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CN101708868B - Process for rapidly producing basic nickel carbonate or basic cobaltous carbonate - Google Patents

Process for rapidly producing basic nickel carbonate or basic cobaltous carbonate Download PDF

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Publication number
CN101708868B
CN101708868B CN2009101865328A CN200910186532A CN101708868B CN 101708868 B CN101708868 B CN 101708868B CN 2009101865328 A CN2009101865328 A CN 2009101865328A CN 200910186532 A CN200910186532 A CN 200910186532A CN 101708868 B CN101708868 B CN 101708868B
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Prior art keywords
washing
dissolving
soda ash
solution
chloride
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CN101708868A (en
Inventor
刘元生
刘小平
蒋良华
汤森进
陈小娟
曾昭昆
于金刚
范金星
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Jiangxi Nuclear Industry Xingzhong Technology Co Ltd
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Jiangxi Nuclear Industry Xingzhong Technology Co Ltd
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Abstract

The invention discloses a process for rapidly producing basic nickel carbonate or basic cobaltous carbonate, comprising the following steps of: dissolving, synthetizing, filtering, water scrubbing and drying. The dissolving proportion by weight of nickel chloride or cobalt chloride in the dissolving process is NiCl2:H2O=1:4-8, CoCl2:H2O=1:4-8, and the dissolving proportion by weight of sodium carbonate is Na2CO3:H2O=1:4-8. Aqueous alkali and a nickel chloride or cobalt chloride solution are added by adopting a spray mode in the synthetic process. The synthetic reaction time is 2-4 hours. The invention not only has simple process, short production cycle, low labor intensity and arbitrary enlargement of production scale but also has simple and practicable operation, low cost, stable quality and high efficiency. The process has the characteristics of fast production, high quality of products and high efficiency; products can be turned out after water scrubbing at one time, and therefore, electricity, water, labor and time are saved. The products have even and superfine granules without crushing and sieving, thereby being beneficial to application.

Description

The quick production technique of basic nickel carbonate or cobaltous dihydroxycarbonate
Technical field
The present invention relates to the quick production technique of a kind of basic nickel carbonate or cobaltous dihydroxycarbonate.
Background technology
Basic nickel carbonate [NiCO 32Ni (OH) 24H 2O], cobaltous dihydroxycarbonate [2CoCO 33Ni (OH) 2H 2O] product is widely used in industries such as accuracy electroplate, electroplating printed circuit board, general-purpose alloy plating, nickel cobalt (alloy) electroforming, ceramic industry, commercial catalysts, and it is widely used, and demand is big.At present the enterprise of this product of domestic production is more, but quality product compares with the import like product bigger gap is arranged, and major cause is that production technique is relatively backward, exists many problems should improve and perfect.
The production technique of these two kinds of products has manual operations and semi-mechanization to produce two kinds at present.With alkali formula carbon nickel method for making is example, pass through complicated procedures of forming such as reaction, washing, filtering separation, drying, pulverizing, screening, just makes basic nickel carbonate finished product (cobaltous dihydroxycarbonate and basic nickel carbonate method for making are basic identical) at last.All more or less there is certain defective in the comprehensive production technique of each enterprise at present.Such as, wash this operation, soon 3-4 days, generally to want just can finish about a week, filtering separation also needs 1-2 days.Add drying, the operation of pulverizing, sieve, not only process cycle is long, and processing parameter be difficult for to grasp, and as drying process, because overlong time, temperature distributing disproportionation are even, causes local temperature too high, causes the product dehydration easily, influences quality product.Above-mentioned in addition explained hereafter operation labour intensity is big, and dust pollution is serious, is unfavorable for health of operators, the production cost height, and industrial scale also is subjected to the influence of production technique.
Summary of the invention
The objective of the invention is to: overcome the defective of existing basic nickel carbonate or cobaltous dihydroxycarbonate production technique, provide that a kind of technology is simple, with short production cycle, labour intensity is little and the basic nickel carbonate of constant product quality or cobaltous dihydroxycarbonate production technique.
Production technique of the present invention may further comprise the steps:
A), dissolving: starting material nickelous chloride or cobalt chloride, soda ash are put into reactor respectively and dissolved, be liquid after the dissolving;
B), synthetic: alkaline solution and nickelous chloride or cobalt chloride solution are added another reactor carry out building-up reactions, add alkaline solution earlier, after add nickelous chloride or cobalt chloride solution, and stir, control sprays and stirring velocity, the pH value of solution value transfers to 〉=7.5~9.5;
C), filter washing: the solution that building-up reactions is good is put in the sheet frame and is washed, and in the washing process, should note the water yield, about dividing, about and the centre washing of changing sides, guarantee the homogeneity of washing, the washing time is 2.5~4.5 hours, constituent contents such as sampling analysis Na, Cl after washing is finished with control washing quality, are controlled at≤the 0.01g/ liter until Na, Cl content, after washing is finished, increase to 0.8~1.6MPa again, extrude moisture content, squeezing after 30 minutes is that dismountable sheet frame takes out filter cake.
D, drying: filter cake is directly entered drying oven carry out drying, control input speed and drying temperature well, temperature controlling will be done wet degree according to filter cake, and general temperature is controlled at about 60~80 ℃.
Nickelous chloride or cobalt chloride dissolving ratio is NiCl by mass ratio in the dissolution process of technology of the present invention 2: H 2O=1: 4~8, CoCl 2: H 2O=1: 4~8, yellow soda ash dissolving ratio by mass ratio is: Na 2CO 3: H 2O=1: 4~8.
Alkaline solution and nickelous chloride or cobalt chloride solution take the spray mode to add in the building-up process of technology of the present invention.
The synthesising reacting time of technology of the present invention is 2~4 hours.
The present invention has realized the fast fast preparation method production of cover basic nickel carbonate, cobalt product.Not only production technique is simple, and is with short production cycle, and labour intensity is little, and industrial scale can enlarge arbitrarily, and operation is simple, and cost is low, steady quality, efficient height.This technology has the advantages that to produce fast, product high-quality, efficient height, washes disposablely just can go out product, compare with traditional method, and power saving, water-saving, the saving of labor saves time, and is laborsaving.Convenient, can save production cost big spoke degree.Product does not need through crushing screening, and product particle is evenly fine again, helps using.Both reduce the pollution of dust in the production, improved the protection of work again, met the requirement of modern production fully.
Embodiment
The present invention is described in detail below in conjunction with embodiment.
Embodiment 1: the basic nickel carbonate preparation
Present embodiment technology may further comprise the steps:
1, change material: nickelous chloride, yellow soda ash are put into the differential responses still respectively dissolve (abbreviationization material), be liquid after the dissolving, nickelous chloride dissolving ratio is: NiCl 2: H 2O=1: 4~8 (mass ratioes), yellow soda ash dissolving ratio is: Na 2CO 3: H 2O=1: 4~8 (mass ratioes).
2, synthetic: alkaline solution and nickel chloride solution are added another reactor carry out building-up reactions, take the spray mode to add alkaline solution earlier, after add the chlorination nickel solution, and stir, control sprays and stirring velocity, the pH value of solution value transfers to 〉=7.5~9.5; Synthesising reacting time is 2~4 hours.
3, filter washing:
Synthetic good soup compound is drawn into washes in the sheet frame, in the washing process, should note the water yield, about the branch, about and middle staggered washing, guarantee the homogeneity of washing, the washing time is 2.5~4.5 hours.Constituent contents such as sampling analysis Na, Cl after washing is finished are with control washing quality.General N a, Cl content are controlled at≤the 0.01g/ liter.After washing was finished, pressure boost was extruded moisture content again, and squeezing after 30 minutes is that dismountable sheet frame takes out filter cake.
4, drying: filter cake is directly entered drying oven carry out drying, control input speed and drying temperature well, temperature controlling will be done wet degree according to filter cake, and general temperature is controlled at about 60~80 ℃, and the size of drying oven is selected according to turnout.Should in time inspect nickel content in the analysed preparation by random samples in drying process, be strict controlled within the technical scope, operator want the parameter in the detail record production, note the rangeability of technical parameter, instruct production by the grasp of parameter.
Embodiment 2: the cobaltous dihydroxycarbonate preparation
Adopt and embodiment 1 same process mode, it comprises following processing step:
1, cobalt chloride, yellow soda ash are put into the differential responses still respectively and dissolved (abbreviationization material), be liquid after the dissolving, nickelous chloride dissolving ratio is: CoCl 2: H 2O=1: 4~8 (mass ratioes), yellow soda ash dissolving ratio is: Na 2CO 3: H 2O=1: 4~8 (mass ratioes).
2, synthetic: alkaline solution and cobalt chloride solution are added another reactor carry out building-up reactions, take the spray mode to add alkaline solution earlier, after add the chlorination cobalt liquor, and stir, control sprays and stirring velocity, the pH value of solution value transfers to 〉=7.5~9.5; Synthesising reacting time is 2~4 hours.
3, filter washing:
Synthetic good soup compound is drawn into washes in the sheet frame, in the washing process, should note the water yield, about the branch, about and middle staggered washing, guarantee the homogeneity of washing, the washing time is 2.5~4.5 hours.Constituent contents such as sampling analysis Na, Cl after washing is finished are with control washing quality.General N a, Cl content are controlled at≤the 0.01g/ liter.After washing was finished, pressure boost was extruded moisture content again, and squeezing after 30 minutes is that dismountable sheet frame takes out filter cake.
4, drying: filter cake is directly entered drying oven carry out drying, control input speed and drying temperature well, temperature controlling will be done wet degree according to filter cake, and general temperature is controlled at about 60~80 ℃, and the size of drying oven is selected according to turnout.Should in time inspect nickel content in the analysed preparation by random samples in drying process, be strict controlled within the technical scope, operator want the parameter in the detail record production, note the rangeability of technical parameter, instruct production by the grasp of parameter.
Embodiment 3: the basic nickel carbonate preparation
Nickelous chloride, yellow soda ash are separated in the molten process in the present embodiment, and nickelous chloride dissolving ratio by mass ratio is: NiCl 2: H 2O=1: 4, yellow soda ash dissolving ratio by mass ratio for being: Na 2CO 3: H 2O=1: 5, other processing step and parameter are identical with embodiment 1.
Embodiment 4, basic nickel carbonate preparation
Nickelous chloride, yellow soda ash are separated in the molten process in the present embodiment, and nickelous chloride dissolving ratio by mass ratio is: NiCl 2: H 2O=1: 8, yellow soda ash dissolving ratio by mass ratio for being: Na 2CO 3: H 2O=1: 8, other processing step and parameter are identical with embodiment 1.
Embodiment 5: the basic nickel carbonate preparation
Nickelous chloride, yellow soda ash are separated in the molten process in the present embodiment, and nickelous chloride dissolving ratio by mass ratio is: NiCl 2: H 2O=1: 7, yellow soda ash dissolving ratio by mass ratio for being: Na 2CO 3: H 2O=1: 4, other processing step and parameter are identical with embodiment 1.
Embodiment 6: the cobaltous dihydroxycarbonate preparation
Cobalt chloride, yellow soda ash are separated in the molten process in the present embodiment, and nickelous chloride dissolving ratio by mass ratio is: CoCl 2: H 2O=1: 4, yellow soda ash dissolving ratio by mass ratio for being: CoCl 2: H 2O=1: 8, other processing step and parameter are identical with embodiment 2.
Embodiment 7: the cobaltous dihydroxycarbonate preparation
Cobalt chloride, yellow soda ash are separated in the molten process in the present embodiment, and nickelous chloride dissolving ratio by mass ratio is: CoCl 2: H 2O=1: 6, yellow soda ash dissolving ratio by mass ratio for being: CoCl 2: H 2O=1: 7, other processing step and parameter are identical with embodiment 2.
Embodiment 8: the cobaltous dihydroxycarbonate preparation
Cobalt chloride, yellow soda ash are separated in the molten process in the present embodiment, and nickelous chloride dissolving ratio by mass ratio is: CoCl 2: H 2O=1: 8, yellow soda ash dissolving ratio by mass ratio is: CoCl 2: H 2O=1: 4, other processing step and parameter are identical with embodiment 2.
The basic nickel carbonate that makes by technology of the present invention, quality standard such as the following table that cobaltous dihydroxycarbonate reaches:
1, basic nickel carbonate
Project Technical specifications (%) Canonical analysis (%)
Nickel (Ni) ≥40 45
Cobalt (CO) ≤0.1000 0.0500
Iron (Fe) ≤0.0020 0.0018
Zinc (Zn) ≤0.0100 0.0050
Hydrochloric acid insoluble substance ≤0.0100 0.0050
Vitriol (SO 4) ≤0.0500 0.0100
Muriate (Cl) ≤0.0100 0.0050
Heavy metal (in Cu) ≤0.0100 0.0080
Sodium oxide (Na 2O) ≤0.1000 0.0100
Alkali and alkaline-earth metal (vitriol) ≤0.7000 0.2000
Granularity 120 orders 200 orders
2, cobaltous dihydroxycarbonate
Project Technical specifications (%) Canonical analysis (%)
Cobalt (CO) ≥46 46.5
Nickel (Ni) ≤0.05000 0.0100
Iron (Fe) ≤0.0100 0.0050
Zinc (Zn) ≤0.0500 0.0050
Hydrochloric acid insoluble substance ≤0.0200 0.0100
Vitriol (SO 4) ≤0.0500 0.0050
Muriate (Cl) ≤0.0100 0.0050
Heavy metal (in Cu) ≤0.1000 0.0100
Sodium oxide (Na 2O) ≤0.0100 0.0080
Alkali and alkaline-earth metal (vitriol) ≤0.7500 0.2000
Granularity 120 orders 150 orders

Claims (2)

1. basic nickel carbonate or the quick production technique of cobaltous dihydroxycarbonate is characterized in that: may further comprise the steps:
A), dissolving: starting material nickelous chloride or cobalt chloride, soda ash are put into reactor respectively and dissolved, be liquid after the dissolving; Nickelous chloride or cobalt chloride dissolving ratio is NiCl by mass ratio in the dissolution process 2: H 2O=1: 4~8, CoCl 2: H 2O=1: 4~8, yellow soda ash dissolving ratio by mass ratio is: Na 2CO 3: H 2O=1: 4~8;
B), synthetic: as the above-mentioned soda ash solution of dissolved and nickelous chloride or cobalt chloride solution to be added another reactor carry out building-up reactions, take the spray mode to add soda ash solution earlier, after add nickelous chloride or cobalt chloride solution, and stir, control spray and stirring velocity, the pH value of solution value transfers to 7.5~9.5;
C), filter washing: the solution that building-up reactions is good is put in the sheet frame and is washed, and in the washing process, should note the water yield, about dividing, about and the centre washing of changing sides, guarantee the homogeneity of washing, the washing time is 2.5~4.5 hours, constituent contents such as sampling analysis Na, Cl after washing is finished with control washing quality, are controlled at≤the 0.01g/ liter until Na, Cl content, after washing is finished, increase to 0.8~1.6MPa again, extrude moisture content, squeezing after 30 minutes is that dismountable sheet frame takes out filter cake;
D, drying: filter cake is directly entered drying oven carry out drying, control input speed and drying temperature well, temperature controlling will be done wet degree according to filter cake, and temperature is controlled at 60~80 ℃.
2. basic nickel carbonate according to claim 1 or the quick production technique of cobaltous dihydroxycarbonate is characterized in that: synthesising reacting time is 2~4 hours.
CN2009101865328A 2009-11-20 2009-11-20 Process for rapidly producing basic nickel carbonate or basic cobaltous carbonate Expired - Fee Related CN101708868B (en)

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US8815186B2 (en) 2009-12-18 2014-08-26 Invista North America S.A.R.L. Nickel compositions for preparing nickel metal and nickel complexes
CN103080119B (en) 2010-09-07 2015-04-08 因温斯特技术公司 Nickel compositions for preparing nickel metal and nickel complexes
JP2014523481A (en) 2011-06-10 2014-09-11 インヴィスタ テクノロジーズ エスアエルエル Firing and reduction processes involving fluidized bed reactors
CN102701293A (en) * 2012-06-13 2012-10-03 赣州逸豪优美科实业有限公司 Production method of basic cobalt carbonate
CN102923794B (en) * 2012-11-23 2015-05-20 长沙矿冶研究院有限责任公司 Method for continuously compounding high-purity alkali nickel carbonate
CN103303960B (en) * 2013-05-23 2014-12-31 东又悦(苏州)电子科技新材料有限公司 Preparation method of spherical basic cupric carbonate powder
CN104556248B (en) * 2013-10-12 2017-06-27 中国电子科技集团公司第十八研究所 The method of continuous production large granular spherical cobalt carbonate
CN106745341B (en) * 2017-01-07 2017-12-08 邵阳学院 The hydrothermal synthesis method of Carbon Dioxide nickel
KR102327114B1 (en) * 2017-03-08 2021-11-16 유미코아 Precursors of cathode materials for a rechargeable lithium ion battery
CN110194492B (en) * 2018-02-27 2021-08-06 荆门市格林美新材料有限公司 Preparation method of basic nickel carbonate
CN110203977B (en) * 2018-02-28 2021-09-10 荆门市格林美新材料有限公司 Preparation method of sodium-containing basic nickel carbonate
CN110759387A (en) * 2018-07-25 2020-02-07 荆门市格林美新材料有限公司 Preparation method of manganese-doped basic cobalt carbonate
CN110028110A (en) * 2019-05-16 2019-07-19 赣州逸豪优美科实业有限公司 A kind of technique that basic cobaltous carbonate is prepared as raw material using copper cobalt ore
TWI703095B (en) * 2019-07-03 2020-09-01 國立成功大學 Method for treating cobalt-containing wastewater by fluidized-bed crystallization
CN111892094B (en) * 2020-06-22 2024-04-12 荆门市格林美新材料有限公司 Mass production method of low-impurity high-solubility basic cobalt carbonate

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