CN101376529B - Method for producing spherical cobaltous carbonate - Google Patents
Method for producing spherical cobaltous carbonate Download PDFInfo
- Publication number
- CN101376529B CN101376529B CN200810143011XA CN200810143011A CN101376529B CN 101376529 B CN101376529 B CN 101376529B CN 200810143011X A CN200810143011X A CN 200810143011XA CN 200810143011 A CN200810143011 A CN 200810143011A CN 101376529 B CN101376529 B CN 101376529B
- Authority
- CN
- China
- Prior art keywords
- tank
- pulp
- cobalt
- reaction
- storage tank
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Fee Related
Links
Images
Landscapes
- Battery Electrode And Active Subsutance (AREA)
Abstract
The invention relates to a manufacturing method of spherical cobalt carbonate. At first, a cobalt chloride solution and an ammonium hydrocarbonate solution are led to flow into a reaction tank according to a certain flow rate, the reaction temperature is controlled between 5 and 9 DEG C by a refrigerator; the reaction is conducted under the condition that the pH value is 7.2 to 7.3; when the liquid level of a ground-paste reaches 1.5m<3> in the reaction tank, the ground-paste is discharged into an ageing tank, the ground-paste in the ageing tank is heated until the temperature ranges from 43 to 47 DEG C, is processed through standing, precipitation and growth, is filtered, pulped and washed after being aged for 18 hours, and then is dried and secondary-recovered by a cyclone separating device and a pouched trapper to obtain the finished product. The manufacturing method is characterized in that the refrigerator is utilized to reduce the reaction temperature during the reaction process, and a product crystal is led to grow canonically and evenly instead of being influenced by temperature no longer and grow to a spheroid finally under the conditions of constant flow, constant temperature and constant pH value. At the same time, the production mode adopts the standing and ageing without stirring to achieve the determinacy on particle nucleation condition and manufacturing time during the product is manufactured, thereby ensuring the controllability on particle diameter and shape of the precipitate particles.
Description
Technical field
The cobaltous carbonate production method that production such as a kind of novel material making method, especially battery material, catalyzer, magneticsubstance, electronic material, Wimet are used.
Background technology
Advanced information society, the mobile electronic device fast development has benefited from the good electro-chemical properties of volt of green lithium-ion secondary cell.The production of lithium ion secondary battery anode material, the most ripe with cobalt acid lithium at present, the critical materials of decision cobalt acid lithium quality is except that the influence that is subjected to cobaltous carbonate density and crystalline structure, and crystal morphology also has very large influence.The suitability for industrialized production of spherical cobaltous carbonate is still blank at home at present, and therefore producing spherical cobaltous carbonate is pressing for of battery industry.
Tradition carbonic acid process for producing cobalt is that cobalt chloride and bicarbonate of ammonia are reacted under hot conditions, easily cause the violent phenomenon of local reaction, the generation particle growth is too fast, pattern (have dendroid, sheet, bar-shaped etc.) of all kinds, add and adopt mechanical stirring in the reaction process, cause the product crystal structure to be damaged easily, can't standard grow equably.In addition, the flow of traditional technology, temperature, pH value are controlled non-constant, inaccurate.In a word, traditional technology easily causes product particle skewness, crystalline form inconsistent, is unfavorable for the stable of quality product, can not produce spherical cobaltous carbonate at all.
Summary of the invention
The purpose of this invention is to provide a kind of method for producing spherical cobaltous carbonate, accomplish that reaction precipitation composition granule particle diameter and form can control, guarantee that pattern is spherical, product has consistence.
Production stage of the present invention is as follows:
1, preparation cobalt chloride solution
In configured slot, add pure water 1m
3, open agitating vane, slowly add the cobalt chloride of certainweight, add pure water to 3m after having thrown cobalt chloride
3, fully dissolving, sampling analysis when cobalt chloride concentration reaches 100 ± g/L, pumps into cobalt liquid storage tank.
2, preparation precipitation agent
In configured slot, add pure water 1m
3, open agitating vane, slowly add the bicarbonate of ammonia of certainweight, add water to 3m again after having thrown bicarbonate of ammonia
3, stir after 20 minutes, fully dissolving when bicarbonate of ammonia concentration reaches 120 ± 5g/L, pumps into the alkali lye storage tank.
3, low temperature is synthetic
In reactive tank, add 150 liters in end water, open refrigerator, control reaction temperature is 7 ± 2 ℃, open cobalt liquid pump and lye pump, open the under meter of cobalt liquid storage tank and alkali lye storage tank respectively, make cobalt chloride solution and ammonium bicarbonate soln flow into reactive tank by certain flow, the pH value after hour in the sampling analysis reactive tank, the control pH value is 7.2～7.3; The slip liquid level reaches 1.5m in reactive tank
3The time, close the under meter of cobalt liquid storage tank and alkali lye storage tank respectively, open the reactive tank bottom valve, groove internal reaction liquid all is discharged to is added with 1m in advance
3In the ageing tank of hot water.
4, staticly settle growth
Slip intensification in the ageing tank is reached 45 ± 2 ℃ of controlled temperature, staticly settle growth; After 18 hours from groove sampling analysis, when the laser particle diameter of ageing precipitation material reaches the 3-6 micron, again aged material is all pumped into pressure filter (model is XMG 30/1000-uK).
5, filtration, pulp and washing
At first compress filter plate, make slip become filter cake behind squeeze and filter, then washing leaching cake unclamps filter plate and unloads filter cake, begins pulp then: add pure water 0.8m toward the pulp groove earlier
3, slowly adding filter cake toward the pulp groove when opening agitating vane, the limit adds the pure water limit stirred 30 minutes, accomplished pulp cmpletely; At last the material after the pulp is pressed into once more and carries out filtration washing in the pressure filter, till do not have white precipitate, detect Cl in filtrate with silver nitrate titration this moment up to washing
-≤ 0.005g/L.
6, drying
The dismounting filter cake dries up the back and sends into drying machine with feeder, sends into hot blast toward drying machine simultaneously; The spiral rotation of hot blast, constantly blot the moisture of material, the drying machine mechanical force is pulverized material, material after the pulverizing is done rotating forward movement with hot blast, wherein macrobead gets rid of under centrifugal action to barrel and drops to the bottom and carry out new pulverizing drying process again, reach the dry particulate that requires and then carried secretly and enter cyclonic separator, enter pouched trapper again after coming out from cyclonic separator, promptly obtain finished product respectively with the secondary recovery device by air-flow.
7, packing
At first two layers of plastics inner bag are inserted in Fibre Bag, the plastics inner bag of again finished product being packed into is discharged gas, fraps plastics inner bag sack, Fibre Bag is sealed to get final product then.
Compared with the prior art, characteristics of the present invention are to use refrigerator to reduce temperature of reaction in reaction process, guarantee not have the generation of vigorous reaction phenomenon, make no longer temperature influence and standard is grown equably of product crystal, under constant current, constant temperature, permanent pH value condition, finally grow into sphere; Adopt the still aging mode of production simultaneously, do not stir, make product in the production process particle nucleation condition, determinacy was arranged on the production time, guaranteed the controllability of precipitate particles particle diameter and form.
Description of drawings
Fig. 1 is the spherical cobaltous carbonate chemical index
Fig. 2 is the spherical cobaltous carbonate physical index
Fig. 3 is the micro-enlarged view of spherical cobaltous carbonate
Embodiment
Embodiment and production stage of the present invention are identical, repeat no more herein.Fig. 3 is the crystal morphology of the spherical cobaltous carbonate produced of the present invention.
Claims (1)
1. method for producing spherical cobaltous carbonate, its production stage is as follows:
A, preparation cobalt chloride solution
In configured slot, add pure water 1m
3, open agitating vane, slowly add the cobalt chloride of certainweight, has thrown cobalt chloride after the benefit pure water to 3m
3, fully dissolving, sampling analysis when cobalt chloride concentration reaches 100 ± 5g/L, pumps into cobalt liquid storage tank;
B, preparation precipitation agent
In configured slot, add pure water 1m
3, open agitating vane, slowly add the bicarbonate of ammonia of certainweight, add water to 3m again after having thrown bicarbonate of ammonia
3, stirred 20 minutes, fully dissolving when bicarbonate of ammonia concentration reaches 120 ± 5g/L, pumps into the alkali lye storage tank;
C, low temperature synthesize
In reactive tank, add 150 liters in end water, open refrigerator, control reaction temperature is 7 ± 2 ℃, open cobalt liquid pump and lye pump, open the under meter of cobalt liquid storage tank and alkali lye storage tank respectively, make cobalt chloride solution and ammonium bicarbonate soln flow into reactive tank by certain flow, the pH value after hour in the sampling analysis reactive tank, the control pH value is 7.2～7.3; The slip liquid level reaches 1.5m in reactive tank
3The time, close the under meter of cobalt liquid storage tank and alkali lye storage tank respectively, open the reactive tank bottom valve, groove internal reaction liquid all is discharged to is added with 1m in advance
3In the ageing tank of hot water;
D, staticly settle growth
Slip intensification in the ageing tank is reached 45 ± 2 ℃ of controlled temperature, staticly settle growth; After 18 hours from groove sampling analysis, when the laser particle diameter of ageing precipitation material reaches the 3-6 micron, again aged material is all pumped into pressure filter;
E, filtration, pulp and washing
At first compress filter plate, make slip become filter cake behind squeeze and filter, then washing leaching cake unclamps filter plate and unloads filter cake, begins pulp then; Add pure water 0.8m toward the pulp groove earlier
3, slowly adding filter cake toward the pulp groove when opening agitating vane, the limit adds the pure water limit stirred 30 minutes, accomplished pulp cmpletely; At last that pulp is good material is pressed into once more and carries out filtration washing in the pressure filter, and till do not have white precipitate, this moment is with the Cl in the silver nitrate titration detection filter up to washing
-≤ 0.005g/L;
F, drying
The dismounting filter cake, dry up the back and send into drying machine with feeder, send into hot blast toward drying machine simultaneously, the spiral rotation of hot blast, constantly blot the moisture of material, the drying machine mechanical force is pulverized material, material after the pulverizing is done rotating forward movement with hot blast, wherein macrobead gets rid of to barrel under centrifugal action and drops to the bottom and carry out new pulverizing drying process again, reaching the dry particulate that requires is then carried secretly by air-flow and enters cyclonic separator, enter pouched trapper again after coming out from cyclonic separator, promptly obtain finished product respectively with the secondary recovery device;
G, packing
At first two layers of plastics inner bag are inserted in the Fibre Bag, the plastics inner bag of again finished product being packed into is discharged gas, fraps plastics inner bag sack, Fibre Bag is sealed to get final product then.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN200810143011XA CN101376529B (en) | 2008-09-24 | 2008-09-24 | Method for producing spherical cobaltous carbonate |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN200810143011XA CN101376529B (en) | 2008-09-24 | 2008-09-24 | Method for producing spherical cobaltous carbonate |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN101376529A CN101376529A (en) | 2009-03-04 |
| CN101376529B true CN101376529B (en) | 2010-10-13 |
Family
ID=40420274
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN200810143011XA Expired - Fee Related CN101376529B (en) | 2008-09-24 | 2008-09-24 | Method for producing spherical cobaltous carbonate |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN101376529B (en) |
Families Citing this family (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101823155B (en) * | 2010-06-10 | 2011-11-23 | 南京寒锐钴业有限公司 | Preparation method for near-spherical aggregation cobalt powder |
| CN101857278B (en) * | 2010-06-25 | 2012-05-23 | 浙江华友钴业股份有限公司 | Method for preparing spherical carbonate |
| CN101973591B (en) * | 2010-09-30 | 2011-11-09 | 安徽亚兰德新能源材料有限公司 | Method for producing spherical cobalt carbonate by continuous process |
| CN102910686A (en) * | 2011-08-04 | 2013-02-06 | 深圳市格林美高新技术股份有限公司 | Cobalt carbonate preparation method and superfine cobalt powder preparation method |
| CN103288144A (en) * | 2012-04-25 | 2013-09-11 | 漳州师范学院 | Synthesis technology of high-purity carbonate |
| CN104722766B (en) * | 2013-12-18 | 2017-07-18 | 格林美股份有限公司 | A kind of high density cobalt powder and its synthetic method |
| DE202022102465U1 (en) | 2022-04-29 | 2022-05-12 | Hte Gmbh The High Throughput Experimentation Company | Device for the production of solid particles |
| WO2023208742A1 (en) | 2022-04-29 | 2023-11-02 | Hte Gmbh The High Throughput Experimentation Company | Device and method for producing solid particles |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1276345A (en) * | 1999-06-02 | 2000-12-13 | 成都蜀都电子粉体材料厂 | Process for preparing nm-class cobalt oxide |
| CN1470460A (en) * | 2003-07-08 | 2004-01-28 | 中信国安盟固利电源技术有限公司 | High-purity spherical cobalto-cobaltic oxide, and its preparing method and use |
-
2008
- 2008-09-24 CN CN200810143011XA patent/CN101376529B/en not_active Expired - Fee Related
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1276345A (en) * | 1999-06-02 | 2000-12-13 | 成都蜀都电子粉体材料厂 | Process for preparing nm-class cobalt oxide |
| CN1470460A (en) * | 2003-07-08 | 2004-01-28 | 中信国安盟固利电源技术有限公司 | High-purity spherical cobalto-cobaltic oxide, and its preparing method and use |
Non-Patent Citations (1)
| Title |
|---|
| JP 特开2002-3222 A,说明书第0010-0021段. |
Also Published As
| Publication number | Publication date |
|---|---|
| CN101376529A (en) | 2009-03-04 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN101376529B (en) | Method for producing spherical cobaltous carbonate | |
| CN101343084B (en) | Process for preparing high-density cobaltous carbonate | |
| CN108258235B (en) | Method for preparing nickel-cobalt-manganese ternary precursor material through hierarchical reaction | |
| CN107324405B (en) | A kind of lithium nickel cobalt manganese oxide precursor and preparation method thereof and lithium ion battery by the precursor preparation | |
| CN104201367B (en) | High density small particle nickel cobalt manganese hydroxide and preparation method thereof | |
| CN107565121B (en) | Preparation method of modified positive electrode material of lithium battery | |
| CN110127777B (en) | Wet zirconium-doped nickel-cobalt-aluminum ternary precursor with gradient concentration and preparation method thereof | |
| CN109761288B (en) | A kind of preparation method of spherical nickel cobalt manganese persursor material | |
| CN107180950A (en) | A kind of ternary cathode material of lithium ion battery NCM, NCA spray drying process preparation method | |
| CN105870409B (en) | A kind of preparation method and lithium ion battery of nickel-cobalt-manganternary ternary anode material | |
| CN108987682B (en) | Preparation method of nickel-rich precursor material capable of preventing particle fracture | |
| CN102259934B (en) | Oxidization process for producing high-density spherical cobaltosic oxide by virtue of low temperature liquid phase precipitation | |
| CN109686966A (en) | A kind of energy storage super large partial size nickel cobalt manganese hydroxide and preparation method thereof | |
| CN107308898A (en) | A kind of Fast back-projection algorithm device of ternary anode material of lithium battery presoma | |
| CN107732212A (en) | A kind of porous nickel cobalt manganese composite hydroxide and preparation method thereof and the application in lithium ion anode material | |
| CN101269848A (en) | High-density spherical cobaltic-cobaltous oxide and method for preparing the same | |
| CN104649336B (en) | A kind of preparation method of spherical nickel-cobalt aluminium hydroxide presoma | |
| CN108264096B (en) | Preparation method of high-density small-particle nickel-cobalt-manganese hydroxide | |
| WO2023207248A1 (en) | Nca positive electrode material precursor having core-shell structure, method for preparing same, and use thereof | |
| CN111072075A (en) | Preparation method of lithium ion battery anode material | |
| WO2023029897A1 (en) | Preparation method and preparation apparatus for high tap density ternary precursor material | |
| CN103803663B (en) | A kind of production method of spherical cobaltic-cobaltous oxide | |
| CN105129869B (en) | A kind of spherical big particle diameter hydroxy cobalt oxide no ammonia continuous production technology | |
| CN1830788B (en) | Technology of transforming common magnesium hydrexide into hexagonal sheel shaped magnesium hydroxide by hydrothermal method | |
| CN108365183A (en) | Ternary material with surface coated with aluminum oxide and preparation method thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| ASS | Succession or assignment of patent right |
Owner name: LOUDI REDSUN POWER SOURCE NEW MATERIALS CO., LTD. Free format text: FORMER OWNER: ZHOU HONGYANG Effective date: 20110504 |
|
| C41 | Transfer of patent application or patent right or utility model | ||
| COR | Change of bibliographic data |
Free format text: CORRECT: ADDRESS; FROM: 417007 LOUDI REDSUN NEW POWER MATERIALS COMPANY, DEVELOPMENT ZONE, WANBAO TOWN, LOUXING DISTRICT, LOUDI CITY, HU NAN PROVINCE TO: 417007 XINZHI VILLAGE, WANBAO TOWN, LOUXING DISTRICT, LOUDI CITY, HU NAN PROVINCE |
|
| TR01 | Transfer of patent right |
Effective date of registration: 20110504 Address after: Loudi City, Hunan Province Wan Bao 417007 Louxing District Xin Zhi Cun Patentee after: Loudi red sun power supply new material Co Ltd Address before: 417007 Loudi City, Hunan province Louxing District Wanbao Town Development Zone Loudi red sun power new material company Patentee before: Zhou Hongyang |
|
| C56 | Change in the name or address of the patentee |
Owner name: HU NAN REDSUN NEW MATERIALS CO., LTD. Free format text: FORMER NAME: LOUDI REDSUN POWER SOURCE NEW MATERIALS CO., LTD. |
|
| CP01 | Change in the name or title of a patent holder |
Address after: Loudi City, Hunan Province Wan Bao 417007 Louxing District Xin Zhi Cun Patentee after: Hunan Red Sun Power Supply New Material Co.,Ltd. Address before: Loudi City, Hunan Province Wan Bao 417007 Louxing District Xin Zhi Cun Patentee before: Loudi red sun power supply new material Co Ltd |
|
| ASS | Succession or assignment of patent right |
Owner name: ZHOU HONGYANG Free format text: FORMER OWNER: HU NAN REDSUN NEW MATERIALS CO., LTD. Effective date: 20150513 |
|
| C41 | Transfer of patent application or patent right or utility model | ||
| TR01 | Transfer of patent right |
Effective date of registration: 20150513 Address after: 417007 Loudi City, Hunan Province Yue Ping Yin Tong District Six neighborhood offices Patentee after: Zhou Hongyang Address before: Loudi City, Hunan Province Wan Bao 417007 Louxing District Xin Zhi Cun Patentee before: Hunan Red Sun Power Supply New Material Co.,Ltd. |
|
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20101013 Termination date: 20150924 |
|
| EXPY | Termination of patent right or utility model |