CN103301794B - Reaction process concentration control method of precursor for lithium battery material - Google Patents
Reaction process concentration control method of precursor for lithium battery material Download PDFInfo
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- CN103301794B CN103301794B CN201310184305.8A CN201310184305A CN103301794B CN 103301794 B CN103301794 B CN 103301794B CN 201310184305 A CN201310184305 A CN 201310184305A CN 103301794 B CN103301794 B CN 103301794B
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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Abstract
The invention relates to a reaction process concentration control method of a precursor for a lithium battery material. The method comprises the steps that: a level controller in a reaction kettle feeds back the change of the charging total quantity at different reaction steps in real time; a PLC (programmable logic controller) control system controls a circulating pump to pump material in the reaction kettle into a concentration tank; the PLC control system adjusts the discharge of concentrated filtrate in the concentration tank in time; concentrated material returns the reaction kettle; the concentrated material continuously remains in the reaction kettle to be fully reacted; the concentration of solid precipitate in the reaction kettle is controlled to reach 5 to 60 percent; the specific gravity of the solid precipitate to a mother liquor mixture is controlled to be 1.1-1.8g/cm3. The method has the advantages that the circulation concentration and automatic discharge of the material in the reaction kettle are controlled through the PLC control system, the automation control level is high, the reaction accuracy is high, the reaction time of the material in the reaction kettle can be effectively prolonged, sufficient reaction is guaranteed, and the capacity and the product quality are improved.
Description
Technical field
The present invention relates to lithium battery technology, being the concentrated control method of lithium battery material presoma reaction process specifically, being applied to lithium electricity positive electrode field, is mainly the production of positive electrode presoma, as cobalt hydroxide, the multielement complex hydroxide of cobalt carbonate and nickel cobalt manganese.
Background technology
Lithium electricity positive electrode market is along with mobile phone, notebook computer, digital camera, popularizing of the electric consumers such as DV, and power vehicle, electric tool, Moped Scooter, the expansion of generating and energy storage device equal energy source power product, the demand of its material presoma constantly promotes, requirement for quality is increasingly strict, and the required presoma of positive electrode is produced particularly important in industrial chain, the existing lithium battery material presoma generally adopting, be mainly cobalt hydroxide, the multielement complex hydroxide of cobalt carbonate and nickel cobalt manganese, with cobalt salt, nickel salt, manganese salt, add precipitating reagent and complexing agent simultaneously, through synthetic its hydroxide of precipitation reaction or carbonate, obtain precursor powder through washes clean, precipitation reaction operation be presoma produce in critical process, the Main Physical Characteristics of lithium battery material, as tap density, particle diameters etc. all depend on the control of the precipitation reaction of presoma, how to improve the efficiency of reactor, the presoma of how controlling well also constantly highlights at series of problems such as the quality of course of reaction.
Existing lithium battery material presoma reactor operation, all adopt continuous charging, mode by overfall continuous pulp discharge is carried out, along with carrying out continuously of charging reaction, initial stage just starts overflow discharge when liquid level in reactor reaches overfall position, the material of now discharging, due to reaction time deficiency, particle diameter is less than normal, tap density is on the low side etc., be equivalent to produce early stage a large amount of defective works, defective work now need to again dissolve or add in qualified material by the mode of mixed batch in the later stage, larger on product quality impact, the Efficiency Decreasing of simultaneous reactions still, also have in initial reaction stage and reduce reinforced total amount to extend the mode in reaction time, but reinforced total amount reduces, reactor production capacity also decreases, and carry out in initial reaction stage and the mode that adopts afterwards the reinforced total amount of adjusting, before and after causing, the stabilizing influence of reaction system is very large, and the mode of overflow is produced, along with reinforced carrying out continuously, material particular diameter, tap density meet the requirements, but the material that each time period discharges exists larger fluctuation, and homogeneity of product is not high.
Summary of the invention
Low for lithium battery material presoma reactor operation reaction efficiency in prior art, production capacity is low, the inconsistent deficiency that waits of product quality, the invention provides the concentrated control method of a kind of lithium battery material presoma reaction process, can improve reactor efficiency, reach the stable reactor material of controlling, guarantee production capacity and product quality simultaneously.
The technical solution used in the present invention is: the concentrated control method of presoma reaction process for a kind of lithium battery material, it is characterized in that adopting solid sediment in enrichment facility realization response still material to concentrate with separating of mother liquor, enrichment facility comprises reactor, fluid level controller, circulating pump, thickener and PLC control system, reactor inner top is provided with fluid level controller, reactor bottom connects thickener through circulating pump, thickener is connected to reactor inner top, and fluid level controller, circulating pump and thickener are all connected PLC control system; The variation of fluid level controller Real-time Feedback reinforced total amount in the time of the differential responses stage in reactor, the material in reactor is pumped into thickener by PLC control system controlled circulation pump, PLC control system is adjusted in time concentrated filtrate in thickener and is discharged, concentrated material turns back in reactor, concentrated material rests on fully reaction in reactor continuously, control solids of sedimentation substrate concentration in reactor and reach 5～60%, the proportion 1.1～1.8g/cm3 of solid sediment and mother liquor mixture.
Further, be also connected with discharge control valve on described circulating pump, what PLC control system was adjusted discharge control valve in time opens discharge qualified products continuously or periodically.
Again further, described thickener is provided with discharge opeing control valve, and PLC control system control discharge opeing control valve switching value makes concentrated filtrate intermittently or continuous mode is discharged.
Compared with prior art, the present invention has the following advantages: thickener has filtering and concentrating function, material in reactor is by after thickener, and concentrated filtrate was discharged by discharge opeing control valve intermittence or continuous mode, and concentrated material turns back in reactor, realize the circular flow of material between thickener and reactor by circulating pump, material rests in reactor material in reactor sufficient reacting after concentrating through circulating continuously, be conducive to discharge material steady quality, uniformity is high; The variation of fluid level controller Real-time Feedback reinforced total amount in the time of the differential responses stage in reactor, by setting PLC control system, adjusts the switching value of discharge opeing control valve in time, further guarantees material in reactor concentration, improves the quality of products stable; After material in reactor is qualified, by setting PLC control system, that realizes discharge control valve discharges qualified products continuously or periodically, guarantees that production capacity is stable.
The present invention adopts the circulation of PLC control system control material in reactor to concentrate and automatic discharge, and its automatic controlling level is high, and reaction precision is high, can effectively extend material reaction time in reactor, guarantees sufficient reacting, improves production capacity and product quality.
Brief description of the drawings
Fig. 1 is the enrichment facility structural representation that the present invention adopts;
Fig. 2 is fundamental diagram of the present invention.
In figure: reactor 1, fluid level controller 2, thickener 3, discharge opeing control valve 4, circulating pump 5, discharge control valve 6, PLC control system 7.
Detailed description of the invention
Below in conjunction with drawings and Examples, the invention will be further described.
Shown in Fig. 1, the enrichment facility that the present invention adopts comprises reactor 1, fluid level controller 2, thickener 3, discharge opeing control valve 4, circulating pump 5, discharge control valve 6 and PLC control system 7.Reactor 1 inner top is provided with fluid level controller 2, reactor 1 bottom connects thickener 3 through circulating pump 5, on circulating pump 5, be also connected with discharge control valve 4, thickener 3 is connected to reactor 1 inner top, thickener 3 is provided with discharge opeing control valve 4, and fluid level controller 2, circulating pump 5, thickener 3, discharge control valve 6 and discharge opeing control valve 4 are all connected PLC control system 7.
The concentrated control method of presoma reaction process for lithium battery material shown in Fig. 2, the variation of fluid level controller Real-time Feedback reinforced total amount in the time of the differential responses stage in reactor, the material in reactor is pumped into thickener by PLC control system controlled circulation pump, after material filtering is concentrated, PLC control system control discharge opeing control valve switching value makes concentrated filtrate intermittently or continuous mode is discharged, concentrated material turns back in reactor, concentrated material rests on fully reaction in reactor continuously, control solids of sedimentation substrate concentration in reactor and reach 5～60%, proportion 1.1～the 1.8g/cm3 of solid sediment and mother liquor mixture, what PLC control system was adjusted discharge control valve in time opens discharge qualified products continuously or periodically.
Claims (1)
1. the concentrated control method of presoma reaction process for lithium battery material, it is characterized in that: adopt solid sediment in enrichment facility realization response still material to concentrate with separating of mother liquor, enrichment facility comprises reactor, fluid level controller, circulating pump, thickener and PLC control system, reactor inner top is provided with fluid level controller, reactor bottom connects thickener through circulating pump, thickener is connected to reactor inner top, and fluid level controller, circulating pump and thickener are all connected PLC control system; The variation of fluid level controller Real-time Feedback reinforced total amount in the time of the differential responses stage in reactor, the material in reactor is pumped into thickener by PLC control system controlled circulation pump, PLC control system is adjusted in time concentrated filtrate in thickener and is discharged, concentrated material turns back in reactor, concentrated material rests on fully reaction in reactor continuously, control solids of sedimentation substrate concentration in reactor and reach 5～60%, the proportion 1.1～1.8g/cm3 of solid sediment and mother liquor mixture; On described circulating pump, be also connected with discharge control valve, what PLC control system was adjusted discharge control valve in time opens discharge qualified products continuously or periodically; Described thickener is provided with discharge opeing control valve, and PLC control system control discharge opeing control valve switching value makes concentrated filtrate intermittently or continuous mode is discharged.
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| CN103301794B true CN103301794B (en) | 2014-08-20 |
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Families Citing this family (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105195075A (en) * | 2015-09-08 | 2015-12-30 | 西达（无锡）生物科技有限公司 | Circulating stirring device |
| CN107308898B (en) * | 2017-07-28 | 2023-09-15 | 格林美（江苏）钴业股份有限公司 | Rapid synthesis device for ternary lithium battery anode material precursor |
| CN107331859B (en) * | 2017-07-28 | 2019-12-10 | 荆门市格林美新材料有限公司 | Method for rapidly synthesizing ternary lithium battery positive electrode material precursor by single kettle |
| CN110600683B (en) * | 2018-06-13 | 2020-07-31 | 浙江帕瓦新能源股份有限公司 | Preparation method of semi-continuous ternary precursor |
| CN109382058A (en) * | 2018-11-02 | 2019-02-26 | 四川思达能环保科技有限公司 | A kind of Novel filtration enrichment facility and main reaction kettle device |
| CN109574093B (en) * | 2018-12-26 | 2021-11-05 | 柳州申通汽车科技有限公司 | Intermittent nickel-cobalt-aluminum precursor preparation method |
| CN110586017B (en) * | 2019-11-01 | 2024-06-14 | 常州市正元干燥工程有限公司 | Purifier |
| CN110756140B (en) * | 2019-11-05 | 2022-07-12 | 华友新能源科技（衢州）有限公司 | Method for concentrating materials in ternary precursor synthesis reaction |
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| WO1995024265A1 (en) * | 1994-03-11 | 1995-09-14 | Hoechst Celanese Corporation | Control system for an acetic acid manufacturing process |
| JP4998162B2 (en) * | 2007-09-12 | 2012-08-15 | 中西金属工業株式会社 | Interprocess conveyor system |
| CN202803228U (en) * | 2012-09-05 | 2013-03-20 | 瓮福（集团）有限责任公司 | Temperature control device for purified iodine reaction kettles |
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2013
- 2013-05-20 CN CN201310184305.8A patent/CN103301794B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO1995024265A1 (en) * | 1994-03-11 | 1995-09-14 | Hoechst Celanese Corporation | Control system for an acetic acid manufacturing process |
| JP4998162B2 (en) * | 2007-09-12 | 2012-08-15 | 中西金属工業株式会社 | Interprocess conveyor system |
| CN202803228U (en) * | 2012-09-05 | 2013-03-20 | 瓮福（集团）有限责任公司 | Temperature control device for purified iodine reaction kettles |
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Address after: 225400 No. 8 Binjiang North Road, Taixing Economic Development Zone, Jiangsu Patentee after: Grammy (Jiangsu) cobalt industry Limited by Share Ltd Address before: 225400 Taixing Economic Development Zone, Jiangsu, Binjiang, North Road, No. 8, No. Patentee before: Jiangsu Cobalt Nickel Metal Co., Ltd. |
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