
Put, treat colloid solidification about 2～4h in battery, be charged 3～5h,.Gained accumulator is followed through 400～500 discharge and recharges
After ring, there is not dry and cracked and glue segregation phenomenon in electrolyte, accumulator is tilted to four direction, surface electroless liquid seepage,
Through subsequent detection, cyclic endurance, up to 800～900 times, has wide market application foreground.
The invention has the beneficial effects as follows:
(1) gained accumulator sol-electrolyte of the present invention is applied in accumulator, can be effectively improved accumulator poor stability, the Yishui River
Change, the problem of thixotropy difference, there is self discharge little, the advantages such as capacity is high, resistance to deep discharge；
(2) utilizing accumulator prepared by electrolyte of the present invention, service life, more conventional accumulator improve more than 2 times, can be effective
Reducing electric motor car, the loss of automobile storage battery and replacement frequency, make accumulator material be fully used, having wide market should
Use prospect.
Detailed description of the invention
Weigh distiller grains 2～3kg, add in the fermentation tank filling 3～5L deionized waters, stir with 300～500r/min rotating speeds
Mix mixing 20～30min, by the 6～8% of inoculum concentration, acetic acid bacteria be seeded in fermentation tank material subsequently, standing for fermentation 5～7 days,
Centrifugation, removes lower sediment, collects to obtain upper strata acidity clear liquid；Measure 200～220mL Polyethylene Glycol octyl phenyls successively
Ether, 150～180mL hexanol, 600～650mL hexamethylene, add in beaker, then beaker is placed in digital display tests the speed constant temperature magnetic force
In agitator, it is 40～45 DEG C in temperature, under the conditions of rotating speed is 400～500r/min, constant temperature stirring mixing 15～20min,
Under constant temperature stirring, in beaker, it is slowly added dropwise 50～60mL above-mentioned gained upper strata acidity clear liquids, controls in 15～20min
Drip off；Waiting to drip complete, continue stirring mixing 8～12min, obtain microemulsion, then raise temperature to 50～55 DEG C, regulation rotating speed is extremely
600～800r/min, under constant temperature stirring, in microemulsion, drip 80～100mL tetraethyl orthosilicates, control 10～
Drip off in 15min, wait to drip complete, continue constant temperature stirring reaction 3～5h；Question response terminates, under stirring, in beaker
Add 50～70mL acetone, with 350～400r/min rotating speed stirring mixing 3～5min, standing 45～60min, sucking filtration, remove filter
Liquid, with absolute ethanol washing filter cake 3～5 times, then proceeds to filter cake in baking oven, is dried to constant weight under the conditions of 105～110 DEG C,
Subsequently dried filter cake is proceeded to Muffle furnace, under the conditions of 680～750 DEG C, calcines 60～90min, cool to room temperature with the furnace,
Obtain white-amorphous superfines；Count by weight, in batch mixer, be sequentially added into 85～100 parts of mass fractions be 58～
60% sulphuric acid, 6～8 parts of above-mentioned gained white-amorphous superfines, 1～3 part of polyacrylamide, 0.6～0.8 part of glycerol, with
1600～1800r/min rotating speed high-speed stirred mixing 8～10h, obtain accumulator sol-electrolyte.
Example 1
Weigh distiller grains 2kg, add in the fermentation tank filling 3L deionized water, with 300r/min rotating speed stirring mixing 20min, subsequently
By the 6% of inoculum concentration, acetic acid bacteria is seeded in fermentation tank material, standing for fermentation 5 days, centrifugation, removes lower sediment, collect
Obtain upper strata acidity clear liquid；Measure 200mL Triton X-100,150mL hexanol, 600mL hexamethylene successively, add and burn
In Bei, then beaker is placed in digital display tests the speed in constant temperature blender with magnetic force, be 40 DEG C in temperature, under the conditions of rotating speed is 400r/min,
Constant temperature stirring mixing 15min, under constant temperature stirring, is slowly added dropwise 50mL above-mentioned gained upper strata acidity clear liquid in beaker,
Control to drip off in 15min；Waiting to drip complete, continue stirring mixing 8min, obtain microemulsion, then raise temperature to 50 DEG C, regulation turns
Speed is to 600r/min, under constant temperature stirring, drips 80mL tetraethyl orthosilicate, control to drip off in 10min in microemulsion,
Wait to drip complete, continue constant temperature stirring reaction 3h；Question response terminates, and under stirring, adds 50mL acetone in beaker, with
350r/min rotating speed stirring mixing 3min, stands 45min, sucking filtration, removes filtrate, with absolute ethanol washing filter cake 3 times, then will filter
Cake proceeds in baking oven, is dried to constant weight under the conditions of 105 DEG C, subsequently dried filter cake is proceeded to Muffle furnace, in 680 DEG C of conditions
Under, calcine 60min, cool to room temperature with the furnace, obtain white-amorphous superfines；Count by weight, in batch mixer, successively
Adding 85 parts of mass fractions is 58% sulphuric acid, and 6 parts of above-mentioned gained white-amorphous superfines, 1 part of polyacrylamide, 0.6 part sweet
Oil, mixes 8h with 1600r/min rotating speed high-speed stirred, obtains accumulator sol-electrolyte.
Gained accumulator sol-electrolyte of the present invention is poured in accumulator electrolyzer, until colloid liquid level exceedes pole plate group
2cm, adds the phosphoric acid (mass fraction is 85%) of sol-electrolyte quality 0.2%, stands, treats colloid solidification about 2h in battery, enter
Row charging 3h,.Gained accumulator is after 400 charge and discharge cycles, and dry and cracked and glue segregation phenomenon does not occurs in electrolyte, will
Accumulator tilts to four direction, surface electroless liquid seepage, and through subsequent detection, cyclic endurance, up to 800 times, has wide
Wealthy market application foreground.
Example 2
Weigh distiller grains 2.5kg, add in the fermentation tank filling 4L deionized water, mix 25min with the stirring of 400r/min rotating speed, with
By the 7% of inoculum concentration, acetic acid bacteria is seeded in fermentation tank material afterwards, standing for fermentation 6 days, centrifugation, removes lower sediment, receive
Collect to obtain upper strata acidity clear liquid；Measure 210mL Triton X-100,160mL hexanol, 620mL hexamethylene successively, add
In beaker, then beaker is placed in digital display testing the speed in constant temperature blender with magnetic force, be 42 DEG C in temperature, rotating speed is 450r/min condition
Under, constant temperature stirring mixing 18min, under constant temperature stirring, in beaker, it is slowly added dropwise 55mL above-mentioned gained upper strata acid clear
Liquid, controls to drip off in 18min；Wait to drip complete, continue stirring mixing 10min, obtain microemulsion, then raise temperature to 52 DEG C, adjust
Joint rotating speed is to 700r/min, under constant temperature stirring, drips 90mL tetraethyl orthosilicate, control in 12min in microemulsion
Drip off, wait to drip complete, continue constant temperature stirring reaction 4h；Question response terminates, and under stirring, adds 60mL third in beaker
Ketone, with 380r/min rotating speed stirring mixing 4min, stands 55min, sucking filtration, removes filtrate, with absolute ethanol washing filter cake 4 times,
Again filter cake is proceeded in baking oven, be dried to constant weight under the conditions of 108 DEG C, subsequently dried filter cake is proceeded to Muffle furnace, in 700
Under the conditions of DEG C, calcine 80min, cool to room temperature with the furnace, obtain white-amorphous superfines；Count by weight, at batch mixer
In, being sequentially added into 95 parts of mass fractions is 59% sulphuric acid, 7 parts of above-mentioned gained white-amorphous superfines, 2 parts of polyacrylamides,
0.7 part of glycerol, mixes 9h with 1700r/min rotating speed high-speed stirred, obtains accumulator sol-electrolyte.
Gained accumulator sol-electrolyte of the present invention is poured in accumulator electrolyzer, until colloid liquid level exceedes pole plate group
3cm, adds the phosphoric acid (mass fraction is 85%) of sol-electrolyte quality 0.3%, stands, treats colloid solidification about 3h in battery, enter
Row charging 4h,.Gained accumulator is after 450 charge and discharge cycles, and dry and cracked and glue segregation phenomenon does not occurs in electrolyte, will
Accumulator tilts to four direction, surface electroless liquid seepage, and through subsequent detection, cyclic endurance, up to 860 times, has wide
Wealthy market application foreground.
Example 3
Weigh distiller grains 3kg, add in the fermentation tank filling 5L deionized water, with 500r/min rotating speed stirring mixing 30min, subsequently
By the 8% of inoculum concentration, acetic acid bacteria is seeded in fermentation tank material, standing for fermentation 7 days, centrifugation, removes lower sediment, collect
Obtain upper strata acidity clear liquid；Measure 220mL Triton X-100,180mL hexanol, 650mL hexamethylene successively, add and burn
In Bei, then beaker is placed in digital display tests the speed in constant temperature blender with magnetic force, be 45 DEG C in temperature, under the conditions of rotating speed is 500r/min,
Constant temperature stirring mixing 20min, under constant temperature stirring, is slowly added dropwise 60mL above-mentioned gained upper strata acidity clear liquid in beaker,
Control to drip off in 20min；Waiting to drip complete, continue stirring mixing 12min, obtain microemulsion, then raise temperature to 55 DEG C, regulation turns
Speed is to 800r/min, under constant temperature stirring, drips 100mL tetraethyl orthosilicate in microemulsion, controls to drip in 15min
Complete, wait to drip complete, continue constant temperature stirring reaction 5h；Question response terminates, and under stirring, adds 70mL third in beaker
Ketone, with 400r/min rotating speed stirring mixing 5min, stands 60min, sucking filtration, removes filtrate, with absolute ethanol washing filter cake 5 times,
Again filter cake is proceeded in baking oven, be dried to constant weight under the conditions of 110 DEG C, subsequently dried filter cake is proceeded to Muffle furnace, in 750
Under the conditions of DEG C, calcine 90min, cool to room temperature with the furnace, obtain white-amorphous superfines；Count by weight, at batch mixer
In, being sequentially added into 100 parts of mass fractions is 60% sulphuric acid, 8 parts of above-mentioned gained white-amorphous superfines, 3 parts of polyacrylamides
Amine, 0.8 part of glycerol, mix 10h with 1800r/min rotating speed high-speed stirred, obtain accumulator sol-electrolyte.
Gained accumulator sol-electrolyte of the present invention is poured in accumulator electrolyzer, until colloid liquid level exceedes pole plate group
4cm, adds the phosphoric acid (mass fraction is 85%) of sol-electrolyte quality 0.4%, stands, treats colloid solidification about 4h in battery, enter
Row charging 5h,.Gained accumulator is after 500 charge and discharge cycles, and dry and cracked and glue segregation phenomenon does not occurs in electrolyte, will
Accumulator tilts to four direction, surface electroless liquid seepage, and through subsequent detection, cyclic endurance, up to 900 times, has wide
Wealthy market application foreground.
Claims (1)
1. the preparation method of an accumulator sol-electrolyte, it is characterised in that concrete preparation process is:
(1) weigh distiller grains 2～3kg, add in the fermentation tank filling 3～5L deionized waters, with 300～500r/min rotating speed stirrings
Mixing 20～30min, is seeded to acetic acid bacteria in fermentation tank material by the 6～8% of inoculum concentration, standing for fermentation 5～7 days subsequently, from
The heart separates, and removes lower sediment, collects to obtain upper strata acidity clear liquid；
(2) 200～220mL Triton X-100s, 150～180mL hexanol, 600～650mL hexamethylenes are measured successively
Alkane, adds in beaker, then beaker is placed in digital display tests the speed in constant temperature blender with magnetic force, is 40～45 DEG C in temperature, and rotating speed is 400
～under the conditions of 500r/min, constant temperature stirring mixing 15～20min, under constant temperature stirring, be slowly added dropwise in beaker 50～
60mL above-mentioned gained upper strata acidity clear liquid, controls to drip off in 15～20min；
(3) waiting to drip complete, continue stirring mixing 8～12min, obtain microemulsion, then raise temperature to 50～55 DEG C, regulation rotating speed is extremely
600～800r/min, under constant temperature stirring, in microemulsion, drip 80～100mL tetraethyl orthosilicates, control 10～
Drip off in 15min, wait to drip complete, continue constant temperature stirring reaction 3～5h；
(4) question response terminates, and under stirring, adds 50～70mL acetone, stir with 350～400r/min rotating speeds in beaker
Mix mixing 3～5min, stand 45～60min, sucking filtration, remove filtrate, with absolute ethanol washing filter cake 3～5 times, then filter cake is turned
Enter in baking oven, be dried to constant weight under the conditions of 105～110 DEG C, subsequently dried filter cake is proceeded to Muffle furnace, in 680～750
Under the conditions of DEG C, calcine 60～90min, cool to room temperature with the furnace, obtain white-amorphous superfines；
(5) counting by weight, in batch mixer, being sequentially added into 85～100 parts of mass fractions is 58～60% sulphuric acid, 6～8 parts
Above-mentioned gained white-amorphous superfines, 1～3 part of polyacrylamide, 0.6～0.8 part of glycerol, with 1600～1800r/min
Rotating speed high-speed stirred mixing 8～10h, obtains accumulator sol-electrolyte.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109273749A (en) * | 2018-09-20 | 2019-01-25 | 王景硕 | A kind of preparation method of the dedicated colloidal electrolyte of flow battery |
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| JPS54114730A (en) * | 1978-02-28 | 1979-09-07 | Shin Kobe Electric Machinery | Method of producing lead storage battery |
| KR101009995B1 (en) * | 2007-05-30 | 2011-01-21 | 오션 베이 인터내셔널 리미티드 | Lead acid battery having gelled electrolyte |
| CN102394318A (en) * | 2011-10-31 | 2012-03-28 | 福州大学 | Colloid electrolyte preparation technology and glue distribution machine thereof for plumbic acid colloid storage battery |
| CN105449293A (en) * | 2014-09-30 | 2016-03-30 | 佛山市高明区(中国科学院)新材料专业中心 | Gel electrolyte used for lead-acid storage battery and preparation method for gel electrolyte |
-
2016
- 2016-08-29 CN CN201610746869.XA patent/CN106159352B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS54114730A (en) * | 1978-02-28 | 1979-09-07 | Shin Kobe Electric Machinery | Method of producing lead storage battery |
| KR101009995B1 (en) * | 2007-05-30 | 2011-01-21 | 오션 베이 인터내셔널 리미티드 | Lead acid battery having gelled electrolyte |
| CN102394318A (en) * | 2011-10-31 | 2012-03-28 | 福州大学 | Colloid electrolyte preparation technology and glue distribution machine thereof for plumbic acid colloid storage battery |
| CN105449293A (en) * | 2014-09-30 | 2016-03-30 | 佛山市高明区(中国科学院)新材料专业中心 | Gel electrolyte used for lead-acid storage battery and preparation method for gel electrolyte |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109273749A (en) * | 2018-09-20 | 2019-01-25 | 王景硕 | A kind of preparation method of the dedicated colloidal electrolyte of flow battery |
| CN109273749B (en) * | 2018-09-20 | 2021-12-21 | 黄春美 | Preparation method of special colloidal electrolyte for flow battery |
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