CN104218270A - Method for preparing tetrabasic lead sulfate by using acid leaching byproduct in production of lead acid storage battery positive electrode plate - Google Patents
Method for preparing tetrabasic lead sulfate by using acid leaching byproduct in production of lead acid storage battery positive electrode plate Download PDFInfo
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- CN104218270A CN104218270A CN201410306028.8A CN201410306028A CN104218270A CN 104218270 A CN104218270 A CN 104218270A CN 201410306028 A CN201410306028 A CN 201410306028A CN 104218270 A CN104218270 A CN 104218270A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G21/00—Compounds of lead
- C01G21/20—Sulfates
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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
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W30/00—Technologies for solid waste management
- Y02W30/50—Reuse, recycling or recovery technologies
- Y02W30/84—Recycling of batteries or fuel cells
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Abstract
The invention relates to a method for preparing tetrabasic lead sulfate by using an acid leaching byproduct in the production of a lead acid storage battery positive electrode plate. The method comprises the following steps: 1, draining water on the surface of the acid leaching byproduct, respectively determining the content of lead sulfate, lead oxide, simple substance lead and water in the acid leaching byproduct through a chemical analysis technology and a gravimetric analysis technology, and determining the percentage content of lead sulfate and lead oxide; 2, adding the surface water drained acid leaching byproduct into a reaction kettle, supplementing lead oxide or lead powder used for producing the lead acid storage battery according to the determination results obtained in step 1 to make a molar ratio of lead oxide to lead sulfate in the reaction kettle reach 3-6.5:1, and using deionized water as a reaction medium in a reaction system; and 3, preparing the tetrabasic lead sulfate. The above raw material is the lead acid battery byproduct and is applied to the production of the lead acid battery, so waste recycling is realized, the production cost of the lead acid storage battery is reduced, the method is environmentally friendly, and the quality of the battery is improved.
Description
Technical field
The present invention relates to a kind of method of utilizing of anode plate for lead acid accumulator accessory substance, particularly a kind of utilization drenched the method that sour accessory substance is prepared four basic lead sulphates in anode plate for lead acid accumulator manufacture.
Background technology
Lead acid accumulator because of possess safety, reliable, manufacture that letter is answered, the advantage such as cheap becomes the chemical power source that society is most widely used.But lead acid accumulator can produce a large amount of leaded accessory substances in process of production.Current most battery manufacturers is peddled the smelting for lead bullion to plumbous returned enterprise after all adopting accessory substance to collect, but the cost control that this way is brought is very low, and lead bullion smelting process also can be brought the pollution of environment.Therefore how to handle that these leaded accessory substances are controlled cost for lead acid accumulator enterprise well and just seem very important as the image of social responsibility enterprise.In addition, there is serious early stage capacitance loss (PCL) problems such as anode plate grid excessive corrosion, active material softening and shedding and negative pole sulfation in lead acid accumulator, has greatly restricted its development.
The pouring acid accessory substance that anode plate for lead acid accumulator produces in manufacturing, is commonly called as in the industry plumbous mud, and the intensive collection and treatment of the general employing of Qian Ni lead acid accumulator enterprise, as giving plumbous returned enterprise containing scrap lead unified sale.But lead acid accumulator is strictly controlled at preparation process Program, also just achieved the stable composition of plumbous mud and formed.Plumbous mud contains lead sulfate, lead oxide, simple substance lead and moisture, also contains in addition a small amount of lead acid accumulator solid for mulation composition.Each component content all can be stablized within the specific limits, therefore can well utilize the stability of plumbous mud to go to carry out processing again of refuse, turns waste into wealth.Positive plate washes away through drenching acid the accessory substance that gets off in addition, and particle is tiny, and other byproducts of preparing with this accessory substance also can be controlled particle diameter and homogeneity better.
Four alkali formula sulfuric acid are generally to be made by lead oxide and lead sulfate melting.Four basic lead sulphates also available lead oxide and lead sulfate aqueous suspension boil and make.Four basic lead sulphates are as Chinese white, the heat stabilizer of plastics and additives of lead-acid battery.Research finds that four basic lead sulphates have the advantages such as crystalline size is large, intercrystalline connection is tight, when existing, anode plate for lead acid accumulator can form the skeleton structure of active material, mechanical strength is high, can suppress PCL phenomenon, extends the cycle life of lead acid accumulator.Therefore if utilized, in anode plate for lead acid accumulator manufacture, drench sour accessory substance and prepare four basic lead sulphates, and four basic lead sulphates of preparation are applied in anode plate for lead acid accumulator, the leaded accessory substance of production process will both can well be disposed, also four basic lead sulphates that accessory substance can be prepared are added into the cycle life that improves battery in battery, can play the effect killing two birds with one stone.
Summary of the invention
The invention provides a kind of utilization and in anode plate for lead acid accumulator manufacture, drench the method that sour accessory substance is prepared four basic lead sulphates.
The technical solution adopted for the present invention to solve the technical problems is:
Utilize in anode plate for lead acid accumulator manufacture and drench the method that sour accessory substance is prepared four basic lead sulphates, the method comprises the steps:
A, determine that positive plate drenches the composition of sour accessory substance: drain the moisture that drenches sour accessory substance surface, by chemical analysis and gravimetry, determine respectively the content that drenches lead sulfate, lead oxide, simple substance lead and moisture in sour accessory substance, and the percentage composition of definite lead sulfate and lead oxide;
B, determine that lead acid accumulator produces the use amount with lead powder: get the sour accessory substance of the pouring draining after surface moisture and add in reactor, according to the measurement result of step a, add lead oxide or lead acid accumulator production lead powder (oxidizability is 70 ~ 85%), the amount of substance ratio of the interior lead oxide of reactor and lead sulfate is reached within the scope of 3 ~ 6.5:1, and reaction system be take deionized water as reaction medium;
The preparation of c, four basic lead sulphates: reaction system is 70 ~ 120 ℃ of temperature, reacts 1 ~ 10 hour under the condition constantly stirring, product ball milling 1 ~ 10 hour under the rotating speed of 100 ~ 300r/min, and then drying and crushing obtains four basic lead sulphate products.
The present invention take anode plate for lead acid accumulator in producing discarded object---drench sour accessory substance for the raw material of preparation four basic lead sulphates, raw material is easy to get, the composition of the pouring acid accessory substance of most of lead acid accumulator manufacturing enterprise is similar to, the inventive method can large-scale promotion.
As preferably, add lead acid accumulator and produce while using lead powder (oxidizability is 70 ~ 85%), with the lead oxide containing in lead powder, calculate the quality of adding lead powder.
As preferably, the preparation detailed process of step c, four basic lead sulphates is as follows: reactor is installed in the homogeneous reactor of 70 ~ 120 ℃, under the condition constantly stirring, reacts 1 ~ 10 hour; After in reactor, reaction finishes, product is proceeded in ball mill, under the rotating speed of 100 ~ 300r/min, ball milling is 1 ~ 10 hour; Product after ball milling carries out drying and crushing and obtains four basic lead sulphate products.
As preferably, free lead content 9.8% ~ 10.1% in the sour accessory substance of described pouring, lead sulfate content 35.0% ~ 36.6%, lead oxide content 18.9% ~ 19.3%, moisture 35.0% ~ 36.5%.
As preferably, the consumption of deionized water is 1 ~ 1.5 times of reactant weight.I haven't seen you for ages makes reactant too sticky for amount of deionized water, and reaction should not be carried out; Cross and affect at most reaction speed.
It is raw material that the present invention utilizes the byproduct in lead acid accumulator production process, by simple method, prepares additive four basic lead sulphates that lead-acid battery can re-use.Both can reduce the production cost of lead acid accumulator, can also slow down capacity attenuation problem in lead acid accumulator early stage, simultaneously can protection of the environment reduce the discharge of pollutant.Lead acid accumulator enterprise can actually carry out large-scale production in conjunction with self.
The conventional preparation method of current four basic lead sulphates is high temperature solid-state method, sintering process and tribasic lead sulfate decomposition method etc.The raw materials for production purity requirement that these methods are used is higher, and production process severe reaction conditions power consumption is simultaneously serious, and easily causes secondary pollution.
The present invention adopts in lead acid accumulator manufacture positive plate to drench sour accessory substance and production is produced four basic lead sulphates with lead powder as raw material, owing to drenching, sour byproduct particles is tiny, stable mass production four basic lead sulphates that are applicable to of material composition, and the four basic lead sulphate particle homogeneous of producing are tiny, short grained four basic lead sulphates are applied to anode additive of lead acid storage battery, can be distributed in uniformly in positive plate, well improve the intensity of positive plate, for slowing down premature capacity loss of lead acid battery phenomenon, there is good effect, improve the cycle life of lead acid accumulator.Raw material sources of the present invention are applied to again lead-acid battery in lead-acid battery accessory substance and produce, and realize refuse cycling and reutilization, and the production cost that can reduce lead acid accumulator is simultaneously environmentally friendly, and can improve the quality of battery, are to achieve many things at one stroke.
Specific embodiment
Below by specific embodiment, technical scheme of the present invention is described in further detail.Should be appreciated that enforcement of the present invention is not limited to the following examples, any pro forma accommodation that the present invention is made and/or change all will fall into protection range of the present invention.
In the present invention, if not refer in particular to, all part, percentages are unit of weight, and the equipment adopting and raw material etc. all can be buied from market or this area is conventional.Method in following embodiment, if no special instructions, is the conventional method of this area.
Drenching sour accessory substance derives from: Chilwee Power Co., Ltd.'s positive plate fabrication stage drenches sour process and washes away the accessory substance that gets off.In the following embodiment of the present invention, drench sour accessory substance chemical composition stability, wherein free lead content 9.5% ~ 10.1%, lead sulfate content 35.0% ~ 36.6%, lead oxide content 18.6% ~ 19.3%, moisture 35.0% ~ 36.5%, wherein, also containing having an appointment 1% additives of lead-acid battery, this part additive does not produce effect to the production of four basic lead sulphates.
embodiment 1:
Accurately take the pouring acid accessory substance that 100g drains surface moisture, by compleximetry, obtain the content of lead sulfate, lead oxide, free lead, by gravimetric analysis, determine the content of moisture; Being respectively lead sulfate content 36.6%, lead oxide content 18.6%, free lead content 9.5%, moisture is 35.0%, and all the other impurity are partly lead acid battery positive electrode formula, and impurity on reaction without impact and content seldom, is not considered.
By calculating the amount of substance of lead oxide, lead sulfate in this 100g accessory substance, this 100g accessory substance is added in reactor, according to lead oxide, be 3:1 proportioning reactant with lead sulfate amount of substance ratio, also need to add in addition 61.5g pure zirconia plumbous, amount to into lead powder for production (oxidizability 75%), namely also need in reactor, add 82g and produce with lead powder (oxidizability 75%), add 200g deionized water as the medium of reaction simultaneously;
Reactor is installed in homogeneous reactor, continuous stirring reaction 9 hours at 70 ℃;
Reactor product proceeds in ball mill under 300r/min condition ball milling 3 hours;
End reaction thing drying and crushing obtains powdery four basic lead sulphates, and purity is 80.4%.
?
embodiment 2
Accurately take the pouring acid accessory substance that 100g drains surface moisture, by chemical analysis, obtain the content of lead sulfate, lead oxide, free lead and moisture;
By calculating the amount of substance of lead oxide in accessory substance, lead sulfate, this 100g accessory substance is added in reactor, according to lead oxide and lead sulfate amount of substance, than add 118g production lead powder (oxidizability 75%) in reactor for 4:1, (produce by the computational methods of lead powder consumption with embodiment 1, lower same), add 250g deionized water as the medium of reaction simultaneously;
Reactor is installed in homogeneous reactor, continuous stirring reaction 7 hours at 90 ℃;
Reactor product proceeds in ball mill under 300r/min condition ball milling 5 hours;
End reaction thing drying and crushing obtains powdery four basic lead sulphates, and purity is 84%.
?
embodiment 3
Accurately take the pouring acid accessory substance that 100g drains surface moisture, by chemical analysis, obtain the content of lead sulfate, lead oxide, free lead and moisture;
By calculating the amount of substance of lead oxide in accessory substance, lead sulfate, this 100g accessory substance is added in reactor, according to lead oxide and lead sulfate amount of substance, than add 154g in reactor for 5:1, produce with lead powder (oxidizability 75%), add 300g deionized water as the medium reacting simultaneously;
Reactor is installed in homogeneous reactor, continuous stirring reaction 4 hours at 100 ℃;
Reactor product proceeds in ball mill under 300r/min condition ball milling 6 hours;
End reaction thing drying and crushing obtains powdery four basic lead sulphates, and purity is 81%.
?
embodiment 4
Accurately take the pouring acid accessory substance that 100g drains surface moisture, by chemical analysis, obtain the content of lead sulfate, lead oxide, free lead and moisture;
By calculating the amount of substance of lead oxide in accessory substance, lead sulfate, this 100g accessory substance is added in reactor, according to lead oxide and lead sulfate amount of substance, than add 150g in reactor for 5:1, produce with lead powder (oxidizability 75%), add a certain amount of deionized water as the medium reacting simultaneously;
Reactor is installed in homogeneous reactor, continuous stirring reaction 4 hours at 110 ℃;
Reactor product proceeds in ball mill under 300r/min condition ball milling 6 hours;
End reaction thing drying and crushing obtains powdery four basic lead sulphates, and purity is 84.4%.
?
embodiment 5
Accurately take the pouring acid accessory substance that 100g drains surface moisture, by chemical analysis, obtain the content of lead sulfate, lead oxide, free lead and moisture;
By calculating the amount of substance of lead oxide in accessory substance, lead sulfate, this 100g accessory substance is added in reactor, according to lead oxide and lead sulfate amount of substance, than add 172g in reactor for 5.5:1, produce with lead powder (oxidizability 75%), add 330g deionized water as the medium reacting simultaneously;
Reactor is installed in homogeneous reactor, continuous stirring reaction 5 hours at 110 ℃;
Reactor product proceeds in ball mill under 200r/min condition ball milling 5 hours;
End reaction thing drying and crushing obtains powdery four basic lead sulphates, and purity is 82.2%.
?
embodiment 6
Accurately take the pouring acid accessory substance that 100g drains surface moisture, by chemical analysis, obtain the content of lead sulfate, lead oxide, free lead and moisture;
By calculating the amount of substance of lead oxide in accessory substance, lead sulfate, this 100g accessory substance is added in reactor, according to lead oxide and lead sulfate amount of substance, than add 190g in reactor for 6:1, produce with lead powder (oxidizability 75%), add 350g deionized water as the medium reacting simultaneously;
Reactor is installed in homogeneous reactor, continuous stirring reaction 2 hours at 120 ℃;
Reactor product proceeds in ball mill under 200r/min condition ball milling 7 hours;
End reaction thing drying and crushing obtains powdery four basic lead sulphates, and purity is 83.4%.
?
embodiment 7
Accurately take the pouring acid accessory substance that 100g drains surface moisture, by chemical analysis, obtain the content of lead sulfate, lead oxide, free lead and moisture;
By calculating the amount of substance of lead oxide in accessory substance, lead sulfate, this 100g accessory substance is added in reactor, according to lead oxide and lead sulfate amount of substance, than add 208g in reactor for 6.5:1, produce with lead powder (oxidizability 75%), add 380g deionized water as the medium reacting simultaneously;
Reactor is installed in homogeneous reactor, continuous stirring reaction 3 hours at 120 ℃;
Reactor product proceeds in ball mill under 200r/min condition ball milling 6 hours;
End reaction thing drying and crushing obtains powdery four basic lead sulphates, and purity is 80.6%.
Raw material of the present invention is to drench sour accessory substance, lead sulfate and particles of lead oxide are tiny, the tiny homogeneous of four basic lead sulphate particle diameters of preparing with this raw material, average grain diameter is below 10 μ m, as additive, add in lead acid battery positive electrode, can be dispersed, for lead acid accumulator cycle performance, there is very large castering action.
Above-described embodiment is a kind of preferably scheme of the present invention, not the present invention is done to any pro forma restriction, also has other variant and remodeling under the prerequisite that does not exceed the technical scheme that claim records.
Claims (5)
1. utilize in anode plate for lead acid accumulator manufacture and drench the method that sour accessory substance is prepared four basic lead sulphates, it is characterized in that the method comprises the steps:
A, determine that positive plate drenches the composition of sour accessory substance: drain the moisture that drenches sour accessory substance surface, by chemical analysis and gravimetry, determine respectively the content that drenches lead sulfate, lead oxide, simple substance lead and moisture in sour accessory substance, and the percentage composition of definite lead sulfate and lead oxide;
B, determine that lead acid accumulator produces the use amount with lead powder: get the sour accessory substance of the pouring draining after surface moisture and add in reactor, according to the measurement result of step a, add lead oxide or lead acid accumulator production lead powder, the amount of substance ratio of the interior lead oxide of reactor and lead sulfate is reached within the scope of 3 ~ 6.5:1, and reaction system be take deionized water as reaction medium;
The preparation of c, four basic lead sulphates: reaction system is 70 ~ 120 ℃ of temperature, reacts 1 ~ 10 hour under the condition constantly stirring, product ball milling 1 ~ 10 hour under the rotating speed of 100 ~ 300r/min, and then drying and crushing obtains four basic lead sulphate products.
2. according to claim 1 utilization in anode plate for lead acid accumulator manufacture drenched the method that sour accessory substance is prepared four basic lead sulphates, it is characterized in that: add lead acid accumulator and produce while using lead powder, with the lead oxide containing in lead powder, calculate the quality of adding lead powder.
3. according to claim 1 and 2 utilization drenched the method that sour accessory substance is prepared four basic lead sulphates in anode plate for lead acid accumulator manufacture, the preparation detailed process that it is characterized in that step c, four basic lead sulphates is as follows: reactor is installed in the homogeneous reactor of 70 ~ 120 ℃, under the condition constantly stirring, reacts 1 ~ 10 hour; After in reactor, reaction finishes, product is proceeded in ball mill, under the rotating speed of 100 ~ 300r/min, ball milling is 1 ~ 10 hour; Product after ball milling carries out drying and crushing and obtains four basic lead sulphate products.
4. according to claim 1 utilization in anode plate for lead acid accumulator manufacture drenched the method that sour accessory substance is prepared four basic lead sulphates, it is characterized in that: lead sulfate content 35.0% ~ 36.6% in the sour accessory substance of described pouring, lead oxide content 18.9% ~ 19.3%.
5. according to claim 4 utilization in anode plate for lead acid accumulator manufacture drenched the method that sour accessory substance is prepared four basic lead sulphates, it is characterized in that: the consumption of deionized water is 1 ~ 1.5 times of reactant weight.
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104767003A (en) * | 2015-03-19 | 2015-07-08 | 安徽中能电源有限公司 | Lead-mud deepening treatment and reuse method in storage battery electrode plate coating process |
| CN105390763A (en) * | 2015-11-06 | 2016-03-09 | 天能电池集团（安徽）有限公司 | Method for preparing tetrabasic lead sulfate from waste lead plaster |
| CN106299521A (en) * | 2016-08-20 | 2017-01-04 | 超威电源有限公司 | A kind of lead-acid accumulator drenches acid scrap lead mud direct circulation and reclaims the method utilized |
| CN106564941A (en) * | 2016-11-04 | 2017-04-19 | 浙江兜兰智能设备股份有限公司 | Method for preparing tetrabasic lead sulfate |
| CN106587141A (en) * | 2016-11-04 | 2017-04-26 | 浙江兜兰智能设备股份有限公司 | Production process and device for tetrabasic lead sulfate (4BS) |
| CN106684463A (en) * | 2016-07-14 | 2017-05-17 | 安徽轰达电源有限公司 | Method for preparing 4BS seed crystal of lead-acid battery employing grinding method |
| CN107265497A (en) * | 2017-05-22 | 2017-10-20 | 朱可可 | It is a kind of to extend the method that yellow lead energy-saving production technology prepares four basic lead sulphates |
| CN109399698A (en) * | 2018-09-30 | 2019-03-01 | 超威电源有限公司 | A method of utilizing leaching clay standby four basic lead sulphates of lead plumbate |
| CN110526284A (en) * | 2019-10-15 | 2019-12-03 | 超威电源集团有限公司 | A kind of preparation method of four basic lead sulphates |
| CN113097443A (en) * | 2021-03-29 | 2021-07-09 | 济源职业技术学院 | Tubular positive plate prepared from tubular positive waste lead paste and preparation method thereof |
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Cited By (13)
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| CN104767003A (en) * | 2015-03-19 | 2015-07-08 | 安徽中能电源有限公司 | Lead-mud deepening treatment and reuse method in storage battery electrode plate coating process |
| CN105390763B (en) * | 2015-11-06 | 2018-06-29 | 天能电池集团（安徽）有限公司 | The method that scrap lead cream prepares four basic lead sulphates |
| CN105390763A (en) * | 2015-11-06 | 2016-03-09 | 天能电池集团（安徽）有限公司 | Method for preparing tetrabasic lead sulfate from waste lead plaster |
| CN106684463A (en) * | 2016-07-14 | 2017-05-17 | 安徽轰达电源有限公司 | Method for preparing 4BS seed crystal of lead-acid battery employing grinding method |
| CN106299521A (en) * | 2016-08-20 | 2017-01-04 | 超威电源有限公司 | A kind of lead-acid accumulator drenches acid scrap lead mud direct circulation and reclaims the method utilized |
| CN106564941A (en) * | 2016-11-04 | 2017-04-19 | 浙江兜兰智能设备股份有限公司 | Method for preparing tetrabasic lead sulfate |
| CN106587141A (en) * | 2016-11-04 | 2017-04-26 | 浙江兜兰智能设备股份有限公司 | Production process and device for tetrabasic lead sulfate (4BS) |
| CN107265497A (en) * | 2017-05-22 | 2017-10-20 | 朱可可 | It is a kind of to extend the method that yellow lead energy-saving production technology prepares four basic lead sulphates |
| CN107265497B (en) * | 2017-05-22 | 2019-11-15 | 安徽徽能化工科技有限公司 | A method of extending yellow lead energy-saving production technology and prepares four basic lead sulphates |
| CN109399698A (en) * | 2018-09-30 | 2019-03-01 | 超威电源有限公司 | A method of utilizing leaching clay standby four basic lead sulphates of lead plumbate |
| CN110526284A (en) * | 2019-10-15 | 2019-12-03 | 超威电源集团有限公司 | A kind of preparation method of four basic lead sulphates |
| CN110526284B (en) * | 2019-10-15 | 2022-03-01 | 超威电源集团有限公司 | Preparation method of tetrabasic lead sulfate |
| CN113097443A (en) * | 2021-03-29 | 2021-07-09 | 济源职业技术学院 | Tubular positive plate prepared from tubular positive waste lead paste and preparation method thereof |
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Application publication date: 20141217 |