CN103337624B - A kind of lead-acid accumulator negative pole lead paste suppressing liberation of hydrogen and preparation method - Google Patents
A kind of lead-acid accumulator negative pole lead paste suppressing liberation of hydrogen and preparation method Download PDFInfo
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- CN103337624B CN103337624B CN201310265588.9A CN201310265588A CN103337624B CN 103337624 B CN103337624 B CN 103337624B CN 201310265588 A CN201310265588 A CN 201310265588A CN 103337624 B CN103337624 B CN 103337624B
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
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- Y02E60/10—Energy storage using batteries
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Abstract
A kind of lead-acid accumulator negative pole lead paste suppressing liberation of hydrogen and preparation method, its technical scheme is: described lead plaster solid material is made up of the material of following weight unit's: Hydrocerussitum (Ceruse) 100, carbon source 1～3, zinc source 0.15～1.0, barium sulfate 0.3～2, sodium lignosulfonate 0.1～0.5, fiber 0.01～0.5.The present invention adds certain zinc compound and different types of carbon at cathode lead plaster, improve size and the microstructure of lead negative material, thus reach to improve the capacity of lead-acid battery, improve charge acceptance, and increase the purpose of charge and discharge cycles stability.Test shows, in cathode lead plaster, the doping of Zinc compounds can make the hydrogen-evolution overpotential of acid accumulator negative pole lead more negative, increase liberation of hydrogen difficulty, reduce hydrogen to separate out, reduce the consumption of electrolyte during using, be conducive to improving the life of storage battery, reduce the possibility that the dangerous accidents such as blast occur the most to a certain extent.
Description
Technical field
The present invention relates to a kind of accumulator lead plaster technology, particularly suppress lead-acid accumulator negative pole lead paste and the preparation method of liberation of hydrogen, belong to battery technology field.
Background technology
Positive/negative plate is the parts of lead-acid accumulator most critical, and the quality of positive/negative plate directly determines discharge capacity and the charge and discharge service life cycle of lead-acid accumulator.Although occurring in that many novel batteries planted with lithium battery as representative in recent years, but lead-acid battery is cheap with it, safe and reliable, steady performance, still has the irreplaceable effect of other types battery in fields such as traffic, electric power, communication, computer, national defence, railways.At present, insider is usually through improving its electric conductivity in the carbon doping of different content to cathode lead plaster, to improve the capacity of battery, extends the lead-acid battery life-span, reaches the purpose under high magnification with good circulation performance.But the hydrogen-evolution overpotential that the doping of carbon will make lead negative pole is shuffled, likely separate out substantial amounts of hydrogen when overcharge and large current charge, increase water consumption, increase the possibility that the unsafe incidents such as blast occur.In view of this, how to solve the negative plate of lead-acid battery adds the gassing aggravation problem that more carbon black brings, reduce hydrogen-separating quantity, thus reduce the consumption of acid, the generation of minimizing accident, become problem demanding prompt solution.
Summary of the invention
The technical problem to be solved is: provide a kind of lead-acid accumulator negative pole lead paste reducing the suppression liberation of hydrogen that hydrogen separates out and preparation method, described method is by adding carbon and zinc compound in proportion in cathode lead plaster, thus increase liberation of hydrogen difficulty improving negative plate performance simultaneously, reduce hydrogen and separate out.
Problem alleged by the present invention is solved by techniques below scheme:
A kind of lead-acid accumulator negative pole lead paste suppressing liberation of hydrogen, its special feature is: described lead plaster solid material is made up of the material of following weight unit's: Hydrocerussitum (Ceruse) 100, carbon source 1～3, zinc source 0.15～1.0, barium sulfate 0.3～2, sodium lignosulfonate 0.1～0.5, fiber 0.01～0.5.
The lead-acid accumulator negative pole lead paste of above-mentioned suppression liberation of hydrogen, described carbon source is the in combination of two or more in graphite, white carbon black, superconductive carbon black, acetylene black, CNT；Described zinc source is the one or more combination of zinc oxide, zinc sulfide, zinc sulfate.
The lead-acid accumulator negative pole lead paste of above-mentioned suppression liberation of hydrogen, described leady oxide amount is 65%～80%, and described barium sulfate is 2500 mesh fine barium sulfates, and described sodium lignosulfonate is Norway's lignin, and described fiber is polyester fiber.
The preparation method of the lead-acid accumulator negative pole lead paste of above-mentioned suppression liberation of hydrogen, it carries out by following operation:
A. dispensing: weigh each raw material by above-mentioned lead plaster proportioning raw materials；
B. premix: by formula ratio carbon source, zinc source, sodium lignosulfonate, barium sulfate and the Hydrocerussitum (Ceruse) of Hydrocerussitum (Ceruse) total amount 0.5%～5%, mix homogeneously, standby；
C. it is dry mixed: the Hydrocerussitum (Ceruse) of remainder is put into paste mixing machine with the above-mentioned raw material through premix and is dry mixed；
D. wet mixing: after 1min～5min is dry mixed, it is quickly poured into and is mixed, by distilled water and proportional quantity fiber, the suspension formed, wherein distilled water is solid material gross weight 10-20%, after stirring 2min～5min, be slowly added to Hydrocerussitum (Ceruse) weight 6～14%, the density 1.400g/cm that is3Sulfuric acid solution, acid adding limit, limit stir, stir 10min～30min, go out cream.
The cathode lead plaster hydrogen precipitation problem that the present invention is directed to solve to reduce doping carbon is improved, break through lead-acid accumulator negative pole lead paste conventional formulation techniques, in cathode lead plaster, certain zinc compound and different types of carbon is added by proportioning, improve size and the microstructure of lead negative material, thus reach to improve the capacity of lead-acid battery, improve charge acceptance, and increase the purpose of charge and discharge cycles stability.Test shows, in cathode lead plaster, the doping of Zinc compounds can make the hydrogen-evolution overpotential of acid accumulator negative pole lead more negative, increase liberation of hydrogen difficulty, reduce hydrogen to separate out, reduce the consumption of electrolyte during using, be conducive to improving the life of storage battery, reduce the possibility that the dangerous accidents such as blast occur the most to a certain extent.Compared with routine techniques, the accumulator capacity using the technology of the present invention to make can improve 5～10%, and acid consumption reduces by 10～20%.
Accompanying drawing explanation
Fig. 1 is the discharge curve that the negative plate prepared in the process of the present invention is assembled into cell；
Fig. 2 is X-ray diffraction (XRD) figure after the negative plate chemical conversion prepared in the process of the present invention；
Fig. 3 is scanning electron microscope (SEM) figure after the negative plate chemical conversion prepared in the process of the present invention；
Fig. 4 is the liberation of hydrogen curve of negative plate and the common negative plate prepared in the process of the present invention；
Fig. 5 is that after the negative plate prepared in the process of the present invention is assembled into cell and conventional accumulators 20 charge and discharge cycles of circulation, the consumption of water compares schematic diagram.
Detailed description of the invention
The key technology of the present invention is to be improved lead-acid accumulator negative pole lead paste proportioning raw materials, adds certain carbon source and zinc source in cathode lead plaster raw material in proportion.Can improve the electric conductivity of active substance as conductive agent after carbon source being added in cathode lead plaster, especially when latter stage of discharging, active substance major part all becomes PbS04Crystal, needs to improve its electric conductivity.While addition carbon source improves its electric conductivity in cathode lead plaster, the hydrogen-evolution overpotential of lead negative pole can be made to shuffle, separate out substantial amounts of hydrogen when overcharge and large current charge, increase water consumption, increase the possibility that the unsafe incidents such as blast occur.To this end, the present invention adds zinc source such as zinc oxide, zinc sulfide, zinc sulfate etc. in cathode lead plaster raw material.The interpolation of Zinc compounds can improve the hydrogen-evolution overpotential of lead-acid accumulator, reduces the consumption of electrolyte during using, and reduces hydrogen and separates out, reduces the possibility that the dangerous accidents such as blast occur to a certain extent.The standard electrode potential of zinc is-1.216V, and the standard electrode potential of lead is-0.54V, and therefore, zinc has more negative electrode potential, it is not easy to be reduced to metallic zinc.Zinc oxide is a kind of water-fast white amphoteric oxide, is wide bandgap semiconductor materials, owing to zinc oxide is big to the affinity of electronics, make hydrion be not readily available electronics and generate the hydrogen molecule of neutrality, therefore, be equivalent to improve the deposition potential of hydrogen, it is possible to reduce the precipitation of hydrogen.Zinc oxide, as a kind of basic anhydride, can precipitate in electrolyte under the effect of sulfuric acid electrolyte, and the Zn content in negative plate reduces, and liberation of hydrogen inhibitory action reduces.The biggest effect to suppression liberation of hydrogen of addition is the most obvious, but the amount of the biggest active substance of addition can reduce accordingly, affects discharge capacity, and the amount of it is possible to additionally incorporate can cause plate active material loose after too much dissolving, and causes and comparatively fast comes off.Therefore, the addition in zinc source it is determined through experimentation.Zinc sulfide, zinc sulfate have the similar mechanism of action with zinc oxide, do not repeat.
Cathode lead plaster solid material proportioning of the present invention is following (mass parts): Hydrocerussitum (Ceruse) 100, carbon source 1～3, zinc source 0.15～1.0, barium sulfate 0.3～2, sodium lignosulfonate 0.1～0.5, fiber 0.01～0.5.Wherein, carbon source is the in combination of two or more (single material with carbon element structure is the most single, and action effect is poor) in graphite, white carbon black, superconductive carbon black, acetylene black, CNT；Described zinc source is the one or more combination of zinc oxide, zinc sulfide, zinc sulfate；Described leady oxide amount is 65%～80%, and described barium sulfate is 2500 mesh fine barium sulfates, and described sodium lignosulfonate is Norway's lignin, and described fiber is polyester fiber, and described sulfuric acid density is 1.400g/cm3。
Being coated in equably on grid by the lead plaster made according to proportioning of the present invention, temperature 30～50 DEG C, solidify 24 hours under conditions of humidity >=85%RH, then temperature 70～100 DEG C, humidity≤40%RH is dried, and i.e. makes negative plate.3 negative plates prepared as stated above and 2 conventional cathode plates are constituted an about 2Ah battery, then at 1.05g/cm3Dilute sulfuric acid be melted into: first shelve 20 minutes, then charge 50min with 300mA electric current, stand 8min, charge 240min with 700mA electric current, stand 10min, charge 480min with 600mA electric current, stand 10min, then 200mA electric current charging 120min.Referring to Fig. 1-5, Fig. 1 is negative plate of the present invention discharge curve under 1.25C multiplying power, and it is 2286mAh that electric discharge terminates capacity, exceeds about 7% than the capacity of regular convention formula battery.Fig. 2 is X-ray diffraction (XRD) figure of negative plate of the present invention, it is seen then that peak type is sharply clear, illustrates that crystal formation is preferable, does not has miscellaneous peak, and the standard card comparison with lead understands, and product is mainly based on simple substance lead.Fig. 3 is the scanning electron microscope diagram after negative plate of the present invention chemical conversion, and as seen from the figure, this negative material granule is less and more uniform.Fig. 4 is the present invention and common negative plate liberation of hydrogen curve under the conditions of identical charging current, visible under identical electric current, the hydrogen-evolution overpotential (A curve) of the battery that inventive formulation makes is more negative, i.e. inventive formulation battery precipitation hydrogen is more difficult, so the consumption of water is less under the same conditions.Fig. 5 is the comparison of the consumption of water after the monocell that negative plate of the present invention is made encloses with regular convention formula circulating battery 20, the battery consumption water yield (A figure) of this formula is 56 milliliters, and the battery consumption water yield of regular convention formula (B figure) is 71 milliliters, illustrating under state-of-charge and cycle-index, the battery consumption water yield that the negative plate of this formula does is less.This is consistent with the result of Fig. 4.
Several specific embodiments of cathode lead plaster proportioning raw materials of the present invention given below:
Embodiment 1, weighs following cathode lead plaster raw material: Hydrocerussitum (Ceruse) 1000g, graphite 10 g, white carbon black 5 g, zinc oxide 1.5 g, barium sulfate 3g, sodium lignosulfonate 1 g, fiber 0.1 g.
Embodiment 2, weighs following cathode lead plaster raw material: Hydrocerussitum (Ceruse) 1000g, white carbon black 10 g, superconductive carbon black 15 g, zinc oxide 3 g, zinc sulfide 1.5 g, barium sulfate 10g, sodium lignosulfonate 5g, fiber 5 g.
Embodiment 3, weighs following cathode lead plaster raw material: Hydrocerussitum (Ceruse) 1000g, graphite 10 g, white carbon black 15 g, acetylene black 5 g, zinc oxide 5 g, barium sulfate 20g, sodium lignosulfonate 4g, fiber 3g.
Embodiment 4, weighs following cathode lead plaster raw material: Hydrocerussitum (Ceruse) 1000g, CNT 5 g, white carbon black 5 g, zinc sulfate 7 g, barium sulfate 12g, sodium lignosulfonate 3 g, fiber 2 g.
Embodiment 5, weighs following cathode lead plaster raw material: Hydrocerussitum (Ceruse) 1000g, graphite 7 g, superconductive carbon black 12 g, white carbon black 5 g, zinc sulfide 10g, barium sulfate 8g, sodium lignosulfonate 2 g, fiber 0.5 g.
Embodiment 6, weighs following cathode lead plaster raw material: Hydrocerussitum (Ceruse) 1000g, CNT 15 g, white carbon black 15 g, zinc sulfide 1g, zinc sulfate 8 g, barium sulfate 12g, sodium lignosulfonate 3 g, fiber 2 g.
The preparation method of cathode lead plaster of the present invention is as follows: a. dispensing: weigh each raw material by above-mentioned lead plaster proportioning raw materials；B. premix: by formula ratio carbon source, zinc source, marasperse BS, barium sulfate etc. and part Hydrocerussitum (Ceruse) (Hydrocerussitum (Ceruse) total amount 0.5%～5%) mix homogeneously, the purpose of Hydrocerussitum (Ceruse) premix is to make additive, particularly carbon source and zinc source is evenly distributed in Hydrocerussitum (Ceruse), simple being dry mixed of paste mixing machine of dependence is difficult to accomplish, if additive and Hydrocerussitum (Ceruse) mixing inequality, the most too much material with carbon element be likely to result in lead plaster come off, the defect such as gassing aggravation.Standby；C. it is dry mixed: the Hydrocerussitum (Ceruse) of remainder is put into paste mixing machine with the above-mentioned raw material through premix and is dry mixed；D. wet mixing: after 1min～5min is dry mixed, it is quickly poured into and is mixed, by distilled water and proportional quantity fiber, the suspension formed, wherein distilled water is solid material gross weight 10-20%, after stirring 2min～5min, be slowly added to Hydrocerussitum (Ceruse) weight 6～14%, the density 1.400g/cm that is3Sulfuric acid solution, acid adding limit, limit stir, stir 10min～30min, go out cream.
Claims (2)
1. the preparation method of the lead-acid accumulator negative pole lead paste suppressing liberation of hydrogen, it is characterised in that: described lead plaster solid material is made up of the material of following weight unit's: Hydrocerussitum (Ceruse) 100, carbon source 1～3, zinc source 0.15～1.0, barium sulfate 0.3～2, sodium lignosulfonate 0.1～0.5, fiber 0.01～0.5；
Described carbon source is the in combination of two or more in graphite, superconductive carbon black, acetylene black, CNT；Described zinc source is the one or more combination of zinc oxide, zinc sulfide, zinc sulfate；
Preparation is carried out by following operation:
A. dispensing: weigh each raw material by above-mentioned lead plaster solid material proportioning；
B. premix: by proportional quantity carbon source, zinc source, sodium lignosulfonate, barium sulfate and the Hydrocerussitum (Ceruse) mix homogeneously of Hydrocerussitum (Ceruse) total amount 0.5%～5%, standby；
C. it is dry mixed: the Hydrocerussitum (Ceruse) of remainder is put into paste mixing machine with the above-mentioned raw material through premix and is dry mixed；
D. wet mixing: after 1min～5min is dry mixed, it is quickly poured into and is mixed, by distilled water and proportional quantity fiber, the suspension formed, wherein distilled water is solid material gross weight 10-20%, after stirring 2min～5min, be slowly added to Hydrocerussitum (Ceruse) weight 6～14%, density be 1.400g/cm3Sulfuric acid solution, acid adding limit, limit stir, stir 10min～30min, go out cream.
The preparation method of the lead-acid accumulator negative pole lead paste of suppression liberation of hydrogen the most according to claim 1, it is characterised in that: described leady oxide amount is 65%～80%, and described barium sulfate is 2500 mesh fine barium sulfates, and described fiber is polyester fiber.
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