CN108258328A - A kind of preparation method of colloidal electrolyte of lead acid accumulator - Google Patents
A kind of preparation method of colloidal electrolyte of lead acid accumulator Download PDFInfo
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- H—ELECTRICITY
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- 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
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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
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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 belongs to Lead-acid Battery Technology fields, especially a kind of preparation method of colloidal electrolyte of lead acid accumulator, solve the problems, such as that colloidal electrolyte aquation lamination is serious in the prior art, resistance is big, short life, the preparation method includes the following steps：Disperse after nano silicon dioxide and distilled water are mixed, then the temperature reaction of methylate trimethoxy silane, obtains mixed liquor A；Sulfate, nano oxidized boron, 1 pi-allyl, 3 methylimidazole villaumite, sodium sulfate of polyethenoxy ether of fatty alcohol and remaining distilled water are stirred, obtain mixed liquid B；Dimethicone, lubricating grease and sulfuric acid are added in mixed liquid B, mix to obtain mixed liquor C；Add stabilizer after mixed liquor A is mixed with mixed liquor C, be uniformly mixed to obtain the final product.Preparation method of the present invention is simple, and preparation condition is mild, at low cost, and gained colloidal electrolyte thixotropy is good, and internal resistance is small, and no leakage acid, non smoke, moisture dissipation speed is slow, and service life is long, is worthy to be popularized.
Description
Technical field
The present invention relates to Lead-acid Battery Technology field more particularly to a kind of preparation sides of colloidal electrolyte of lead acid accumulator
Method.
Background technology
In accumulator, lead-acid accumulator has that technology maturation, cheap, charge-discharge performance is good, safe to use etc. excellent
Point, and most important stabilized power source and DC power supply are used as, it is widely used in aviation, railway, automobile, ship, communication, gold
Melt, in the industry-by-industries such as national defence, it has also become indispensable energy products in social production and human lives.Lead-acid accumulator refers to
Electrode is mainly made of lead and its oxide, and electrolyte is a kind of accumulator of sulfuric acid solution.Under lead-acid accumulator discharge condition,
Anode main component is brown lead oxide, and cathode main component is lead；Under charged state, the main component of positive and negative anodes is sulfuric acid
Lead.Gelled lead acid battery is the improvement to the common lead-acid accumulator of liquid electrolyte, has been replaced sulfuric acid with colloidal electrolyte
Electrolyte makes moderate progress compared with common batteries in safety, charge capacity, discharge performance and service life etc., is to plumbic acid
One larger innovating reform of accumulator.In the prior art, gelled lead acid battery uses Ludox more with colloidal electrolyte
Be formulated, due to raw material select and dosage it is lack of standardization, the limitation of existing colloidal electrolyte preparation process, leads in addition
Cause its generally existing gelation time is short, gel strength is poor, thixotropy is poor, gel stability is poor, colloidal electrolyte aquation layering
The defects of phenomenon is serious, resistance is big, short life.Number of patent application 201110455808.5 discloses a kind of colloidal lead-acid storage battery
Electrolyte, preparation method and lead-acid accumulator, the colloidal electrolyte of lead acid accumulator include：The sulphur of 40wt%~47wt%
Acid；The nano silicon dioxide of 0.8wt%~1wt%；The hydroxyethyl cellulose of 0.1wt%~0.5wt%；0.1wt%~
The ammonium sulfate of 0.5wt%；The phosphoric acid of 0.1wt%~0.5wt%；Surplus is water.The patent forms lead using hydroxyethyl cellulose
Acid accumulator colloidal electrolyte, though during it can effectively reduce battery use to a certain degree electrolyte moisture loss, carry
The cycle life of plumbic acid accumulator, but the phosphoric acid added in its formula can reduce the appearance of some initial cycles of lead-acid accumulator
Amount reduces the speed that lead sulfate is oxidized to brown lead oxide so that the poor performance at low temperatures of lead-acid accumulator, there are gel stabilities
The defects of difference, short life.Based on above statement, the present invention proposes a kind of preparation method of colloidal electrolyte of lead acid accumulator.
Invention content
The purpose of the present invention is to solve exist in the prior art gelation time is short, gel strength is poor, thixotropy is poor,
The problem of gel stability is poor, colloidal electrolyte aquation lamination is serious, resistance is big, short life, and a kind of plumbic acid proposed
The preparation method of storage-battery colloidal electrolyte.
A kind of preparation method of colloidal electrolyte of lead acid accumulator, includes the following steps：
S1, preparation prepare colloidal electrolyte of lead acid accumulator raw material, by weight percentage, including nano silicon dioxide
3~8%, methyltrimethoxysilane 0.02~0.06%, dimethicone 1~3%, sulfate 0.5~0.9%, nanometer
Boron oxide 0.2~0.5%, 1- pi-allyl -3- methylimidazole villaumites 0.3~0.7%, lubricating grease 0.08~0.15%, fatty alcohol
Polyethenoxy ether sodium sulfate 0.1~0.5%, stabilizer 0.1~0.3%, sulfuric acid 35~44%, surplus are distilled water；
S2, nano silicon dioxide is added in ultrasonic disperser, adds distilled water to the quality point of nano silicon dioxide
Number is 5~8%, after 12~20min of ultrasonic disperse, adds in methyltrimethoxysilane, 80~88 are warming up in ultrasonic disperse
DEG C, after reacting 20~40min, obtain mixed liquor A；
S3, by sulfate, nano oxidized boron, 1- pi-allyl -3- methylimidazole villaumites, sodium sulfate of polyethenoxy ether of fatty alcohol
It is added in blender jointly with remaining distilled water, 8~15min is stirred with the rotating speed of 350~500r/min, obtains mixed liquid B；
S4, it keeps the rotating speed in step S3 constant, dimethicone, lubricating grease and sulfuric acid is added to mixed liquor jointly
In B, after being uniformly mixed, mixed liquor C is obtained；
S5, mixed liquor A and mixed liquor C are added in glue making machine jointly, 20 is stirred with the rotating speed of 1000~1200r/min
~30min, then adds in stabilizer, continues to be uniformly mixed to get colloidal electrolyte.
Preferably, colloidal electrolyte of lead acid accumulator raw material is prepared in the step S1, by weight percentage, including
Nano silicon dioxide 4~7%, methyltrimethoxysilane 0.03~0.05%, dimethicone 1.5~2.5%, sulfate
0.6~0.8%, nano oxidized boron 0.3~0.4%, 1- pi-allyl -3- methylimidazole villaumites 0.4~0.6%, lubricating grease 0.1~
0.14%th, sodium sulfate of polyethenoxy ether of fatty alcohol 0.2~0.4%, stabilizer 0.15~0.25%, sulfuric acid 38~42%, surplus
For distilled water.
Preferably, colloidal electrolyte of lead acid accumulator raw material is prepared in the step S1, by weight percentage, including
Nano silicon dioxide 6%, methyltrimethoxysilane 0.04%, dimethicone 2%, sulfate 0.7%, nano oxidized boron
0.35%th, 1- pi-allyls -3- methylimidazole villaumites 0.5%, lubricating grease 0.12%, sodium sulfate of polyethenoxy ether of fatty alcohol 0.3%,
Stabilizer 0.2%, sulfuric acid 40%, surplus are distilled water.
Preferably, the density of sulfuric acid solution is 1.48~1.56g/cm in the step S13。
Preferably, it is 1~1.8 that sulfate, which is mass ratio, in the step S1:0.5~1.2:2~3:0.3~0.7:1.5
~2.5 lead sulfate, cobaltous sulfate, sodium sulphate, STANNOUS SULPHATE CRYSTALLINE and aluminum sulfate compounding agent.
Preferably, it is 1~30 that the stabilizer, which is mass ratio,:30~1 polyacrylamide and the group of carboxymethyl cellulose
Close object.
The preparation method of a kind of colloidal electrolyte of lead acid accumulator proposed by the present invention, using methyltrimethoxysilane pair
The nanometer titanium dioxide silicon emulsion of dispersion is modified, and can effectively improve the thermally and chemically stability of nano silicon dioxide, increase
Its specific surface area improves its reactivity and thixotropy；Sulfate addition can effectively prevent sulfation, increase electrode
Actual surface area enhances its corrosion resistance, inhibits the early stage capacity failure of lead-acid accumulator, improves the deeper cavity service life of battery；
The addition of 1- pi-allyl -3- methylimidazole villaumites and nano oxidized boron can reduce water loss, accelerate lead sulfate and be oxidized to dioxy
Change the speed of lead, increase the utilization rate of positive active material；The addition of lubricating grease and sodium sulfate of polyethenoxy ether of fatty alcohol accelerates
The migration of ion and gas, diffusion, make gel networks high resilience and thixotropy, avoid aquation lamination,
Sulfation can be effectively prevented, extends the service life of lead-acid accumulator；The stabilizer being eventually adding has good water suction, water conservation
With the effect for delaying colloid solidification, can effectively reduce the fluid loss of lead-acid accumulator, improve colloidal electrolyte stability,
Alleviate the aquation layering of colloidal electrolyte, convenient for the filling of colloidal electrolyte, preparation method of the present invention is simple, preparation condition temperature
With manufacturing cost is low, and gained colloidal electrolyte thixotropy is good, and internal resistance is small, without leakage acid, non smoke, moisture dissipation speed during charging
Slowly, service life is long, and pole plate corrosion and deformation, prevention active material can be inhibited to come off, be greatly improved lead-acid accumulator
Cycle life is worthy to be popularized.
Specific embodiment
The present invention is made with reference to specific embodiment further to explain.
Embodiment one
A kind of preparation method of colloidal electrolyte of lead acid accumulator proposed by the present invention, includes the following steps：
S1, preparation prepare colloidal electrolyte of lead acid accumulator raw material, by weight percentage, including nano silicon dioxide
8%th, methyltrimethoxysilane 0.06%, dimethicone 3%, sulfate 0.9%, nano oxidized boron 0.5%, 1- allyls
Base -3- methylimidazole villaumites 0.7%, lubricating grease 0.15%, sodium sulfate of polyethenoxy ether of fatty alcohol 0.5%, stabilizer 0.3%,
Sulfuric acid 44%, surplus are distilled water, and wherein the density of sulfuric acid solution is 1.56g/cm3, sulfate be that mass ratio is 1.8:1.2:
3:0.7:2.5 lead sulfate, cobaltous sulfate, sodium sulphate, STANNOUS SULPHATE CRYSTALLINE and aluminum sulfate compounding agent；Stabilizer is that mass ratio is 1:30
The composition of polyacrylamide and carboxymethyl cellulose；
S2, nano silicon dioxide is added in ultrasonic disperser, adds distilled water to the quality point of nano silicon dioxide
Number is 8%, after ultrasonic disperse 20min, adds in methyltrimethoxysilane, 88 DEG C are warming up in ultrasonic disperse, react 40min
Afterwards, mixed liquor A is obtained；
S3, by sulfate, nano oxidized boron, 1- pi-allyl -3- methylimidazole villaumites, sodium sulfate of polyethenoxy ether of fatty alcohol
It is added in blender jointly with remaining distilled water, 15min is stirred with the rotating speed of 500r/min, obtains mixed liquid B；
S4, it keeps the rotating speed in step S3 constant, dimethicone, lubricating grease and sulfuric acid is added to mixed liquor jointly
In B, after being uniformly mixed, mixed liquor C is obtained；
S5, mixed liquor A and mixed liquor C are added in glue making machine jointly, 30min are stirred with the rotating speed of 1200r/min, so
After add in stabilizer, continue to be uniformly mixed to get colloidal electrolyte.
Embodiment two
A kind of preparation method of colloidal electrolyte of lead acid accumulator proposed by the present invention, includes the following steps：
S1, preparation prepare colloidal electrolyte of lead acid accumulator raw material, by weight percentage, including nano silicon dioxide
6%th, methyltrimethoxysilane 0.04%, dimethicone 2%, sulfate 0.7%, nano oxidized boron 0.35%, 1- alkene
Propyl -3- methylimidazole villaumites 0.5%, lubricating grease 0.12%, sodium sulfate of polyethenoxy ether of fatty alcohol 0.3%, stabilizer
0.2%th, sulfuric acid 40%, surplus are distilled water, and wherein the density of sulfuric acid solution is 1.52g/cm3, sulfate be that mass ratio is
1.4:0.8:2.5:0.5:2 lead sulfate, cobaltous sulfate, sodium sulphate, STANNOUS SULPHATE CRYSTALLINE and aluminum sulfate compounding agent；Stabilizer is mass ratio
It is 1:1 polyacrylamide and the composition of carboxymethyl cellulose；
S2, nano silicon dioxide is added in ultrasonic disperser, adds distilled water to the quality point of nano silicon dioxide
Number is 6.5%, after ultrasonic disperse 16min, adds in methyltrimethoxysilane, 84 DEG C is warming up in ultrasonic disperse, reaction
After 30min, mixed liquor A is obtained；
S3, by sulfate, nano oxidized boron, 1- pi-allyl -3- methylimidazole villaumites, sodium sulfate of polyethenoxy ether of fatty alcohol
It is added in blender jointly with remaining distilled water, 12min is stirred with the rotating speed of 420r/min, obtains mixed liquid B；
S4, it keeps the rotating speed in step S3 constant, dimethicone, lubricating grease and sulfuric acid is added to mixed liquor jointly
In B, after being uniformly mixed, mixed liquor C is obtained；
S5, mixed liquor A and mixed liquor C are added in glue making machine jointly, 25min are stirred with the rotating speed of 1100r/min, so
After add in stabilizer, continue to be uniformly mixed to get colloidal electrolyte.
Embodiment three
A kind of preparation method of colloidal electrolyte of lead acid accumulator proposed by the present invention, includes the following steps：
S1, preparation prepare colloidal electrolyte of lead acid accumulator raw material, by weight percentage, including nano silicon dioxide
3%th, methyltrimethoxysilane 0.02%, dimethicone 1%, sulfate 0.5%, nano oxidized boron 0.2%, 1- allyls
Base -3- methylimidazole villaumites 0.3%, lubricating grease 0.08%, sodium sulfate of polyethenoxy ether of fatty alcohol 0.1%, stabilizer 0.1%,
Sulfuric acid 35%, surplus are distilled water, and wherein the density of sulfuric acid solution is 1.48g/cm3, sulfate be that mass ratio is 1:0.5:2:
0.3:1.5 lead sulfate, cobaltous sulfate, sodium sulphate, STANNOUS SULPHATE CRYSTALLINE and aluminum sulfate compounding agent；Stabilizer is that mass ratio is 30:1 it is poly-
The composition of acrylamide and carboxymethyl cellulose；
S2, nano silicon dioxide is added in ultrasonic disperser, adds distilled water to the quality point of nano silicon dioxide
Number is 5%, after ultrasonic disperse 12min, adds in methyltrimethoxysilane, 80 DEG C are warming up in ultrasonic disperse, react 20min
Afterwards, mixed liquor A is obtained；
S3, by sulfate, nano oxidized boron, 1- pi-allyl -3- methylimidazole villaumites, sodium sulfate of polyethenoxy ether of fatty alcohol
It is added in blender jointly with remaining distilled water, 8min is stirred with the rotating speed of 350r/min, obtains mixed liquid B；
S4, it keeps the rotating speed in step S3 constant, dimethicone, lubricating grease and sulfuric acid is added to mixed liquor jointly
In B, after being uniformly mixed, mixed liquor C is obtained；
S5, mixed liquor A and mixed liquor C are added in glue making machine jointly, 20min are stirred with the rotating speed of 1000r/min, so
After add in stabilizer, continue to be uniformly mixed to get colloidal electrolyte.
The stabilizer in above-described embodiment one and two is changed into polyacrylamide or carboxymethyl cellulose respectively, at other
In the case that part is constant, colloidal electrolyte of lead acid accumulator is made, comparative example one and two is set.
The colloidal electrolyte of lead acid accumulator prepared in the embodiment of the present invention one~tri- and comparative example one and two are tested respectively
The comprehensive performance of the colloidal electrolyte of lead acid accumulator of middle preparation obtains following parameter：
By above table it is found that using the combination of polyacrylamide and carboxymethyl cellulose in the embodiment of the present invention one~tri-
Object is stabilizer, and required colloidal electrolyte of lead acid accumulator is prepared, and comprehensive performance, which is far superior in comparative example one, adopts
It is to use carboxymethyl cellulose as colloidal lead-acid storage battery made of stabilizer in stabilizer and comparative example two with polyacrylamide
Electrolyte.
Using acid filling machine by the colloidal electrolyte of lead acid accumulator prepared in the embodiment of the present invention one~tri- and comparative example one,
The colloidal electrolyte of lead acid accumulator prepared in two is injected separately into battery, is obtained lead-acid accumulator, is detected lead acid storage battery respectively
The cycle life in pond obtains following result：
By above table it is found that using the combination of polyacrylamide and carboxymethyl cellulose in the embodiment of the present invention one~tri-
Object is stabilizer, and required colloidal electrolyte of lead acid accumulator is prepared, and the cycle life of manufactured lead-acid accumulator is remote
It is more than in comparative example one and uses polyacrylamide by carboxymethyl cellulose being used to be made of stabilizer in stabilizer and comparative example two
Manufactured lead-acid accumulator after colloidal electrolyte of lead acid accumulator.
Colloidal electrolyte of lead acid accumulator is prepared by above-described embodiment one, and utilizes acid filling machine by the lead-acid accumulator of preparation
Colloidal electrolyte is injected separately into battery, obtains lead-acid accumulator, and polyacrylamide and carboxymethyl are fine in stable testing agent respectively
The cycle life of the asynchronous lead-acid accumulator of mass ratio of element is tieed up, obtains following result：
As seen from the above table：The mass ratio of polyacrylamide and carboxymethyl cellulose is 1 in stabilizer:10-10:When 1, it is made
Lead-acid accumulator electrolyte injection battery in obtain cycle life of lead-acid accumulator longer, particularly when polypropylene in stabilizer
The mass ratio of amide and carboxymethyl cellulose is 1:When 1, plumbic acid storage is obtained in lead-acid accumulator electrolyte injection battery obtained
Battery cycle life longest.
The foregoing is only a preferred embodiment of the present invention, but protection scope of the present invention be not limited thereto,
Any one skilled in the art in the technical scope disclosed by the present invention, according to the technique and scheme of the present invention and its
Inventive concept is subject to equivalent substitution or change, should be covered by the protection scope of the present invention.
Claims (6)
1. a kind of preparation method of colloidal electrolyte of lead acid accumulator, which is characterized in that include the following steps：
S1, preparation prepare colloidal electrolyte of lead acid accumulator raw material, by weight percentage, including nano silicon dioxide 3~
8%th, methyltrimethoxysilane 0.02~0.06%, dimethicone 1~3%, sulfate 0.5~0.9%, nano oxidized
Boron 0.2~0.5%, 1- pi-allyl -3- methylimidazole villaumites 0.3~0.7%, lubricating grease 0.08~0.15%, fatty alcohol polyoxy
Ethylene ether sodium sulfate 0.1~0.5%, stabilizer 0.1~0.3%, sulfuric acid 35~44%, surplus are distilled water；
S2, nano silicon dioxide is added in ultrasonic disperser, the mass fraction for adding distilled water to nano silicon dioxide is 5
After~8%, 12~20min of ultrasonic disperse, methyltrimethoxysilane is added in, 80~88 DEG C are warming up in ultrasonic disperse, instead
After answering 20~40min, mixed liquor A is obtained；
S3, by sulfate, nano oxidized boron, 1- pi-allyl -3- methylimidazole villaumites, sodium sulfate of polyethenoxy ether of fatty alcohol with it is surplus
Remaining distilled water is added in blender jointly, is stirred 8~15min with the rotating speed of 350~500r/min, is obtained mixed liquid B；
S4, it keeps the rotating speed in step S3 constant, dimethicone, lubricating grease and sulfuric acid is added in mixed liquid B jointly,
After being uniformly mixed, mixed liquor C is obtained；
S5, mixed liquor A and mixed liquor C are added in glue making machine jointly, with the rotating speed of 1000~1200r/min stirring 20~
Then 30min adds in stabilizer, continue to be uniformly mixed to get colloidal electrolyte.
A kind of 2. preparation method of colloidal electrolyte of lead acid accumulator according to claim 1, which is characterized in that the step
Colloidal electrolyte of lead acid accumulator raw material is prepared in rapid S1, by weight percentage, including nano silicon dioxide 4~7%, first
Base trimethoxy silane 0.03~0.05%, dimethicone 1.5~2.5%, sulfate 0.6~0.8%, nano oxidized boron
0.3~0.4%, 1- pi-allyls -3- methylimidazole villaumites 0.4~0.6%, lubricating grease 0.1~0.14%, aliphatic alcohol polyethenoxy
Ether sodium sulfate 0.2~0.4%, stabilizer 0.15~0.25%, sulfuric acid 38~42%, surplus are distilled water.
A kind of 3. preparation method of colloidal electrolyte of lead acid accumulator according to claim 1, which is characterized in that the step
Colloidal electrolyte of lead acid accumulator raw material is prepared in rapid S1, by weight percentage, including nano silicon dioxide 6%, methyl
Trimethoxy silane 0.04%, dimethicone 2%, sulfate 0.7%, nano oxidized boron 0.35%, 1- pi-allyl -3- first
Base imidazoles villaumite 0.5%, lubricating grease 0.12%, sodium sulfate of polyethenoxy ether of fatty alcohol 0.3%, stabilizer 0.2%, sulfuric acid
40%th, surplus is distilled water.
A kind of 4. preparation method of colloidal electrolyte of lead acid accumulator according to claim 1, which is characterized in that the step
The density of sulfuric acid solution is 1.48~1.56g/cm in rapid S13。
A kind of 5. preparation method of colloidal electrolyte of lead acid accumulator according to claim 1, which is characterized in that the step
It is 1~1.8 that sulfate, which is mass ratio, in rapid S1:0.5~1.2:2~3:0.3~0.7:1.5~2.5 lead sulfate, cobaltous sulfate,
The compounding agent of sodium sulphate, STANNOUS SULPHATE CRYSTALLINE and aluminum sulfate.
6. the preparation method of a kind of colloidal electrolyte of lead acid accumulator according to claim 1, which is characterized in that described steady
It is 1~30 that determine agent, which be mass ratio,:30~1 polyacrylamide and the composition of carboxymethyl cellulose.
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