CN108336422A - A kind of low temperature resistant battery liquid and preparation method thereof - Google Patents
A kind of low temperature resistant battery liquid and preparation method thereof Download PDFInfo
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- CN108336422A CN108336422A CN201810214743.7A CN201810214743A CN108336422A CN 108336422 A CN108336422 A CN 108336422A CN 201810214743 A CN201810214743 A CN 201810214743A CN 108336422 A CN108336422 A CN 108336422A
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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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- 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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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
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Abstract
The invention discloses a kind of low temperature resistant battery liquids and preparation method thereof, belong to accumulator manufacturing technology field.The battery liquid, by percentage to the quality, composition includes：Water 60 65%, sulfuric acid 30~35%, tannin 0.1~0.5%, lignosulphonic acid magnesium 0.05~0.3%, lithium sulfite 0.02~0.1%, stannous sulfate 0.02~0.1%, poly-epoxy succinic acid or polyepoxy sodium succinate 3~10%, hydroxymethyl cellulose 0.05~0.3%.The present invention adds the new component poly-epoxy succinic acid for reducing polar plate sulfation or polyepoxy sodium succinate to slow down the use failure of lignin components in cathode additive agent in the electrolytic solution, improves the service life of accumulator, while increasing the cryogenic property of accumulator；The present invention adds the special tannin of accumulator alternatively in accumulator, to improve the cryogenic property of accumulator, lignosulphonic acid magnesium and metal salt component is added, to avoid accumulator dendrite short circuit and polar plate sulfation.
Description
Technical field
The present invention relates to accumulator manufacturing technology fields, and in particular to a kind of low temperature resistant battery liquid and its preparation
Method.
Background technology
Expected service life is not achieved during lead-acid accumulator use in most cases, main problem is that capacity declines in advance
Subtract and fail, influencing a main cause of service life of lead accumulator is：It is hard to generate white that is, on pole plate for polar plate sulfation
Hard lead sulfate crystallization, when charging is again extremely difficult to be converted into active material, referred to as " sulfation ".In simple, it is exactly
The pole plate of lead-acid accumulator is covered by sulfuric acid leading crystal, leads to battery capacity decline or deterioration.
The reason of generating this lead sulfate is overdischarge or is placed for a long time after discharging that lead sulfate particle is molten in the electrolytic solution
Solution is in saturation state, these lead sulfates recrystallize when the temperature is low, i.e. the lead sulfate particle of the precipitation of lead sulfate, precipitation exists
It growing, develops because of temperature variation again and again, crystal grain is made to increase, the electric conductivity of this lead sulfate is bad, resistance is big,
Solubility and solution rate very little again, when charging, restore difficult, thus reduce as capacity and the reason of the lost of life, in energy storage
It is showed with the accumulator used in terms of start and stop especially prominent.
Important component of the electrolyte as battery, played between the positive and negative electrode of lead-acid accumulator conveying metal from
The effect of son, is known as " blood " of lead-acid accumulator.It is to the specific capacity of battery, operating temperature range, cycle efficieny and safety
The vital effect such as performance；It is to obtain high-energy density, long circulation life and good security to select suitable electrolyte
Lead-acid accumulator key, therefore it is extremely important developing the electrolyte that meets lead-acid accumulator demand.
Application publication number discloses lead-acid accumulator graphene electrolyte for the patent document of CN105680102A, including：
Graphene aqueous solution, sulfate, stannous sulfate, Ludox, sodium carboxymethylcellulose, surplus are sulfuric acid solution.It is adopted in the formula
Increase the flowing activity of electrolyte with graphene aqueous solution, increase the respond of electrolyte and active material, increases electrode table
The activation energy in face reduces the obstruction that the lead sulfate film on lead surface conducts electronics, increases oxygen cycle efficiency, reduces the sulphur of bulky grain
Hydrochlorate extends the service life of deeper cavity.
In recent years, many accumulator property indexs increased the examination to cryogenic property, in European standard and national standard
Low temperature property requirements are increasingly stringenter, such as are increased to low in starting battery national standard national standard GB/T5008-2013
Subzero 29 DEG C of the detection of temperature, capacity check has been adjusted to -20 DEG C of temperature by -15 DEG C of detections under low temperature in power battery national standard
Lower carry out capacity check is increased to Low temperature property requirements from production standard aspect, to adapt to the more and more harsh market demand.
Therefore, how to be improved that the service life caused by improve current polar plate sulfation terminates in advance accumulator asks
The high standards for inscribing and meeting cryogenic property is the research topic that battery industry faces.
Invention content
The purpose of the present invention is to provide a kind of low temperature resistant battery liquids, to solve accumulator in the prior art
The problem that poor performance at low temperatures, polar plate sulfation cause service life short.
To achieve the above object, the present invention adopts the following technical scheme that：
A kind of low temperature resistant battery liquid, by percentage to the quality, composition includes：Water 60-65%, sulfuric acid 30~
35%, tannin 0.1~0.5%, lignosulphonic acid magnesium 0.05~0.3%, lithium sulfite 0.02~0.1%, stannous sulfate 0.02~
0.1%, poly-epoxy succinic acid or polyepoxy sodium succinate 3~10%, hydroxymethyl cellulose 0.05~0.3%.
The tannin uses the special tannin extract of accumulator.The usual special tannin of accumulator is added as low-temperature storage battery negative plate
Agent uses, and since tannin is only adsorbed on the surface of metallic lead, without being adsorbed on the lead sulfate plane of crystal newly formed, makes
The effective area that negative plate participates in the active material of reaction is guaranteed, and to slow down the passivation of negative plate, and improves low temperature
The performance of accumulator.The present invention alternatively adds tannin in the electrolytic solution, to improve the cryogenic property of accumulator.
Compared to sodium lignosulfonate, the solubility higher of lignosulphonic acid magnesium in the solution, while being capable of providing more free
Lignosulphonic acid radical ion uses cryogenic property to be better than sodium lignosulfonate in the electrolytic solution.
The present invention adds tannin and lignosulphonic acid magnesium to improve both substance ions in the electrolytic solution in the electrolytic solution
Solubility avoids the too fast dissolving of both additives in pole plate from causing to fail, to maintain effect of both additives in pole plate
With avoiding polar plate sulfation, improve cryogenic property and the service life of pole plate.
The present invention adds stannous sulfate and lithium sulfite in the electrolytic solution, mainly enhances electrolyte conductance, improves electric power storage
The charging and discharging capabilities in pond inhibit the growth of cathode lead dendritic crystal, prevent lead dendritic crystal short-circuit, larger lead sulfate particle is made easily to be gone back
Original inhibits early stage capacitance loss.
Since tin and lithium ratio lead are active, stannous sulfate and lithium sulfite are generated in the time priority of electric discharge, is then regenerated
Lead sulfate, and stannous sulfate and lithium sulfite do not crystallize, charging when, will not generate the lead sulfate crystallization of bulk, in this way can be with
The vulcanization for reducing battery generates, and then extends the service life of battery.
In addition from the formation mechanism of lead sulfate, the formation of lead sulfate is by after tiny lead sulfate dissolving, then to more
Big lead sulfate surface Precipitation grows into coarse lead sulfate crystallization hard to tolerate, therefore, can pass through and add sulfate ligands
Dopant forms complex, since the compound that sulfate ligands dopant is formed is unstable in acid medium, does not lead
The sulfation layer of electricity, will gradually dissolve back in solution, and then sulfation generation is reduced or avoided.Stannous sulfate and Asia
Lithium sulfate can avoid the lead sulfate sulfate that generation is shelved in overdischarge in short-term as sulfate ligands dopant complex
Change.
The present invention adds poly-epoxy succinic acid or polyepoxy sodium succinate (PESA), poly-epoxy succinic acid in the electrolytic solution
Or the amount of activated group of polyepoxy sodium succinate has certain chelating ability to free lead cation, after adding PESA, can seal
Lock section divides lead cationic, inhibits its reacting with sulfate ion, to prevent lead sulfate from crystallizing.
Since the PESA of addition has special adsorption capacity to the active site of nucleus and crystal in lead sulfate small crystals, and
It can be adsorbed on above by physically or chemically acting on, interface enable to greatly increase, interface can be higher, and the critical radius of crystal is got over
Greatly, small crystals is precipitated more difficult from water.
In addition, PESA has distortion of lattice effect, inhibit the regular growth of sulfuric acid leading crystal, to big havoc crystallization
Regularity makes lattice deformability, due to the lead sulfate crystal shape very irregular being distorted, it is difficult to pass through orderly close-packed arrays shape
At hard sulfuric acid lead, to achieve the purpose that avoid polar plate sulfation.
Preferably, the battery liquid, by percentage to the quality, composition includes：Water 60~63%, sulfuric acid 32~
34%, tannin 0.3~0.4%, lignosulphonic acid magnesium 0.15~0.2%, lithium sulfite 0.07~0.08%, stannous sulfate 0.06~
0.08%, poly-epoxy succinic acid or polyepoxy sodium succinate 4~6%, hydroxymethyl cellulose 0.07~0.2%.
More preferably, the battery liquid, by percentage to the quality, composition includes：Water 63%, sulfuric acid 32%, list
Peaceful 0.3%, lignosulphonic acid magnesium 0.2%, lithium sulfite 0.08%, stannous sulfate 0.06%, poly-epoxy succinic acid or polycyclic oxygen
Sodium succinate 4%, hydroxymethyl cellulose 0.07%.
The conductivity of the water is less than 0.3 μ S/cm.
It is a further object to provide the method for preparing above-mentioned low temperature resistant battery liquid, the method packets
It includes：
(1) each raw material is weighed according to formula ratio；
(2) water for accounting for water gross mass 15~25% is heated to 80~90 DEG C, tannin is added, stirs evenly, is cooled to 60
~70 DEG C, lignosulphonic acid magnesium is added, is uniformly mixed, stands to room temperature, mixed liquor I is made；
(3) water for accounting for water gross mass 15~25% is heated to 50~60 DEG C, poly-epoxy succinic acid or polycyclic oxygen is added
Sodium succinate after stirring evenly, is added lithium sulfite and stannous sulfate, is uniformly mixed, and stands to room temperature, mixed liquor II is made；
(4) sulfuric acid and the water of surplus are mixed, prepares aqueous sulfuric acid, stood to room temperature, mixed liquor I and mixing is added
Liquid II, stirs evenly, and adds hydroxymethyl cellulose, increases stir speed (S.S.) after mixing and carries out shear agitation, then in negative pressure item
It is stood under part, the low temperature resistant battery liquid is made.
Preferably, in step (2)-(4), a kind of raw material is often added, is stirred with the rate of 100~400 turns/min
Mixing.
Specifically, in step (2), after tannin is added, 20~30min is stirred with the rate of 300~400 turns/min.It is added
After lignosulphonic acid magnesium, 10~20min is stirred with the rate of 100~200 turns/min.
In step (3), after poly-epoxy succinic acid or polyepoxy sodium succinate is added, with the rate of 100~200 turns/min
Stir 10~20min.
In step (4), after mixed liquor I and mixed liquor II is added, 5~10min is stirred with the rate of 100~200 turns/min；
After hydroxymethyl cellulose is added, 5~10min is stirred with the rate of 100~200 turns/min, high speed is carried out in adjustment stir speed (S.S.)
Shear agitation.
Preferably, the rate of the shear agitation is 2000~3000 turns/min.The time of shear agitation be 30~
50min。
Due to generating a large amount of bubbles in whipping process, using being stood under condition of negative pressure, gas in liquid is contributed to be discharged.Make
To be preferred, in step (4), the condition of negative pressure is -0.1~-0.2MPa.
The advantageous effect that the present invention has：
The present invention adds the new component poly-epoxy succinic acid or polycyclic oxygen amber for reducing polar plate sulfation in the electrolytic solution
Meticortene Solu-Delta-cortef fails to slow down the use of lignin components in cathode additive agent, improves the service life of accumulator, while increasing accumulator
Cryogenic property；The present invention adds the special tannin of accumulator alternatively in accumulator, to improve the cryogenic property of accumulator,
Lignosulphonic acid magnesium and metal salt component are added, to avoid accumulator dendrite short circuit and polar plate sulfation.
Specific implementation mode
The present invention is further explained in the light of specific embodiments.
Comparative example 1
1, battery liquid formula：It is pure water (conductivity be less than 0.3 μ S/cm) 66kg, sulfuric acid (analysis is pure) 34kg, anhydrous
Sodium sulphate 15g/L electrolyte.
2, preparation method
Sulfuric acid is slowly injected into water, is stirred simultaneously, cooling measure is opened, continues cooling down after acid adding, wait for temperature
Degree is down to 45 DEG C hereinafter, addition anhydrous sodium sulfate, stirs evenly and can be used.
Embodiment 1
1, battery liquid formula：Pure water (conductivity is less than 0.3 μ S/cm) 63kg, sulfuric acid (analysis is pure) 32kg, tannin
(accumulator is special) 0.3kg, lignosulphonic acid magnesium 0.2kg, lithium sulfite 0.08kg, stannous sulfate 0.06kg, poly-epoxy succinic acid
4kg, hydroxymethyl cellulose 0.7kg.
2, preparation method
(1) it by 6.4kg formula water heating, is kept for 80 DEG C tannin is then added, 30 points is stirred with 400r/min speed
Clock ensures that tannin uniformly mixes in water, solution temperature is down to 60 DEG C, lignosulphonic acid magnesium is then added, with 200r/min speed
Degree is stirred 20 minutes, is ensured that lignosulphonic acid magnesium uniformly mixes in the solution, is stood for use to room temperature.
(2) it by 20% formula water heating, is kept for 50 DEG C poly-epoxy succinic acid is then added, is stirred with 200r/min speed
It mixes 20 minutes, ensures that poly-epoxy succinic acid uniformly mixes in the solution, keep temperature that lithium sulfite and stannous sulfate is then added,
Stirring 5 minutes is stood for use to room temperature.
(3) formula sulfuric acid is mixed with surplus formula water, sulfuric acid is poured slowly into water, configures aqueous sulfuric acid, and standing arrives
After room temperature, mixed solution made from the 2nd, the 3rd step is added, is stirred 5min minutes with 200r/min speed, hydroxyl is then added
Methylcellulose, speed is adjusted to 2000r/min high shear agitations 30 after being stirred 5min minutes with 200r/min speed
Minute, negative pressure -0.2MPa can be used after standing 1h.
Embodiment 2
1, battery liquid formula：Pure water (conductivity is less than 0.3 μ S/cm) 66kg, sulfuric acid (analysis is pure) 34kg, tannin
(accumulator is special) 0.4kg, lignosulphonic acid magnesium 0.15kg, lithium sulfite 0.07kg, stannous sulfate 0.08kg, poly-epoxy succinic acid
6kg, hydroxymethyl cellulose 0.2kg.
2, preparation method
(1) it by 6.4kg formula water heating, is kept for 90 DEG C tannin is then added, 20 points is stirred with 300r/min speed
Clock ensures that tannin uniformly mixes in water, solution temperature is down to 70 DEG C, lignosulphonic acid magnesium is then added, with 100r/min speed
Degree is stirred 10 minutes, is ensured that lignosulphonic acid magnesium uniformly mixes in the solution, is stood for use to room temperature.
(2) it by 20% formula water heating, is kept for 60 DEG C poly-epoxy succinic acid is then added, is stirred with 100r/min speed
It mixes 10 minutes, ensures that poly-epoxy succinic acid uniformly mixes in the solution, keep temperature that lithium sulfite and stannous sulfate is then added,
Stirring 10 minutes is stood for use to room temperature.
(3) formula sulfuric acid is mixed with surplus formula water, sulfuric acid is poured slowly into water, configures aqueous sulfuric acid, and standing arrives
After room temperature, mixed solution made from the 2nd, the 3rd step is added, is stirred 10min minutes with 100r/min speed, hydroxyl is then added
Methylcellulose, speed is adjusted to 3000r/min high shear agitations 30 after being stirred 10min minutes with 100r/min speed
Minute, negative pressure -0.1MPa can be used after standing 2h.
Application examples
Comparative example 1 is respectively adopted, battery liquid prepared by Examples 1 and 2, model is assembled into according to common process
6-QW-60 maintenance-free battery (capacity：60Ah low-temperature high-current discharge Icc 500A), reference standard GB/T5008.1-2013
The accumulator of assembling is detected.
1, idle capacity
Detection method：It is discharged with 25A in 25 DEG C of ± 2 DEG C of environment temperatures, 10.5 ± 0.05v of final voltage records the time.
2, -18 DEG C of low temperature detections
Detection method：It is kept not less than for 24 hours in -18 DEG C of ± 1 DEG C of environment temperatures.With 500A discharge 30s, record 10s,
30s voltages, static 20s, with 300A electric discharge 40s, voltage when recording 40s, 10.5 ± 0.05v of final voltage records the time.
3,20h rated capacities
Detection method：It is discharged with 3A in 25 DEG C of ± 2 DEG C of environment temperatures, 10.5 ± 0.05v of final voltage records the time.
4, -29 DEG C of low temperature detections
Detection method：It is kept not less than for 24 hours in -29 DEG C of ± 1 DEG C of environment temperatures.With 400A discharge 30s, record 10s,
30s voltages, static 20s, with 240A electric discharge 40s, voltage when recording 40s, 10.5 ± 0.05v of final voltage records the time.
5, charge acceptance
Detection method：Be maintained at after accumulator is fully charged in 25 DEG C of ± 2 DEG C of environment temperatures, with I0 (6.4A) discharge 5h,
20h is placed in 0 DEG C of ± 1 DEG C of environment temperature, takes out in 1min and charges by 14.4 ± 0.10v voltages, after ten minutes record charging
Electric current Ica.
6, retention of charge is tested
Detection method：It is placed 49 days in 40 ± 2 DEG C of water baths after battery is fully charged, -18 DEG C is carried out with 300A electric currents
Cold-starting discharges, and records 30S voltages.
7, cycle life
Detection method：It is tested according to 5.9.2 cycling durables I in GB/T5008.1-2013.
The results are shown in Table 1.
Table 1
From the above, it is seen that using the accumulator of the electrolyte of embodiment 1 and embodiment 2 assembling in low temperature, charged guarantor
Hold the indexs such as ability, service life has raising by a relatively large margin than the accumulator property of comparative example 1, it was demonstrated that skill using the present invention
Art scheme makes accumulator low temperature resistant and reduces polar plate sulfation, and the performance for improving charge acceptance etc. significantly carries
It rises.
Claims (9)
1. a kind of low temperature resistant battery liquid, which is characterized in that by percentage to the quality, composition includes：Water 60-65%,
Sulfuric acid 30~35%, tannin 0.1~0.5%, lignosulphonic acid magnesium 0.05~0.3%, lithium sulfite 0.02~0.1%, sulfuric acid are sub-
Tin 0.02~0.1%, poly-epoxy succinic acid or polyepoxy sodium succinate 3~10%, hydroxymethyl cellulose 0.05~0.3%.
2. low temperature resistant battery liquid as described in claim 1, which is characterized in that by percentage to the quality, composition packet
It includes：Water 60~63%, sulfuric acid 32~34%, tannin 0.3~0.4%, lignosulphonic acid magnesium 0.15~0.2%, lithium sulfite 0.07
~0.08%, stannous sulfate 0.06~0.08%, poly-epoxy succinic acid or polyepoxy sodium succinate 4~6%, hydroxylmethyl cellulose
Element 0.07~0.2%.
3. low temperature resistant battery liquid as claimed in claim 2, which is characterized in that by percentage to the quality, composition packet
It includes：Water 63%, tannin 0.3%, lignosulphonic acid magnesium 0.2%, lithium sulfite 0.08%, stannous sulfate 0.06%, gathers sulfuric acid 32%
Epoxysuccinic acid or polyepoxy sodium succinate 4%, hydroxymethyl cellulose 0.07%.
4. low temperature resistant battery liquid as described in any one of claims 1-3, which is characterized in that the conductivity of the water
Less than 0.3 μ S/cm.
5. the preparation method of low temperature resistant battery liquid according to any one of claims 1-4, which is characterized in that packet
It includes：
(1) each raw material is weighed according to formula ratio；
(2) water for accounting for water gross mass 15~25% is heated to 80~90 DEG C, tannin is added, stirs evenly, is cooled to 60~70
DEG C, lignosulphonic acid magnesium is added, is uniformly mixed, stands to room temperature, mixed liquor I is made；
(3) water for accounting for water gross mass 15~25% is heated to 50~60 DEG C, poly-epoxy succinic acid or poly- epoxy succinic is added
Sour sodium after stirring evenly, is added lithium sulfite and stannous sulfate, is uniformly mixed, and stands to room temperature, mixed liquor II is made；
(4) sulfuric acid and the water of surplus are mixed, prepares aqueous sulfuric acid, stood to room temperature, mixed liquor I and mixed liquor is added
II, it stirs evenly, adds hydroxymethyl cellulose, increase stir speed (S.S.) after mixing and carry out shear agitation, then in condition of negative pressure
The low temperature resistant battery liquid is made in lower standing.
6. preparation method as claimed in claim 5, which is characterized in that in step (2)-(4), a kind of raw material is often added, with 100
The rate of~400 turns/min is stirred mixing.
7. preparation method as claimed in claim 6, which is characterized in that in step (2), be added tannin after, with 300~400 turns/
The rate of min stirs 20~30min.
8. preparation method as claimed in claim 5, which is characterized in that in step (4), the rate of the shear agitation is 2000
~3000 turns/min.
9. preparation method as claimed in claim 5, which is characterized in that in step (4), the condition of negative pressure be -0.1~-
0.2MPa。
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| CN111934010A (en) * | 2020-08-05 | 2020-11-13 | 湖南省长城新能源科技有限公司 | Lead-acid storage battery electrolyte and preparation method thereof |
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