CN102134094A - Method for preparing high-purity lead-acid barium conductive material for lead-acid storage battery - Google Patents
Method for preparing high-purity lead-acid barium conductive material for lead-acid storage battery Download PDFInfo
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- CN102134094A CN102134094A CN2011100401427A CN201110040142A CN102134094A CN 102134094 A CN102134094 A CN 102134094A CN 2011100401427 A CN2011100401427 A CN 2011100401427A CN 201110040142 A CN201110040142 A CN 201110040142A CN 102134094 A CN102134094 A CN 102134094A
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- barium
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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 relates to a method for preparing a high-purity lead-acid barium conductive material for a lead-acid storage battery, in particular to a lead-acid barium conductive material applied to a lead-acid storage battery. Lead monoxide and barium oxide are used as main raw materials; and the material is prepared by the steps of proportioning, salinization, co-precipitation, drying, sintering, crushing and the like. The lead-acid barium material is a powdery material with good electric conductivity, and can be used as a conductive additive and applied in a storage battery polar plate. The internal resistance of the battery is reduced, the initial capacity of the battery is increased, and good charge receiving capacity is obtained.
Description
Technical field
The invention belongs to chemical power source material field, be specifically related to a kind of production technology that can be used for the plumbic acid barium electro-conductive material of polar plate of lead acid storage battery.
Background technology
The performance of anode plate for lead acid accumulator is the main determining factor of cell integrated performance.In positive plate lead plaster, add an amount of conductive additive, can reduce the internal resistance of battery, increase the initial capacity of battery, and make battery have charge acceptance preferably.Conductive additive at present commonly used is carbon materialses such as graphite, acetylene black, has poor stability, shortcoming that rate of loss is high.Plumbic acid barium has good conductivity, stable high characteristics, uses as the conductive additive in the anode diachylon to have important use value, but in application process material purity is had relatively high expectations.Therefore how preparing high purity plumbic acid barium is the technical bottleneck of this material widespread use, only addresses this problem plumbic acid barium material is used widely in store battery, constantly promotes the store battery product performance.
Summary of the invention
The object of the present invention is to provide a kind of preparation method of high purity plumbic acid barium electro-conductive material, constantly advance the progress of lead acid cell product.
The present invention includes following steps:
A. salinization reaction: yellow lead oxide and the barium oxide ratio that with mol ratio be 1.08～1.02:1 of purity more than chemical pure mixed with acetum, stir to clarify transparent, formation salinization reaction solution;
B. coprecipitation reaction: oxalic acid solution is added in the salinization reaction solution, and reaction obtains the coprecipitate of lead oxalate and barium oxalate;
C. separate: remove supernatant, get coprecipitate;
D. sintering: get coprecipitate sintering under 800～850 ℃ of environment, after product to be sintered is cooled to room temperature, pulverizes and obtain plumbic acid barium electro-conductive material.
The present invention is a main raw material with the yellow lead oxide and the barium oxide of purity more than chemical pure, at first obtains the plumbic acetate and the barium acetate of solubility through the peracetate processing; Secondly make the lead salt of solubility and barium salt that co-precipitation take place in solution by adding oxalic acid, obtain highly purified lead oxalate, barium oxalate coprecipitate; Generate high-purity plumbic acid barium with the coprecipitate separation and by high temperature sintering then; At last through pulverizing the black powder shape product that promptly obtains high-purity plumbic acid barium.Use higher yellow lead oxide of purity and barium oxide product purity is improved, reduce foreign matter content as main raw material; Method by chemical coprecipitation prepares intermediate product, and lead element and barium element are mixed in the molecule rank, helps the conversion of product in the sintering process, has ensured the high purity of product.High-purity plumbic acid barium is applied in the positive plate lead plaster as conductive additive, can reduces the internal resistance of battery, increase the initial capacity of battery, and make battery have charge acceptance preferably, improve the overall performance of store battery product.
In addition, among the step a, the molar ratio of used acetic acid and yellow lead oxide is 4.2～4.5:1, and the working concentration of acetum is 12～20 wt %.Molar ratio 4.2～4.5:1 according to acetic acid and yellow lead oxide reacts, and helps plumbic acetate and barium acetate blend that yellow lead oxide in the reactant and barium oxide are converted into solubility fully; The working concentration of acetum is 12～20 wt %, can guarantee that reactant reacts rapidly, improves reaction efficiency.
Among the step b, the molar ratio of used oxalic acid and yellow lead oxide is 2.5～2.8:1, and oxalic acid solution concentration is 10～15 wt %.Molar ratio 2.5～2.8:1 according to oxalic acid and yellow lead oxide reacts, and the plumbic acetate and the barium acetate blend that help solubility are converted into lead oxalate and barium oxalate coprecipitate fully; The working concentration of oxalic acid solution is 10～15 wt %, can guarantee that coprecipitation reaction takes place rapidly for oxalic acid and plumbic acetate and barium acetate, improves reaction efficiency.
In the steps d, sintering time is 6～8 hours.Sintering time is too short, is unfavorable for the generation of product plumbic acid barium, has reduced production efficiency; Sintering time is long, can cause waste again, has increased production cost.Select sintering time 6～8 hours under 800～850 ℃ of environment, both can having guaranteed reacts completely carries out, and can not increase production cost again, is suitable reaction conditions.
Embodiment
One, example 1:
1, the barium oxide 153.3g (1.00mol) more than chemical pure mixes at yellow lead oxide 234.2g (1.05mol) more than the chemical pure and purity accurately to take by weighing purity.
2, preparation 1720g concentration is the acetum (acetic acid 4.3mol) of 15wt% and the oxalic acid solution (oxalic acid 2.6mol) that 1950g concentration is 12 wt%.
At first, the yellow lead oxide that proportioning is good and plumbic acid barium add in the acetum, stir to clarify transparently, finish the salinization reaction, produce plumbic acetate and barium acetate; Secondly, oxalic acid solution is slowly joined in the salinization reaction solution, do not stop to stir, coprecipitation reaction takes place, obtain the coprecipitate of lead oxalate and barium oxalate; At last, through separating, get coprecipitate in 800 ℃ of following sintering 8h, after product to be sintered was cooled to room temperature, pulverizing and obtaining purity was 98% black plumbic acid barium dust shape product, and promptly lead acid cell is with high purity plumbic acid barium electro-conductive material.
Two, example 2:
1, the barium oxide 153.3g (1.00mol) more than chemical pure mixes at yellow lead oxide 227.5g (1.02mol) more than the chemical pure and purity accurately to take by weighing purity.
2, preparation 1467g concentration is the acetum (acetic acid 4.4mol) of 18wt% and the oxalic acid solution (oxalic acid 2.8mol) that 1680g concentration is 15 wt%.
At first, the yellow lead oxide that proportioning is good and plumbic acid barium add in the acetum, stir to clarify transparently, finish the salinization reaction, produce plumbic acetate and barium acetate; Secondly, oxalic acid solution is slowly joined in the salinization reaction solution, do not stop to stir, coprecipitation reaction takes place, obtain the coprecipitate of lead oxalate and barium oxalate; At last, after the coprecipitate separation, in 850
oSintering 6h under the C, after product to be sintered was cooled to room temperature, pulverizing and obtaining purity was 99% black plumbic acid barium dust shape product, promptly lead acid cell is with high purity plumbic acid barium electro-conductive material.
Claims (4)
1. lead acid cell is characterized in that may further comprise the steps with the preparation method of high purity plumbic acid barium electro-conductive material:
A. salinization reaction: yellow lead oxide and the barium oxide ratio that with mol ratio be 1.08～1.02:1 of purity more than chemical pure mixed with acetum, stir to clarify transparent, formation salinization reaction solution;
B. coprecipitation reaction: oxalic acid solution is added in the salinization reaction solution, and reaction obtains the coprecipitate of lead oxalate and barium oxalate;
C. separate: remove supernatant, get coprecipitate;
D. sintering: get coprecipitate sintering under 800～850 ℃ of environment, after product to be sintered is cooled to room temperature, pulverizes and obtain plumbic acid barium electro-conductive material.
2. according to the preparation method of the described lead acid cell of claim 1, it is characterized in that among the step a that the molar ratio of used acetic acid and yellow lead oxide is 4.2～4.5:1, and acetum concentration is 12～20 wt % with high purity plumbic acid barium electro-conductive material.
3. according to the preparation method of the described lead acid cell of claim 1, it is characterized in that among the step b that the molar ratio of used oxalic acid and yellow lead oxide is 2.5～2.8:1, and oxalic acid solution concentration is 10～15 wt % with high purity plumbic acid barium electro-conductive material.
4. according to the preparation method of the described lead acid cell of claim 1, it is characterized in that in the steps d that sintering time is 6～8 hours with high purity plumbic acid barium electro-conductive material.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2011100401427A CN102134094A (en) | 2011-02-18 | 2011-02-18 | Method for preparing high-purity lead-acid barium conductive material for lead-acid storage battery |
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| CN2011100401427A CN102134094A (en) | 2011-02-18 | 2011-02-18 | Method for preparing high-purity lead-acid barium conductive material for lead-acid storage battery |
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| CN102134094A true CN102134094A (en) | 2011-07-27 |
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| CN2011100401427A Pending CN102134094A (en) | 2011-02-18 | 2011-02-18 | Method for preparing high-purity lead-acid barium conductive material for lead-acid storage battery |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102660683A (en) * | 2012-03-13 | 2012-09-12 | 北京科技大学 | Method for preparing barium plumbate powder by coprecipitation of copper anode mud silver separating residue of circuit board |
| CN102683708A (en) * | 2012-05-18 | 2012-09-19 | 湖南维邦新能源有限公司 | Negative plate of battery, preparation method thereof and battery comprising negative plate |
| CN106784805A (en) * | 2015-11-25 | 2017-05-31 | 衡阳瑞达电源有限公司 | Anode material of lead-acid battery and lead accumulator |
| CN111697201A (en) * | 2019-08-12 | 2020-09-22 | 福州伯瑞电源科技有限公司 | Production of high-power lead-acid storage battery positive plate |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS63210057A (en) * | 1987-02-27 | 1988-08-31 | 株式会社デンソー | Manufacture of high temperature ptc material |
| RO116136B1 (en) * | 1995-05-30 | 2000-10-30 | Inst De Fizica Si Tehnologia M | PROCESS FOR PRODUCING THIN CONDUCTIVE LAYERS OF BaPbO3 |
-
2011
- 2011-02-18 CN CN2011100401427A patent/CN102134094A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS63210057A (en) * | 1987-02-27 | 1988-08-31 | 株式会社デンソー | Manufacture of high temperature ptc material |
| RO116136B1 (en) * | 1995-05-30 | 2000-10-30 | Inst De Fizica Si Tehnologia M | PROCESS FOR PRODUCING THIN CONDUCTIVE LAYERS OF BaPbO3 |
Non-Patent Citations (4)
| Title |
|---|
| 《Journal of Alloys and Compounds》 20061004 Masahiro Yasukawa et al. Preparation of dense BaPbO3-based ceramics by a coprecipitation and their thermoelectric properties 第420-425页 1-4 第426卷, 2 * |
| 《功能材料》 19991231 宋练鹏 化学液相法制备BaPbO3 导电陶瓷 第392-393页 1-4 第30卷, 第4期 2 * |
| 《湘潭矿业学院学报》 20030630 刘心宇等 液相共沉淀法制备BaPbO3导电陶瓷粉末 第44-47页 1-4 第18卷, 第2期 2 * |
| 《硅酸盐学报》 20030630 刘心宇等 液相共沉淀法制备BaPbO3导电陶瓷的研究 第547-551页 1-4 第31卷, 第6期 2 * |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102660683A (en) * | 2012-03-13 | 2012-09-12 | 北京科技大学 | Method for preparing barium plumbate powder by coprecipitation of copper anode mud silver separating residue of circuit board |
| CN102683708A (en) * | 2012-05-18 | 2012-09-19 | 湖南维邦新能源有限公司 | Negative plate of battery, preparation method thereof and battery comprising negative plate |
| CN106784805A (en) * | 2015-11-25 | 2017-05-31 | 衡阳瑞达电源有限公司 | Anode material of lead-acid battery and lead accumulator |
| CN111697201A (en) * | 2019-08-12 | 2020-09-22 | 福州伯瑞电源科技有限公司 | Production of high-power lead-acid storage battery positive plate |
| CN111697201B (en) * | 2019-08-12 | 2023-04-11 | 福州伯瑞电源科技有限公司 | Production of high-power lead-acid storage battery positive plate |
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Application publication date: 20110727 |