CN103301794A - 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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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 that lithium battery material concentrates control method with the presoma reaction process specifically, being applied to lithium electricity positive electrode field, mainly is the production of positive electrode presoma, such 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 production of positive electrode is particularly important in industrial chain, the existing lithium battery material presoma that generally adopts, be mainly cobalt hydroxide, the multielement complex hydroxide of cobalt carbonate and nickel cobalt manganese, with cobalt salt, nickel salt, manganese salt, add simultaneously precipitating reagent and complexing agent, through synthetic its hydroxide of precipitation reaction or carbonate, obtain precursor powder through washes clean, the precipitation reaction operation be that presoma produces in critical process, the Main Physical Characteristics of lithium battery material, such as tap density, particle diameters etc. all depend on the control of the precipitation reaction of presoma, how to improve the efficient of reactor, the presoma of how controlling well also constantly highlights at the series of problems such as quality of course of reaction.
Existing lithium battery material presoma reactor operation, all adopt continuous charging, mode by the overfall continuous pulp discharge is carried out, along with carrying out continuously of charging reaction, initial stage liquid level in reactor reaches the overfall position and just begins the overflow discharge, the material that discharge this moment, because the reaction time is not enough, particle diameter is less than normal, tap density is on the low side etc., is equivalent to produce early stage a large amount of defective works, and the defective work of this moment needs again dissolving or the mode by mixed batch adds in the qualified material in the later stage, larger on the product quality impact, the Efficiency Decreasing of simultaneous reactions still; Also have in initial reaction stage and reduce reinforced total amount to prolong the mode in reaction time, but reinforced total amount reduces, the reactor production capacity also decreases, and carry out with adopting afterwards the mode of regulating reinforced total amount in initial reaction stage, the stabilizing influence of reaction system is very large before and after causing, and the mode of overflow is produced, along with reinforced carrying out continuously, material particular diameter, tap density meet the requirements, but there is larger fluctuation in the material that each time period discharges, and homogeneity of product is not high.
Summary of the invention
Low for lithium battery material presoma reactor operation reaction efficiency in the prior art, production capacity is low, the inconsistent deficiency that waits of product quality, the invention provides a kind of lithium battery material concentrated control method of presoma reaction process, can improve reactor efficient, reach stable control reactor material, guarantee simultaneously production capacity and product quality.
The technical solution used in the present invention is: a kind of lithium battery material concentrates control method with the presoma reaction process, it is characterized in that adopting the interior solid sediment of enrichment facility realization response still material concentrated with separating of mother liquor, enrichment facility comprises reactor, fluid level controller, circulating pump, thickener and PLC control system, the reactor inner top is provided with fluid level controller, the reactor bottom connects thickener through circulating pump, thickener is connected to the reactor inner top, and fluid level controller, circulating pump and thickener are connected and are connected the PLC control system; The fluid level controller Real-time Feedback is in the variation of differential responses reinforced total amount during the stage in the reactor, PLC control system controlled circulation pump pumps into thickener with the material in the reactor, the PLC control system is in time adjusted concentrated filtrate discharge in the thickener, concentrated material turns back in the reactor, concentrated material rests on fully reaction in the reactor continuously, the solids of sedimentation substrate concentration reaches 5～60%, the proportion 1.1～1.8g/cm3 of solid sediment and mother liquor mixture in the control reactor.
Further, also be connected with the discharge control valve on the described circulating pump, what the PLC control system was in time adjusted the discharge control valve opens the discharge qualified products continuously or periodically.
Again further, described thickener is provided with the 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 the filtering and concentrating function, material in the reactor is by behind the thickener, and concentrated filtrate was discharged by discharge opeing control valve intermittence or continuous mode, and concentrated material turns back in the reactor, realize the circular flow of material between thickener and reactor by circulating pump, after material is concentrated through circulation, rest on continuously in the reactor material in reactor sufficient reacting, be conducive to discharge the material steady quality, uniformity is high; The fluid level controller Real-time Feedback by setting the PLC control system, is in time adjusted the switching value of discharge opeing control valve in the variation of differential responses reinforced total amount during the stage in the reactor, further guarantees material in reactor concentration, improves the quality of products stable; After material in reactor was qualified, by setting the PLC control system, that realizes the discharge control valve discharged qualified products continuously or periodically, guaranteed 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 the reaction precision is high, can effectively prolong material in the reactor internal reaction time, guarantees sufficient reacting, improves production capacity and product quality.
Description of drawings
Fig. 1 is the enrichment facility structural representation that the present invention adopts;
Fig. 2 is fundamental diagram of the present invention.
Among the 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.
The specific embodiment
The invention will be further described below in conjunction with drawings and Examples.
Shown in Figure 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, also be connected with discharge control valve 4 on the circulating pump 5, 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 are connected and are all connected PLC control system 7.
Lithium battery material shown in Figure 2 concentrates control method with the presoma reaction process, the fluid level controller Real-time Feedback is in the variation of differential responses reinforced total amount during the stage in the reactor, PLC control system controlled circulation pump pumps into thickener with the material in the reactor, 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 the reactor, concentrated material rests on fully reaction in the reactor continuously, the solids of sedimentation substrate concentration reaches 5～60%, the proportion 1.1～1.8g/cm3 of solid sediment and mother liquor mixture in the control reactor; What the PLC control system was in time adjusted the discharge control valve opens the discharge qualified products continuously or periodically.
Claims (3)
1. a lithium battery material concentrates control method with the presoma reaction process, it is characterized in that: adopt the interior solid sediment of enrichment facility realization response still material concentrated with separating of mother liquor, enrichment facility comprises reactor, fluid level controller, circulating pump, thickener and PLC control system, the reactor inner top is provided with fluid level controller, the reactor bottom connects thickener through circulating pump, thickener is connected to the reactor inner top, and fluid level controller, circulating pump and thickener are connected and are connected the PLC control system; The fluid level controller Real-time Feedback is in the variation of differential responses reinforced total amount during the stage in the reactor, PLC control system controlled circulation pump pumps into thickener with the material in the reactor, the PLC control system is in time adjusted concentrated filtrate discharge in the thickener, concentrated material turns back in the reactor, concentrated material rests on fully reaction in the reactor continuously, the solids of sedimentation substrate concentration reaches 5～60%, the proportion 1.1～1.8g/cm3 of solid sediment and mother liquor mixture in the control reactor.
2. lithium battery material according to claim 1 concentrates control method with the presoma reaction process, it is characterized in that: also be connected with the discharge control valve on the described circulating pump, what the PLC control system was in time adjusted the discharge control valve opens the discharge qualified products continuously or periodically.
3. lithium battery material according to claim 1 concentrates control method with the presoma reaction process, it is characterized in that: described thickener is provided with the 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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Cited By (7)
| 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 |
| CN107308898A (en) * | 2017-07-28 | 2017-11-03 | 荆门市格林美新材料有限公司 | A kind of Fast back-projection algorithm device of ternary anode material of lithium battery presoma |
| CN107331859A (en) * | 2017-07-28 | 2017-11-07 | 荆门市格林美新材料有限公司 | A kind of method of one-pot Fast back-projection algorithm ternary anode material of lithium battery presoma |
| 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 |
| CN109574093A (en) * | 2018-12-26 | 2019-04-05 | 柳州申通汽车科技有限公司 | A kind of intermittent nickel cobalt aluminium precursor preparation method |
| CN110600683A (en) * | 2018-06-13 | 2019-12-20 | 浙江帕瓦新能源股份有限公司 | Preparation method of semi-continuous ternary precursor |
| CN110756140A (en) * | 2019-11-05 | 2020-02-07 | 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
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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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 |
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Cited By (12)
| 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 |
| CN107308898A (en) * | 2017-07-28 | 2017-11-03 | 荆门市格林美新材料有限公司 | A kind of Fast back-projection algorithm device of ternary anode material of lithium battery presoma |
| CN107331859A (en) * | 2017-07-28 | 2017-11-07 | 荆门市格林美新材料有限公司 | A kind of method of one-pot Fast back-projection algorithm ternary anode material of lithium battery presoma |
| 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 |
| 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 |
| CN110600683A (en) * | 2018-06-13 | 2019-12-20 | 浙江帕瓦新能源股份有限公司 | Preparation method of semi-continuous ternary precursor |
| 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 |
| CN109574093A (en) * | 2018-12-26 | 2019-04-05 | 柳州申通汽车科技有限公司 | A kind of intermittent nickel cobalt aluminium precursor preparation method |
| 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 |
| CN110756140A (en) * | 2019-11-05 | 2020-02-07 | 华友新能源科技（衢州）有限公司 | Method for concentrating materials in ternary precursor synthesis reaction |
| 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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| CN103301794B (en) | 2014-08-20 |
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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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