CN103682329A - Internal formation lead plaster preparation process - Google Patents
Internal formation lead plaster preparation process Download PDFInfo
- Publication number
- CN103682329A CN103682329A CN201310574636.2A CN201310574636A CN103682329A CN 103682329 A CN103682329 A CN 103682329A CN 201310574636 A CN201310574636 A CN 201310574636A CN 103682329 A CN103682329 A CN 103682329A
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- China
- Prior art keywords
- lead plaster
- cream
- lead
- add
- sulfuric acid
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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
-
- 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
-
- 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
Abstract
The invention discloses an internal formation lead plaster preparation process. The internal formation lead plaster preparation technology comprises the following steps in sequence: step one. adding water so as to prepare preparatory liquid; step two. adding lead powder; and step three. adding dilute sulphuric acid so as to form the lead plaster. According to the internal formation lead plaster preparation technology, pure water is used as a solvent and a dispersing agent so as to completely and uniformly disperse materials, so that the uniformity and the consistency of components in the lead plaster are improved, and by adopting a wet-process addition process, the pollution of dust generated during the addition of powder materials to environments is avoided. Compared with a dry-process technology, the internal formation lead plaster preparation process has the advantages that the non-uniform stirring caused by the difference of the powder materials in specific gravity can be solved, meanwhile, the stirring time can aslo be shortened, the production efficiency is improved, as the stirring time is shortened, the good effect of the lead plaster is ensured, and the difficulty in application of the lead plaster is avoided. The self discharge of storage batteries prepared from the lead plaster is obviously reduced, and the heavy current cycle life is obviously prolonged.
Description
Technical field
The invention belongs to Lead-acid Battery Technology field, relate to a kind of lead plaster preparation technology that is internalized into.
Background technology
Traditional cream technique that closes is all first will under various powder additive dry states, to mix with lead powder, be dry mixed and add again later formula water, the dry agitation mechanism that routine is closed cream machine is to utilize stirrer paddle to force mixing, be subject to the impact of stirrer paddle stroke size, peripheral stirring strength will obviously be greater than the strength of heart portion, cause each position and stir the fluctuation of collision rate generation shaped form, because the proportion of powder additives is had nothing in common with each other, adding proportion is few again, the proportion of lead powder is larger, under Action of Gravity Field, finally cause the material that proportion is lighter to concentrate on the shortest heart portion position of mixer stroke.Therefore, under dry state, each material and lead powder being done to simple mechanical agitation can not fully mix it, even if time expand, does not reach the effect mixing yet, under hygrometric state, need again the longer time of stirring just can make it mix, long mixing time has reduced production efficiency, also makes on the other hand lead plaster be difficult to fill.
Application number is to disclose a kind of plumbous charcoal superbattery negative pole preparation technology in 201210375188.9 Chinese patent application, Carbon Materials powder is uniformly dispersed through high-speed stirred separately in water, then mixes, be uniformly dispersed with lead powder and other cathode additive agent.In the process that this preparation technology's high speed stirs, really can make system dispersion effect good, but while adding material and even be difficult to guarantee system when the later stage stirs and remain in good dispersity at every turn.
Because of the effect of each additive in lead plaster most important, therefore, if additive mixes inhomogeneous meeting and causes each local part proportional imbalance in the lead plaster after the system of closing, adopt the pole plate consistency of making under traditional handicraft poor, use the middle and later periods to cause a large amount of batteries to be return because of single reason that only falls behind, therefore it is most important that, lead plaster closes the uniformity consistency of system.
Summary of the invention
Technical problem to be solved by this invention is just to provide a kind of lead plaster preparation technology that is internalized into, the present invention is a kind of brand-new storage battery lead plaster preparation technology that is internalized into, utilize pure water as solvent and dispersant, each material to be thoroughly uniformly dispersed, improve the uniformity consistency of each component in lead plaster, the technique that wet method is added, the dust pollution on the environment while simultaneously having avoided powder body material to add.
For solving the problems of the technologies described above, the present invention adopts following technical scheme: a kind of lead plaster preparation technology that is internalized into, comprises the following steps successively:
Step 1, add water and make preparation liquid: short fiber and additive are added to the water, and high speed shear stirs, and mixing time is 3～8min, obtains preparation liquid; Object is to allow to be dissolvable in water the formulation additives of water water-soluble in advance, also makes water-fast additive dispersed, the pollution of the dust while simultaneously also having avoided powder body material to add to environment;
Step 2, add lead powder: lead powder is added to the preparation liquid obtaining in step 1, continue to stir 6～8min, obtain preparation and close cream; Wherein, described lead powder can be Shimadzu formula lead powder or Ba Dunshi lead powder.Continue stirring and can allow lead powder further be oxidized, and allow lead oxide generate lead hydroxide, plumbous conversion process is accelerated greatly, shortened mixing time, enhanced productivity, simultaneously because mixing time shortens, be conducive to guarantee the good result of lead plaster, avoid lead plaster to be difficult to fill.
Step 3, add dilute sulfuric acid and close cream: the preparation that slowly at the uniform velocity adds step 2 to make dilute sulfuric acid is closed in cream, constantly stirs simultaneously, continue to stir 10～20min after adding dilute sulfuric acid, complete and close cream, until temperature, go out cream during lower than 45 ℃.Preferably dilute sulfuric acid at the uniform velocity adds in 13～18min, to allow lead plaster change into basic lead sulphate.
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, putting into a small amount of fiber stirs, just can find intuitively that fiber is stereo suspending shape disorderly to dispersion, and long-time placement do not have too large variation; But also having the dispersiveness of some fibers of not handling well in water not quite desirable, after stirring, may disperse, is a batt layer but just can float after a while.
In the present invention, through high speed shear, stir, under the effect of shearing force, short fiber and additive can be uniformly dispersed in water, compare with dry stirring, can solve the inhomogeneous problem of stirring that various powder proportion differences cause, also can shorten mixing time, enhance productivity, avoid lead plaster to be difficult to fill simultaneously.
Preferably, in described step 1, when being added to the water, short fiber and additive also add polyether-type dispersant.Polyether-type dispersant solvent chain is mainly homopolymers and the copolymer of the materials such as oxirane, expoxy propane, oxolane, wherein mainly comprises the copolymer of oxirane and expoxy propane.The synthetic of this class hyper-dispersant can be initiator with anchoring group, and under the condition existing at heating, pressurization and catalyst, the ring-opening reaction by cyclic ethers material makes.For example, while making initiator with diethyl ethylene diamine, to inorganic pigment, the dispersion in the strong polarizable medium such as alcohol, ether has extraordinary effect to the hyper-dispersant of the lower array structure obtaining.
Preferably, the copolymer that described polyether-type dispersant is oxirane and expoxy propane.
Preferably, in described step 3, add in the process of dilute sulfuric acid, the temperature that cream is closed in preparation remains on 60～70 ℃.Closing the mechanical mixture that cream process is not various materials, is that chemical reaction occurs, and has heat to emit simultaneously.The temperature of closing lead plaster in cream process can affect the composition of lead plaster, and therefore controlling temperature has good quality to guarantee the lead plaster making.
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 utilizes pure water as solvent and dispersant, each material to be thoroughly uniformly dispersed, improve the uniformity consistency of each component in lead plaster, the technique that wet method is added, the dust pollution on the environment while simultaneously having avoided powder body material to add.The present invention compares with dry process, can solve the inhomogeneous problem of stirring that various powder proportion differences cause, also can shorten mixing time simultaneously, enhance productivity, because mixing time shortens, be conducive to guarantee the good result of lead plaster simultaneously, avoid lead plaster to be difficult to fill.And the storage battery self discharge of being made by it obviously reduces, the large current cycle life-span obviously improves.
Below in conjunction with embodiment, the invention will be further described:
Embodiment
A kind of lead plaster preparation technology embodiment 1 that is internalized into of the present invention, comprises the following steps successively:
Step 1, add water and make preparation liquid: short fiber and additive are added to the water, and high speed shear stirs, and mixing time is 3min, obtains preparation liquid; Object is to allow to be dissolvable in water the formulation additives of water water-soluble in advance, also makes water-fast additive dispersed, the pollution of the dust while simultaneously also having avoided powder body material to add to environment;
Step 2, add lead powder: lead powder is added to the preparation liquid obtaining in step 1, continue to stir 6min, obtain preparation and close cream; Wherein, described lead powder can be Shimadzu formula lead powder or Ba Dunshi lead powder.Continue stirring and can allow lead powder further be oxidized, and allow lead oxide generate lead hydroxide, plumbous conversion process is accelerated greatly, shortened mixing time, enhanced productivity, simultaneously because mixing time shortens, be conducive to guarantee the good result of lead plaster, avoid lead plaster to be difficult to fill.
Step 3, add dilute sulfuric acid and close cream: slowly at the uniform velocity add step 2 to make dilute sulfuric acid
Preparation close in cream, constantly stir simultaneously, continue to stir 10min after adding dilute sulfuric acid, complete and close cream, until temperature, go out cream during lower than 45 ℃.Preferably dilute sulfuric acid at the uniform velocity adds in 13～18min, to allow lead plaster change into basic lead sulphate.
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, putting into a small amount of fiber stirs, just can find intuitively that fiber is stereo suspending shape disorderly to dispersion, and long-time placement do not have too large variation; But also having the dispersiveness of some fibers of not handling well in water not quite desirable, after stirring, may disperse, is a batt layer but just can float after a while.
In the present invention, through high speed shear, stir, under the effect of shearing force, short fiber and additive can be uniformly dispersed in water, compare with dry stirring, can solve the inhomogeneous problem of stirring that various powder proportion differences cause, also can shorten mixing time, enhance productivity, avoid lead plaster to be difficult to fill simultaneously.In described step 1, when being added to the water, short fiber and additive also add polyether-type dispersant.Polyether-type dispersant solvent chain is mainly homopolymers and the copolymer of the materials such as oxirane, expoxy propane, oxolane, wherein mainly comprises the copolymer of oxirane and expoxy propane.The synthetic of this class hyper-dispersant can be initiator with anchoring group, and under the condition existing at heating, pressurization and catalyst, the ring-opening reaction by cyclic ethers material makes.For example, while making initiator with diethyl ethylene diamine, to inorganic pigment, the dispersion in the strong polarizable medium such as alcohol, ether has extraordinary effect to the hyper-dispersant of the lower array structure obtaining.
Described polyether-type dispersant is the copolymer of oxirane and expoxy propane.
In described step 3, add in the process of dilute sulfuric acid, the temperature that cream is closed in preparation remains on 60 ℃.Closing the mechanical mixture that cream process is not various materials, is that chemical reaction occurs, and has heat to emit simultaneously.The temperature of closing lead plaster in cream process can affect the composition of lead plaster, and therefore controlling temperature has good quality to guarantee the lead plaster making.
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%.
A kind of lead plaster preparation technology embodiment 2 that is internalized into of the present invention, comprises the following steps successively:
Step 1, add water and make preparation liquid: short fiber and additive are added to the water, and high speed shear stirs, and mixing time is 8min, obtains preparation liquid;
Step 2, add lead powder: lead powder is added to the preparation liquid obtaining in step 1, continue to stir 8min, obtain preparation and close cream; Wherein, described lead powder can be Shimadzu formula lead powder or Ba Dunshi lead powder.
Step 3, add dilute sulfuric acid and close cream: the preparation that slowly at the uniform velocity adds step 2 to make dilute sulfuric acid is closed in cream, constantly stirs simultaneously, continue to stir 20min after adding dilute sulfuric acid, complete and close cream, until temperature, go out cream during lower than 45 ℃.
In described step 1, when being added to the water, 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, add in the process of dilute sulfuric acid, the temperature that cream is closed in preparation remains on 70 ℃.
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%.
A kind of lead plaster preparation technology embodiment 3 that is internalized into of the present invention, comprises the following steps successively:
Step 1, add water and make preparation liquid: short fiber and additive are added to the water, and high speed shear stirs, and mixing time is 5min, obtains preparation liquid;
Step 2, add lead powder: lead powder is added to the preparation liquid obtaining in step 1, continue to stir 7min, obtain preparation and close cream; Wherein, described lead powder can be Shimadzu formula lead powder or Ba Dunshi lead powder.
Step 3, add dilute sulfuric acid and close cream: the preparation that slowly at the uniform velocity adds step 2 to make dilute sulfuric acid is closed in cream, constantly stirs simultaneously, continue to stir 13min after adding dilute sulfuric acid, complete and close cream, until temperature, go out cream during lower than 45 ℃.
In described step 1, when being added to the water, 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, add in the process of dilute sulfuric acid, the temperature that cream is closed in preparation remains on 65 ℃.
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: the lead plaster that lead plaster preparation technology embodiment 1～3 of the present invention is made is produced battery, carries out cycle life test, and contrasts with prior art, and result is as shown in table 1:
Table 1
| ? | Circulating battery number of times |
| Embodiment 1 | 710 |
| Embodiment 2 | 658 |
| Embodiment 3 | 663 |
| Comparative example | 408 |
Illustrate: by above-mentioned data, can find out, the performance of the lead plaster that cream technique makes of closing of the present invention is apparently higher than the performance index of prior art, and the storage battery self discharge of being made by it obviously reduces, and the large current cycle life-span obviously improves.
The foregoing is only specific embodiments of the invention, but technical characterictic of the present invention is not limited to this, any those skilled in the art is in the field of the invention, and the variation of doing or modification are all encompassed among the scope of the claims of the present invention.
Claims (6)
1. be internalized into a lead plaster preparation technology, it is characterized in that: comprise the following steps successively:
Step 1, add water and make preparation liquid: short fiber and additive are added to the water, and high speed shear stirs, and mixing time is 3～8min, obtains preparation liquid;
Step 2, add lead powder: lead powder is added to the preparation liquid obtaining in step 1, continue to stir 6～8min, obtain preparation and close cream;
Step 3, add dilute sulfuric acid and close cream: the preparation that slowly at the uniform velocity adds step 2 to make dilute sulfuric acid is closed in cream, constantly stirs simultaneously, continue to stir 10～20min after adding dilute sulfuric acid, complete and close cream, until temperature, go out cream during lower than 45 ℃.
2. a kind of lead plaster preparation technology that is internalized into as claimed in claim 1, is characterized in that: in described step 1, also add polyether-type dispersant when short fiber and additive are added to the water.
3. a kind of lead plaster preparation technology that is internalized into as claimed in claim 2, is characterized in that: described polyether-type dispersant is the copolymer of oxirane and expoxy propane.
4. a kind of lead plaster preparation technology that is internalized into as claimed in claim 1, is characterized in that: in described step 3, add in the process of dilute sulfuric acid, the temperature that cream is closed in preparation remains on 60～70 ℃.
5. a kind of lead plaster preparation technology that is internalized into as claimed in claim 1, 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.
6. a kind of lead plaster preparation technology that is internalized into as claimed in claim 1, is characterized in that: the mass percent concentration of described sulfuric acid is 45%.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310574636.2A CN103682329A (en) | 2013-11-15 | 2013-11-15 | Internal formation lead plaster preparation process |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310574636.2A CN103682329A (en) | 2013-11-15 | 2013-11-15 | Internal formation lead plaster preparation process |
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| CN103682329A true CN103682329A (en) | 2014-03-26 |
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| CN201310574636.2A Pending CN103682329A (en) | 2013-11-15 | 2013-11-15 | Internal formation lead plaster preparation process |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107359312A (en) * | 2017-06-16 | 2017-11-17 | 超威电源有限公司 | A kind of preparation method of lead plaster and its detection method of carbon material dispersion effect |
| CN108933233A (en) * | 2017-05-22 | 2018-12-04 | 湖北润阳新能源有限公司 | A kind of lead-acid accumulator anode diachylon and the method that pole plate is prepared using the lead plaster |
| CN115889786A (en) * | 2022-09-23 | 2023-04-04 | 湖州德旭科技有限公司 | Preparation process of lead powder for long-life lead-acid storage battery |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102074695A (en) * | 2010-12-21 | 2011-05-25 | 江苏永达电源股份有限公司 | High-temperature paste mixing process for prolonging cycle life of battery |
| CN102931380A (en) * | 2012-11-26 | 2013-02-13 | 苏州大学 | Power type lead-acid storage battery positive electrode plate |
-
2013
- 2013-11-15 CN CN201310574636.2A patent/CN103682329A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102074695A (en) * | 2010-12-21 | 2011-05-25 | 江苏永达电源股份有限公司 | High-temperature paste mixing process for prolonging cycle life of battery |
| CN102931380A (en) * | 2012-11-26 | 2013-02-13 | 苏州大学 | Power type lead-acid storage battery positive electrode plate |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108933233A (en) * | 2017-05-22 | 2018-12-04 | 湖北润阳新能源有限公司 | A kind of lead-acid accumulator anode diachylon and the method that pole plate is prepared using the lead plaster |
| CN107359312A (en) * | 2017-06-16 | 2017-11-17 | 超威电源有限公司 | A kind of preparation method of lead plaster and its detection method of carbon material dispersion effect |
| CN107359312B (en) * | 2017-06-16 | 2020-02-21 | 超威电源集团有限公司 | Preparation method of lead plaster and detection method of carbon material dispersion effect of lead plaster |
| CN115889786A (en) * | 2022-09-23 | 2023-04-04 | 湖州德旭科技有限公司 | Preparation process of lead powder for long-life lead-acid storage battery |
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