CN102689933A - Method for producing hydroxy cobalt oxide - Google Patents
Method for producing hydroxy cobalt oxide Download PDFInfo
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- CN102689933A CN102689933A CN2012100681530A CN201210068153A CN102689933A CN 102689933 A CN102689933 A CN 102689933A CN 2012100681530 A CN2012100681530 A CN 2012100681530A CN 201210068153 A CN201210068153 A CN 201210068153A CN 102689933 A CN102689933 A CN 102689933A
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Abstract
The invention discloses a method for producing hydroxy cobalt oxide, comprising the following steps of: firstly, preparing a cobaltous sulfate solution with cobalt content of 75-85g/l; adjusting a pH value of the solution to be 3.0-4.5; adding EDTA (Ethylene Diamine Tetraacetic Acid) into the solution according to the proportion of cobalt to EDTA of 100:(1-3); preparing sodium hydroxide solution with alkali concentration of 7-9mol; performing cocurrent flow on two solutions and flowing into a reaction groove; introducing the air for performing synthetic reaction; controlling the reaction temperature to be between 50 and 70 and a pH value to be between 10.0 and 12.0 for reacting for 15-25 hours; flowing into an aging groove for aging for 50-60 minutes; and finally, filtering, washing and slurrying to prepare a hydroxy cobalt oxide solid product. According to the method, the production process is controllable, particles of the product are uniformly distributed with good consistency, the shape is spherical and the product has good dispersibility; and the production process is free of ammonia nitrogen pollution, so that continuous production is realized, and the equipment utilization rate and the production efficiency are improved.
Description
Technical field
The present invention relates to the hydroxyl oxidize process for producing cobalt that production such as a kind of novel material making method, especially battery material, catalyzer, magneticsubstance, electronic material, wimet are used.。
Background technology
Hydroxy cobalt oxide is mainly used in makes high-quality tricobalt tetroxide, and battery high-quality for producing, that have extended cycle life is established solid raw material basis.There is following defective in existing manufacturing technique:
1, the precipitation agent that adopts is a carbonate, and the ammonia nitrogen refuse intractable that produces in the production process is prone to contaminate environment.
2, adopt the mode of production of being interrupted of a groove one groove, can not continuous production.When material reach a certain height in reactive tank and each processing condition when reaching, can only the whole emptyings of material in the groove be produced again again.
3, product particle skewness, particle diameter and form can't be controlled, and consistence is poor, quality is unstable.
Summary of the invention
The purpose of this invention is to provide a kind of hydroxyl oxidize process for producing cobalt, accomplish serialization production, controllability of improving the quality of products and stability, pollution-free.
Production stage of the present invention is following:
1, preparation cobalt sulfate solution
According to the cobalt contents of cobalt sulfate solution raw material, the sour cobalt contents controlling index 75～85g/l that makes the groove nominal volume and wait to prepare cobalt liquor; Calculated in advance goes out the add-on that needs of cobalt sulfate solution raw material; By calculating good add-on the cobalt sulfate solution raw material is added Preparation tank, open agitating vane, add pure water to Preparation tank nominal volume absolute altitude place; Stirred 5～10 minutes, and made the solution thorough mixing; Add hydrochloric acid, adjustment pH value of solution value is 3.0～4.5, the sampling analysis cobalt contents, by cobalt: EDTA=100: 1～3 ratio adding additive EDTA pumps into high-order cobalt liquid storage tank then.
2, preparation sodium hydroxide solution
According to concentration, the Preparation tank nominal volume of sodium hydroxide solution raw material and wait to prepare the controlling index 7～9mol of concentration of lye; Calculated in advance goes out the add-on that needs of sodium hydroxide solution raw material, by calculating good add-on the sodium hydroxide solution raw material is added Preparation tank, opens agitating vane; Add pure water to Preparation tank nominal volume absolute altitude place; Stirred 5～10 minutes, and made the solution thorough mixing, pump into high-order alkali lye storage tank then.
3, building-up reactions
With the cobalt sulfate solution for preparing and sodium hydroxide solution respectively with 100～00L/h flow and 60～350L/h flow simultaneously and flow in the reactive tank, the feeding flow is 8～15m in the reaction solution
3The air of/h, control reaction temperature are 50～70 ℃, and the pH value is 10.0～12.0; React and generate after 15～25 hours in hydroxy cobalt oxide slip and the riser inflow ageing tank of beginning on reactive tank; Digestion time is 50～60 minutes, impels grain growing even, and a material pattern is more complete.
4, filter, wash and a pulp
Slip in the ageing tank is all pumped into the 1# pressure filter, at first compress filter plate, make slip after press filtration, become filter cake; Then washing leaching cake unclamps filter plate and unloads filter cake, on one side discharging adding pulp groove, add pure water to pulp groove riser place on one side, carry out the pulp first time, stir pulp 10～20 minutes, filter cake is broken up fully; Open pulp groove blow-off valve then; 70～90 ℃ of hot pure water 2.5～3.5m have been added in advance
31# medial launder discharge.
5, filtration, washing and secondary pulp
When the material in the 1# medial launder reaches 5m3, the material in the 1# medial launder is pumped into the 2# pressure filter, pump limit, limit adds 70～90 ℃ of hot pure water toward the 2# pressure filter, till material all pumps into the 2# pressure filter.After press filtration for the second time, the washing; Dismantle the 2# cake of filter-press on one side and add the pulp groove; Add pure water to pulp groove riser place on one side, carry out the pulp second time, stir pulp 10～20 minutes; Open pulp groove blow-off valve toward 2# medial launder discharge, the 2# medial launder is added with 70～90 ℃ of pure hot water 2.5～3.5m in advance
3Material in the 2# medial launder reaches 5m
3The time, pumping into the 3# pressure filter, pump limit, limit adds 70～90 ℃ hot pure water, till material all pumps into the 3# pressure filter; After the press filtration of 3# pressure filter finished, with 70～90 ℃ of hot pure water washings 25～30 minutes, assurance Na ionic concn was unclamped the 3# filter press filter board at last less than 0.01g/l, unloads filter cake, promptly obtains the hydroxy cobalt oxide solid phase prod.
Compared with present technology, the present invention has following characteristics:
1, production process is controlled, constant product quality.
Owing to can effectively regulate and control important parameters such as stirrer rotating speed, pH value, temperature and reaction soln flow velocitys in the production process; And used additive EDTA to regulate, so product particle is evenly distributed high conformity; Pattern type of being is spherical, has good dispersiveness and stability.
2, serialization production improves plant factor and working efficiency.
The suitable height location of reactive tank has riser; When material reaches riser in the groove; The building-up reactions of cobalt liquid and alkali lye is accomplished basically, and the slip of generation directly flows out from the reactive tank riser, so the slip outflow reactive tank of cobalt liquid, alkali lye entering reactive tank and generation carries out simultaneously; Serialization production be can realize, plant factor and working efficiency improved.
3, production process does not have ammonia and nitrogen pollution.
Since adopt sodium hydroxide to replace carbonate, so no ammonia nitrogen class refuse produce in the production process as precipitation agent, therefore free from environmental pollution.
Description of drawings
Fig. 1 is hydroxy cobalt oxide product chemical ingredients, physicals table.
Fig. 2 is the hydroxy cobalt oxide product structure figure that the present invention produces.
Embodiment
Embodiment one
Production stage is following:
1, preparation cobalt sulfate solution
When the cobalt contents controlling index of cobalt liquor to be prepared is 80g/l, at nominal volume 10m
3Preparation tank in to add cobalt contents be the cobalt sulfate solution raw material 8m of 100g/l
3, open agitating vane, add pure water to Preparation tank nominal volume absolute altitude place; Stirred 5～10 minutes, and added hydrochloric acid, adjustment pH value of solution value is 3.5; The sampling analysis cobalt contents, in cobalt: EDTA=100: 2 ratio adds additive EDTA, pumps into high-order cobalt liquid storage tank then.
2, preparation sodium hydroxide solution
When concentration of lye controlling index to be prepared is 8mol, at nominal volume 10m
3Preparation tank in add the sodium hydroxide solution 6.67m of concentration when being 12mol
3, open agitating vane, add pure water to Preparation tank nominal volume absolute altitude place, stirred 5～10 minutes, pump into high-order alkali lye storage tank then.
3, building-up reactions
Cobalt sulfate solution with 300L/h flow, sodium hydroxide solution simultaneously and flow in the reactive tank with 200L/h, the feeding flow is 12m in the reaction solution
3The air of/h, control reaction temperature are 50～70 ℃, and the pH value is 10.0～12.0, react to generate after 15～25 hours in hydroxy cobalt oxide slip and the riser inflow ageing tank of beginning on reactive tank, and digestion time is 50～60 minutes.
4, filter, wash and a pulp
Slip in the ageing tank is pumped into the press filtration of 1# pressure filter, washing leaching cake, on one side discharging adding pulp groove; Add pure water to pulp groove riser place on one side, carry out the pulp first time, stir pulp 10～20 minutes; Open pulp groove blow-off valve then, added 70～90 ℃ of hot pure water 2.5～3.5m in advance
31# medial launder discharge.
5, filtration, washing and secondary pulp
Material in the 1# medial launder reaches 5m
3The time, the material in the 1# medial launder is pumped into the 2# pressure filter, pump limit, limit adds 70～90 ℃ of hot pure water toward the 2# pressure filter, till material all pumps into the 2# pressure filter.After press filtration for the second time, the washing, add the pulp groove, carry out the pulp second time (identical) with pulp first time operating procedure Yi Bian dismantle the 2# cake of filter-press.Pulp groove discharge is to being added with 70～90 ℃ of hot pure water 2.5～3.5m in advance
3The 2# medial launder; When the material of 2# medial launder reaches 5m
3The time, the material in the 2# medial launder is pumped into the 3# pressure filter, pump limit, limit adds 70～90 ℃ hot pure water, till material all pumps into the 3# pressure filter.After the press filtration of 3# pressure filter finishes,, guarantee that the Na ionic concn is less than 0.01g/l with 70～90 ℃ of hot pure water washings 25～30 minutes; Unload filter cake at last, promptly obtain the hydroxy cobalt oxide solid phase prod.
Embodiment two
This routine production stage 1 is basic identical with embodiment one, and have only following parameters different: the cobalt contents controlling index of cobalt sulfate solution to be prepared is 75g/l, is the rose vitriol 8.33m of 90g/l toward the interior adding of Preparation tank cobalt contents
3, adjustment solution pH value is 3.0, press cobalt: EDTA=100: 1 adds additive EDTA.
This routine production stage 2 is basic identical with embodiment one, and have only following parameters different: alkali concn controlling index to be prepared is 7mol, is the sodium hydroxide solution 7m of 10mol toward the interior adding of Preparation tank concentration
3
This routine production stage 3 is basic identical with embodiment one, and have only following parameters different: the flow of cobalt sulfate solution is 100L/h, and the flow of sodium hydroxide solution is 60L/h, and air flow quantity is 8m
3/ h.
This routine production stage 3,4 and embodiment one are identical.
Embodiment three
This routine production stage 1 is basic identical with embodiment one, and have only following parameters different: the cobalt contents controlling index of cobalt sulfate solution to be prepared is 85g/l, is the rose vitriol 7.73m of 110g/l toward the interior adding of Preparation tank cobalt contents
3, adjustment pH value of solution value is 4.5, press cobalt: EDTA=100: 3 add additive EDTA.
This routine production stage 2 is basic identical with embodiment one, and have only following parameters different: alkali concn controlling index to be prepared is 9mol, is the sodium hydroxide solution 6m of 15mol toward the interior adding of Preparation tank concentration
3
This routine production stage 3 is basic identical with embodiment one, and have only following parameters different: the flow of cobalt sulfate solution is 500L/h, and the flow of sodium hydroxide solution is 350L/h, and air flow quantity is 15m
3/ h.
This routine production stage 3,4 and embodiment one are identical.
Claims (1)
1. hydroxyl oxidize process for producing cobalt is characterized in that production stage is following:
A, preparation cobalt sulfate solution
According to cobalt contents, the Preparation tank nominal volume of cobalt sulfate solution raw material and wait to prepare the cobalt contents controlling index 75～85g/l of cobalt liquor; Calculated in advance goes out the add-on that needs of cobalt sulfate solution raw material; By calculating good add-on the cobalt sulfate solution raw material is added Preparation tank, open agitating vane, add pure water to Preparation tank nominal volume absolute altitude place; Stirred 5～10 minutes, and made the solution thorough mixing; Add hydrochloric acid, adjustment pH value of solution value is 3.0～4.5, the sampling analysis cobalt contents, and by cobalt: EDTA=100: 1～3 ratio adding additive EDTA pumps into high-order cobalt liquid storage tank then;
B, preparation sodium hydroxide solution
Based on concentration, the make-up tank nominal volume of sodium hydroxide solution raw material and wait to prepare the control index 7～9mol of concentration of lye; Calculated in advance goes out the addition that needs of sodium hydroxide solution raw material; By calculating good addition the sodium hydroxide solution raw material is added make-up tank; Open stirring vane; Add pure water to make-up tank nominal volume absolute altitude place; Stirred 5～10 minutes, solution is fully mixed, pump into high-order alkali lye storage tank then;
C, building-up reactions
With the cobalt sulfate solution for preparing and sodium hydroxide solution respectively with 100～500L/h flow and 60～350L/h flow simultaneously and flow in the reactive tank, the feeding flow is 8～15m in the reaction solution
3The air of/h, control reaction temperature are 50～70 ℃, and the pH value is 10.0～12.0, react to generate after 15～25 hours in hydroxy cobalt oxide slip and the riser inflow ageing tank of beginning on reactive tank, and digestion time is 50～60 minutes;
D, filtration, washing and a pulp
Slip in the ageing tank is all pumped into the 1# pressure filter, at first compress filter plate, make slip after press filtration, become filter cake; Then washing leaching cake unclamps filter plate and unloads filter cake; Discharging on one side adds the pulp groove; Add pure water to pulp groove riser place on one side, carry out the pulp first time, stir pulp 10～20 minutes, filter cake is broken up fully; Open pulp groove blow-off valve then, added 70～90 ℃ of hot pure water 2.5～3.5m in advance
31# medial launder discharge;
E, filtration, washing and secondary pulp
When the material in the 1# medial launder reaches 5m3, the material in the 1# medial launder is pumped into the 2# pressure filter, pump limit, limit adds 70～90 ℃ of hot pure water toward the 2# pressure filter, till material all pumps into the 2# pressure filter; After press filtration for the second time, the washing; Dismantle the 2# cake of filter-press on one side and add the pulp groove; Add pure water to pulp groove riser place on one side, carry out the pulp second time, stir pulp 10～20 minutes; Open pulp groove blow-off valve toward 2# medial launder discharge, the 2# medial launder is added with 70～90 ℃ of hot pure water 2.5～3.5m in advance
3Material in the 2# medial launder reaches 5m
3The time, the material in the 2# medial launder is pumped into the 3# pressure filter, pump limit, limit adds 70～90 ℃ hot pure water, till material all pumps into the 3# pressure filter; After the press filtration of 3# pressure filter finishes,, guarantee that the Na ionic concn is less than 0.01g/l with 70～90 ℃ of hot pure water washings 25～30 minutes; Unclamp the 3# filter press filter board at last, unload filter cake, promptly obtain the hydroxy cobalt oxide solid phase prod.
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| CN2012100681530A CN102689933A (en) | 2012-03-15 | 2012-03-15 | Method for producing hydroxy cobalt oxide |
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Cited By (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102881896A (en) * | 2012-10-22 | 2013-01-16 | 吉林吉恩亚融科技有限公司 | Cobalt coating method for spherical nickel hydroxide by mechanical fusion |
| CN103232075A (en) * | 2013-04-11 | 2013-08-07 | 湖南雅城新材料发展有限公司 | Preparation method for large-grained spherical cobalt oxyhydroxide |
| CN103466722A (en) * | 2013-08-26 | 2013-12-25 | 无锡中经金属粉末有限公司 | Synthesis technology of nano cobalt oxyhydroxide |
| CN103482710A (en) * | 2013-08-27 | 2014-01-01 | 江苏华东锂电技术研究院有限公司 | Preparation method of spherical hydroxy cobalt oxide |
| CN103490062A (en) * | 2013-08-27 | 2014-01-01 | 江苏华东锂电技术研究院有限公司 | Preparation method of lithium cobalt oxide |
| CN104056489A (en) * | 2014-03-31 | 2014-09-24 | 成都易态科技有限公司 | Cross flow filtration method of metal sulfate solution |
| CN105129869A (en) * | 2015-08-28 | 2015-12-09 | 上饶市鼎鑫金属化工有限公司 | Novel ammonia-free continuous production technology of spherical large-particle-size CoOOH |
| CN105869916A (en) * | 2016-06-23 | 2016-08-17 | 华中科技大学 | Method for preparing hydroxyl cobaltous oxide nanotube electrode |
| CN108928847A (en) * | 2017-05-27 | 2018-12-04 | 江苏凯力克钴业股份有限公司 | A kind of copper sulfide purifying technique and device |
| CN111233051A (en) * | 2020-03-04 | 2020-06-05 | 陕西师范大学 | Method for preparing submicron spherical cobalt carbonate |
| CN111348688A (en) * | 2018-12-24 | 2020-06-30 | 格林美（江苏）钴业股份有限公司 | Post-treatment device and post-treatment process for cobaltosic oxide synthetic material |
| CN111924890A (en) * | 2020-07-01 | 2020-11-13 | 陕西师范大学 | Preparation method of CoO (OH) nanoflower |
| CN112645392A (en) * | 2021-03-11 | 2021-04-13 | 金驰能源材料有限公司 | Laminated high-density sphere-like cobalt oxyhydroxide precursor and preparation method thereof |
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Cited By (23)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102881896B (en) * | 2012-10-22 | 2014-06-18 | 吉林吉恩亚融科技有限公司 | Cobalt coating method for spherical nickel hydroxide by mechanical fusion |
| CN102881896A (en) * | 2012-10-22 | 2013-01-16 | 吉林吉恩亚融科技有限公司 | Cobalt coating method for spherical nickel hydroxide by mechanical fusion |
| CN103232075B (en) * | 2013-04-11 | 2015-06-03 | 湖南雅城新材料发展有限公司 | Preparation method for cobalt oxyhydroxide |
| CN103232075A (en) * | 2013-04-11 | 2013-08-07 | 湖南雅城新材料发展有限公司 | Preparation method for large-grained spherical cobalt oxyhydroxide |
| CN103466722A (en) * | 2013-08-26 | 2013-12-25 | 无锡中经金属粉末有限公司 | Synthesis technology of nano cobalt oxyhydroxide |
| CN103466722B (en) * | 2013-08-26 | 2015-05-27 | 无锡中经金属粉末有限公司 | Synthesis technology of nano cobalt oxyhydroxide |
| CN103490062A (en) * | 2013-08-27 | 2014-01-01 | 江苏华东锂电技术研究院有限公司 | Preparation method of lithium cobalt oxide |
| WO2015027821A1 (en) * | 2013-08-27 | 2015-03-05 | 江苏华东锂电技术研究院有限公司 | Preparation method of lithium cobalt oxide |
| WO2015027841A1 (en) * | 2013-08-27 | 2015-03-05 | 江苏华东锂电技术研究院有限公司 | Method for preparing spherical cobalt oxyhydroxide |
| CN103490062B (en) * | 2013-08-27 | 2016-05-04 | 江苏华东锂电技术研究院有限公司 | The preparation method of cobalt acid lithium |
| CN103482710A (en) * | 2013-08-27 | 2014-01-01 | 江苏华东锂电技术研究院有限公司 | Preparation method of spherical hydroxy cobalt oxide |
| CN104056489B (en) * | 2014-03-31 | 2016-08-17 | 成都易态科技有限公司 | The cross flow filter method of solution of metal sulfates |
| CN104056489A (en) * | 2014-03-31 | 2014-09-24 | 成都易态科技有限公司 | Cross flow filtration method of metal sulfate solution |
| CN105129869A (en) * | 2015-08-28 | 2015-12-09 | 上饶市鼎鑫金属化工有限公司 | Novel ammonia-free continuous production technology of spherical large-particle-size CoOOH |
| CN105869916A (en) * | 2016-06-23 | 2016-08-17 | 华中科技大学 | Method for preparing hydroxyl cobaltous oxide nanotube electrode |
| CN105869916B (en) * | 2016-06-23 | 2018-04-24 | 华中科技大学 | A kind of preparation method of hydroxy cobalt oxide nanotube electrode |
| CN108928847A (en) * | 2017-05-27 | 2018-12-04 | 江苏凯力克钴业股份有限公司 | A kind of copper sulfide purifying technique and device |
| CN108928847B (en) * | 2017-05-27 | 2023-05-12 | 格林美（江苏）钴业股份有限公司 | Copper sulfide purification process and device |
| CN111348688A (en) * | 2018-12-24 | 2020-06-30 | 格林美（江苏）钴业股份有限公司 | Post-treatment device and post-treatment process for cobaltosic oxide synthetic material |
| CN111348688B (en) * | 2018-12-24 | 2023-11-21 | 格林美（江苏）钴业股份有限公司 | Device and process for post-treatment of cobaltosic oxide synthetic material |
| CN111233051A (en) * | 2020-03-04 | 2020-06-05 | 陕西师范大学 | Method for preparing submicron spherical cobalt carbonate |
| CN111924890A (en) * | 2020-07-01 | 2020-11-13 | 陕西师范大学 | Preparation method of CoO (OH) nanoflower |
| CN112645392A (en) * | 2021-03-11 | 2021-04-13 | 金驰能源材料有限公司 | Laminated high-density sphere-like cobalt oxyhydroxide precursor and preparation method thereof |
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Application publication date: 20120926 |