CN103682330B - One is internalized into lead plaster and closes technique processed - Google Patents
One is internalized into lead plaster and closes technique processed Download PDFInfo
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- CN103682330B CN103682330B CN201310578728.8A CN201310578728A CN103682330B CN 103682330 B CN103682330 B CN 103682330B CN 201310578728 A CN201310578728 A CN 201310578728A CN 103682330 B CN103682330 B CN 103682330B
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- lead
- hydroxide solution
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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
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
- H01M4/56—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of lead
- H01M4/57—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of lead of "grey lead", i.e. powders containing lead and lead oxide
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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
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
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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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- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Inorganic Chemistry (AREA)
- Compositions Of Macromolecular Compounds (AREA)
- Battery Electrode And Active Subsutance (AREA)
Abstract
The invention discloses one to be internalized into lead plaster and to close technique processed, comprise the following steps successively: step one, add dilute sulfuric acid making preparation liquid, step 2, prefabricated lead hydroxide solution, step 3, preparation liquid mix with lead hydroxide solution three steps such as closing cream.The present invention is dissolved in acid in advance in order to the additive making to be dissolvable in water acid, also makes the additive being insoluble to acid dispersed simultaneously, first by short fiber and additive in advance with dilute sulfuric acid shear agitation, make system high degree of dispersion; Then will add in this dispersion through prefabricated lead hydroxide solution, realize wet method to feed in raw material, various material can be made dispersed, improve the uniformity consistency of each component in lead plaster, the technique that wet method is added, avoid dust pollution on the environment when powder body material adds, and the storage battery self discharge of being made up of it obviously reduces, big current cycle life significantly improves simultaneously.
Description
Technical field
The invention belongs to Lead-acid Battery Technology field, relate to one and be internalized into lead plaster conjunction technique processed.
Background technology
Traditional conjunction cream technique is all mix under various powder additive dry state with lead powder, because the proportion of additive is had nothing in common with each other, adding proportion is few again, simple mechanical agitation can not make it fully mix, because the effect of each additive in lead plaster is most important, therefore, if additive mixes uneven meeting and causes closing each local part proportional imbalance in the lead plaster after making, the pole plate consistency made under adopting traditional handicraft is poor, use the middle and later periods a large amount of batteries can be caused to return because of single laggard reason, therefore, the uniformity consistency of lead plaster conjunction system is most important.
Application number is disclose a kind of plumbous charcoal superbattery negative pole preparation technology in the Chinese patent application of 201210375188.9, is uniformly dispersed separately by Carbon Materials powder in water through high-speed stirred, then mixes with lead powder and other cathode additive agent, be uniformly dispersed.Really system dispersion effect can be made good in the process that this preparation technology's high speed stirs, but when adding material and even be difficult to guarantee system when the later stage stirs and remain in good dispersity at every turn.
Summary of the invention
Technical problem to be solved by this invention is just to provide one and is internalized into lead plaster conjunction technique processed, the present invention is that a kind of brand-new lead plaster closes technique processed, mainly change the addition manner of formula materials (additive), due to be internalized into lead acid accumulator have in formula materials water insoluble but be dissolved in acid additive add, as bismuth oxide is water insoluble, dissolve in acid, in order to better additive be disperseed, therefore adopt the technique shifted to an earlier date with acid mixing dispersion, by this technique, bismuth oxide just can dissolving acid completely, better disperses in acid solution.
First each powder body material is uniformly mixed through cutter and the dilute sulfuric acid (density is: 1.35-1.45g/cm325 DEG C) after weighing by device for inhaling powdery substances by technique of the present invention, dilute sulfuric acid is utilized thoroughly to be uniformly dispersed by each material as solvent and dispersant, then this solution is added in lead powder, by this technological improvement, various material can be made dispersed, improve the uniformity consistency of each component in lead plaster.The technique that wet method is added, avoids dust pollution on the environment when powder body material adds simultaneously.
For solving the problems of the technologies described above, the present invention adopts following technical scheme: one is internalized into lead plaster and closes technique processed, comprises the following steps successively:
Step one, add dilute sulfuric acid and make preparation liquid: add in dilute sulfuric acid by short fiber and additive, high shear agitation is even, and mixing time is 3 ~ 6min, then quick freeze, obtains preparation liquid; Load weighted short fiber and additive are drawn in cutter by device for inhaling powdery substances, mixing shearing 3 ~ 6min, object allows the additive being dissolvable in water acid be dissolved in acid in advance, as bismuth oxide is water insoluble, dissolve in acid, in order to better additive be disperseed, therefore adopt the technique shifted to an earlier date with acid mixing dispersion, by this technique, bismuth oxide just can dissolving acid completely, better disperses in acid solution.Also the additive making to be insoluble to acid is dispersed, also avoid dust when powder body material adds to the pollution of environment simultaneously;
Step 2, prefabricated lead hydroxide solution: lead powder preheating also slowly stirred, mixing time is 6 ~ 8min; Be added to the water by preheated lead powder, high shear agitation is even, and mixing time is 5 ~ 8min, obtains lead hydroxide solution; Wherein, described lead powder can be Shimadzu formula lead powder or Ba Dunshi lead powder.Preheating is also slowly stirred and lead powder can be allowed to be oxidized further; Preferably add in 2min, then continue stirring 5 ~ 8 minutes, this process allows lead oxide generate lead hydroxide.
Step 3, preparation liquid mix with lead hydroxide solution and close cream: lead hydroxide solution step 2 obtained slowly at the uniform velocity adds in the obtained preparation liquid of step one, constantly stir simultaneously, continue stirring 10 ~ 20min after adding lead hydroxide solution, complete conjunction cream, go out cream until temperature lower than when 45 DEG C.Preferably dilute sulfuric acid at the uniform velocity adds in 13 ~ 18min, changes into basic lead sulphate to allow lead plaster.
Because fiber adopts different active agent formulations to process to its surface in process of production, make fiber chance water dispersed, generally in pure water or dilute sulfuric acid, put into a small amount of fiber to stir, just spatially suspension is random in dispersion can to find fiber intuitively, and long-time placement does not have too large change; But also there is the dispersiveness of some fibers do not handled well in water not quite desirable, may disperse after stirring, but just to float after a while be a batt layer.
Through high shear agitation in the present invention, under the effect of shearing force, short fiber and additive are first disperseed with dilute sulfuric acid, the additive being dissolvable in water acid is made to be dissolved in acid in advance, as bismuth oxide is water insoluble, dissolve in acid, in order to better additive be disperseed, also make the additive being insoluble to acid dispersed simultaneously, then stop stirring rear short fiber and additive conglomeration again to prevent, so adopt freezing method, by freezing for preparation liquid system good for dispersed with stirring cooling, the motion of various material molecule or group in system is slowed down rapidly, maintain in the state of dispersion.
Preferably, in described step one, cryogenic temperature is 0 ~ 5 DEG C.The motion of material molecule various in system or group can be remained in very slow state, avoid water freezing simultaneously, so that follow-up and carrying out that be cream step.
Preferably, in described step one, while adding in dilute sulfuric acid by short fiber and additive, also add polyether-type dispersant.Polyether-type dispersant solvent chain is the homopolymers of the material such as oxirane, expoxy propane, oxolane and copolymer mainly, wherein mainly comprises the copolymer of oxirane and expoxy propane.The synthesis of this kind of hyper-dispersant can be initiator with anchoring group, under heating, pressurization and catalyst existent condition, is obtained by the ring-opening reaction of cyclic ethers material.Such as, when making initiator with diethyl ethylene diamine, the hyper-dispersant of the having structure obtained has extraordinary effect to the dispersion of inorganic pigment in the strong polarizable medium such as alcohol, ether.
Preferably, described polyether-type dispersant is the copolymer of oxirane and expoxy propane.
Preferably, in described step 3, lead hydroxide solution step 2 obtained slowly at the uniform velocity adds in the process of the obtained preparation liquid of step one, and the temperature of preparation liquid remains on 60 ~ 70 DEG C.Close the mechanical mixture that cream process is not various material, be that chemical reaction occurs, have heat to release simultaneously.The temperature of closing lead plaster in cream process can affect the composition of lead plaster, and therefore control temperature is to ensure that the lead plaster obtained has good quality.
Preferably, described short fiber is at least one in polypropylene fibre, polyvinyl chloride fibre, acrylic fiber, polyacrylonitrile fibre, polypyrrole fiber, polythiophene fiber.
Preferably, the mass percent concentration of described sulfuric acid is 45%.
Compared with prior art, advantage of the present invention is: the present invention is dissolved in acid in advance in order to make the additive being dissolvable in water acid, as bismuth oxide is water insoluble, dissolve in acid, in order to better additive be disperseed, also make the additive being insoluble to acid dispersed simultaneously, first by short fiber and additive in advance with dilute sulfuric acid (density is: 1.35-1.45g/cm325 DEG C) shear agitation, the additive being dissolvable in water acid is made to be dissolved in acid in advance, also make the additive being insoluble to acid dispersed simultaneously, make system high degree of dispersion; Then will add in this dispersion through prefabricated lead hydroxide solution, realize wet method to feed in raw material, various material can be made dispersed, improve the uniformity consistency of each component in lead plaster, the technique that wet method is added, avoid dust pollution on the environment when powder body material adds, and the storage battery self discharge of being made up of it obviously reduces, big current cycle life significantly improves simultaneously.
Below in conjunction with embodiment, the invention will be further described:
Embodiment
One of the present invention is internalized into lead plaster and closes process example 1 processed, comprises the following steps successively:
Step one, add dilute sulfuric acid and make preparation liquid: add in dilute sulfuric acid by short fiber and additive, high shear agitation is even, and mixing time is 3min, then quick freeze, obtains preparation liquid; Load weighted short fiber and additive are drawn in cutter by device for inhaling powdery substances, mixing shearing 3 ~ 6min, object allows the additive being dissolvable in water acid be dissolved in acid in advance, as bismuth oxide is water insoluble, dissolve in acid, in order to better additive be disperseed, therefore adopt the technique shifted to an earlier date with acid mixing dispersion, by this technique, bismuth oxide just can dissolving acid completely, better disperses in acid solution.Also the additive making to be insoluble to acid is dispersed, also avoid dust when powder body material adds to the pollution of environment simultaneously;
Step 2, prefabricated lead hydroxide solution: lead powder preheating also slowly stirred, mixing time is 6min; Be added to the water by preheated lead powder, high shear agitation is even, and mixing time is 5min, obtains lead hydroxide solution; Wherein, described lead powder can be Shimadzu formula lead powder or Ba Dunshi lead powder.Preheating is also slowly stirred and lead powder can be allowed to be oxidized further; Preferably add in 2min, then continue stirring 5 ~ 8 minutes, this process allows lead oxide generate lead hydroxide.
Step 3, preparation liquid mix with lead hydroxide solution and close cream: lead hydroxide solution step 2 obtained slowly at the uniform velocity adds in the obtained preparation liquid of step one, constantly stir simultaneously, continue to stir 10min after adding lead hydroxide solution, complete conjunction cream, go out cream until temperature lower than when 45 DEG C.Preferably dilute sulfuric acid at the uniform velocity adds in 13 ~ 18min, changes into basic lead sulphate to allow lead plaster.
Because fiber adopts different active agent formulations to process to its surface in process of production, make fiber chance water dispersed, generally in pure water or dilute sulfuric acid, put into a small amount of fiber to stir, just spatially suspension is random in dispersion can to find fiber intuitively, and long-time placement does not have too large change; But also there is the dispersiveness of some fibers do not handled well in water not quite desirable, may disperse after stirring, but just to float after a while be a batt layer.
Through high shear agitation in the present invention, under the effect of shearing force, short fiber and additive are first disperseed with dilute sulfuric acid, the additive being dissolvable in water acid is made to be dissolved in acid in advance, as bismuth oxide is water insoluble, dissolve in acid, in order to better additive be disperseed, also make the additive being insoluble to acid dispersed simultaneously, then stop stirring rear short fiber and additive conglomeration again to prevent, so adopt freezing method, by freezing for preparation liquid system good for dispersed with stirring cooling, the motion of various material molecule or group in system is slowed down rapidly, maintain in the state of dispersion.
In described step one, cryogenic temperature is 2 DEG C.The motion of material molecule various in system or group can be remained in very slow state, avoid water freezing simultaneously, so that follow-up and carrying out that be cream step.
In described step one, while adding in dilute sulfuric acid by short fiber and additive, also add polyether-type dispersant.Polyether-type dispersant solvent chain is the homopolymers of the material such as oxirane, expoxy propane, oxolane and copolymer mainly, wherein mainly comprises the copolymer of oxirane and expoxy propane.The synthesis of this kind of hyper-dispersant can be initiator with anchoring group, under heating, pressurization and catalyst existent condition, is obtained by the ring-opening reaction of cyclic ethers material.Such as, when making initiator with diethyl ethylene diamine, the hyper-dispersant of the having structure obtained has extraordinary effect to the dispersion of inorganic pigment in the strong polarizable medium such as alcohol, ether.
Described polyether-type dispersant is the copolymer of oxirane and expoxy propane.
In described step 3, lead hydroxide solution step 2 obtained slowly at the uniform velocity adds in the process of the obtained preparation liquid of step one, and the temperature of preparation liquid remains on 60 DEG C.Close the mechanical mixture that cream process is not various material, be that chemical reaction occurs, have heat to release simultaneously.The temperature of closing lead plaster in cream process can affect the composition of lead plaster, and therefore control temperature is to ensure that the lead plaster obtained has good quality.
Described short fiber is at least one in polypropylene fibre, polyvinyl chloride fibre, acrylic fiber, polyacrylonitrile fibre, polypyrrole fiber, polythiophene fiber.
The mass percent concentration of described sulfuric acid is 45%.
One of the present invention is internalized into lead plaster and closes process example 2 processed, comprises the following steps successively:
Step one, add dilute sulfuric acid and make preparation liquid: add in dilute sulfuric acid by short fiber and additive, high shear agitation is even, and mixing time is 6min, then quick freeze, obtains preparation liquid;
Step 2, prefabricated lead hydroxide solution: lead powder preheating also slowly stirred, mixing time is 8min; Be added to the water by preheated lead powder, high shear agitation is even, and mixing time is 8min, obtains lead hydroxide solution; Wherein, described lead powder can be Shimadzu formula lead powder or Ba Dunshi lead powder.
Step 3, preparation liquid mix with lead hydroxide solution and close cream: lead hydroxide solution step 2 obtained slowly at the uniform velocity adds in the obtained preparation liquid of step one, constantly stir simultaneously, continue to stir 20min after adding lead hydroxide solution, complete conjunction cream, go out cream until temperature lower than when 45 DEG C.
In described step one, cryogenic temperature is 5 DEG C.
In described step one, while adding in dilute sulfuric acid by short fiber and additive, also add polyether-type dispersant.
Described polyether-type dispersant is the copolymer of oxirane and expoxy propane.
In described step 3, lead hydroxide solution step 2 obtained slowly at the uniform velocity adds in the process of the obtained preparation liquid of step one, and the temperature of preparation liquid remains on 70 DEG C.
Described short fiber is at least one in polypropylene fibre, polyvinyl chloride fibre, acrylic fiber, polyacrylonitrile fibre, polypyrrole fiber, polythiophene fiber.
The mass percent concentration of described sulfuric acid is 45%.
One of the present invention is internalized into lead plaster and closes process example 3 processed, comprises the following steps successively:
Step one, add dilute sulfuric acid and make preparation liquid: add in dilute sulfuric acid by short fiber and additive, high shear agitation is even, and mixing time is 5min, then quick freeze, obtains preparation liquid;
Step 2, prefabricated lead hydroxide solution: lead powder preheating also slowly stirred, mixing time is 8min; Be added to the water by preheated lead powder, high shear agitation is even, and mixing time is 8min, obtains lead hydroxide solution; Wherein, described lead powder can be Shimadzu formula lead powder or Ba Dunshi lead powder.
Step 3, preparation liquid mix with lead hydroxide solution and close cream: lead hydroxide solution step 2 obtained slowly at the uniform velocity adds in the obtained preparation liquid of step one, constantly stir simultaneously, continue to stir 13min after adding lead hydroxide solution, complete conjunction cream, go out cream until temperature lower than when 45 DEG C.
In described step one, cryogenic temperature is 3 DEG C.
In described step one, while adding in dilute sulfuric acid by short fiber and additive, also add polyether-type dispersant.
Described polyether-type dispersant is the copolymer of oxirane and expoxy propane.
In described step 3, lead hydroxide solution step 2 obtained slowly at the uniform velocity adds in the process of the obtained preparation liquid of step one, and the temperature of preparation liquid remains on 65 DEG C.
Described short fiber is at least one in polypropylene fibre, polyvinyl chloride fibre, acrylic fiber, polyacrylonitrile fibre, polypyrrole fiber, polythiophene fiber.
The mass percent concentration of described sulfuric acid is 45%.
Performance Detection: lead plaster lead plaster of the present invention being closed process example 1 ~ 3 processed obtained produces battery, and carry out cycle life test, and contrast with prior art, result is as shown in table 1:
Table 1
| Circulating battery number of times | |
| Embodiment 1 | 684 |
| Embodiment 2 | 702 |
| Embodiment 3 | 655 |
| Comparative example | 408 |
Illustrate: can be found out by above-mentioned data, lead plaster of the present invention closes the performance index of performance apparently higher than prior art of the lead plaster that technique processed obtains, and the storage battery self discharge of being made up of it obviously reduces, and big current cycle life significantly improves.
The foregoing is only specific embodiments of the invention, but technical characteristic of the present invention is not limited thereto, any those skilled in the art is in the field of the invention, and the change done or modification are all encompassed among the scope of the claims of the present invention.
Claims (5)
1. be internalized into lead plaster and close a technique processed, it is characterized in that: comprise the following steps successively:
Step one, add dilute sulfuric acid and make preparation liquid: add in dilute sulfuric acid by short fiber and additive, add polyether-type dispersant simultaneously, high shear agitation is even, and mixing time is 3 ~ 6min, then quick freeze, and cryogenic temperature is 0 ~ 5 DEG C, obtains preparation liquid;
Step 2, prefabricated lead hydroxide solution: lead powder preheating also slowly stirred, mixing time is 6 ~ 8min; Be added to the water by preheated lead powder, high shear agitation is even, and mixing time is 5 ~ 8min, obtains lead hydroxide solution;
Step 3, preparation liquid mix with lead hydroxide solution and close cream: lead hydroxide solution step 2 obtained slowly at the uniform velocity adds in the obtained preparation liquid of step one, constantly stir simultaneously, continue stirring 10 ~ 20min after adding lead hydroxide solution, complete conjunction cream, go out cream until temperature lower than when 45 DEG C.
2. one as claimed in claim 1 is internalized into lead plaster and closes technique processed, it is characterized in that: described polyether-type dispersant is the copolymer of oxirane and expoxy propane.
3. one as claimed in claim 1 is internalized into lead plaster and closes technique processed, it is characterized in that: in described step 3, lead hydroxide solution step 2 obtained slowly at the uniform velocity adds in the process of the obtained preparation liquid of step one, and the temperature of preparation liquid remains on 60 ~ 70 DEG C.
4. one as claimed in claim 1 is internalized into lead plaster and closes technique processed, it is characterized in that: described short fiber is at least one in polypropylene fibre, polyvinyl chloride fibre, acrylic fiber, polyacrylonitrile fibre, polypyrrole fiber, polythiophene fiber.
5. one as claimed in claim 1 is internalized into lead plaster and closes technique processed, it is characterized in that: the mass percent concentration of described sulfuric acid is 45%.
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| CN201310578728.8A CN103682330B (en) | 2013-11-15 | 2013-11-15 | One is internalized into lead plaster and closes technique processed |
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| CN103682330B true CN103682330B (en) | 2016-04-06 |
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| CN110890526B (en) * | 2019-10-15 | 2022-01-07 | 浙江南都电源动力股份有限公司 | Lead plaster additive adding process |
| CN113976106A (en) * | 2021-09-27 | 2022-01-28 | 达斯玛环境科技（北京）有限公司 | Preparation method and system of aluminum-based catalyst |
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| CN101740759A (en) * | 2008-11-24 | 2010-06-16 | 台湾神户电池股份有限公司 | Diachylon composition and preparation method and lead storage battery thereof |
| CN101969126A (en) * | 2010-09-15 | 2011-02-09 | 超威电源有限公司 | Formula of positive lead paste |
| CN102931410A (en) * | 2012-10-24 | 2013-02-13 | 超威电源有限公司 | High-capacity formation lead paste and preparation method thereof |
| CN102931380A (en) * | 2012-11-26 | 2013-02-13 | 苏州大学 | Power type lead-acid storage battery positive electrode plate |
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| CN1161877A (en) * | 1996-04-10 | 1997-10-15 | 财团法人工业技术研究院 | Composition of mixed silicon series defoaming agent |
| CN1767248A (en) * | 2004-10-25 | 2006-05-03 | 深圳市理士奥电源技术有限公司 | Nanometer-level high composite electrolyte and its preparing method |
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Address after: 313100 Zhejiang province Huzhou city Changxing County town pheasant emerging industrial park Chaowei Power Co. Ltd Patentee after: Chaowei Power Group Co.,Ltd. Address before: 313100 Zhejiang province Huzhou city Changxing County town pheasant emerging industrial park Chaowei Power Co. Ltd Patentee before: CHILWEE POWER Co.,Ltd. |
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Effective date of registration: 20191217 Address after: 336400 Jiangxi city of Yichun province Shanggao County Industrial Park gold heap Patentee after: JIANGXI XINWEI POWER ENERGY TECHNOLOGY Co.,Ltd. Address before: 313100 Zhejiang province Huzhou city Changxing County town pheasant emerging industrial park Chaowei Power Co. Ltd Patentee before: Chaowei Power Group Co.,Ltd. |