CN1277752C - Process for preparing cobaltosic oxide powder by solid-phase catalytic oxidation of cobaltous chloride - Google Patents

Process for preparing cobaltosic oxide powder by solid-phase catalytic oxidation of cobaltous chloride Download PDF

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Publication number
CN1277752C
CN1277752C CN 200410024898 CN200410024898A CN1277752C CN 1277752 C CN1277752 C CN 1277752C CN 200410024898 CN200410024898 CN 200410024898 CN 200410024898 A CN200410024898 A CN 200410024898A CN 1277752 C CN1277752 C CN 1277752C
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co3o4
powder
cobalt chloride
technology
solid
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CN 200410024898
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CN1704340A (en
Inventor
张慧
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Tianjin Lishen Battery JSCL
Ningbo Ronbay Lithium Battery Material Co Ltd
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NINGBO JINHE NEW MATERIAL CO Ltd
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Abstract

The present invention relates to a technology for preparing Co3O4 powder by the solid-phase catalytic oxidation of cobalt chloride, which belongs to the field of fine chemical industry. The publicly known Co3O4 powder is mainly applied to the synthesis of the positive material LiCoO2 of a lithium ion battery, and has the basic requirements for Co3O4, which comprise thin granularity, high density and narrow grain size distribution. At present, the Co3O4 powder is industrially produced almost by using the liquid phase precipitation method; the liquid phase precipitation method for producing the Co3O4 powder has the disadvantages that the process is long; in the precipitation process, technological parameters, such as temperature, the pH value, staying time, stirring intensity, flow speed of a precipitating agent, etc., are too many and have poor maneuverability and repeatability. The technology of the present invention has the essential points that the technological process comprises the following steps that: cobalt chloride and a catalyst are mixed according to the compounding ratio, dried, pulverized and calcined. The technology for preparing Co3O4 powder by the solid-phase catalytic oxidation of cobalt chloride of the present invention has the advantages of short technological process, strong maneuverability of the technological parameters, high uniformity of identical batch order of products, high consistency of different batch orders and narrow grain size distribution; in addition, the granule size can be conveniently adjusted and controlled.

Description

The technology of cobaltosic oxide powder is produced in the oxidation of cobalt chloride solid catalysis
Technical field
The present invention relates to field of fine chemical, is the preparation technology that cobaltosic oxide powder is produced in the oxidation of a kind of cobalt chloride solid catalysis.
Background technology
Known cobaltosic oxide powder is mainly used in anode material for lithium-ion batteries LiCoO 2Synthetic.Fine size, density height, narrow diameter distribution are to CO 3O 4Basic demand.Present industrial production cobaltosic oxide powder adopts liquid-phase precipitation method mostly, its significant disadvantages is a long flow path, processing parameter majorities such as precipitation process temperature, pH value, the residence time, stirring intensity, precipitation agent flow velocity and controllability, poor reproducibility, the cobaltosic oxide powder density of producing is little, size distribution is wide, and batch the homogeneity and the consistence of different batches can not effectively guarantee together.
Summary of the invention
The objective of the invention is to overcome existing technology shortcoming, propose that a kind of flow process is brief, processing parameter is few and controllability is strong, product evenly reaches high conformity, narrow diameter distribution, globule size be the production technique of conveniently regulating and controlling, is the technology that cobaltosic oxide powder is produced in the oxidation of a kind of cobalt chloride solid catalysis.
The technology of cobaltosic oxide powder is produced in cobalt chloride solid catalysis of the present invention oxidation, may further comprise the steps:
1), batching cobalt chloride, catalyzer mix by 100: 0.5～2.5 (weight ratio) proportioning.Described catalyzer is NH 4Cl, NH 4NO3, CH 3-(CH 2) 17NH 2In a kind of or its mixture;
2), dry with 1) batching in the step dries under 100～120 ℃ of temperature;
3), pulverize will prepare burden 2) in material after drying be crushed to 60 orders;
4), calcining will go on foot and gather 3) pyrolysis in calcining of gained powder, 350～450 ℃, 2～4 hours.
The production technique of working out by the present invention has that flow process is short, unfavorable factor is easy to control, quality product is good, cost is relatively low, adapts to produce in enormous quantities.
Embodiment
Embodiment one, takes by weighing cobalt chloride (COCl respectively 26H 2O) 3000 grams, NH 4The Cl30 gram mixes it, dries under 100～120 ℃ of temperature, and again that drying is good material is crushed to 60 orders, then with the pyrolysis in calcining furnace of gained powder, 350～450 ℃, 3 hours.Gained cobaltosic oxide particle diameter is normal distribution, d 509.0 μ m, loose density 1.10g/cm 3
Embodiment two, take by weighing cobalt chloride (COCl respectively 26H 2O) 3000 grams, NH 4The Cl75 gram mixes it, dries under 100～120 ℃ of temperature, and again that drying is good material is crushed to 60 orders, then with the pyrolysis in calcining furnace of gained powder, 350～450 ℃, 3 hours.Gained cobaltosic oxide particle diameter is normal distribution, d 505.8 μ m, loose density 0.75g/cm 3
Embodiment three, take by weighing cobalt chloride (COCl respectively 26H 2O) 3000 grams, NH 4The Cl60 gram mixes it, dries under 100～120 ℃ of temperature, and again that drying is good material is crushed to 60 orders, then with the pyrolysis in calcining furnace of gained powder, 350～450 ℃, 3 hours.Gained cobaltosic oxide particle diameter is normal distribution, d 507.0 μ m, loose density 0.90g/cm 3
Example example four takes by weighing cobalt chloride (COCl respectively 26H 2O) 3000 grams, NH 4The Cl30 gram, NH 4NO 330 grams, CH 3-(CH 2) 17NH 215 grams mix it, dry under 100～120 ℃ of temperature, again the exsiccant material are crushed to 60 orders, then with the pyrolysis in calcining furnace of gained powder, 350～450 ℃, 3 hours.Gained cobaltosic oxide particle diameter is normal distribution, d 505.0 μ m, loose density 0.69g/cm 3
The comparative example, electrolytic metal cobalt nitric acid dissolve, cobalt contents 160g/l, free acid 10g/l; With the boiling deionized water oxalic acid is dissolved, proportion 1.04 adds ammoniacal liquor and transfers PH4.5,70 ℃ of temperature; 45 ℃ of cobalt nitrate solution temperature slowly add oxalic acid ammonia in the stirring, and final PH1.0 continues to stir 20 minutes; Filter and with seething with excitement deionized water wash 8 times, 400 ℃ of roastings 5 hours are sieved.Gained cobaltosic oxide powder size distribution abnormal, loose density 0.40g/cm 3

Claims (1)

1, the technology of cobaltosic oxide powder is produced in the oxidation of a kind of cobalt chloride solid catalysis, it is characterized in that this technology may further comprise the steps:
1), batching cobalt chloride, catalyzer mix by 100: 0.5～2.5 (weight ratio) proportioning, described catalyzer is NH 4Cl, NH 4NO 3, CH 3-(CH 2) 17NH 2In a kind of or its mixture;
2), drying is dried the batching of step 1) under 100～120 ℃ of temperature;
3), pulverize will prepare burden 2) dried material of drying is crushed to 60 orders;
4), calcining will go on foot and gather 3) pyrolysis in calcining of gained powder, 350～450 ℃, 2～4 hours.
CN 200410024898 2004-06-03 2004-06-03 Process for preparing cobaltosic oxide powder by solid-phase catalytic oxidation of cobaltous chloride Active CN1277752C (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN 200410024898 CN1277752C (en) 2004-06-03 2004-06-03 Process for preparing cobaltosic oxide powder by solid-phase catalytic oxidation of cobaltous chloride

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN 200410024898 CN1277752C (en) 2004-06-03 2004-06-03 Process for preparing cobaltosic oxide powder by solid-phase catalytic oxidation of cobaltous chloride

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CN1704340A CN1704340A (en) 2005-12-07
CN1277752C true CN1277752C (en) 2006-10-04

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102978419B (en) * 2012-12-17 2014-06-18 江西稀有稀土金属钨业集团有限公司 Electrically-heating and integrally-rotating resistance furnace capable of sintering anhydrous cobalt chloride into cobalt oxide product

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Assignee: NINGBO COBOTO COBALT & NICKEL Co.,Ltd.

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Denomination of invention: Process for preparing cobaltosic oxide powder by solid-phase catalytic oxidation of cobaltous chloride

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