CN108258328B - Preparation method of lead-acid storage battery colloidal electrolyte - Google Patents
Preparation method of lead-acid storage battery colloidal electrolyte Download PDFInfo
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- CN108258328B CN108258328B CN201810198663.7A CN201810198663A CN108258328B CN 108258328 B CN108258328 B CN 108258328B CN 201810198663 A CN201810198663 A CN 201810198663A CN 108258328 B CN108258328 B CN 108258328B
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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
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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
Abstract
The invention belongs to the technical field of lead-acid storage batteries, in particular to a preparation method of a lead-acid storage battery colloidal electrolyte, which solves the problems of serious hydration and delamination phenomenon, large resistance and short service life of the colloidal electrolyte in the prior art, and comprises the following steps: mixing and dispersing nano silicon dioxide and distilled water, and then adding methyltrimethoxysilane for heating reaction to obtain a mixed solution A; stirring and mixing sulfate, nano boron oxide, 1-allyl-3-methylimidazole chloride, fatty alcohol-polyoxyethylene ether sodium sulfate and the rest of distilled water to obtain a mixed solution B; adding dimethyl polysiloxane, lubricating grease and sulfuric acid into the mixed solution B, and mixing to obtain a mixed solution C; and mixing the mixed solution A and the mixed solution C, adding a stabilizer, and uniformly mixing to obtain the composite material. The preparation method is simple, the preparation conditions are mild, the cost is low, the prepared colloidal electrolyte has good thixotropy, small internal resistance, no acid leakage, no smoke, low water loss speed and long service life, and is worthy of popularization.
Description
Technical Field
The invention relates to the technical field of lead-acid storage batteries, in particular to a preparation method of a lead-acid storage battery colloidal electrolyte.
Background
Among the storage batteries, the lead-acid storage battery has the advantages of mature technology, low price, good charge and discharge performance, safe use and the like, is widely applied to various industries such as aviation, railway, automobile, ship, communication, finance, national defense and the like as the most main stable power supply and direct-current power supply, and becomes an indispensable energy product in social production and human life. Lead-acid storage battery is a storage battery with electrodes mainly made of lead and lead oxide and electrolyte of sulfuric acid solution. In the discharge state of the lead-acid storage battery, the main component of the positive electrode is lead dioxide, and the main component of the negative electrode is lead; in a charged state, the main components of the positive electrode and the negative electrode are lead sulfate. The colloid lead-acid accumulator is an improvement on the common lead-acid accumulator with liquid electrolyte, and the colloid electrolyte is used to replace sulfuric acid electrolyte, so that it has improved safety, capacity, discharge performance and service life. In the prior art, colloidal electrolytes for colloidal lead-acid storage batteries are mostly prepared from silica sol, and due to the nonstandard selection and dosage of raw materials and the limitation of the existing preparation process of the colloidal electrolytes, the colloidal lead-acid storage batteries generally have the defects of short gelation time, poor gel strength, poor thixotropy, poor gel stability, serious hydration and delamination phenomena of the colloidal electrolytes, large resistance, short service life and the like. Patent application No. 201110455808.5 discloses a lead-acid storage battery gel electrolyte, a preparation method thereof and a lead-acid storage battery, wherein the lead-acid storage battery gel electrolyte comprises: 40 to 47 weight percent of sulfuric acid; 0.8 wt% -1 wt% of nano silicon dioxide; 0.1 to 0.5 weight percent of hydroxyethyl cellulose; 0.1 to 0.5 weight percent of ammonium sulfate; 0.1 to 0.5 weight percent of phosphoric acid; the balance being water. According to the lead-acid storage battery colloid electrolyte formed by the hydroxyethyl cellulose, although the loss of electrolyte moisture in the use process of the battery can be effectively reduced to a certain extent, the cycle life of the lead-acid storage battery is prolonged, the phosphoric acid added in the formula can reduce the initial cyclic capacity of the lead-acid storage battery, and the speed of oxidizing lead sulfate into lead dioxide is reduced, so that the low-temperature performance of the lead-acid storage battery is poor, and the defects of poor gel stability, short service life and the like exist. Based on the statement, the invention provides a preparation method of a lead-acid storage battery colloidal electrolyte.
Disclosure of Invention
The invention aims to solve the problems of short gelation time, poor gel strength, poor thixotropy, poor gel stability, serious hydration and delamination phenomena of a colloidal electrolyte, large resistance and short service life in the prior art, and provides a preparation method of a lead-acid storage battery colloidal electrolyte.
A preparation method of lead-acid storage battery colloidal electrolyte comprises the following steps:
s1, preparing a raw material for preparing a lead-acid storage battery colloidal electrolyte, which comprises, by weight, 3-8% of nano silicon dioxide, 0.02-0.06% of methyltrimethoxysilane, 1-3% of dimethylpolysiloxane, 0.5-0.9% of sulfate, 0.2-0.5% of nano boron oxide, 0.3-0.7% of 1-allyl-3-methylimidazolium chloride, 0.08-0.15% of lubricating grease, 0.1-0.5% of fatty alcohol polyoxyethylene ether sodium sulfate, 0.1-0.3% of a stabilizer, 35-44% of sulfuric acid and the balance of distilled water;
s2, adding nano silicon dioxide into an ultrasonic disperser, adding distilled water until the mass fraction of the nano silicon dioxide is 5-8%, ultrasonically dispersing for 12-20 min, adding methyltrimethoxysilane, ultrasonically dispersing while heating to 80-88 ℃, and reacting for 20-40 min to obtain a mixed solution A;
s3, adding sulfate, nano boron oxide, 1-allyl-3-methylimidazole chloride salt, fatty alcohol-polyoxyethylene ether sodium sulfate and the rest of distilled water into a stirrer together, and stirring at the rotating speed of 350-500 r/min for 8-15 min to obtain a mixed solution B;
s4, keeping the rotating speed in the step S3 unchanged, adding the dimethyl polysiloxane, the lubricating grease and the sulfuric acid into the mixed solution B together, and stirring and mixing uniformly to obtain a mixed solution C;
and S5, adding the mixed solution A and the mixed solution C into a glue making machine together, stirring at the rotating speed of 1000-1200 r/min for 20-30 min, then adding a stabilizer, and continuously stirring and uniformly mixing to obtain the colloidal electrolyte.
Preferably, the raw material for preparing the lead-acid storage battery colloidal electrolyte in the step S1 comprises, by weight, 4-7% of nano silicon dioxide, 0.03-0.05% of methyltrimethoxysilane, 1.5-2.5% of dimethylpolysiloxane, 0.6-0.8% of sulfate, 0.3-0.4% of nano boron oxide, 0.4-0.6% of 1-allyl-3-methylimidazolium chloride, 0.1-0.14% of lubricating grease, 0.2-0.4% of sodium fatty alcohol polyoxyethylene ether sulfate, 0.15-0.25% of a stabilizer, 38-42% of sulfuric acid, and the balance of distilled water.
Preferably, the raw material for preparing the lead-acid storage battery colloidal electrolyte in step S1 includes, by weight, 6% of nano-silica, 0.04% of methyltrimethoxysilane, 2% of dimethylpolysiloxane, 0.7% of sulfate, 0.35% of nano-boron oxide, 0.5% of 1-allyl-3-methylimidazolium chloride, 0.12% of grease, 0.3% of sodium fatty alcohol polyoxyethylene ether sulfate, 0.2% of a stabilizer, 40% of sulfuric acid, and the balance of distilled water.
Preferably, the density of the sulfuric acid solution in the step S1 is 1.48-1.56 g/cm3。
Preferably, the sulfate in the step S1 is a compound agent of lead sulfate, cobalt sulfate, sodium sulfate, tin sulfate and aluminum sulfate in a mass ratio of 1-1.8: 0.5-1.2: 2-3: 0.3-0.7: 1.5-2.5.
Preferably, the stabilizer is a composition of polyacrylamide and carboxymethyl cellulose with a mass ratio of 1-30: 30-1.
According to the preparation method of the colloidal electrolyte of the lead-acid storage battery, disclosed by the invention, the dispersed nano-silica emulsion is modified by adopting methyl trimethoxy silane, so that the thermal and chemical stability of the nano-silica can be effectively improved, the specific surface area of the nano-silica is increased, and the reaction activity and thixotropy of the nano-silica are improved; the addition of the sulfate can effectively prevent sulfation, increase the actual surface area of the electrode, enhance the corrosion resistance of the electrode, inhibit the early capacity failure of the lead-acid storage battery and prolong the deep cycle life of the battery; the addition of the 1-allyl-3-methylimidazole chlorine salt and the nano boron oxide can reduce water loss, accelerate the oxidation of lead sulfate into lead dioxide and increase the utilization rate of positive active substances; the addition of the lubricating grease and the fatty alcohol-polyoxyethylene ether sodium sulfate accelerates the migration and diffusion of ions and gases, so that the gel network structure is rich in elasticity and thixotropy, the hydration layering phenomenon is avoided, the sulfation can be effectively prevented, and the service life of the lead-acid storage battery is prolonged; the added stabilizer has good effects of absorbing water, retaining water and delaying colloid solidification, can effectively reduce the water loss of the lead-acid storage battery, improves the stability of the colloid electrolyte, relieves the hydration layering of the colloid electrolyte, and is convenient for the filling of the colloid electrolyte.
Detailed Description
The present invention will be further illustrated with reference to the following specific examples.
Example one
The invention provides a preparation method of lead-acid storage battery colloidal electrolyte, which comprises the following steps:
s1, preparing a raw material for preparing a lead-acid storage battery colloidal electrolyte, which comprises 8% of nano silicon dioxide, 0.06% of methyltrimethoxysilane, 3% of dimethyl polysiloxane, 0.9% of sulfate, 0.5% of nano boron oxide, 0.7% of 1-allyl-3-methylimidazolium chloride, 0.15% of lubricating grease, 0.5% of fatty alcohol-polyoxyethylene ether sodium sulfate, 0.3% of stabilizer, 44% of sulfuric acid and the balance of distilled water by weight percentage, wherein the density of the sulfuric acid solution is 1.56g/cm3The sulfate is a compound agent of lead sulfate, cobalt sulfate, sodium sulfate, tin sulfate and aluminum sulfate with the mass ratio of 1.8:1.2:3:0.7: 2.5; the stabilizer is a composition of polyacrylamide and carboxymethyl cellulose with the mass ratio of 1: 30;
s2, adding nano silicon dioxide into an ultrasonic disperser, adding distilled water until the mass fraction of the nano silicon dioxide is 8%, ultrasonically dispersing for 20min, adding methyltrimethoxysilane, heating to 88 ℃ while ultrasonically dispersing, and reacting for 40min to obtain a mixed solution A;
s3, adding sulfate, nano boron oxide, 1-allyl-3-methylimidazole chloride salt, fatty alcohol-polyoxyethylene ether sodium sulfate and the residual distilled water into a stirrer together, and stirring at the rotating speed of 500r/min for 15min to obtain a mixed solution B;
s4, keeping the rotating speed in the step S3 unchanged, adding the dimethyl polysiloxane, the lubricating grease and the sulfuric acid into the mixed solution B together, and stirring and mixing uniformly to obtain a mixed solution C;
and S5, adding the mixed solution A and the mixed solution C into a glue making machine together, stirring at the rotating speed of 1200r/min for 30min, then adding a stabilizer, and continuously stirring and uniformly mixing to obtain the colloidal electrolyte.
Example two
The invention provides a preparation method of lead-acid storage battery colloidal electrolyte, which comprises the following steps:
s1, preparing a raw material for preparing a lead-acid storage battery colloidal electrolyte, which comprises, by weight, 6% of nano silicon dioxide, 0.04% of methyltrimethoxysilane, 2% of dimethylpolysiloxane, 0.7% of sulfate, 0.35% of nano boron oxide, 0.5% of 1-allyl-3-methylimidazolium chloride, 0.12% of lubricating grease, 0.3% of sodium fatty alcohol polyoxyethylene ether sulfate, 0.2% of a stabilizer, 40% of sulfuric acid and the balance of distilled water, wherein the density of the sulfuric acid solution is 1.52g/cm3The sulfate is a compound agent of lead sulfate, cobalt sulfate, sodium sulfate, tin sulfate and aluminum sulfate in a mass ratio of 1.4:0.8:2.5:0.5: 2; the stabilizer is a composition of polyacrylamide and carboxymethyl cellulose with the mass ratio of 1: 1;
s2, adding nano silicon dioxide into an ultrasonic disperser, adding distilled water until the mass fraction of the nano silicon dioxide is 6.5%, ultrasonically dispersing for 16min, adding methyltrimethoxysilane, heating to 84 ℃ while ultrasonically dispersing, and reacting for 30min to obtain a mixed solution A;
s3, adding sulfate, nano boron oxide, 1-allyl-3-methylimidazole chloride salt, fatty alcohol-polyoxyethylene ether sodium sulfate and the residual distilled water into a stirrer together, and stirring at the rotating speed of 420r/min for 12min to obtain a mixed solution B;
s4, keeping the rotating speed in the step S3 unchanged, adding the dimethyl polysiloxane, the lubricating grease and the sulfuric acid into the mixed solution B together, and stirring and mixing uniformly to obtain a mixed solution C;
and S5, adding the mixed solution A and the mixed solution C into a glue making machine together, stirring at the rotating speed of 1100r/min for 25min, then adding a stabilizer, and continuously stirring and uniformly mixing to obtain the colloidal electrolyte.
EXAMPLE III
The invention provides a preparation method of lead-acid storage battery colloidal electrolyte, which comprises the following steps:
s1, preparing raw materials for preparing the lead-acid storage battery colloidal electrolyte, wherein the raw materials comprise nano-dioxygen3% of silicon oxide, 0.02% of methyltrimethoxysilane, 1% of dimethylpolysiloxane, 0.5% of sulfate, 0.2% of nano boron oxide, 0.3% of 1-allyl-3-methylimidazolium chloride, 0.08% of lubricating grease, 0.1% of fatty alcohol-polyoxyethylene ether sodium sulfate, 0.1% of stabilizer, 35% of sulfuric acid and the balance of distilled water, wherein the density of the sulfuric acid solution is 1.48g/cm3The sulfate is a compound agent of lead sulfate, cobalt sulfate, sodium sulfate, tin sulfate and aluminum sulfate in a mass ratio of 1:0.5:2:0.3: 1.5; the stabilizer is a composition of polyacrylamide and carboxymethyl cellulose with the mass ratio of 30: 1;
s2, adding nano silicon dioxide into an ultrasonic disperser, adding distilled water until the mass fraction of the nano silicon dioxide is 5%, ultrasonically dispersing for 12min, adding methyltrimethoxysilane, ultrasonically dispersing while heating to 80 ℃, and reacting for 20min to obtain a mixed solution A;
s3, adding sulfate, nano boron oxide, 1-allyl-3-methylimidazole chloride salt, sodium fatty alcohol polyoxyethylene ether sulfate and the rest of distilled water into a stirrer together, and stirring at the rotating speed of 350r/min for 8min to obtain a mixed solution B;
s4, keeping the rotating speed in the step S3 unchanged, adding the dimethyl polysiloxane, the lubricating grease and the sulfuric acid into the mixed solution B together, and stirring and mixing uniformly to obtain a mixed solution C;
and S5, adding the mixed solution A and the mixed solution C into a glue making machine together, stirring at the rotating speed of 1000r/min for 20min, then adding a stabilizer, and continuously stirring and uniformly mixing to obtain the colloidal electrolyte.
The stabilizers in the first and second examples are respectively replaced by polyacrylamide or carboxymethyl cellulose, lead-acid battery colloidal electrolytes are prepared under the condition that other conditions are not changed, and the first and second comparative examples are set.
The lead-acid battery colloidal electrolyte prepared in the first to third examples of the invention and the lead-acid battery colloidal electrolyte prepared in the first and second comparative examples were tested for comprehensive performance, respectively, and the following parameters were obtained:
as can be seen from the above table, the required lead-acid battery colloidal electrolyte prepared by using the composition of polyacrylamide and carboxymethylcellulose as the stabilizer in the first to third examples of the invention has far better comprehensive properties than the lead-acid battery colloidal electrolyte prepared by using polyacrylamide as the stabilizer in the first comparative example and carboxymethylcellulose as the stabilizer in the second comparative example.
Respectively injecting the lead-acid storage battery colloidal electrolyte prepared in the first to third embodiments of the invention and the lead-acid storage battery colloidal electrolyte prepared in the first and second embodiments of the invention into a battery by using an acid filling machine to obtain lead-acid storage batteries, and respectively detecting the cycle life of the lead-acid storage batteries to obtain the following results:
from the above table, it can be seen that the lead-acid storage battery prepared by using the composition of polyacrylamide and carboxymethylcellulose as the stabilizer in the first to third embodiments of the present invention has a cycle life far longer than that of the lead-acid storage battery prepared by using polyacrylamide as the stabilizer in the first embodiment and using carboxymethylcellulose as the stabilizer in the second embodiment.
Preparing the lead-acid storage battery colloidal electrolyte according to the first embodiment, respectively injecting the prepared lead-acid storage battery colloidal electrolyte into a battery by using an acid filling machine to obtain the lead-acid storage battery, and respectively testing the cycle life of the lead-acid storage battery when the mass ratio of polyacrylamide to carboxymethylcellulose in the stabilizer is different, thereby obtaining the following results:
from the above table, it can be seen that: when the mass ratio of the polyacrylamide to the carboxymethyl cellulose in the stabilizer is 1:10-10:1, the prepared lead-acid storage battery electrolyte is injected into the battery to obtain the lead-acid storage battery with longer cycle life, and particularly when the mass ratio of the polyacrylamide to the carboxymethyl cellulose in the stabilizer is 1:1, the prepared lead-acid storage battery electrolyte is injected into the battery to obtain the lead-acid storage battery with the longest cycle life.
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art should be considered to be within the technical scope of the present invention, and the technical solutions and the inventive concepts thereof according to the present invention should be equivalent or changed within the scope of the present invention.
Claims (5)
1. The preparation method of the lead-acid storage battery colloidal electrolyte is characterized by comprising the following steps:
s1, preparing a raw material for preparing a lead-acid storage battery colloidal electrolyte, which comprises, by weight, 3-8% of nano silicon dioxide, 0.02-0.06% of methyltrimethoxysilane, 1-3% of dimethylpolysiloxane, 0.5-0.9% of sulfate, 0.2-0.5% of nano boron oxide, 0.3-0.7% of 1-allyl-3-methylimidazolium chloride, 0.08-0.15% of lubricating grease, 0.1-0.5% of fatty alcohol polyoxyethylene ether sodium sulfate, 0.1-0.3% of a stabilizer, 35-44% of a sulfuric acid solution and the balance of distilled water;
s2, adding nano silicon dioxide into an ultrasonic disperser, adding distilled water until the mass fraction of the nano silicon dioxide is 5-8%, ultrasonically dispersing for 12-20 min, adding methyltrimethoxysilane, ultrasonically dispersing while heating to 80-88 ℃, and reacting for 20-40 min to obtain a mixed solution A;
s3, adding sulfate, nano boron oxide, 1-allyl-3-methylimidazole chloride salt, fatty alcohol-polyoxyethylene ether sodium sulfate and the rest of distilled water into a stirrer together, and stirring at the rotating speed of 350-500 r/min for 8-15 min to obtain a mixed solution B;
s4, keeping the rotating speed in the step S3 unchanged, adding the dimethyl polysiloxane, the lubricating grease and the sulfuric acid solution into the mixed solution B together, and stirring and mixing uniformly to obtain mixed solution C;
s5, adding the mixed solution A and the mixed solution C into a glue making machine together, stirring at the rotating speed of 1000-1200 r/min for 20-30 min, then adding a stabilizer, and continuously stirring and uniformly mixing to obtain a colloidal electrolyte;
the density of the sulfuric acid solution in the step S1 is 1.48-1.56 g/cm 3.
2. The method for preparing the lead-acid storage battery colloidal electrolyte according to claim 1, wherein the raw materials for preparing the lead-acid storage battery colloidal electrolyte in the step S1 comprise, by weight, 4-7% of nano-silica, 0.03-0.05% of methyltrimethoxysilane, 1.5-2.5% of dimethylpolysiloxane, 0.6-0.8% of sulfate, 0.3-0.4% of nano-boron oxide, 0.4-0.6% of 1-allyl-3-methylimidazolium chloride, 0.1-0.14% of lubricating grease, 0.2-0.4% of sodium fatty alcohol polyoxyethylene ether sulfate, 0.15-0.25% of stabilizer, 38-42% of sulfuric acid solution, and the balance of distilled water.
3. The method of claim 1, wherein the raw materials for preparing the lead-acid battery colloidal electrolyte in step S1 comprise, by weight, 6% of nano-silica, 0.04% of methyltrimethoxysilane, 2% of dimethylpolysiloxane, 0.7% of sulfate, 0.35% of nano-boron oxide, 0.5% of 1-allyl-3-methylimidazolium chloride, 0.12% of grease, 0.3% of sodium fatty alcohol polyoxyethylene ether sulfate, 0.2% of a stabilizer, 40% of a sulfuric acid solution, and the balance of distilled water.
4. The method for preparing the lead-acid storage battery colloidal electrolyte according to claim 1, wherein the sulfate in the step S1 is a compound agent of lead sulfate, cobalt sulfate, sodium sulfate, tin sulfate and aluminum sulfate in a mass ratio of 1-1.8: 0.5-1.2: 2-3: 0.3-0.7: 1.5-2.5.
5. The preparation method of the lead-acid storage battery colloidal electrolyte according to claim 1, wherein the stabilizer is a composition of polyacrylamide and carboxymethylcellulose in a mass ratio of 1-30: 30-1.
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