CN1193605A - Preparation of high density and activity spherical nickle hydroxide - Google Patents
Preparation of high density and activity spherical nickle hydroxide Download PDFInfo
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- CN1193605A CN1193605A CN97100691A CN97100691A CN1193605A CN 1193605 A CN1193605 A CN 1193605A CN 97100691 A CN97100691 A CN 97100691A CN 97100691 A CN97100691 A CN 97100691A CN 1193605 A CN1193605 A CN 1193605A
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- mother liquor
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- 230000000694 effects Effects 0.000 title claims abstract description 9
- 238000002360 preparation method Methods 0.000 title claims description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 title claims description 4
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims abstract description 32
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 32
- BFDHFSHZJLFAMC-UHFFFAOYSA-L nickel(ii) hydroxide Chemical compound [OH-].[OH-].[Ni+2] BFDHFSHZJLFAMC-UHFFFAOYSA-L 0.000 claims abstract description 31
- 239000007788 liquid Substances 0.000 claims abstract description 22
- 239000002245 particle Substances 0.000 claims abstract description 22
- 229910021529 ammonia Inorganic materials 0.000 claims abstract description 16
- 238000006243 chemical reaction Methods 0.000 claims abstract description 14
- LGQLOGILCSXPEA-UHFFFAOYSA-L nickel sulfate Chemical compound [Ni+2].[O-]S([O-])(=O)=O LGQLOGILCSXPEA-UHFFFAOYSA-L 0.000 claims abstract description 12
- 229910000363 nickel(II) sulfate Inorganic materials 0.000 claims abstract description 12
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 claims abstract description 5
- 230000032683 aging Effects 0.000 claims abstract description 4
- 238000003483 aging Methods 0.000 claims abstract description 4
- 238000001035 drying Methods 0.000 claims abstract description 4
- 238000005406 washing Methods 0.000 claims abstract description 4
- 239000012452 mother liquor Substances 0.000 claims description 42
- 230000029087 digestion Effects 0.000 claims description 14
- 239000000203 mixture Substances 0.000 claims description 8
- 238000000926 separation method Methods 0.000 claims description 6
- 239000000654 additive Substances 0.000 claims description 5
- 230000000996 additive effect Effects 0.000 claims description 5
- 238000002425 crystallisation Methods 0.000 claims description 4
- 230000008025 crystallization Effects 0.000 claims description 4
- 238000003756 stirring Methods 0.000 claims description 3
- RFYUQSQGLHNNOY-UHFFFAOYSA-N cobalt;sulfuric acid Chemical compound [Co].OS(O)(=O)=O RFYUQSQGLHNNOY-UHFFFAOYSA-N 0.000 claims description 2
- HVTHJRMZXBWFNE-UHFFFAOYSA-J sodium zincate Chemical compound [OH-].[OH-].[OH-].[OH-].[Na+].[Na+].[Zn+2] HVTHJRMZXBWFNE-UHFFFAOYSA-J 0.000 claims description 2
- 239000012295 chemical reaction liquid Substances 0.000 claims 1
- 230000001143 conditioned effect Effects 0.000 claims 1
- 239000007864 aqueous solution Substances 0.000 abstract description 7
- 230000008901 benefit Effects 0.000 abstract description 3
- 238000004519 manufacturing process Methods 0.000 abstract 2
- 239000000243 solution Substances 0.000 description 18
- 238000000034 method Methods 0.000 description 10
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 7
- 230000008569 process Effects 0.000 description 7
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 description 6
- 230000000052 comparative effect Effects 0.000 description 6
- 229910052938 sodium sulfate Inorganic materials 0.000 description 6
- 235000011152 sodium sulphate Nutrition 0.000 description 6
- 239000003513 alkali Substances 0.000 description 5
- 239000010808 liquid waste Substances 0.000 description 5
- 238000005516 engineering process Methods 0.000 description 4
- 230000004907 flux Effects 0.000 description 4
- 150000002815 nickel Chemical class 0.000 description 4
- 241000220317 Rosa Species 0.000 description 3
- 229910052759 nickel Inorganic materials 0.000 description 3
- NWONKYPBYAMBJT-UHFFFAOYSA-L zinc sulfate Chemical compound [Zn+2].[O-]S([O-])(=O)=O NWONKYPBYAMBJT-UHFFFAOYSA-L 0.000 description 3
- 229910000368 zinc sulfate Inorganic materials 0.000 description 3
- 229960001763 zinc sulfate Drugs 0.000 description 3
- 235000011114 ammonium hydroxide Nutrition 0.000 description 2
- 150000003863 ammonium salts Chemical class 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 238000007599 discharging Methods 0.000 description 2
- 239000010419 fine particle Substances 0.000 description 2
- 238000003672 processing method Methods 0.000 description 2
- 239000011541 reaction mixture Substances 0.000 description 2
- 230000001105 regulatory effect Effects 0.000 description 2
- 239000002699 waste material Substances 0.000 description 2
- 240000007594 Oryza sativa Species 0.000 description 1
- 235000007164 Oryza sativa Nutrition 0.000 description 1
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 description 1
- 230000002411 adverse Effects 0.000 description 1
- OJIJEKBXJYRIBZ-UHFFFAOYSA-N cadmium nickel Chemical compound [Ni].[Cd] OJIJEKBXJYRIBZ-UHFFFAOYSA-N 0.000 description 1
- 235000013339 cereals Nutrition 0.000 description 1
- 238000005352 clarification Methods 0.000 description 1
- 238000004891 communication Methods 0.000 description 1
- 239000008139 complexing agent Substances 0.000 description 1
- 239000008367 deionised water Substances 0.000 description 1
- 229910021641 deionized water Inorganic materials 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 239000006260 foam Substances 0.000 description 1
- 230000008676 import Effects 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 239000006101 laboratory sample Substances 0.000 description 1
- 238000011068 loading method Methods 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 229910001453 nickel ion Inorganic materials 0.000 description 1
- 238000010899 nucleation Methods 0.000 description 1
- 230000006911 nucleation Effects 0.000 description 1
- 239000007774 positive electrode material Substances 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 230000004044 response Effects 0.000 description 1
- 235000009566 rice Nutrition 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
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- Battery Electrode And Active Subsutance (AREA)
- Manufacture And Refinement Of Metals (AREA)
Abstract
A process for preparing high-density, high-activity spherical nickel hydroxide used as active positive electrode of secondary alkaline accumulator features that the aqueous solution of nickel sulfate containing ammonia and ammonium and the aqueous solution of sodium hydroxide containing ammonia are continuously input to reactor, where they take part in reaction to generate nickel hydroxid particles and mother liquid, and the nickel hydroxide particles and mother liquid are discharged from reactor via own outlets. The nickel hydroxide particles go through separator by size, ageing, washing and drying, and the mother liquid is processed for reuse. Its advantages are uniform granularity, and low cost of production.
Description
The invention relates to the positive electrode active materials of secondary Edison battery--the preparation method of nickel hydroxide.
Along with the develop rapidly and the electric vehicle engineering of portable communication equipment and portable computer progressively moves towards practicability, people constantly propose higher requirement to the specific energy of secondary cells such as ni-mh, NI-G.Traditional sintered type technology for preparing electrode more and more can not satisfy this requirement.Exploitation in recent years be the specific energy that the non-sintered type technology for preparing electrode of collector has improved battery greatly with nickel foam and fiber nickel.Positive electrode active materials--nickel hydroxide has sphere for the ni-mh of non-sintered type high-energy-density and nickel-cadmium cell requirement, high-density and advantage of high activity.The more representational processing method of preparation high-density ball-shape nickel hydroxide is the scheme that JP2-6340 proposes.Its main points are: nickel salt aqueous solution, alkali aqueous solution and ammonia or ammonium salt aqueous solution import reactor respectively continuously, and reaction blended (nickel hydroxide particle and mother liquor) is discharged reactor continuously in the overflow mode, and the reaction solution pH value is 9-12, and temperature of reaction is 20-80 ℃.Reaction mixture is through solid-liquid separation, and washing and drying obtain product.The subject matter of this method is that product granularity is restive, be easy to generate two kinds of deflections: the one, more newborn nickel hydroxide fine particle is taken out of reactor by mother liquor, and the bigger particle of part may be stranded in and continues in the reactor to grow up the long period, to making Granularity Distribution wide; The 2nd, particle meeting sometimes " is grown up " synchronously, and to making product granularity excessive, density descends on the contrary.In order to overcome " growing up synchronously " problem, JP3-252318 has improved the technology that JP2-6340 proposes.Main improvement is: by periodically adjusting the method for pH value, obtain reasonably Granularity Distribution.But prepare in the processing condition of ball-shape nickel hydroxide at crystallization process, PH is one of the most responsive factor.It is not only influential to the granular size and the density of product, and its electrochemical activity is also had considerable influence.The frequent pH value of adjusting is difficult to guarantee the stable of product performance, in addition, does not all consider the multiplexing with topic of mother liquor in the above-mentioned patent.
The purpose of this invention is to provide a kind of processing method for preparing high density and activity spherical nickle hydroxide, make that the particle size distribution of product is narrow, stable performance, the mother liquor reusable cuts down the consumption of energy, and reduces liquid waste disposal amount ratio.
The present invention is achieved like this: with single nickel salt, sodium hydroxide, ammoniacal liquor or ammonium salt and a small amount of active additive (rose vitriol and zinc sulfate) are initial feed, in dissolver, be mixed with the nickel sulfate solution that contains ammonia, ammonium and additive sulfuric acid cobalt, contain the aqueous sodium hydroxide solution of ammonia and additive sodium zincate.This feed liquid is transported in the reactor continuously, and the pH value of control reaction solution and temperature of reaction and continuous the stirring make it that chemical reaction take place in reactor, and wherein nickel salt and alkali generate nickel hydroxide, and ammonia is used for regulating the degree of saturation of crossing of nickel ion as a kind of complexing agent.Under in reactor, constantly stirring, nickel hydroxide crystal process nucleation that constantly generates and the sphere and the similar spheroidal particle of growing up and forming a certain size gradually, and generate the mother liquor that mainly contains sodium sulfate simultaneously.Above-mentioned said nickel hydroxide particle and mother liquor are discharged continuously from two outlets of reactor respectively, and wherein nickel hydroxide particle enters digestion tank after hydromechanics granular size separator separates, and mother liquor also is input in the digestion tank behind the mother liquor settler.Mother liquor and nickel hydroxide mix and ageing once more in digestion tank, mixture carries out solid-liquid separation through solid-liquid separator then, obtain product after the washing of nickel hydroxide particle process, the drying, and mother liquor is removed most of sodium sulfate through crystallization, wherein 90 percent return dissolver and prepare burden, 10 handle the back through the liquid waste disposal device again discharges.The PH of above-mentioned said reactor control reaction solution is 10.00-13.00, temperature of reaction 30-70 ℃, and reaction times 5-10 hour.
Fig. 1 is a process flow sheet of the present invention.Among Fig. 1: 1 is dissolver, and 2 is reactor, and 3 is the mother liquor settler, and 4 is hydromechanics granular size separator, and 5 is digestion tank, 6 is solid-liquid separator, and 7 is washer, and 8 is moisture eliminator, and 9 is the sulfate crystal device, 10 is the liquid waste disposal device, and C is an initial feed, and A is a product, and B is a waste liquid.
Below in conjunction with Fig. 1 technical process of the present invention is described.By the continuous supply response device 2 of stock liquid of dissolver 1 preparation, the mother liquor that generates in reactor 2 is transported in the digestion tank 5 after settler 3 clarifications, and the nickel hydroxide particle that generates enters digestion tank 5 through hydromechanics granular size separator 4.Mother liquor and nickel hydroxide mix and ageing after entering digestion tank 5 respectively once more, and mother liquor and nickel hydroxide mixture carry out solid-liquid separation through solid-liquid separator 6 then.Nickel hydroxide particle becomes product A again behind washer 7 and moisture eliminator 8.After mother liquor is removed most of sodium sulfate through crystallizer 9, wherein 90 percent return dissolver 1 batching, the 10 waste liquid B dischargings after liquid waste disposal device 10 is handled again.
Through the mother liquor contains sodium sulfate 30-40 grams per liter that crystallizer 9 is handled, ammonia 0.2-0.5 mol.The nickel sulfate solution nickel concentration of mother liquor preparation is the 1.0-2.0 mol thus, and ammonia concentration is the 0.1-0.4 mol; Thus mother liquor and ammoniacal liquor the preparation alkali lye, naoh concentration is the 2-6 mol, ammonia concentration 0.2-1.5 mol.
Fig. 2 has provided reactor 2 in Fig. 1 flow process, mother liquor settler 3, hydromechanics granular size separator 4, the principle of operation figure of digestion tank 5.Among Fig. 2,2. reactor, 3. mother liquor settler, 4. hydromechanics granular size separator, 5. digestion tank, 11. nickel sulfate solutions, 12. aqueous sodium hydroxide solutions, 13. volume pumps, 14. upflow tubes.
Under steady operation conditions, enter the nickel sulfate solution 11 of reactor and the total flux of aqueous sodium hydroxide solution 12 and should equal from the total flux of upflow tube 14 effusive mother liquors and nickel hydroxide mixture.At this moment, when the mother liquid flow rate by volume pump 13 during greater than the total flux of nickel sulfate solution 11 and aqueous sodium hydroxide solution 12, partial mother liquid will be from digestion tank 5 by hydromechanics granular size separator Returning reactor 2.Mother liquor that returns and the back-setting effect of nickel hydroxide particle waterpower granular size separator of discharging have so just been caused from reactor 2, this back-setting effect is exactly the isolating hydraulic principle of granular size, and the particularly newly-generated nickel hydroxide fine particle that part is little will be taken back reactor by the mother liquor of adverse current.If adjust the flow proportional of volume pump 13 control mother liquors and nickel sulfate solution 11 and aqueous sodium hydroxide solution 12, thereby control is returned the flow velocity of mother liquor by hydromechanics granular size separator 4, just can control the size and the distribution of the nickel hydroxide particle that enters digestion tank 5.
The invention has the advantages that:
(1) owing to adopted the size and the distribution of hydraulic method control product particle, not only make the product granularity size more suitable, narrow distribution range has avoided traditional technology to control the unsettled shortcoming of product performance that product granularity may cause by adjusting pH value merely simultaneously.
(2) the present invention has adopted the flow process that mother liquor is recycled, and can effectively save starting material, and for example: the multiplexing amount of ammonia accounts for 70 percent of total consumption.Liquid waste disposal amount (generally adopting evaporative crystallization to handle) has reduced 90 percent simultaneously, can cut down the consumption of energy greatly.Therefore, the present invention has big industrial value.
Embodiment one reactor useful volume is 200 liters.
Nickel sulfate solution (before mother liquor is multiplexing): concentration of nickel sulfate is 1.7 mol, rose vitriol 0.043 mol, do not contain ammonia or ammonium, PH=2-3, the multiplexing back of mother liquor: concentration of nickel sulfate 1.7 mol, rose vitriol: 0.043 mol, ammonia and ammonium total concn 0.3 mol, sodium sulfate concentration 0.25 mol, PH=4-5,14.5 liters of flows/time.
Alkali aqueous solution (before mother liquor is multiplexing): naoh concentration 4.5 mol, zinc sulfate: 0.11 mol, ammonia concentration 1.2 mol.The multiplexing back of mother liquor: naoh concentration 4.5 mol, zinc sulfate 0.11 mol, ammonia concentration 0.8 mol, sodium sulfate concentration 0.2 mol, average discharge be about 10.5 liters/time, by regulating alkali aqueous solution flow control reaction solution PH=11.00 ± 0.02.Temperature of reaction is 50 ℃.
Mother liquor is through settler, and nickel hydroxide is discharged from reactor respectively through hydromechanics granular size separator.29 liters of mother liquid flow rates/time.
Embodiment two
Reactor effective volume: 2 meters
3The nickel sulfate solution flow: 145 liters/time, about 105 liters of flux of alkaline liquor/time, 290 liters of mother liquid flow rates/time, other conditions are with embodiment one.
Comparative example one
Mother liquor is not multiplexing.Single nickel salt and sodium hydroxide are prepared by deionized water.Composition and concentration are respectively with multiplexing each the preceding solution of mother liquor among the embodiment one.Other conditions are with embodiment one.
Comparative example two
Reaction mixture (mother liquor and nickel hydroxide) is discharged reactor from same overflow port, does not establish hydromechanics granular size tripping device.Other conditions are with embodiment two.
The size-grade distribution of above-mentioned four groups of laboratory samples and the measurement result of other performances are listed in the table 1.
Table 1
Size-grade distribution embodiment one embodiment two comparative examples one comparative example two
(differential rice) % % % %
000 3.8 40-50,0 0.1 0 2.5 30-40,1.9 2.1 1.7 4.3 20-30,3.2 3.4 4.1 8.8 15-20,12.6 11.4 13.1 14.7 10-15,32.3 26.5 34.9 33.8 8-10,36.5 35.3 32.1 12.4 6-8 10.3 15.7 11.6 10.7 4-6,0.6 0.8 0.4 2.4 average grain diameters below 3.6 5.7 3.1 6.6 4 (micron), 11.52 11.04 11.73 12.46 tap density (gram per centimeters more than 503) 2.17 2.15 2.18 2.14 loading capacities (MAH/gram)＞260＞260＞260＞260
Embodiment one, two and comparative example one contrast, mother liquor reclaims use and does not reclaim use, and product performance are basic identical, and the multiplexing product performance that do not influence of mother liquor are described.Embodiment one, two and comparative example two contrasts illustrate that the present invention adopts hydromechanics granular size lock out operation, and product particle degree distribution range obviously narrows down.
Claims (2)
1. preparation method who prepares high density and activity spherical nickle hydroxide, to contain ammonia, the nickel sulfate solution of ammonium and additive sulfuric acid cobalt, the aqueous sodium hydroxide solution that contains ammonia and additive sodium zincate is an original liquid, be transported to this feed liquid in the reactor continuously, the PH of conditioned reaction liquid and temperature of reaction in reactor, constantly stir, make it that chemical reaction take place, nickel hydroxide particle that generates and mother liquor are discharged reactor and are carried out solid-liquid separation, its nickel hydroxide particle washs, thereby the dry product that obtains, the nickel hydroxide particle and the mother liquor that it is characterized in that above-mentioned said generation are to discharge continuously from two outlets of reactor, wherein nickel hydroxide particle enters digestion tank through hydromechanics granular size separator, and mother liquor enters digestion tank through the mother liquor settler, above-mentioned nickel hydroxide and mother liquor mix and ageing in digestion tank once more, its mixture carries out solid-liquid separation, nickel hydroxide particle washing after the separation, obtain product after the drying, and mother liquor is after crystallization treatment, its mother liquor of 90 percent returns as feed liquid multiplexing, and 10 mother liquor discharges after treatment.
2. by aforesaid right requirement 1 described preparation method, it is characterized in that the PH of reaction solution in the described reactor is controlled at 10.00-13.00, temperature is controlled at 30-70 ℃.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN97100691A CN1053646C (en) | 1997-03-14 | 1997-03-14 | Preparation of high density and activity spherical nickle hydroxide |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN97100691A CN1053646C (en) | 1997-03-14 | 1997-03-14 | Preparation of high density and activity spherical nickle hydroxide |
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| Publication Number | Publication Date |
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| CN1193605A true CN1193605A (en) | 1998-09-23 |
| CN1053646C CN1053646C (en) | 2000-06-21 |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1091075C (en) * | 1998-10-21 | 2002-09-18 | 中国科学院金属腐蚀与防护研究所 | Method for producing spherical nickel hydroxide-based powder |
| CN1101341C (en) * | 1998-10-29 | 2003-02-12 | 中国科学院金属腐蚀与防护研究所 | Manufacturing equipment of spherical nickelous hydroxide series powder |
| CN100385712C (en) * | 2004-10-26 | 2008-04-30 | 深圳市比克电池有限公司 | Multicomponent metal oxide, lithium ion battery anode material and its preparing method |
| CN107623124A (en) * | 2017-09-30 | 2018-01-23 | 金驰能源材料有限公司 | A kind of preparation method of spherical nickel cobalt manganese persursor material |
| CN109205685A (en) * | 2017-07-03 | 2019-01-15 | 东莞东阳光科研发有限公司 | A kind of continuous preparation method of the nickelic ternary precursor of lithium ion battery |
| CN109574094A (en) * | 2019-01-24 | 2019-04-05 | 广东迈纳科技有限公司 | A kind of preparation method of stable particle size and its distribution nickel cobalt aluminium hydroxide |
Family Cites Families (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4244938A (en) * | 1978-11-20 | 1981-01-13 | Mooney Chemicals, Inc. | Preparation of transition metal hydrates by direct metal reaction |
| JPS6191855A (en) * | 1984-10-09 | 1986-05-09 | Matsushita Electric Ind Co Ltd | Sealed battery |
| JPS6340427A (en) * | 1986-08-06 | 1988-02-20 | Mitsubishi Electric Corp | Modulation system |
| CN1075697A (en) * | 1993-04-09 | 1993-09-01 | 河南师范大学 | Preparation method of corpuscle ball type nickel hydroxide |
| CN1107442A (en) * | 1994-02-26 | 1995-08-30 | 王维波 | Process for preparing nickel hydroxide |
| CN1037957C (en) * | 1994-05-24 | 1998-04-08 | 中国科学技术大学 | Preparation process for ultramicro particle nickel oxide |
-
1997
- 1997-03-14 CN CN97100691A patent/CN1053646C/en not_active Expired - Fee Related
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1091075C (en) * | 1998-10-21 | 2002-09-18 | 中国科学院金属腐蚀与防护研究所 | Method for producing spherical nickel hydroxide-based powder |
| CN1101341C (en) * | 1998-10-29 | 2003-02-12 | 中国科学院金属腐蚀与防护研究所 | Manufacturing equipment of spherical nickelous hydroxide series powder |
| CN100385712C (en) * | 2004-10-26 | 2008-04-30 | 深圳市比克电池有限公司 | Multicomponent metal oxide, lithium ion battery anode material and its preparing method |
| CN109205685A (en) * | 2017-07-03 | 2019-01-15 | 东莞东阳光科研发有限公司 | A kind of continuous preparation method of the nickelic ternary precursor of lithium ion battery |
| CN109205685B (en) * | 2017-07-03 | 2022-04-26 | 东莞东阳光科研发有限公司 | Continuous preparation method of high-nickel ternary precursor for lithium ion battery |
| CN107623124A (en) * | 2017-09-30 | 2018-01-23 | 金驰能源材料有限公司 | A kind of preparation method of spherical nickel cobalt manganese persursor material |
| CN107623124B (en) * | 2017-09-30 | 2020-04-07 | 金驰能源材料有限公司 | Preparation method of spherical nickel-cobalt-manganese precursor material |
| CN109574094A (en) * | 2019-01-24 | 2019-04-05 | 广东迈纳科技有限公司 | A kind of preparation method of stable particle size and its distribution nickel cobalt aluminium hydroxide |
| CN109574094B (en) * | 2019-01-24 | 2022-03-08 | 广东迈纳科技有限公司 | Preparation method of nickel-cobalt-aluminum hydroxide with stable particle size and particle size distribution |
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| CN1053646C (en) | 2000-06-21 |
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