CN108565503B - Lead-acid storage battery electrolyte and preparation method thereof - Google Patents
Lead-acid storage battery electrolyte and preparation method thereof Download PDFInfo
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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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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
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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
- H01M10/12—Construction or manufacture
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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
- H01M2300/0002—Aqueous electrolytes
- H01M2300/0005—Acid electrolytes
- H01M2300/0011—Sulfuric acid-based
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- Y02E60/10—Energy storage using batteries
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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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Abstract
The invention belongs to the technical field of lead-acid storage batteries, and particularly relates to a lead-acid storage battery electrolyte and a preparation method thereof. The electrolyte comprises electrolyte mother liquor and an additive, wherein the electrolyte mother liquor is prepared from the following raw materials in parts by weight: 45-50 parts of sulfuric acid; 10-15 parts of nano fumed silica; 3-4 parts of potassium sulfate; 3-4 parts of magnesium sulfate; 0.3-0.5 part of stannous sulfate; 6-8 parts of lithium sulfate; 0.01-0.05 part of cerium sulfate; 80-100 parts of deionized water; the additive is prepared from the following raw materials in parts by weight: 2-3 parts of hydroxyethyl cellulose; 0.1-0.5 part of carboxymethyl chitosan; 0.1-0.5 part of silicon dioxide whisker; the dosage of the additive is 8-12% of the mass of the electrolyte mother liquor. The lead-acid storage battery electrolyte can prolong the cycle life of a storage battery to over 620 times; the preparation method is scientific, reasonable, simple and feasible.
Description
Technical Field
The invention belongs to the technical field of lead-acid storage batteries, and particularly relates to a lead-acid storage battery electrolyte and a preparation method thereof.
Background
Lead acid batteries have been invented since 1859, and have been in history for over one hundred and fifty years to date. The lead-acid storage battery has the advantages of simple structure, stable performance, high safety, convenient use, easy obtainment of raw materials, low price and the like, is widely applied to a plurality of fields in national economy such as transportation, communication, national defense and the like, and becomes an indispensable energy product in social production and human life.
While many new batteries are beginning to appear, lead acid batteries have a position for replacement in many areas. The lead-acid storage battery comprises five major components, namely a positive electrode, a negative electrode, a diaphragm, electrolyte and a battery shell, wherein the electrolyte is one of main factors influencing the performance of the battery.
At present, after a lead-acid storage battery is used for a period of time, the charge acceptance is poor, the actual charge capacity and storage capacity are reduced, and the actual application is seriously influenced. In addition, the surface of the negative electrode is seriously sulfated, and the large-particle sulfate causes the mechanical deformation and expansion of the polar plate, thereby causing the performance loss of the battery; and the sponge lead cannot be effectively converted back, so that the cycle life of the battery is limited. Therefore, how to increase the service life of the battery is a problem to be solved urgently.
Chinese patent CN 104681881A discloses a lead-acid battery electrolyte, which is characterized in that the service life of a battery added with the electrolyte is only terminated after the battery is cycled for 200 times by adding a plurality of additives, thereby prolonging the service life of the battery. However, the additive contains a large amount of organic matters, is unstable in the electrolyte of a lead-acid storage battery, has limited solubility in the electrolyte, and has very limited improvement on the service life of the battery.
Disclosure of Invention
Aiming at the defects of the prior art, the invention aims to provide the lead-acid storage battery electrolyte which can effectively prolong the service life of a storage battery; the invention also provides a preparation method of the composition, which is scientific, reasonable, simple and feasible.
The lead-acid storage battery electrolyte comprises an electrolyte mother solution and an additive, wherein the electrolyte mother solution is prepared from the following raw materials in parts by weight:
the additive is prepared from the following raw materials in parts by weight:
2-3 parts of hydroxyethyl cellulose;
0.1-0.5 part of carboxymethyl chitosan;
0.1-0.5 part of silicon dioxide whisker;
the dosage of the additive is 8-12% of the mass of the electrolyte mother liquor.
Wherein:
the mass concentration of the sulfuric acid is 70-80%.
The particle size of the nano fumed silica is 25-40 nm.
The diameter of the silicon dioxide crystal whisker is 0.1-0.5 μm, and the length is 0.1-2 μm.
The preparation method of the lead-acid storage battery electrolyte comprises the following steps:
(1) preparing an electrolyte mother solution:
a. adding 30-45 parts of deionized water into a stirring kettle, adding nano fumed silica in batches, and stirring to obtain a silica mother solution;
b. adding the rest deionized water into the stirring kettle, adding potassium sulfate, magnesium sulfate, stannous sulfate, lithium sulfate and cerium sulfate, stirring until the potassium sulfate, the magnesium sulfate, the stannous sulfate, the lithium sulfate and the cerium sulfate are dissolved, adding sulfuric acid, and stirring to obtain sulfuric acid mother liquor;
c. adding the silicon dioxide mother liquor into sulfuric acid mother liquor, and uniformly stirring to obtain electrolyte mother liquor;
(2) adding hydroxyethyl cellulose and carboxymethyl chitosan into the electrolyte mother liquor, heating to 30-35 ℃, and stirring for 3-4 hours to obtain a colloid dispersion liquid;
(3) and (3) adding the silicon dioxide whiskers under continuous stirring, and then continuously stirring for 1-2 hours to obtain the lead-acid storage battery electrolyte.
In the step (2), the stirring speed is 500-1000 rpm.
In the step (3), the stirring speed is 3000-4000 rpm.
The nanometer fumed silica forms a nanometer silica particle framework which is mainly combined by hydrogen bonds in the colloid electrolyte. The hydrogen bonding has the advantages that the rheological property of the colloid has reversibility, and the phenomenon of hydration and delamination can not occur.
The hydroxyethyl cellulose is a non-ionic surfactant, has stronger water retention capacity and good flow regulation performance, and can effectively reduce the loss of electrolyte water in the use process of the battery, thereby prolonging the cycle life of the storage battery.
Carboxymethyl chitosan is a polyelectrolyte, and in an acidic environment, amino groups on molecules are converted into positive ions. In the discharge process of the battery, positive ions migrate to the surface of the negative electrode under the action of an electric field. In the migration process, due to the coordination effect of the carboxymethyl chitosan polyelectrolyte and the hydrogen sulfate radical, the hydrogen sulfate radical is effectively driven to migrate to the negative electrode, the migration speed of the hydrogen sulfate radical is improved, the charge and discharge performance of the storage battery is improved, the concentration of the hydrogen sulfate radical negative ions at the negative electrode is increased, the utilization rate of the negative electrode active substances is improved, and therefore the battery capacity is improved. The addition of the carboxymethyl chitosan improves the response speed of the sulfuric acid concentration in the colloidal electrolyte at the electrode interface layer, effectively improves the utilization efficiency of the active substance, and inhibits the sulfation of the active substance.
The silicon dioxide crystal whisker and the electrolyte system form hydrogen bond association, and under the shearing force with the rotating speed of 3000-4000 r/min, the silicon dioxide crystal whisker particles are quickly oriented along the external force, so that the colloidal electrolyte system is broken down, and the viscosity is quickly reduced. The smoothness of glue filling is greatly improved, the colloidal electrolyte with good gel performance is obtained, the gelation time is prolonged, the electrolyte has sufficient time to keep a flowing state after being prepared, the filling is convenient, the use process is not hydrated and layered, and the stability is good.
In conclusion, the beneficial effects of the invention are as follows:
(1) the lead-acid storage battery electrolyte comprises an additive, hydroxyethyl cellulose, carboxymethyl chitosan and silicon dioxide whiskers, and the synergistic effect of the additive, the hydroxyethyl cellulose, the carboxymethyl chitosan and the silicon dioxide whiskers prolongs the service life of the battery, so that the cycle life of the storage battery can be prolonged to more than 620 times.
(2) The lead-acid storage battery electrolyte contains the silicon dioxide whiskers, and the nano gas-phase silicon dioxide and the silicon dioxide whiskers act together to form a more stable mutually-interwoven net structure, so that the lead-acid storage battery electrolyte has stronger inhibition capability on glue separation, has good dispersibility and prolongs the cycle life of a storage battery.
(3) The additive has small dosage, and the adopted additive is stable in the lead-acid storage battery and cannot be oxidized to lose the effect.
(4) The preparation method is scientific, reasonable, simple and feasible, and is suitable for industrial large-scale production.
Detailed Description
The present invention will be further described with reference to the following examples.
All the starting materials used in the examples are commercially available.
Example 1
The electrolyte mother solution is prepared from the following raw materials in parts by weight:
the additive is prepared from the following raw materials in parts by weight:
2.5 parts of hydroxyethyl cellulose;
0.3 part of carboxymethyl chitosan;
0.3 part of silicon dioxide whisker;
the dosage of the additive is 10 percent of the mass of the electrolyte mother liquor.
The mass concentration of the sulfuric acid is 75%.
The particle size of the nano fumed silica is 25-40 nm.
The diameter of the silicon dioxide crystal whisker is 0.1-0.5 μm, and the length is 0.1-2 μm.
The preparation method comprises the following steps:
(1) preparing an electrolyte mother solution:
a. adding 36 parts of deionized water into a stirring kettle, adding nano fumed silica in batches, and stirring to obtain a silica mother solution;
b. adding the rest deionized water into the stirring kettle, adding potassium sulfate, magnesium sulfate, stannous sulfate, lithium sulfate and cerium sulfate, stirring until the potassium sulfate, the magnesium sulfate, the stannous sulfate, the lithium sulfate and the cerium sulfate are dissolved, adding sulfuric acid, and stirring to obtain sulfuric acid mother liquor;
c. adding the silicon dioxide mother liquor into sulfuric acid mother liquor, and uniformly stirring to obtain electrolyte mother liquor;
(2) adding hydroxyethyl cellulose and carboxymethyl chitosan into the electrolyte mother liquor, heating to 35 ℃, and stirring for 3 hours to obtain a colloid dispersion liquid;
(3) and (3) adding the silicon dioxide whiskers under continuous stirring, and then continuously stirring for 2 hours after the silicon dioxide whiskers are added to obtain the lead-acid storage battery electrolyte.
In the step (2), the stirring speed is 800 revolutions per minute.
In the step (3), the stirring speed is 3500 rpm.
Example 2
The electrolyte mother solution is prepared from the following raw materials in parts by weight:
the additive is prepared from the following raw materials in parts by weight:
3 parts of hydroxyethyl cellulose;
0.1 part of carboxymethyl chitosan;
0.1 part of silicon dioxide whisker;
the dosage of the additive is 8 percent of the mass of the electrolyte mother liquor.
The mass concentration of the sulfuric acid is 70%.
The nano fumed silica and the silica whiskers are the same as in example 1.
The preparation method comprises the following steps:
(1) preparing an electrolyte mother solution:
a. adding 45 parts of deionized water into a stirring kettle, adding nano fumed silica in batches, and stirring to obtain a silica mother solution;
b. adding the rest deionized water into the stirring kettle, adding potassium sulfate, magnesium sulfate, stannous sulfate, lithium sulfate and cerium sulfate, stirring until the potassium sulfate, the magnesium sulfate, the stannous sulfate, the lithium sulfate and the cerium sulfate are dissolved, adding sulfuric acid, and stirring to obtain sulfuric acid mother liquor;
c. adding the silicon dioxide mother liquor into sulfuric acid mother liquor, and uniformly stirring to obtain electrolyte mother liquor;
(2) adding hydroxyethyl cellulose and carboxymethyl chitosan into the electrolyte mother liquor, heating to 30 ℃, and stirring for 4 hours to obtain a colloid dispersion liquid;
(3) and (3) adding the silicon dioxide whiskers under continuous stirring, and then continuously stirring for 1 hour after the silicon dioxide whiskers are added to obtain the lead-acid storage battery electrolyte.
In the step (2), the stirring speed is 500 rpm.
In the step (3), the stirring speed is 4000 revolutions per minute.
Example 3
The electrolyte mother solution is prepared from the following raw materials in parts by weight:
the additive is prepared from the following raw materials in parts by weight:
2 parts of hydroxyethyl cellulose;
0.5 part of carboxymethyl chitosan;
0.5 part of silicon dioxide whisker;
the dosage of the additive is 12 percent of the mass of the electrolyte mother liquor.
The mass concentration of the sulfuric acid is 80%.
The nano fumed silica and the silica whiskers are the same as in example 1.
The preparation method comprises the following steps:
(1) preparing an electrolyte mother solution:
a. adding 30 parts of deionized water into a stirring kettle, adding nano fumed silica in batches, and stirring to obtain a silica mother solution;
b. adding the rest deionized water into the stirring kettle, adding potassium sulfate, magnesium sulfate, stannous sulfate, lithium sulfate and cerium sulfate, stirring until the potassium sulfate, the magnesium sulfate, the stannous sulfate, the lithium sulfate and the cerium sulfate are dissolved, adding sulfuric acid, and stirring to obtain sulfuric acid mother liquor;
c. adding the silicon dioxide mother liquor into sulfuric acid mother liquor, and uniformly stirring to obtain electrolyte mother liquor;
(2) adding hydroxyethyl cellulose and carboxymethyl chitosan into the electrolyte mother liquor, heating to 35 ℃, and stirring for 3 hours to obtain a colloid dispersion liquid;
(3) and (3) adding the silicon dioxide whiskers under continuous stirring, and then continuously stirring for 2 hours after the silicon dioxide whiskers are added to obtain the lead-acid storage battery electrolyte.
In the step (2), the stirring speed is 1000 rpm.
In the step (3), the stirring speed is 3000 r/min.
Comparative example 1
The procedure of example 1 was repeated except that no additive was used.
Comparative example 2
The additive was the same as in example 1 except that hydroxyethyl cellulose was not used.
Comparative example 3
The additive was the same as in example 1 except that carboxymethyl chitosan was not used.
Comparative example 4
The additive was the same as in example 1 except that no silica whiskers were used.
And (3) effect testing:
1. the lead-acid storage battery electrolytes prepared in examples 1-3 and comparative examples 1-4 are added into a single battery assembled into 2V and 400mAh by a traditional process, and a cycle life test is carried out after formation.
2. The cycling conditions were as follows:
1)C20detecting qualified batteries, and performing the following cycle system after the batteries are fully charged;
5I20current of (2) discharging for 2 hours and 0.5C200.2C after charging to 2.45V20Charging to 120% C20Let stand for 30 minutes, thus a cycle.
2) Cycle termination conditions:
after each 20 cycles, 5I was used20The current was discharged to 1.75V, and the capacity C was measured. When the capacity is reduced to 0.5C20The experiment was terminated after the following.
3. The test results are shown in Table 1.
TABLE 1 end of life times of batteries
| Example 1 | 655 times of |
| Example 2 | 638 times of |
| Example 3 | 624 times |
| Comparative example 1 | 432 times |
| Comparative example 2 | 531 times (n) |
| Comparative example 3 | 515 times |
| Comparative example 4 | 481 times |
4. And (4) analyzing results:
the battery made from electrolyte without additive has the end of life after 432 cycles, and the life of the battery with some additive is increased, but the effect is far less than that of the battery with all additive components. The additive has a synergistic effect among the three, and the service life of the battery can be obviously prolonged.
Claims (7)
1. The lead-acid storage battery electrolyte is characterized in that: the electrolyte comprises electrolyte mother liquor and an additive, wherein the electrolyte mother liquor is prepared from the following raw materials in parts by weight:
the additive is prepared from the following raw materials in parts by weight:
2-3 parts of hydroxyethyl cellulose;
0.1-0.5 part of carboxymethyl chitosan;
0.1-0.5 part of silicon dioxide whisker;
the dosage of the additive is 8-12% of the mass of the electrolyte mother liquor.
2. The lead-acid battery electrolyte of claim 1, wherein: the mass concentration of the sulfuric acid is 70-80%.
3. The lead-acid battery electrolyte of claim 1, wherein: the particle size of the nano fumed silica is 25-40 nm.
4. The lead-acid battery electrolyte of claim 1, wherein: the diameter of the silicon dioxide crystal whisker is 0.1-0.5 μm, and the length is 0.1-2 μm.
5. A method of formulating the electrolyte for lead-acid batteries according to any one of claims 1 to 4, characterized in that: the method comprises the following steps:
(1) preparing an electrolyte mother solution:
a. adding 30-45 parts of deionized water into a stirring kettle, adding nano fumed silica in batches, and stirring to obtain a silica mother solution;
b. adding the rest deionized water into the stirring kettle, adding potassium sulfate, magnesium sulfate, stannous sulfate, lithium sulfate and cerium sulfate, stirring until the potassium sulfate, the magnesium sulfate, the stannous sulfate, the lithium sulfate and the cerium sulfate are dissolved, adding sulfuric acid, and stirring to obtain sulfuric acid mother liquor;
c. adding the silicon dioxide mother liquor into sulfuric acid mother liquor, and uniformly stirring to obtain electrolyte mother liquor;
(2) adding hydroxyethyl cellulose and carboxymethyl chitosan into the electrolyte mother liquor, heating to 30-35 ℃, and stirring for 3-4 hours to obtain a colloid dispersion liquid;
(3) and (3) adding the silicon dioxide whiskers under continuous stirring, and then continuously stirring for 1-2 hours to obtain the lead-acid storage battery electrolyte.
6. The method of formulating a lead-acid battery electrolyte according to claim 5, wherein: in the step (2), the stirring speed is 500-1000 rpm.
7. The method of formulating a lead-acid battery electrolyte according to claim 5, wherein: in the step (3), the stirring speed is 3000-4000 rpm.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102044711A (en) * | 2010-12-08 | 2011-05-04 | 华南师范大学 | Storage battery colloidal electrolyte containing acicular nano crystal whisker and preparation method thereof |
| CN102394319A (en) * | 2011-11-03 | 2012-03-28 | 广西天鹅蓄电池有限责任公司 | Colloidal electrolyte of storage battery |
| CN102522596B (en) * | 2011-12-30 | 2014-05-07 | 山东宏艺电源技术有限公司 | Lead-acid storage battery collide electrolyte, preparation method thereof and lead-acid storage battery |
| CN105355984A (en) * | 2015-09-28 | 2016-02-24 | 芜湖日升重型机床有限公司 | Battery electrolyte for numerical control machine tool and preparation method of battery electrolyte and battery |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102044711A (en) * | 2010-12-08 | 2011-05-04 | 华南师范大学 | Storage battery colloidal electrolyte containing acicular nano crystal whisker and preparation method thereof |
| CN102394319A (en) * | 2011-11-03 | 2012-03-28 | 广西天鹅蓄电池有限责任公司 | Colloidal electrolyte of storage battery |
| CN102522596B (en) * | 2011-12-30 | 2014-05-07 | 山东宏艺电源技术有限公司 | Lead-acid storage battery collide electrolyte, preparation method thereof and lead-acid storage battery |
| CN105355984A (en) * | 2015-09-28 | 2016-02-24 | 芜湖日升重型机床有限公司 | Battery electrolyte for numerical control machine tool and preparation method of battery electrolyte and battery |
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