CN102616865B - Preparation method of cobalt carbonate for battery - Google Patents
Preparation method of cobalt carbonate for battery Download PDFInfo
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- CN102616865B CN102616865B CN2012100798120A CN201210079812A CN102616865B CN 102616865 B CN102616865 B CN 102616865B CN 2012100798120 A CN2012100798120 A CN 2012100798120A CN 201210079812 A CN201210079812 A CN 201210079812A CN 102616865 B CN102616865 B CN 102616865B
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Abstract
The invention discloses a preparation method of cobalt carbonate for a battery. The preparation method comprises the following steps of: firstly adding an ammonium bicarbonate solution as a base solution; then adding a cobalt liquid for the neutralization precipitation reaction again; adding the ammonium bicarbonate solution and the cobalt liquid at the same time to a reaction system by adopting a simultaneous feeding mode till the pH of the reaction system is 6-7; moreover, keeping the pH of the whole system to be stabled to be 6-8 in the feeding process; also monitoring the dimension of cobalt carbonate particles; stopping feeding when D50 in the average particle size distribution index of cobalt carbonate reaches the stipulated requirement, thus the whole neutralization precipitation reaction is finished; and filtering and drying discharged materials after the reaction products in a reaction tank is subjected to heat preservation and aging continuously, thereby obtaining the required cobalt carbonate. The preparation method provided by the invention is simple and has low cost, two stage matching of the neutralization precipitation reaction is reasonable, the appropriate matched parameters are optimized, thereby preparing and obtaining the similar-spherical cobalt carbonate with great apparent density and uniform and controllable particle size.
Description
Technical field
The present invention relates to new material technology field, relate in particular to the battery material technology, be specifically related to a kind of preparation method of battery carbon acid cobalt.
Background technology
Progress along with society, the tempo of science and technology is progressively accelerated, the arrival of information age, promoting especially the continuous renewal of electronic product, increase in demand as the energy source device-secondary cell of portable electric appts, the positive electrode material of the secondary cell of present stage is used cobalt acid lithium as leading,, as the quality of the presoma (cobaltous carbonate) of the sour lithium of cobalt, has determined the performance of battery material.
Conventional cobaltous carbonate production is all to adopt anti-addition, is about to cobalt liquid and adds in ammonium bicarbonate soln and carry out neutralization precipitation,, by the adjustment to feed rate, feed temperature and feed concentration, controls size-grade distribution and the loose specific weight of the cobaltous carbonate of generation.
Yet in this neutralization precipitation process, due to constantly carrying out of precipitation, the acidity of system is constantly changing; In addition, also along with the carrying out of precipitation constantly consuming, and the volume of system constantly increases as the bicarbonate of ammonia of end liquid, thereby makes bicarbonate of ammonia concentration reduce; These situations all cause the continuous variation of precipitation environment, and the cobaltous carbonate that therefore generates on physicals, can't guarantee the consistence of front and back, and size-grade distribution is wide, and granular size is inhomogeneous, and profile is also irregular.Finally cause the cell positive material performance of working it out to differ, affect the consistence of battery product.
Summary of the invention
The object of the invention is to the deficiency that exists for prior art, a kind of evenly method of the spherical battery carbon acid cobalt of controlled, class of the Da Song of preparation ratio, particle diameter is provided.
Above-mentioned purpose of the present invention is achieved by following scheme:
Existing technique of producing cobaltous carbonate, its whole reaction is all to complete under greater than 7 environment at pH value, the inventor is by studying rear discovery to existing defective workmanship, neutralization-precipitation reaction is divided into two stages to carry out, and after in two stages, the parameters such as reactive mode, reaction system PH and temperature being carried out corresponding optimization, can obtain better experiment effect, thereby propose a kind of preparation method of battery carbon acid cobalt, this preparation method specifically comprises the steps;
Step 1 neutralization-precipitation reaction
Add ammonium bicarbonate soln as end liquid, then add cobalt liquid to carry out neutralization-precipitation reaction, to reaction system PH=6～7;
Step 2 neutralization-precipitation reaction
When the reaction system PH=6 of step 1～7, adopt the mode of charging simultaneously, add simultaneously ammonium bicarbonate soln and cobalt liquid in the reaction system of step 1, and keep whole system PH to be stabilized between 6～8 in reinforced process, and the size of monitoring cobalt carbonate particle, when the D50 in the average particle size distribution index of cobaltous carbonate reaches specified requirement, stop feeding in raw material, whole neutralization-precipitation reaction finishes;
Step 3 ageing
The material that step 2 is completely reacted is proceeded to be incubated ageing in reactive tank after, discharging is filtered, oven dry, obtains required cobaltous carbonate.
In above-mentioned steps 1, the concentration of ammonium bicarbonate soln is 150～250g/L; Cobalt liquid refers to cobalt chloride solution, cobalt sulfate solution or cobalt nitrate solution etc., and its concentration is in cobalt metal amount 60～120g/L.
In above-mentioned steps 1, add bicarbonate of ammonia as end liquid, the add-on of bicarbonate of ammonia is advisable can just open to stir.
In above-mentioned steps 1, add bicarbonate of ammonia as end liquid, then add cobalt liquid to carry out neutralization-precipitation reaction, cobalt liquid need to slowly add, and specifically can add according to the flow of 2～4L/h, and controlling the neutralization-precipitation reaction temperature is 40～50 ℃.
In above-mentioned steps 1, the temperature of neutralization-precipitation reaction is that the contriver determines after data-optimized, because the contriver finds the main task of this process, is the nucleus that forms cobaltous carbonate.The contriver finds through research: if the growth of the too low particle of temperature is too slow, and pattern is bad, if and temperature is too high, particle growth is too fast, Song Bixiao, do not reach requirement, and pattern is also bad, and therefore according to the result of optimization experiment, the neutralization-precipitation reaction temperature in step 1 of the present invention adopts 40～50 ℃, the nucleus good dispersity of producing in the temperature range of this optimization, might as well based on the granule-morphology of this nuclei growth.
In above-mentioned steps 2, in reinforced process, the concentration of ammonium bicarbonate soln is to adopt the ammonium bicarbonate soln concentration identical with step 1 simultaneously, and cobalt liquid concentration is to adopt the cobalt liquid concentration identical with step 1.
In above-mentioned steps 2, the flow of cobalt liquid be in step 1 the cobalt flow quantity 3/4; The flow of ammonium bicarbonate soln calculates by following method of calculation: cobalt liquid concentration * cobalt flow quantity * (3.5～4.5)/bicarbonate of ammonia concentration, the cobalt flow quantity that described cobalt flow quantity is step 2.
In above-mentioned steps 2, the neutralization-precipitation reaction temperature is 50～70 ℃.The inventor finds by research, and step 2 neutralization-precipitation reaction temperature is slightly higher than step 1 neutralization-precipitation reaction temperature, can look after better the speed of growth and the pattern of granularity and the relation between density of granularity.If temperature is too low, particle growth is slow, but pattern is relative with density better, if temperature is too high, particle manufacture is quick, but the poor density of pattern is poorer.Therefore the contriver is by after optimizing, and adopting step 2 neutralization-precipitation reaction temperature is 50～70 ℃, thereby takes well the balance of three aspects: into account.
In above-mentioned steps 2, the size of described monitoring cobalt carbonate particle, the D50 in the average particle size distribution index that detects the cobaltous carbonate of producing that refers to take a sample; When described D50 until cobaltous carbonate reaches specified requirement, stop feeding in raw material, while referring to the D50=6.5 of cobaltous carbonate～15 μ m, stop feeding in raw material.
In above-mentioned steps 2, if the D50 of cobaltous carbonate does not also reach the requirement of D50, and reactor has been filled material, stops feeding in raw material, and standing clarification after extracting the supernatant liquor of half out, then continues the charging reaction.
In above-mentioned steps 3, the inventor finds by research: after having carried out two step neutralization-precipitation reactions of step 1 and step 2, the ripening of arranging in pairs or groups again, can effectively help advancing of product purity one walk to improve, the impurity that removal is carried secretly, also can repair particle surface in microcosmic ground simultaneously, make its more nodularization, surface more smooth.Therefore, the contriver is studied and optimizes the condition of ageing again, reaches a conclusion as: Aging Temperature needs higher than step 2 neutralization-precipitation reaction temperature, and is concrete high 0～10 ℃; Digestion time is 2～8 hours.
In above-mentioned preparation method, the ratio of total consumption of bicarbonate of ammonia and total consumption of cobalt metal is (3.5～4.5): 1, and weight ratio.
, through the cobaltous carbonate of above-mentioned steps preparation, find after testing its even particle distribution, individual microscopic appearance rule, surfacing, class spheroidization.
Compared with prior art, the present invention has following beneficial effect:
1. existing cobaltous carbonate production technique is mainly to adopt a neutralization-precipitation reaction, at PH, completes under greater than 7 reaction system environment; And the present invention is the neutralization-precipitation reaction that adopts two steps, first neutralization-precipitation reaction adopts the reactive mode of the anti-addition of carbon ammonium, its temperature optimization, whole PH adopts the environment less than 7, the nucleus that these measures all make first neutralization-precipitation reaction generate is finer and close, and the apposition growth of the cobalt carbonate particle that generates for second neutralization-precipitation reaction provides good basis;
2. in first neutralization-precipitation reaction of the present invention, the low temperature during nucleation makes the motion of molecule can be very inviolent, is conducive to the dispersion of molecule; Low PH makes the content of cobaltous hydroxide in the cobaltous carbonate of generation less;
3. in second neutralization-precipitation reaction of the present invention, adopt reinforced simultaneously reactive mode, and controlling flow will be lower than the flow of first neutralization-precipitation reaction, so just can be under a metastable environment, cobalt carbonate particle carries out all to growth, thereby guarantee to produce even particle size distribution, Da Song ratio, the spherical cobaltous carbonate of class;
4. the present invention is by reducing the feed rate of second neutralization-precipitation reaction, control the quantity of newly-increased cobaltous carbonate, grow up thereby can be attached on the particle that first neutralization-precipitation reaction generates, can not pile up and grow up too much and voluntarily because of newly-generated quantity, guarantee the homogeneity of cobalt carbonate particle;
5. in two neutralization-precipitation reactions of the present invention, the flow of cobalt liquid adopts different numerical value, the cobalt flow quantity of second reaction is 3/4 of first reaction cobalt flow quantity, because the inventor finds by such adjustment, can reduce the generation of new nucleus, realize all being attached on original nucleus growing up, thus can be so that the particle growth energy be even, fine and close, pattern is good and Song Bida;
6. preparation method of the present invention two stage collocation simple, with low cost, neutralization-precipitation reaction are reasonable, and the parameter optimization of appropriate mix, thereby prepare the evenly controlled spherical cobaltous carbonate of class of Da Song ratio, particle diameter.
Description of drawings
Fig. 1 is the SEM figure that embodiment 1 prepares the gained cobaltous carbonate; Fig. 2 is the SEM figure that embodiment 2 prepares the gained cobaltous carbonate.
Embodiment
Below in conjunction with specific embodiment, the present invention is done further and describes, but specific embodiment is not done any restriction to the present invention.
Embodiment 1
The preparation method of the present embodiment cobaltous carbonate, specifically comprise the steps:
Step 1 neutralization-precipitation reaction
The ammonium bicarbonate soln (concentration of ammonium bicarbonate soln is 250 g/L) that adds a certain amount of (guarantee open stir get final product) in reaction tank bottom is as end liquid, open the water-bath heat-insulation system, ammonium bicarbonate soln in groove is warming up to 40 ℃, speed take the quantimeter displayed value as 2.5L/h joins cobalt liquid in groove intracellular bicarbonate ammonium solution and carries out neutralization-precipitation reaction afterwards, described cobalt liquid refers to that concentration is that in reaction process, temperature remains unchanged in the cobalt chloride solution of cobalt metal amount 100 g/L;
Step 2 neutralization-precipitation reaction
Reacting system PH value until step 1 reaches at 6.8 o'clock, reduce the cobalt chloride solution flow to 1.8L/h, rising system temperature to 50 ℃, start to add ammonium bicarbonate soln simultaneously, the flow of ammonium bicarbonate soln is 2.8L/h, and in reactive tank, pH value remains between 7.3 ± 0.2;
Fill in groove, stopped stirring 5 minutes this moment, supernatant liquor is extracted away 2.5L, continuation adds cobalt chloride solution and ammonium bicarbonate soln in aforesaid mode, stops after filling stirring 5 minutes again, and supernatant liquor is extracted away 2.5L, continue again to add cobalt chloride solution and ammonium bicarbonate soln, until cobaltous carbonate D50=9～during 10 μ m, stop feeding in raw material, thereby finish neutralization-precipitation reaction;
In above-mentioned steps 2, the concentration of cobalt chloride solution is 100 g/L, and ammonium bicarbonate soln concentration is 250 g/L.
Step 3 ageing
The material that step 2 is completely reacted is incubated ageing under 50 ℃ in reactive tank, digestion time is after 2 hours, and discharging is filtered, and prepares the required cobaltous carbonate of the present embodiment after oven dry, sampling analysis, and the SEM figure of cobaltous carbonate is as shown in Figure 1.
In above-mentioned preparation method, the ratio of total consumption of bicarbonate of ammonia and total consumption of cobalt metal is: 3.8:1, weight ratio.
The sampling analysis result shows: D10=6.914 in the average particle size distribution index of the cobaltous carbonate of the present embodiment preparation, D50=9.715, D90=13.724, Unusually narrow particle size distribution, even particle distribution, individual microscopic appearance rule, class nodularization, any surface finish.
Embodiment 2
The preparation method of the present embodiment cobaltous carbonate, specifically comprise the steps:
Step 1 neutralization-precipitation reaction
The ammonium bicarbonate soln (concentration of ammonium bicarbonate soln is 180 g/L) that adds a certain amount of (guarantee open stir get final product) in reaction tank bottom is as end liquid, open the water-bath heat-insulation system, ammonium bicarbonate soln in groove is warming up to 50 ℃, speed take the quantimeter displayed value as 2.0L/h joins cobalt liquid in groove intracellular bicarbonate ammonium solution and carries out neutralization-precipitation reaction afterwards, described cobalt liquid refers to that concentration is the cobalt chloride solution of 100 g/L, and in reaction process, temperature remains unchanged;
Step 2 neutralization-precipitation reaction
Reacting system PH value until step 1 reaches at 6.5 o'clock, reduces the cobalt chloride solution flow to 1.5L/h, and rising system temperature to 65 ℃, start to add ammonium bicarbonate soln simultaneously, and its flow is 3.3L/h, and in reactive tank, pH value remains between 7.0 ± 0.2;
Fill in groove, stopped stirring 5 minutes this moment, supernatant liquor is extracted away 2.5L, continuation adds cobalt chloride solution and ammonium bicarbonate soln in aforesaid mode, stops after filling stirring 5 minutes again, and supernatant liquor is extracted away 2.5L, continuing to add cobalt chloride solution and ammonium bicarbonate soln, until cobaltous carbonate D50 while reaching 15 μ m, stops feeding in raw material, thereby finish neutralization-precipitation reaction;
In above-mentioned steps 2, the concentration of cobalt chloride solution is that ammonium bicarbonate soln concentration is 180 g/L in cobalt metal amount 100 g/L.
Step 3 ageing
The material that step 2 is completely reacted is incubated ageing under 70 ℃ in reactive tank, digestion time is after 6 hours, and discharging is filtered, the required cobaltous carbonate of oven dry the present embodiment, and sampling analysis, the SEM figure of cobaltous carbonate is as shown in Figure 2.
In above-mentioned preparation method, the ratio of total consumption of bicarbonate of ammonia and total consumption of cobalt metal is: 4.0:1, weight ratio.
The sampling analysis result shows: D10=10.157 in the average particle size distribution index of the cobaltous carbonate of the present embodiment preparation, D50=15.221, D90=23.115, Unusually narrow particle size distribution, even particle distribution, individual microscopic appearance rule, class nodularization, any surface finish.
Claims (5)
1. the preparation method of a battery carbon acid cobalt, specifically comprise the steps:
Step 1, neutralization-precipitation reaction
Add ammonium bicarbonate soln as end liquid, then add cobalt liquid to carry out neutralization-precipitation reaction, to reaction system pH=6 ~ 7, wherein, the flow of cobalt liquid is 2 ~ 4L/h, and the neutralization-precipitation reaction temperature is 40 ~ 50 ℃;
Step 2, neutralization-precipitation reaction
When the reaction system pH=6 of step 1～7, adopt the mode of charging simultaneously, add simultaneously ammonium bicarbonate soln and cobalt liquid in the reaction system of step 1, and keep whole system pH to be stabilized between 6～8 in reinforced process, the neutralization-precipitation reaction temperature is controlled between 50 ~ 70 ℃, and the D50 in monitoring cobaltous carbonate average particle size distribution index, when the D50 of cobaltous carbonate is 6.5～15 μ m, stop feeding in raw material, whole neutralization-precipitation reaction finishes;
Wherein, the flow of cobalt liquid be in step 1 the cobalt flow quantity 3/4;
The flow of ammonium bicarbonate soln is cobalt liquid concentration * cobalt flow quantity * (3.5～4.5)/bicarbonate of ammonia concentration, the cobalt flow quantity that described cobalt flow quantity is step 2;
Step 3, ageing
The material that step 2 is completely reacted is proceeded to be incubated ageing in reactive tank after, discharging is filtered, oven dry, obtains required cobaltous carbonate.
2. the preparation method of a kind of battery carbon acid cobalt according to claim 1, is characterized in that in step 1, and the concentration of described ammonium bicarbonate soln is 150～250g/L; Described cobalt liquid refers to cobalt chloride solution, cobalt sulfate solution or cobalt nitrate solution, and its concentration is in cobalt metal amount 60～120g/L.
3. the preparation method of a kind of battery carbon acid cobalt according to claim 1, it is characterized in that in described step 2, in reinforced process, the concentration of ammonium bicarbonate soln is to adopt the ammonium bicarbonate soln concentration identical with step 1 simultaneously, and cobalt liquid concentration is to adopt the cobalt liquid concentration identical with step 1.
4. the preparation method of a kind of battery carbon acid cobalt according to claim 1, is characterized in that in described step 3, and Aging Temperature is higher 0～10 ℃ than the neutralization-precipitation reaction temperature of step 2.
5. the preparation method of according to claim 1 or 4 described a kind of battery carbon acid cobalts, is characterized in that in described step 3, and digestion time is 2～8 hours.
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| CN105600839A (en) * | 2014-11-20 | 2016-05-25 | 四川顺应金属材料科技有限公司 | Preparation method of battery-grade cobalt carbonate |
| CN106430332A (en) * | 2016-10-08 | 2017-02-22 | 南京寒锐钴业股份有限公司 | Method for reducing mother liquor emission and precipitant unit consumption in precipitation process |
| CN106711449B (en) * | 2017-01-06 | 2019-12-31 | 苏州宇量电池有限公司 | Synthesis method of nano linear cobalt carbonate negative electrode material |
| CN109467135B (en) * | 2018-10-31 | 2021-02-09 | 眉山顺应动力电池材料有限公司 | Preparation method of battery-grade cobalt carbonate and prepared cobalt carbonate |
| CN113292109B (en) * | 2020-02-24 | 2023-11-07 | 荆门市格林美新材料有限公司 | Preparation method of low-sodium superfine cobalt carbonate |
| CN113800573A (en) * | 2020-06-16 | 2021-12-17 | 荆门市格林美新材料有限公司 | Low-chloride ion washing method for cobalt carbonate |
| CN114735760A (en) * | 2022-03-25 | 2022-07-12 | 江西理工大学 | Method for controllably preparing superfine sphere-like cobalt carbonate by liquid phase precipitation method |
| CN114940515B (en) * | 2022-06-15 | 2023-11-03 | 荆门市格林美新材料有限公司 | Aluminum-doped cobalt carbonate and preparation method and application thereof |
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| CN101343084A (en) * | 2008-08-20 | 2009-01-14 | 周红阳 | Process for preparing high-density cobaltous carbonate |
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| CN101973592A (en) * | 2010-10-18 | 2011-02-16 | 南京寒锐钴业有限公司 | Preparation method of high-gravity spherical cobalt carbonate |
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| JPS54131597A (en) * | 1978-04-04 | 1979-10-12 | Sumitomo Metal Mining Co | Manufacture of high reactive basic cobalt carbonate |
| KR20090109733A (en) * | 2008-04-16 | 2009-10-21 | 메탈화학(주) | Method for producing high purity cobalt carbonate |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101343084A (en) * | 2008-08-20 | 2009-01-14 | 周红阳 | Process for preparing high-density cobaltous carbonate |
| CN101830521A (en) * | 2010-04-22 | 2010-09-15 | 江苏凯力克钴业股份有限公司 | Method for producing cobalt carbonate |
| CN101973592A (en) * | 2010-10-18 | 2011-02-16 | 南京寒锐钴业有限公司 | Preparation method of high-gravity spherical cobalt carbonate |
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Address after: 513056 Guangdong city of Qingyuan province city green town German Jiana Metal Technology Co Ltd Patentee after: GUANGDONG JIANA ENERGY TECHNOLOGY CO., LTD. Address before: German Green Town Qingyuan city Guangdong province 513056 Patentee before: Yingde Jiana Metal Technology Co., Ltd. |