CN1297488C - Production equipment and technique for ultramicro powder of cobalt carbonate - Google Patents
Production equipment and technique for ultramicro powder of cobalt carbonate Download PDFInfo
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- CN1297488C CN1297488C CNB2005100314546A CN200510031454A CN1297488C CN 1297488 C CN1297488 C CN 1297488C CN B2005100314546 A CNB2005100314546 A CN B2005100314546A CN 200510031454 A CN200510031454 A CN 200510031454A CN 1297488 C CN1297488 C CN 1297488C
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- reactor
- cobalt
- cobalt salt
- cobalt carbonate
- header tank
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- 238000004519 manufacturing process Methods 0.000 title claims abstract description 31
- 239000000843 powder Substances 0.000 title claims description 39
- ZOTKGJBKKKVBJZ-UHFFFAOYSA-L cobalt(2+);carbonate Chemical compound [Co+2].[O-]C([O-])=O ZOTKGJBKKKVBJZ-UHFFFAOYSA-L 0.000 title claims description 26
- 229910021446 cobalt carbonate Inorganic materials 0.000 title claims description 23
- 238000000034 method Methods 0.000 title claims description 7
- 150000001868 cobalt Chemical class 0.000 claims abstract description 26
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 22
- 238000001556 precipitation Methods 0.000 claims abstract description 22
- 238000003756 stirring Methods 0.000 claims abstract description 16
- 238000006243 chemical reaction Methods 0.000 claims abstract description 12
- 239000000243 solution Substances 0.000 claims abstract description 11
- 230000032683 aging Effects 0.000 claims abstract description 10
- 239000012266 salt solution Substances 0.000 claims abstract description 9
- 239000007788 liquid Substances 0.000 claims description 26
- 239000003513 alkali Substances 0.000 claims description 22
- 239000000463 material Substances 0.000 claims description 8
- 230000008676 import Effects 0.000 claims description 6
- 230000001105 regulatory effect Effects 0.000 claims description 6
- 230000000087 stabilizing effect Effects 0.000 claims description 4
- 230000029087 digestion Effects 0.000 claims description 3
- 239000002994 raw material Substances 0.000 claims description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 2
- 229910052799 carbon Inorganic materials 0.000 claims description 2
- 238000005516 engineering process Methods 0.000 abstract description 6
- 230000001376 precipitating effect Effects 0.000 abstract 6
- ZJRWDIJRKKXMNW-UHFFFAOYSA-N carbonic acid;cobalt Chemical compound [Co].OC(O)=O ZJRWDIJRKKXMNW-UHFFFAOYSA-N 0.000 abstract 4
- 239000012527 feed solution Substances 0.000 abstract 1
- 239000002245 particle Substances 0.000 description 10
- 239000000047 product Substances 0.000 description 8
- 229910017052 cobalt Inorganic materials 0.000 description 6
- 239000010941 cobalt Substances 0.000 description 6
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 6
- IVMYJDGYRUAWML-UHFFFAOYSA-N cobalt(II) oxide Inorganic materials [Co]=O IVMYJDGYRUAWML-UHFFFAOYSA-N 0.000 description 5
- 238000001149 thermolysis Methods 0.000 description 4
- 229910000001 cobalt(II) carbonate Inorganic materials 0.000 description 3
- MULYSYXKGICWJF-UHFFFAOYSA-L cobalt(2+);oxalate Chemical compound [Co+2].[O-]C(=O)C([O-])=O MULYSYXKGICWJF-UHFFFAOYSA-L 0.000 description 2
- IUYLTEAJCNAMJK-UHFFFAOYSA-N cobalt(2+);oxygen(2-) Chemical compound [O-2].[Co+2] IUYLTEAJCNAMJK-UHFFFAOYSA-N 0.000 description 2
- 239000006185 dispersion Substances 0.000 description 2
- 238000007701 flash-distillation Methods 0.000 description 2
- 238000007429 general method Methods 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 238000010298 pulverizing process Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 235000008331 Pinus X rigitaeda Nutrition 0.000 description 1
- 235000011613 Pinus brutia Nutrition 0.000 description 1
- 241000018646 Pinus brutia Species 0.000 description 1
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 1
- 239000012190 activator Substances 0.000 description 1
- 239000013543 active substance Substances 0.000 description 1
- 239000007795 chemical reaction product Substances 0.000 description 1
- 238000010924 continuous production Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 230000004907 flux Effects 0.000 description 1
- 239000000543 intermediate Substances 0.000 description 1
- 230000001788 irregular Effects 0.000 description 1
- 239000011259 mixed solution Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 230000006911 nucleation Effects 0.000 description 1
- 238000010899 nucleation Methods 0.000 description 1
- 239000007774 positive electrode material Substances 0.000 description 1
- 239000012254 powdered material Substances 0.000 description 1
- 239000000725 suspension Substances 0.000 description 1
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- Inorganic Compounds Of Heavy Metals (AREA)
- Battery Electrode And Active Subsutance (AREA)
Abstract
The present invention discloses a device for producing ultramicrofine cobalt carbonate powder and technology thereof. The production device comprises a cobalt salt high-level tank, a precipitating agent high-level tank, a reactor, a stirrer, a sieve plate and an aging tank, wherein the reactor is arranged on the lower parts of the cobalt salt high-level tank and the precipitating agent high-level tank; the stirrer is arranged in the reactor; the sieve plate which is fixed on a controllable stirring shaft rotating at high speed is arranged on the upper part of the reactor; the aging tank is arranged on a discharge opening on the lower end of the reactor; feed openings are arranged on the tops of the cobalt salt high-level tank and the precipitating agent high-level tank, and feed solution outlets are arranged on the lower parts of the cobalt salt high-level tank and the precipitating agent high-level tank. The production technology comprises the following conditions that: a cobalt salt solution contains 20 to 80 g/l of Co<2+>; the concentration of a precipitating agent solution is 15 to 35 wt%; the adding speed of the cobalt salt solution is from 20 to 100 L/min; the adding speed of a precipitating agent is from 60 to 400 L/min; the temperature of a precipitation reaction is from 25 to 60DEGC; the pH value of the precipitation reaction is from 6.5 to 7.5; the stirring speed is from 500 to 1000 r/min; the ageing time is from 0.5 to 2.0 hours. When the device for producing ultramicrofine cobalt carbonate powder and the technology thereof of the present invention are used for producing cobalt carbonate powder, production can be continuously carried out; the productive efficiency can be improved by many times; the product quality is stable; the purpose that the prospective ultramicrofine cobalt carbonate powder is produced can be easily realized.
Description
Technical field
The present invention relates to a kind of production equipment and technology of ultramicro powder of cobalt carbonate.
Background technology
Cobalt such as super fine cobalt powder, cobaltous oxide product is widely used in many fields such as battery material, catalyzer as powdered material.Activator in particular as high tension battery---cobalt oxyhydrogen powder, not only the Chemical Composition requirement is very harsh, and the requirement of physical and chemical performance is higher.The equipment of preparation cobalt oxyhydrogen powder is the settling bath of belt stirrer at present, and the preparation method adopts precipitation agent (Na
2CO
3, NH
4HCO
3Or (NH
4)
2 2C
2O
4) directly join to precipitate in the cobalt saline solution settling bath and produce intermediates such as cobaltous carbonate or cobalt oxalate.Use this production equipment, production can only be carried out by intermittent type, and production efficiency is low, and unstable product quality, the pH value of the temperature of precipitin reaction, reaction soln etc. also are difficult to regulate; And this direct sedimentary charging process, a fatal shortcoming is more arranged, be easy to generate alkali exactly, the cobaltous carbonate of gained or cobalt oxalate powder distribution are inhomogeneous, and globule size and pattern are irregular, it is big to be difficult to prepare specific surface area, like the globular minuteness particle, thereby it is big to be difficult to make specific surface area with this powder of cobalt carbonate as raw material, and globule size is even, pattern is seemingly spherical, loose than little, active good cobalt oxyhydrogen powder.
Summary of the invention
But the object of the present invention is to provide a kind of continuous production, production efficiency height, the powder of cobalt carbonate production equipment of constant product quality.
Another object of the present invention is to provide a kind of production technique of ultramicro powder of cobalt carbonate of good product quality, the powder of cobalt carbonate that use the present invention's production technique makes, by thermolysis, it is big to obtain specific surface area, globule size is even, pattern is seemingly spherical, the cobalt oxyhydrogen powder of Song Bixiao.
The objective of the invention is to be achieved through the following technical solutions.
The present invention's powder of cobalt carbonate production equipment comprises the cobalt salt header tank, the precipitation agent header tank, be positioned at the reactor of described two header tank bottoms, be provided with agitator in the described reactor, top is provided with sieve plate, described sieve plate is fixed on the stir shaft of controlled high speed rotating, under the discharge gate of reactor lower end, is provided with ageing tank; Described cobalt salt header tank and precipitation agent header tank top are provided with liquor inlet and alkali lye import, and the bottom is respectively equipped with material liquid outlet and alkali lye outlet.Below be preferred version: described cobalt salt header tank side wall upper part also is provided with the feed liquid overflow port, and the bottom is provided with the feed temperature setter, and the material liquid outlet place is provided with under meter; Described precipitation agent header tank side wall upper part also is provided with the alkali lye overflow port, and the bottom is provided with the alkali liquid temperature setter, and the alkali lye exit is provided with under meter; Described reactor also is provided with pH value setter and thermoswitch; Described liquor inlet carries pump outlet to be communicated with by pipeline and adjusting; The alkali lye import carries pump outlet to be communicated with by pipeline and adjusting.
When using the above device to carry out the production of powder of cobalt carbonate, precipitant solution in cobalt salt solution in the cobalt salt header tank and the precipitation agent header tank, continuously flow in the reactor respectively, when described solution arrives sieve plate, because sieve plate is fixed on the stir shaft of controlled high speed rotating, the mixed solution of the two can obtain abundant dispersed with stirring, through fully disperseing to stir the ultra tiny CoCO that generates
3Particle suspension enters ageing tank continuously from the discharge gate of reactor lower end, and feed liquid after a certain constant time stirs, is directly pressed general method and filtered in ageing tank, just can obtain containing H
2The CoCO of O 40～70%
3Product.Flow into the constant flow of reactor at certain certain value by under meter and/or flow director may command.Can stablize the liquid level of two header tanks by two adjusting transferpumps and/or overflow port.Temperature of reaction and pH value can be regulated by the thermoswitch and the pH-meter that are contained on the reactor.
The method of utilizing the production equipment of the present invention's ultramicro powder of cobalt carbonate to carry out ultramicro powder of cobalt carbonate production is: the raw material cobalt salt solution contains Co
2+20-80g/l, precipitation agent (soluble carbon hydrochlorate) strength of solution 15wt%-35wt%; Adding speed: cobalt salt solution 20-100L/min, precipitation agent 60-400L/min; Precipitation reaction temperature 25-60 ℃: pH value 6.5-7.5; Stirring velocity 500-1000r/min (speed control by frequency variation); Regulate inlet amount=generation CoCO
3The output of sedimentary solution keeps reactor liquid level stabilizing 10-90cm under sieve plate; Digestion time 0.5-2.0 hour.
Use the present invention's powder of cobalt carbonate production equipment and ultramicro powder of cobalt carbonate production technique to carry out the production of powder of cobalt carbonate, production can be carried out continuously, and production efficiency can improve several times, constant product quality; The preferred version of its production equipment, owing to can adjust precipitation reaction temperature and pH value as required at any time, control feed liquid and flux of alkaline liquor, thereby very help realizing making expection superfine CoCO
3The purpose of particle.
With prepared superfine CoCO
3Powder just can obtain satisfactory cobaltous oxide powder by flash distillation oven dry pulverizing, thermolysis.
Description of drawings
Accompanying drawing is the structural representation of the present invention's powder of cobalt carbonate production equipment one embodiment.
Embodiment
Below in conjunction with accompanying drawing, at first powder of cobalt carbonate production equipment one embodiment to the present invention is illustrated; Then, introduction utilizes this device to carry out superfine CoCO
3The embodiment that powder is produced.
Present embodiment powder of cobalt carbonate production equipment comprises cobalt salt header tank 3, precipitation agent header tank 4, be positioned at the reactor 2 of described two header tanks 3 and 4 bottoms, be provided with agitator 1 in the reactor 2, top is provided with sieve plate 9, sieve plate 9 is fixed on the stir shaft of controlled agitator 1 high speed rotating, under the discharge gate of reactor 2 lower ends, is provided with ageing tank 20; Cobalt salt header tank 3 and precipitation agent header tank 4 tops are respectively equipped with liquor inlet 19, alkali lye import 13, and the bottom is respectively equipped with material liquid outlet 12, alkali lye outlet 16; Cobalt salt header tank 3 side wall upper part are provided with feed liquid overflow port 10, and the bottom is provided with feed temperature setter 14, and material liquid outlet 12 places are provided with under meter 5; Precipitation agent header tank 4 side wall upper part also are provided with alkali lye overflow port 11, and the bottom is provided with alkali liquid temperature setter 15, and alkali lye exports 16 places and is provided with under meter 6; Described reactor 2 also is provided with pH value setter 8 and thermoswitch 7; Liquor inlet 19 is communicated with the outlet of regulating transferpump 17 by pipeline, and alkali lye import 13 is communicated with the outlet of regulating transferpump 18 by pipeline.
Cobalt salt solution and alkali lye continuously flow on the sieve plate 9 of reactor 2 by material liquid outlet 12, alkali lye outlet 16 and under meter 5,6 from cobalt salt header tank 3 and precipitation agent header tank 4 respectively, continuously flow on the sieve plate 9 of reactor 2 the ultra tiny CoCO that the abundant dispersion stirring of warp generates through living alkali lye outlet 16 of abundant dispersion stirring and under meter 5,6
3Particle solution enters ageing tank 20 continuously from the discharge gate of reactor 2 lower ends, and feed liquid is directly pressed general method and filtered after a certain constant time stirs in ageing tank 20, just can obtain containing H
2O 40～70%CoCO
3Product.By the flow of under meter 5 and 6 control inflow reactors 2, make the constant position at distance sieve plate 9 10-90 centimetres of liquid level in the reactor 2.For keeping two flow quantities constant, regulate transferpump 17 and 18 and overflow port 10 and 11 by two liquid, to stablize the liquid level of two header tanks.Temperature of reaction and pH value are regulated by the thermoswitch 7 and the pH-meter 8 that are contained on the reactor 2, realize requiring to obtain ultra micro CoCO
3Particle; By flash distillation oven dry pulverizing, thermolysis, just can obtain satisfactory CoO powder again.
According to device shown in Figure 1, under different reaction conditionss,, just can produce the cobaltous carbonate particulate of different-grain diameter, and and then make D by reactor reaction
501～10 μ m, specific surface area 6～20m
2The end product CoO ultramicro powder of/g.
The CoCO that obtains under the different condition
3Particle detects by Central South University's country's powder inspection center's laser diffraction granularity analyser (model MALV ≡ RN), as cobalt salt concentration C o
2+40g/l, when other condition is constant, the CoCO that obtains
3: D
50=3.16 μ m, specific surface area=5.7019m
2/ g; As cobalt salt concentration C o
2+70g/l, when other condition is identical, the D that records
50=0.65 μ m, specific surface area=13.5833m
2/ g.As seen CoCl in the stoste
2It is bigger to contain Co concentration, and product granularity diminishes, and along with Co
2+Concentration reduces, resulting CoCO
3D
50Increase.Stoste CoCl
2Contain Co
2+40g/l, NH
4HCO
3Concentration 20%, mol ratio is pressed CoCl
2: NH
4HCO
3=1: 3.2, when two liquid flow into respectively when being fixed on the sieve plate that runs up on the reactor stir shaft, be evenly dispersed on the liquid level under the sieve plate, react nucleation (CoCO fast
3And follow nuclei growth nucleus).Regulate inlet amount=generation CoCO
3The output of sedimentary solution keeps reactor liquid level stabilizing 10-90cm under sieve plate, just can obtain granularity D
50The CoCO of=3.16 μ m
3Particle.
The superfine CoCO that utilizes the above powder of cobalt carbonate production equipment to make
3Powder by thermolysis, can obtain the active substance CoO powder as secondary battery positive electrode material: specific surface area＞12m
2/ g, globule size is even, pattern is seemingly spherical, and pine is than＞0.3 μ m, Fisher particle size 0.2～0.5 μ m.
Below introducing utilizes this device to carry out superfine CoCO
3Two embodiment that powder is produced.
Work as CoCl
2Contain Co
2+70g/l, NH
4HCO
3Concentration 20wt%, adding speed: cobalt salt solution 60L/min, precipitation agent 180L/min; 40 ℃ of precipitation reaction temperature: pH value 7.0; Stirring velocity 700r/min (speed control by frequency variation); Regulate inlet amount=generation CoCO
3The output of sedimentary solution keeps reactor liquid level stabilizing 50cm under sieve plate; Digestion time 1.5 hours.
The CoCO that obtains
3Fine powder, particle diameter D
50=0.65 μ m.
Work as CoCl
2Contain Co
2+40g/l, NH
4HCO
3Concentration 20wt%, other conditions are with embodiment 1.
The CoCO that obtains
3Fine powder, particle diameter D
50=3.16 μ m.
Claims (4)
1, a kind of ultramicro powder of cobalt carbonate production equipment, it is characterized in that, comprise cobalt salt header tank (3), precipitation agent header tank (4) is positioned at the reactor (2) of described two header tanks (3) and (4) bottom, is provided with agitator (1) in the described reactor (2), top is provided with sieve plate (9), described sieve plate (9) is fixed on the stir shaft of controlled high speed rotating, under the discharge gate of reactor (2) lower end, is provided with ageing tank (20); Described cobalt salt header tank (3) top is provided with liquor inlet (19), and the bottom is provided with material liquid outlet (12), and described precipitation agent header tank (4) top is provided with alkali lye import (13), and the bottom is provided with alkali lye outlet (16).
2, ultramicro powder of cobalt carbonate production equipment according to claim 1, it is characterized in that, described cobalt salt header tank (3) side wall upper part also is provided with feed liquid overflow port (10), and the bottom is provided with feed temperature setter (14), and material liquid outlet (12) locates to be provided with under meter (5); Precipitation agent header tank (4) side wall upper part also is provided with alkali lye overflow port (11), and the bottom is provided with alkali liquid temperature setter (15), and alkali lye outlet (16) locates to be provided with under meter (6); Described reactor (2) also is provided with pH value setter (8) and thermoswitch (7).
3, the production equipment of ultramicro powder of cobalt carbonate according to claim 1 and 2 is characterized in that, described liquor inlet (19) is communicated with the outlet of regulating transferpump (17) by pipeline; Alkali lye import (13) is communicated with the outlet of regulating transferpump (18) by pipeline.
4, utilize the production equipment of claim 1 or 2 or 3 described ultramicro powder of cobalt carbonate to carry out the method that ultramicro powder of cobalt carbonate is produced, it is characterized in that the raw material cobalt salt solution contains Co
2+20-80g/l, soluble carbon hydrochlorate precipitant solution concentration 15wt%-35wt%; Adding speed: cobalt salt solution 20-100L/min, precipitation agent 60-400L/min; Precipitation reaction temperature 25-60 ℃: pH value 6.5-7.5; Adopt the stirring velocity 500-1000r/min of speed control by frequency variation; Regulate inlet amount=generation CoCO
3The output of sedimentary solution keeps reactor liquid level stabilizing 10-90cm under sieve plate; Digestion time 0.5-2.0 hour.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2005100314546A CN1297488C (en) | 2005-04-15 | 2005-04-15 | Production equipment and technique for ultramicro powder of cobalt carbonate |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2005100314546A CN1297488C (en) | 2005-04-15 | 2005-04-15 | Production equipment and technique for ultramicro powder of cobalt carbonate |
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| Publication Number | Publication Date |
|---|---|
| CN1686828A CN1686828A (en) | 2005-10-26 |
| CN1297488C true CN1297488C (en) | 2007-01-31 |
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ID=35304870
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|---|---|---|---|
| CNB2005100314546A Expired - Fee Related CN1297488C (en) | 2005-04-15 | 2005-04-15 | Production equipment and technique for ultramicro powder of cobalt carbonate |
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Families Citing this family (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100439014C (en) * | 2006-01-26 | 2008-12-03 | 湖南凯丰新材料有限公司 | Preparation method and equipment for nano-grade superfine cobalt powder |
| CN104418388B (en) * | 2013-08-26 | 2016-09-14 | 荆门市格林美新材料有限公司 | The technique of a kind of ultra-fine powder of cobalt carbonate of continuous production and device thereof |
| CN106830101A (en) * | 2017-04-01 | 2017-06-13 | 来安县万博丰环保科技有限公司 | A kind of novel ultra-fine powder of cobalt carbonate process units |
| CN110589900B (en) * | 2019-10-11 | 2021-11-16 | 合肥融捷金属科技有限公司 | Spherical cobalt carbonate production equipment and operation method thereof |
| CN113292110B (en) * | 2020-02-24 | 2023-08-15 | 荆门市格林美新材料有限公司 | Preparation method of superfine and highly dispersed spherical cobalt carbonate |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| RU2154029C2 (en) * | 1998-05-05 | 2000-08-10 | ОАО "Комбинат Североникель" Российского акционерного общества по производству цветных и драгоценных металлов | Method of preparing cobalt carbonate from chloride solution |
| CN1344682A (en) * | 2001-11-13 | 2002-04-17 | 山东大学 | Prepn of nano-cobaltosic oxide powder |
| JP2003313030A (en) * | 2002-04-23 | 2003-11-06 | Sumitomo Metal Mining Co Ltd | High tap density basic cobalt carbonate powder and method for producing the same |
| RU2240287C1 (en) * | 2003-03-17 | 2004-11-20 | Институт химии и технологии редких элементов и минерального сырья им. И.В. Тананаева Кольского научного центра Российской академии наук | Bivalent cobalt carbonate production method |
-
2005
- 2005-04-15 CN CNB2005100314546A patent/CN1297488C/en not_active Expired - Fee Related
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| RU2154029C2 (en) * | 1998-05-05 | 2000-08-10 | ОАО "Комбинат Североникель" Российского акционерного общества по производству цветных и драгоценных металлов | Method of preparing cobalt carbonate from chloride solution |
| CN1344682A (en) * | 2001-11-13 | 2002-04-17 | 山东大学 | Prepn of nano-cobaltosic oxide powder |
| JP2003313030A (en) * | 2002-04-23 | 2003-11-06 | Sumitomo Metal Mining Co Ltd | High tap density basic cobalt carbonate powder and method for producing the same |
| RU2240287C1 (en) * | 2003-03-17 | 2004-11-20 | Институт химии и технологии редких элементов и минерального сырья им. И.В. Тананаева Кольского научного центра Российской академии наук | Bivalent cobalt carbonate production method |
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