CN108336422B - Low-temperature-resistant storage battery electrolyte and preparation method thereof - Google Patents
Low-temperature-resistant 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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- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
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- H01M2300/0002—Aqueous electrolytes
- H01M2300/0005—Acid electrolytes
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Abstract
The invention discloses a low-temperature-resistant storage battery electrolyte and a preparation method thereof, and belongs to the technical field of storage battery manufacturing. The electrolyte of the storage battery comprises the following components in percentage by mass: 60-65% of water, 30-35% of sulfuric acid, 0.1-0.5% of tannin, 0.05-0.3% of magnesium lignosulfonate, 0.02-0.1% of lithium sulfite, 0.02-0.1% of stannous sulfate, 3-10% of polyepoxysuccinic acid or sodium polyepoxysuccinate and 0.05-0.3% of hydroxymethyl cellulose. The polyepoxysuccinic acid or the polyepoxysuccinic acid sodium which is a new component for reducing the sulfation of the polar plate is added into the electrolyte to slow down the use failure of the lignin component in the negative electrode additive, prolong the service life of the storage battery and simultaneously increase the low-temperature performance of the storage battery; the invention adds special tannin for the storage battery into the storage battery in another way to improve the low-temperature performance of the storage battery, and adds magnesium lignosulfonate and metal salt components to avoid dendrite short circuit and polar plate sulfation of the storage battery.
Description
Technical Field
The invention relates to the technical field of storage battery manufacturing, in particular to a low-temperature-resistant storage battery electrolyte and a preparation method thereof.
Background
The service life expectancy under most circumstances in the lead-acid storage battery use, the main problem is that capacity attenuates and loses efficacy in advance, and one of the main reasons that influence the lead-acid storage battery life is: the plate sulfation, that is, white hard lead sulfate crystals are generated on the plate, and the lead sulfate crystals are very difficult to be converted into active substances during charging, which is called sulfation for short. In simple terms, it is the plates of a lead acid battery that are covered by lead sulfate crystals, resulting in a decrease in battery capacity or a decline in function.
The reason for the generation of such lead sulfate is that fine particles of lead sulfate are dissolved in an electrolyte to be saturated when the lead sulfate is left for a long period of time after overdischarge or discharge, and the lead sulfate is recrystallized at a low temperature, that is, precipitation of lead sulfate, and the precipitated lead sulfate particles grow and progress again and again due to temperature fluctuation to increase crystal grains.
The electrolyte is used as an important component of the battery, plays a role in conveying metal ions between the positive electrode and the negative electrode of the lead-acid storage battery, and is called as 'blood' of the lead-acid storage battery. The material plays a vital role in the specific capacity, the working temperature range, the cycle efficiency, the safety performance and the like of the battery; the selection of proper electrolyte is the key to obtain a lead-acid storage battery with high energy density, long cycle life and good safety, so that the development of the electrolyte meeting the requirements of the lead-acid storage battery is very important.
Patent document with application publication number CN105680102A discloses a graphene electrolyte for lead-acid storage batteries, comprising: graphene water solution, sulfate, stannous sulfate, silica sol, sodium carboxymethylcellulose and the balance of sulfuric acid solution. In the formula, the graphene aqueous solution is adopted to increase the flowing activity of the electrolyte, increase the reaction capacity of the electrolyte and an active substance, increase the activation energy of the electrode surface, reduce the obstruction of a lead sulfate film on the lead surface to electron conduction, increase the oxygen circulation efficiency, reduce the sulfation of large particles and prolong the service life of deep circulation.
In recent years, the performance indexes of a plurality of storage batteries increase the examination on low-temperature performance, and the requirements on the low-temperature performance in European standards and national standards are more and more strict, for example, the detection on the low temperature of 29 ℃ below zero is increased in the national standard GB/T5008-2013 of the starting storage battery, the capacity detection in the national standard of the power battery at the low temperature is adjusted from the detection at the temperature of 15 ℃ below zero to the detection at the temperature of 20 ℃ below zero for capacity detection, and the requirements on the low-temperature performance are increased from the production standard level so as to adapt to the more and more rigorous market requirements.
Therefore, how to improve the storage battery to improve the problem of the prior end of life caused by plate sulfation and meet the high standard requirement of low-temperature performance is a research topic faced by the storage battery industry.
Disclosure of Invention
The invention aims to provide a low-temperature-resistant storage battery electrolyte to solve the problems of poor low-temperature performance of a storage battery and short service life caused by sulfation of a polar plate in the prior art.
In order to achieve the purpose, the invention adopts the following technical scheme:
the low-temperature-resistant storage battery electrolyte comprises the following components in percentage by mass: 60-65% of water, 30-35% of sulfuric acid, 0.1-0.5% of tannin, 0.05-0.3% of magnesium lignosulfonate, 0.02-0.1% of lithium sulfite, 0.02-0.1% of stannous sulfate, 3-10% of polyepoxysuccinic acid or sodium polyepoxysuccinate and 0.05-0.3% of hydroxymethyl cellulose.
The tannin adopts special tannin extract for storage batteries. Usually, the special tannin of battery is used as the low temperature battery negative plate additive, because tannin only adsorbs on the surface of metallic lead, and can not adsorb on the newly-formed lead sulfate crystal surface, makes the active material's that the negative plate participated in the reaction effective area obtain guaranteeing to slow down the passivation of negative plate, and improve low temperature battery's performance. The invention adds tannin into the electrolyte in another way to improve the low-temperature performance of the storage battery.
Compared with sodium lignosulfonate, the magnesium lignosulfonate has higher solubility in a solution, can provide more free lignosulfonate ions, and has better low-temperature performance than the sodium lignosulfonate when used in an electrolyte.
According to the invention, tannin and magnesium lignosulfonate are added into the electrolyte to improve the solubility of ions of the two substances in the electrolyte, so that the two additives in the polar plate are prevented from being dissolved too fast to cause failure, the effects of the two additives in the polar plate are maintained, the sulfation of the polar plate is avoided, and the low-temperature performance and the service life of the polar plate are improved.
According to the invention, stannous sulfate and lithium sulfite are added into the electrolyte, so that the conductivity of the electrolyte is enhanced, the charge and discharge capacity of the storage battery is improved, the growth of negative lead dendrites is inhibited, the short circuit of the lead dendrites is prevented, larger lead sulfate particles are easy to reduce, and the early capacity loss is inhibited.
Because tin and lithium are more active than lead, stannous sulfate and lithium sulfite are preferentially generated in the discharging time, and then lead sulfate is generated, and stannous sulfate and lithium sulfite are not crystallized, so that large blocks of lead sulfate crystals are not generated in the charging process, the sulfuration of the battery can be reduced, and the service life of the battery is further prolonged.
In addition, according to the analysis of the forming mechanism of the lead sulfate, the formation of the lead sulfate is that fine lead sulfate is dissolved and then the fine lead sulfate is precipitated and separated on the surface of larger lead sulfate to grow into coarse lead sulfate crystals which are difficult to dissolve, therefore, a coordination compound can be formed by adding a sulfate coordination dopant, and the compound formed by the sulfate coordination dopant is unstable in an acid medium, so that a non-conductive sulfated layer is gradually dissolved back into the solution, and the generation of sulfation is reduced or avoided. Stannous sulfate and lithium sulfite are used as a sulfate coordination dopant coordination compound, so that the sulfation of lead sulfate generated by overdischarge for a short time can be avoided.
According to the invention, polyepoxysuccinic acid or sodium Polyepoxysuccinate (PESA) is added into the electrolyte, part of active groups of the polyepoxysuccinic acid or sodium polyepoxysuccinate have certain chelating force on free lead cations, and after the PESA is added, part of the lead cations can be blocked, and the reaction of the lead cations and sulfate ions can be inhibited, so that the crystallization of lead sulfate is prevented.
The added PESA has special adsorption capacity on crystal nuclei and active points of the crystals in the lead sulfate small crystals and can be adsorbed on the lead sulfate small crystals through physical or chemical action, so that the interface energy is greatly increased, the higher the interface energy is, the larger the critical radius of the crystals is, and the more difficult the small crystals are separated out from water.
In addition, the PESA has the lattice distortion effect and inhibits the regular growth of lead sulfate crystals, so that the regularity of the crystals is greatly damaged, the lattices are deformed, and hard lead sulfate blocks are difficult to form through orderly and compact arrangement due to the irregular shape of the distorted lead sulfate crystals, thereby achieving the purpose of avoiding the sulfation of the polar plate.
Preferably, the battery electrolyte comprises the following components in percentage by mass: 60-63% of water, 32-34% of sulfuric acid, 0.3-0.4% of tannin, 0.15-0.2% of magnesium lignosulfonate, 0.07-0.08% of lithium sulfite, 0.06-0.08% of stannous sulfate, 4-6% of polyepoxysuccinic acid or sodium polyepoxysuccinate and 0.07-0.2% of hydroxymethyl cellulose.
More preferably, the battery electrolyte comprises the following components in percentage by mass: 63% of water, 32% of sulfuric acid, 0.3% of tannin, 0.2% of magnesium lignosulfonate, 0.08% of lithium sulfite, 0.06% of stannous sulfate, 4% of polyepoxysuccinic acid or sodium polyepoxysuccinate and 0.07% of hydroxymethyl cellulose.
The conductivity of the water is less than 0.3 [ mu ] S/cm.
Another object of the present invention is to provide a method for preparing the above low temperature-resistant battery electrolyte, the method comprising:
(1) weighing the raw materials according to the formula ratio;
(2) heating water accounting for 15-25% of the total mass of the water to 80-90 ℃, adding tannin, stirring uniformly, cooling to 60-70 ℃, adding magnesium lignosulfonate, mixing uniformly, and standing to normal temperature to obtain a mixed solution I;
(3) heating water accounting for 15-25% of the total mass of the water to 50-60 ℃, adding polyepoxysuccinic acid or sodium polyepoxysuccinate, stirring uniformly, adding lithium sulfite and stannous sulfate, mixing uniformly, and standing to normal temperature to prepare a mixed solution II;
(4) mixing sulfuric acid and the balance of water, preparing a sulfuric acid aqueous solution, standing to normal temperature, adding the mixed solution I and the mixed solution II, uniformly stirring, adding hydroxymethyl cellulose, mixing, increasing the stirring speed, shearing and stirring, and standing under a negative pressure condition to prepare the low-temperature-resistant storage battery electrolyte.
Preferably, in the steps (2) to (4), each raw material is added, and stirring and mixing are carried out at the speed of 100-400 r/min.
Specifically, in the step (2), after the tannin is added, stirring is carried out for 20-30 min at the speed of 300-400 r/min. After adding the magnesium lignosulphonate, stirring at the speed of 100-200 r/min for 10-20 min.
And (3) adding polyepoxysuccinic acid or polyepoxysuccinic acid sodium, and stirring at the speed of 100-200 rpm for 10-20 min.
In the step (4), adding the mixed solution I and the mixed solution II, and stirring at the speed of 100-200 revolutions per minute for 5-10 min; adding hydroxymethyl cellulose, stirring at the speed of 100-200 rpm for 5-10 min, and adjusting the stirring speed to perform high-speed shearing stirring.
Preferably, the speed of the shear stirring is 2000-3000 r/min. The shearing and stirring time is 30-50 min.
Because a large amount of bubbles are generated in the stirring process, the stirring device is kept still under the negative pressure condition, and the gas in the liquid is discharged. Preferably, in the step (4), the negative pressure condition is-0.1 to-0.2 MPa.
The invention has the following beneficial effects:
the polyepoxysuccinic acid or the polyepoxysuccinic acid sodium which is a new component for reducing the sulfation of the polar plate is added into the electrolyte to slow down the use failure of the lignin component in the negative electrode additive, prolong the service life of the storage battery and simultaneously increase the low-temperature performance of the storage battery; the invention adds special tannin for the storage battery into the storage battery in another way to improve the low-temperature performance of the storage battery, and adds magnesium lignosulfonate and metal salt components to avoid dendrite short circuit and polar plate sulfation of the storage battery.
Detailed Description
The present invention will be further described with reference to the following specific examples.
Comparative example 1
1. The formula of the electrolyte of the storage battery is as follows: 66kg of pure water (the conductivity is less than 0.3 mu S/cm), 34kg of sulfuric acid (analytically pure) and 15g/L of anhydrous sodium sulfate.
2. Preparation method
Slowly injecting sulfuric acid into water, stirring, cooling to below 45 deg.C, adding anhydrous sodium sulfate, and stirring.
Example 1
1. The formula of the electrolyte of the storage battery is as follows: 63kg of pure water (the conductivity is less than 0.3 mu S/cm), 32kg of sulfuric acid (analytically pure), 0.3kg of tannin (special for storage batteries), 0.2kg of magnesium lignosulfonate, 0.08kg of lithium sulfite, 0.06kg of stannous sulfate, 4kg of polyepoxysuccinic acid and 0.7kg of hydroxymethyl cellulose.
2. Preparation method
(1) Heating 6.4kg of formula water, keeping the temperature at 80 ℃, then adding tannin, stirring for 30 minutes at the speed of 400r/min to ensure that the tannin is uniformly mixed in the water, cooling the solution to 60 ℃, then adding magnesium lignosulfonate, stirring for 20 minutes at the speed of 200r/min to ensure that the magnesium lignosulfonate is uniformly mixed in the solution, and standing to normal temperature for later use.
(2) Heating 20% formula water, keeping the temperature at 50 ℃, then adding polyepoxysuccinic acid, stirring for 20 minutes at the speed of 200r/min to ensure that the polyepoxysuccinic acid is uniformly mixed in the solution, keeping the temperature, then adding lithium sulfite and stannous sulfate, stirring for 5 minutes, and standing to normal temperature for later use.
(3) Mixing the formula sulfuric acid with the balance of formula water, slowly pouring the sulfuric acid into the water, preparing a sulfuric acid aqueous solution, standing to normal temperature, adding the mixed solution prepared in the steps 2 and 3, stirring for 5 minutes at the speed of 200r/min, then adding the hydroxymethyl cellulose, stirring for 5 minutes at the speed of 200r/min, adjusting the speed to 2000r/min, shearing and stirring for 30 minutes at a high speed, and standing for 1 hour under the negative pressure of-0.2 MPa.
Example 2
1. The formula of the electrolyte of the storage battery is as follows: 66kg of pure water (the conductivity is less than 0.3 mu S/cm), 34kg of sulfuric acid (analytically pure), 0.4kg of tannin (special for storage batteries), 0.15kg of magnesium lignosulfonate, 0.07kg of lithium sulfite, 0.08kg of stannous sulfate, 6kg of polyepoxysuccinic acid and 0.2kg of hydroxymethyl cellulose.
2. Preparation method
(1) Heating 6.4kg of formula water, keeping the temperature at 90 ℃, then adding tannin, stirring for 20 minutes at the speed of 300r/min to ensure that the tannin is uniformly mixed in the water, cooling the solution to 70 ℃, then adding magnesium lignosulfonate, stirring for 10 minutes at the speed of 100r/min to ensure that the magnesium lignosulfonate is uniformly mixed in the solution, and standing to normal temperature for later use.
(2) Heating 20% formula water, keeping the temperature at 60 ℃, then adding polyepoxysuccinic acid, stirring for 10 minutes at the speed of 100r/min to ensure that the polyepoxysuccinic acid is uniformly mixed in the solution, keeping the temperature, then adding lithium sulfite and stannous sulfate, stirring for 10 minutes, and standing to normal temperature for later use.
(3) Mixing the formula sulfuric acid with the balance of formula water, slowly pouring the sulfuric acid into the water, preparing a sulfuric acid aqueous solution, standing to normal temperature, adding the mixed solution prepared in the steps 2 and 3, stirring at the speed of 100r/min for 10min, then adding the hydroxymethyl cellulose, stirring at the speed of 100r/min for 10min, adjusting the speed to 3000r/min, shearing and stirring at a high speed for 30min, and standing at a negative pressure of-0.1 MPa for 2 h.
Application example
The storage battery electrolytes prepared in comparative example 1 and examples 1 and 2 are respectively assembled into a 6-QW-60 maintenance-free storage battery (capacity: 60Ah \ low-temperature large-current discharge Icc 500A) according to a conventional process, and the assembled storage battery is detected according to a standard GB/T5008.1-2013.
1. Reserve capacity
The detection method comprises the following steps: discharging at 25 deg.C + -2 deg.C under 25A, stopping at voltage of 10.5 + -0.05 v, and recording time.
2. Low temperature detection at-18 deg.C
The detection method comprises the following steps: keeping the temperature at minus 18 +/-1 ℃ for not less than 24 h. The voltage was recorded at 500A for 30s, 10s and 30s, at rest for 20s, at 300A for 40s, at 40s, the voltage was recorded, the final voltage was 10.5 + -0.05 v, and the recording time was recorded.
3. Rated capacity of 20h
The detection method comprises the following steps: discharging at 25 + -2 deg.C with 3A, stopping at 10.5 + -0.05 v, and recording time.
4. Low temperature detection at-29 deg.C
The detection method comprises the following steps: keeping the temperature at minus 29 +/-1 ℃ for not less than 24 h. The voltage was recorded at 400A for 30s, 10s, 30s, rest for 20s, at 240A for 40s, end voltage 10.5 + -0.05 v, recording time.
5. Charge acceptance capability
The detection method comprises the following steps: after the storage battery is completely charged, the storage battery is kept at the ambient temperature of 25 +/-2 ℃, is discharged for 5h by I0(6.4A), is placed at the ambient temperature of 0 +/-1 ℃ for 20h, is taken out for 1min and is charged according to the voltage of 14.4 +/-0.10 v, and the charging current Ica is recorded after 10 min.
6. Charge retention capacity test
The detection method comprises the following steps: after the cell was fully charged, the cell was placed in a 40. + -. 2 ℃ water bath for 49 days, and discharge was initiated at a low temperature of-18 ℃ with a current of 300A, and the voltage was recorded for 30S.
7. Cycle life
The detection method comprises the following steps: the test was carried out according to 5.9.2 cycle endurance I test in GB/T5008.1-2013.
The results are shown in Table 1.
TABLE 1
It can be seen from the above that the performance of the storage battery assembled by using the electrolytes of examples 1 and 2 is greatly improved in indexes such as low temperature, charge retention capacity, service life and the like compared with that of the storage battery of comparative example 1, and it is proved that the performance of the storage battery in the aspects of low temperature resistance, polar plate sulfation reduction, charging acceptance capacity improvement and the like is remarkably improved by using the technical scheme of the invention.
Claims (6)
1. The low-temperature-resistant storage battery electrolyte is characterized by comprising the following components in percentage by mass: 60-65% of water, 30-35% of sulfuric acid, 0.1-0.5% of tannin, 0.05-0.3% of magnesium lignosulfonate, 0.02-0.1% of lithium sulfite, 0.02-0.1% of stannous sulfate, 3-10% of polyepoxysuccinic acid or sodium polyepoxysuccinate and 0.05-0.3% of hydroxymethyl cellulose;
the preparation method of the low-temperature-resistant storage battery electrolyte comprises the following steps:
(1) weighing the raw materials according to the formula ratio;
(2) heating water accounting for 15-25% of the total mass of the water to 80-90 ℃, adding tannin, stirring uniformly, cooling to 60-70 ℃, adding magnesium lignosulfonate, mixing uniformly, and standing to normal temperature to obtain a mixed solution I;
(3) heating water accounting for 15-25% of the total mass of the water to 50-60 ℃, adding polyepoxysuccinic acid or sodium polyepoxysuccinate, stirring uniformly, adding lithium sulfite and stannous sulfate, mixing uniformly, and standing to normal temperature to prepare a mixed solution II;
(4) mixing sulfuric acid and the balance of water to prepare a sulfuric acid aqueous solution, standing to normal temperature, adding the mixed solution I and the mixed solution II, uniformly stirring, adding hydroxymethyl cellulose, mixing, increasing the stirring rate, shearing and stirring, and standing under a negative pressure condition to prepare the low-temperature-resistant storage battery electrolyte;
in the step (2), after the tannin is added, stirring at the speed of 300-400 r/min for 20-30 min; after adding magnesium lignosulphonate, stirring at the speed of 100-200 r/min for 10-20 min;
in the step (3), adding polyepoxysuccinic acid or polyepoxysuccinic acid sodium, and stirring at the speed of 100-200 r/min for 10-20 min;
in the step (4), adding the mixed solution I and the mixed solution II, and stirring at the speed of 100-200 revolutions per minute for 5-10 min; after the hydroxymethyl cellulose is added, stirring for 5-10 min at the speed of 100-200 rpm, and then adjusting the stirring speed to carry out shearing stirring.
2. The low temperature-resistant battery electrolyte of claim 1 wherein the composition comprises, in mass percent: 60-63% of water, 32-34% of sulfuric acid, 0.3-0.4% of tannin, 0.15-0.2% of magnesium lignosulfonate, 0.07-0.08% of lithium sulfite, 0.06-0.08% of stannous sulfate, 4-6% of polyepoxysuccinic acid or sodium polyepoxysuccinate and 0.07-0.2% of hydroxymethyl cellulose.
3. The low temperature-resistant battery electrolyte of claim 2 wherein the composition comprises, in mass percent: 63% of water, 32% of sulfuric acid, 0.3% of tannin, 0.2% of magnesium lignosulfonate, 0.08% of lithium sulfite, 0.06% of stannous sulfate, 4% of polyepoxysuccinic acid or sodium polyepoxysuccinate and 0.07% of hydroxymethyl cellulose.
4. The low temperature tolerant battery electrolyte of any one of claims 1-3 wherein the water has an electrical conductivity of less than 0.3 μ S/cm.
5. The low temperature resistant battery electrolyte of claim 1 wherein in step (4) the shear agitation is at a rate of 2000 to 3000 rpm.
6. The low temperature resistant battery electrolyte of claim 1 wherein in step (4), the negative pressure condition is-0.1 to-0.2 MPa.
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Address after: 313100 Zhejiang city of Huzhou province Changxing County Meishan Industrial Park Applicant after: Tianneng Battery Group Co., Ltd. Address before: 313100 Zhejiang city of Huzhou province Changxing County Meishan Industrial Park Applicant before: Tianneng Battery Group Co., Ltd. |
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| GR01 | Patent grant | ||
| GR01 | Patent grant | ||
| TR01 | Transfer of patent right | ||
| TR01 | Transfer of patent right |
Effective date of registration: 20210107 Address after: 313103 Chengnan industrial functional zone, Changxing Economic and Technological Development Zone, Huzhou City, Zhejiang Province Patentee after: Zhejiang Tianneng Automobile Battery Co.,Ltd. Address before: 313100 Coal Mountain Industrial Park, Changxing County, Huzhou City, Zhejiang Province Patentee before: TIANNENG BATTERY GROUP Co.,Ltd. |