CN102154549B - Production method for high-purity hard-agglomeration-free superfine nickel oxide or cobalt and nickel or cobalt powder - Google Patents
Production method for high-purity hard-agglomeration-free superfine nickel oxide or cobalt and nickel or cobalt powder Download PDFInfo
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Abstract
The invention discloses a production method for high-purity hard-agglomeration-free superfine nickel oxide or cobalt and nickel or cobalt powder; the production method comprises the following steps of: adopting P204 and P507 to extract nickel nitrate, adopting P204 to extract cobalt nitrate, adding addition agents A and B, and sodium hydroxide into a nickel nitrate solution or a nickel nitrate solution for reaction under a temperature of 80 to 100 DEG C, freezing, drying and smashing washed or filtered nickel hydroxide or cobalt filter cake which is reduced into nickel or cobalt powder in a hydrogen furnace; or roasting the washed or filtered nickel hydroxide or cobalt filter cake in a calcining kiln so as to obtain nickel oxide or cobalt powder; the nickel oxide or cobalt powder is free of hard-agglomeration, the D50 is 2 to 3 microns, the content of purities is 20 to 100ppm, and the cost is low; a production system mainly adopting China patents of ''an exhaust gas absorption device for nitrate production'', ''an inorganic salt precipitate continuous washing machine '', ''a drying and grinding all-in-one machine'', ''an inorganic salt uniform roasting rotary kiln'' and a continuous production method can increase quality and production efficiency and reduces cost and environmental pollution.
Description
Technical field
The invention belongs to chemical field, exactly is production method and the production system and the continuous producing method of ultra-fine nickel oxide of high-purity hard aggregation-free or cobalt and nickel or cobalt powder.
Background technology
In the last few years; Continuous development and progress along with science and technology; Chemical industry, electronics, metallurgical increasing to the demand of nickel oxide (cobalt) and nickel (cobalt) powder; And it is also more and more harsher to its quality requirement; By existing national standard production, satisfied not on the market nickel oxide (cobalt) and the requirement of nickel (cobalt) opaque amount, ultra-fine nickel (cobalt) powder has great bulk effect and skin effect; Demonstrate many special nature at aspects such as magnetic, interior pressure, thermal resistance, light absorption, chemisms, having a wide range of applications aspect catalyst, sintering activator, conductive slurry, battery, carbide alloy, production electrodes in base metal multilayer ceramic capacitor (BME--MLCC) or the like.In addition, ultra-fine nickel (cobalt) powder also is widely used at porous material, chiral material, sprayed on material, nano compound electroplating material and at aspects such as improving the lubricating oil friction and wear behavior.
At present, produce ultra-fine nickel (cobalt) powder method and have following several kinds:
1, carbonyl nickel (cobalt) thermal decomposition method: this method technology is simple, and cost is low, and powder purity is high; But the powder easy-sintering, size distribution is wide, and crystallinity is poor, and carbonyl nickel (cobalt) has severe toxicity, is prone to pollute, and needs strict safety precaution.
2, evaporation-condensation method: nickel (cobalt) the powder purity of producing with this method is high, good crystallinity, and mass color is clean, and oxidation resistance is strong; But complex equipments, production efficiency is low, and cost is high.
3, gamma-rays radiation synthetic method: advantage is that industry degree narrowly distributing oxidation resistance is strong, but at present technology that is that all right is ripe.
4, CVD method: advantage is that powder is regular sphere, even particle size distribution, controlled amount, good crystallinity, powder activity height and heat-shrinkable is low; But reactor is designed with specific (special) requirements.
5, High Pressure Hydrogen reducing process: simple to operate, raw material is extensive, and powder size is little; But need high-tension apparatus, cost is high.
6, liquid phase reduction: high simple operations is easy fully, pattern, controllable granularity; The bad easy thermal contraction of crystallinity.
7, microemulsion method: pattern is good, is evenly distributed, and particle diameter is controlled; But productive rate is low, and cost is high, and powder crystallization is bad, is prone to thermal contraction.
8, ultrasonic atomizatio-thermal decomposition method: target component is prone to control, and the predecessor pattern that is easy to get is controlled; But it is wide that powder size distributes, exhaust-gas treatment difficulty after the thermal decomposition.
9, argon shield mechanical ball milling: but continued operation, and production capacity is bigger; But size distribution is inhomogeneous, the difficult control of pattern.
10, electrolysis: pattern and size are easily by Current Control: powder is thicker, and energy consumption is high.
Ultra-fine (nanometer) nickel (cobalt) powder of producing in batches on the international market at present mainly contains the expert on Japan and crosses chemical vapour deposition technique; Canada is through carbonyl nickel (cobalt) decomposition method; And the evaporation-condensation method of U.S. Quantumsphere Inc. (QuantumSphere) and ningbo of china employing; These method production equipments are complicated, cost is high, cause ultra-fine (nanometer) nickel (cobalt) powder per kilogram price on the present international market about 1200 dollars.
Summary of the invention
The purpose of this invention is to provide the production method of ultra-fine nickel of a kind of high-purity hard aggregation-free or cobalt powder and nickel oxide or cobalt, this method comprises:
1) nickel nitrate adopts P204, P507 extraction, and cobalt nitrate extracts with P204, with highly purified nickel nitrate of 60g-100g/L or cobalt liquor, heats 80-100 ℃, is added in the agitated reactor, by per 1 * 10
3L nickel nitrate or cobalt liquor, doping A 14-16 kilogram stirs, and described additive A is by the ratio preparation in by volume 1: 1: 1 of acetone, hexylene glycol, alcohol;
2) add the 7-10g/L additive B again; Addition is nickel nitrate or cobalt liquor volume 2 times; Described additive B is by the ratio preparation in 1: 1: 1 by weight of urea, amine carbonate, ammoniacal liquor, and the concentration of ammoniacal liquor is 20-25%, stirs while adding; Added in 40-60 minute, the temperature of agitated reactor remains on 80-100 ℃;
3) add 40-60g/L sodium hydroxide solution with the additive B equal volume again, stir while adding, added in 40-60 minute, keep 80-100 ℃ of temperature, continue to keep temperature to stir 3 hours;
4) washing, filtration get nickel hydroxide or cobalt filter cake;
5) freezing nickel hydroxide of refrigerator or cobalt filter cake are to icing the knot state;
6) drying and crushing gets high pure and ultra-fine nickel hydroxide or cobalt dust;
7) high pure and ultra-fine nickel hydroxide or cobalt dust are reduced to high pure and ultra-fine nickel or cobalt powder in hydrogen reduction furnace; Or get high pure and ultra-fine nickel oxide or cobalt powder at the roasting roasting in kilns;
The described drying and crushing of step 6) adopts the drying and crushing all-in-one, notification number: CN201413016 drying and crushing;
Described highly purified nickel nitrate or cobalt liquor are 70g-80g/L; Doping A 14-15 kilogram, additive B is 7-8g/L;
Preferred highly purified nickel nitrate or cobalt liquor are 70g/L; 14 kilograms of doping A, additive B are 7g/L; Sodium hydroxide solution is 40g/L;
Described nickel nitrate or cobalt liquor adopt band " to produce the exhaust gas absorption device of nitrate " with metallic nickel or cobalt and salpeter solution, and the consersion unit of CN201410354 is produced;
Be preferably: in the reaction of hydro-oxidation sodium, and continue to keep temperature to stir after 3 hours, adopt inorganic salt precipitates continous way rinsing maching; Notification number: CN201454169U after the washing, adds water with nickel hydroxide or cobalt pulp; Pass through the plate and frame filter press press filtration again, get nickel hydroxide or cobalt filter cake, freezing nickel hydroxide of refrigerator or cobalt filter cake are to icing the knot state; Or outdoor temperature is freezed outdoor below-10 ℃ the time; Inorganic salt uniform calcination rotary kiln, notification number: CN201289292 are adopted in roasting.
Another object of the present invention provides the production system of the ultra-fine nickel oxide of high-purity hard aggregation-free or cobalt powder and nickel or cobalt powder; It comprises: agitated reactor 1, agitated reactor 2, agitated reactor 3, agitated reactor 4, inorganic salt precipitates continous way rinsing maching; Notification number: CN201454169U, nickel hydroxide or cobalt pulp device, plate and frame filter press, freezing equipment, drying and crushing all-in-one; Publication number: CN201413016 and a kind of inorganic salt uniform calcination rotary kiln, notification number: CN201289292 or hydrogen reduction furnace; Described agitated reactor 1, agitated reactor 2, agitated reactor 3, agitated reactor 4 are equipped with overflow pipe; Link to each other with agitated reactor 2 through overflow pipe in the agitated reactor 1; Link to each other with agitated reactor 3 through overflow pipe in the agitated reactor 2; Link to each other with agitated reactor 4 through overflow pipe in the agitated reactor 3, the overflow pipe of agitated reactor 4 links to each other with inorganic salt precipitates continous way rinsing maching charging aperture.
Another object of the present invention provides the continuous producing method of the ultra-fine nickel oxide of high-purity hard aggregation-free or cobalt powder and nickel or cobalt powder, and it comprises:
1) after nickel nitrate adopted P204, P507 extraction or cobalt nitrate with the P204 extraction, compound concentration was 60g-100g/L, by per 1 * 10
3L nickel nitrate or cobalt liquor; Doping A 14-16 kilogram, and in the continuous adding of the stream agitated reactor 1, stir while adding; Overall flow rate is 1-2.5L/min; The temperature of agitated reactor remains on 80-100 ℃, and described additive A is by by volume 1: 1: 1 ratio of acetone, hexylene glycol, alcohol, temperature 50-100 ℃ of preparation;
When overflowing to agitated reactor 2 after 2) question response still 1 is filled it up with; And the stream adding 7-10g/L additive B aqueous solution, flow velocity is 2-5L/min, stirs; Described additive B is by urea, amine carbonate, ammoniacal liquor ratio preparation in 1: 1: 1 by weight, and the concentration of ammoniacal liquor is 20-25%;
When overflowing to agitated reactor 3 after 3) question response still 2 is filled it up with, and stream adding 40-60g/L sodium hydroxide solution, stirring, flow velocity is 2-5L/min, agitated reactor 3 is filled it up with in the back overflow agitated reactor 4;
The molten long-pending of described agitated reactor 1,2,3,4 is 5 * 10
3L; Reaction temperature all remains on 80-100 ℃;
4) in agitated reactor 4, continue to stir, after stream is full, overflows in the inorganic salt precipitates continous way rinsing maching and wash;
5) behind the nickel hydroxide or cobalt pulp after will washing, the plate and frame filter press press filtration becomes filter cake;
6) filter cake is refrigerated to freeze all; The drying and crushing all-in-one is pulverized dry; Get high pure and ultra-fine nickel hydroxide or cobalt dust;
7) high pure and ultra-fine nickel hydroxide or cobalt dust are reduced to high pure and ultra-fine nickel or cobalt powder in hydrogen reduction furnace, or roasting in a kind of inorganic salt uniform calcination rotary kiln, high pure and ultra-fine nickel oxide or cobalt powder got.
The production method of ultra-fine nickel oxide of high-purity hard aggregation-free provided by the invention or cobalt and nickel or cobalt powder, nickel nitrate adopt P204, P507 extraction, and cobalt nitrate extracts with P204; With highly purified nickel nitrate of 60g-100g/L or cobalt liquor, under 80-100 ℃ of temperature, doping A, B, NaOH react; Nickel hydroxide or cobalt filter cake after washing, the filtration; Carry out freezingly again, drying and crushing is reduced to high pure and ultra-fine nickel or cobalt powder in hydrogen reduction furnace; Or get high pure and ultra-fine nickel oxide or cobalt powder at the roasting roasting in kilns; Do not have hard aggregation, D50 is the 2-3 micron, and impurity content is 20-100ppm, and cost is low.
Adopt Chinese patent " to produce the exhaust gas absorption device of nitrate "; " inorganic salt precipitates continous way rinsing maching "; " drying and crushing all-in-one ", " a kind of inorganic salt uniform calcination rotary kiln " are high pure and ultra-fine nickel oxide or the production system of cobalt powder and nickel or cobalt powder and the continuous producing method of high pure and ultra-fine nickel oxide or cobalt powder and nickel or cobalt powder of capital equipment, can improve the quality and the production efficiency of product; Reduce cost, reduce environmental pollution.
Description of drawings
Figure is the continuous process system sketch map of the ultra-fine nickel oxide of the high-purity hard aggregation-free of the present invention or cobalt powder and nickel or cobalt powder.
The specific embodiment
Embodiment 1 highly purified nickel nitrate or cobalt liquor preparation
With metallic nickel or cobalt and salpeter solution, adopt Chinese patent, " producing the exhaust gas absorption device of nitrate ", the consersion unit of CN201410354 is produced, and realizes pollution-free environmental protection production nickel nitrate or cobalt liquor; Concentration is the nickel nitrate solution of 50-190g/L, adopts metal impurities, P507 abstraction impurity removal matter such as P204 extraction copper removal, lead, zinc, manganese, or cobalt nitrate solution employing P204 extraction, obtains highly purified nickel nitrate or cobalt liquor.
The production method of the embodiment ultra-fine nickel of 2 high-purity hard aggregation-frees or cobalt powder and nickel oxide or cobalt
1) with highly purified nickel nitrate of 60g-100g/L or cobalt liquor, heat 80-100 ℃, be added in the agitated reactor, by per 1 * 10
3L nickel nitrate or cobalt liquor, doping A 14-16 kilogram stirs, and described additive A is by by volume 1: 1: 1 ratio of acetone, hexylene glycol, alcohol, temperature 50-100 ℃ of preparation;
2) add the 7-10g/L additive B again; Addition is nickel nitrate or cobalt liquor volume 2 times; Described additive B is by the ratio preparation in 1: 1: 1 by weight of urea, amine carbonate, ammoniacal liquor, and the concentration of ammoniacal liquor is 20-25%, stirs while adding; Added in 40-60 minute, the temperature of agitated reactor remains on 80-100 ℃;
3) add again and add the 40-60g/L sodium hydroxide solution of B equal volume, stir while adding, added in 40-60 minute, keep 80-100 ℃ of temperature, continue to keep temperature stirring 3 hours;
4) washing, filtration get nickel hydroxide or cobalt filter cake;
5) freezing nickel hydroxide of refrigerator or cobalt filter cake are to icing the knot state;
6) drying and crushing gets high pure and ultra-fine nickel hydroxide or cobalt dust;
7) high pure and ultra-fine nickel hydroxide or cobalt dust are reduced to high pure and ultra-fine nickel or cobalt powder in hydrogen reduction furnace.Or get high pure and ultra-fine nickel oxide or cobalt powder at the roasting roasting in kilns.
The production method of the embodiment ultra-fine nickel of 3 high-purity hard aggregation-frees or cobalt powder or nickel oxide or cobalt
1) with highly purified nickel nitrate of 70g-80g/L or cobalt liquor, heat 80-100 ℃, be added in the agitated reactor, by per 1 * 10
3L nickel nitrate or cobalt liquor, doping A 14-15 kilogram stirs, and described additive A is by by volume 1: 1: 1 ratio of acetone, hexylene glycol, alcohol, temperature 50-100 ℃ of preparation;
2) add the 7-8g/L additive B again; Addition is nickel nitrate or cobalt liquor volume 2 times; Described additive B is by the ratio preparation in 1: 1: 1 by weight of urea, amine carbonate, ammoniacal liquor, and the concentration of ammoniacal liquor is 20-25%, stirs while adding; Added in 40-60 minute, the temperature of agitated reactor remains on 80-100 ℃;
3) add again and add the 40-60g/L sodium hydroxide solution of B equal volume, stir while adding, added in 40-60 minute, keep 80-100 ℃ of temperature, continue to keep temperature stirring 3 hours;
4) washing, filtration get nickel hydroxide or cobalt filter cake;
5) freezing nickel hydroxide of refrigerator or cobalt filter cake are to icing the knot state;
6) drying and crushing gets high pure and ultra-fine nickel hydroxide or cobalt dust;
7) high pure and ultra-fine nickel hydroxide or cobalt dust are reduced to high pure and ultra-fine nickel or cobalt powder in hydrogen reduction furnace.Or get high pure and ultra-fine nickel oxide or cobalt powder at the roasting roasting in kilns.
The production method of the embodiment ultra-fine nickel of 4 high-purity hard aggregation-frees or cobalt powder or nickel oxide or cobalt
1) with highly purified nickel nitrate of 60g/L or cobalt liquor, heat 80 ℃, be added in the agitated reactor, by per 1 * 10
3L nickel nitrate or cobalt liquor, 15 kilograms of doping A stir, and described additive A is by by volume 1: 1: 1 ratio of interior ketone, hexylene glycol, alcohol, temperature 50-100 ℃ of preparation;
2) add the 7g/L additive B again; Addition is nickel nitrate or cobalt liquor volume 2 times; Described additive B is by the ratio preparation in 1: 1: 1 by weight of urea, amine carbonate, ammoniacal liquor, and the concentration of ammoniacal liquor is 20-25%, stirs while adding; Added in 40-60 minute, the temperature of agitated reactor remains on 80 ℃;
3) add again and add the 40g/L sodium hydroxide solution of B equal volume, stir while adding, added in 40 minutes, keep 80 ℃ of temperature, continue to keep temperature stirring 3 hours;
4) washing, filtration get nickel hydroxide or cobalt filter cake;
5) freezing nickel hydroxide of refrigerator or cobalt filter cake are to icing the knot state;
6) drying and crushing gets high pure and ultra-fine nickel hydroxide or cobalt dust;
7) high pure and ultra-fine nickel hydroxide or cobalt dust are reduced to high pure and ultra-fine nickel or cobalt powder in hydrogen reduction furnace.Or get high pure and ultra-fine nickel oxide or cobalt powder at the roasting roasting in kilns.
The production method of the embodiment ultra-fine nickel of 5 high-purity hard aggregation-frees or cobalt powder or nickel oxide or cobalt
The reaction of hydro-oxidation sodium, and continue to keep temperature to stir after 3 hours, adopt the inorganic salt precipitates continous way rinsing maching of inventor's invention; Notification number: CN201454169U after the washing, adds water with nickel hydroxide or cobalt pulp; Pass through the plate and frame filter press press filtration again, nickel hydroxide or cobalt filter cake, freezing nickel hydroxide of refrigerator or cobalt filter cake are after ice the knot state; Or outdoor temperature after outdoor freezing, adopts the drying and crushing all-in-one of inventor's invention below-10 ℃ the time; Notification number: CN201413016, pure high pure and ultra-fine nickel hydroxide or the cobalt dust of getting of xeraphium, the inorganic salt uniform calcination rotary kiln of inventor's invention is adopted in roasting; Notification number: CN201289292, other is with embodiment 2,3 or 4.
The production system of the embodiment ultra-fine nickel oxide of 6 high-purity hard aggregation-frees or cobalt powder and nickel or cobalt powder
Referring to accompanying drawing; The production system of high pure and ultra-fine nickel oxide or cobalt powder and nickel or cobalt powder; It comprises: agitated reactor 1, agitated reactor 2, agitated reactor 3, agitated reactor 4, inorganic salt precipitates continous way rinsing maching (notification number: CN201454169U), nickel hydroxide or cobalt pulp device, plate and frame filter press, freezing equipment, drying and crushing all-in-one (publication number: CN201413016) and a kind of inorganic salt uniform calcination rotary kiln, notification number: CN201289292 or hydrogen reduction furnace; Described agitated reactor 1, agitated reactor 2, agitated reactor 3, agitated reactor 4 are equipped with overflow pipe; Link to each other with agitated reactor 2 through overflow pipe in the agitated reactor 1; Link to each other with agitated reactor 3 through overflow pipe in the agitated reactor 2; Link to each other with agitated reactor 4 through overflow pipe in the agitated reactor 3, the overflow pipe of agitated reactor 4 links to each other with inorganic salt precipitates continous way rinsing maching charging aperture;
The continuous producing method of the embodiment ultra-fine nickel oxide of 7 high-purity hard aggregation-frees or cobalt powder and nickel or cobalt powder
Referring to accompanying drawing.
1) highly purified nickel nitrate (cobalt) solution that embodiment 1 is made, compound concentration is 60g-100g/L, by per 1 * 10
3L nickel nitrate (cobalt) solution, doping A 14-16 kilogram, and stream adds in the agitated reactor 1; Stir while adding; Overall flow rate is 1-2.5L/min, and the temperature of agitated reactor remains on 80-100 ℃, and described additive A is by volume to be prepared in 1: 1: 1 ratio by acetone, hexylene glycol, alcohol; The volume of described agitated reactor 1 is 5 * 10
3L;
When overflowing to agitated reactor 2 after 2) question response still 1 is filled it up with; And stream adds the 7-10g/L additive B aqueous solution; Flow velocity is 2-5L/min, stirs, and described additive B is by urea, amine carbonate, ammoniacal liquor ratio preparation in 1: 1: 1 by weight by weight; The concentration of ammoniacal liquor is 20-25%, and it is 5 * 10 that agitated reactor 2 dissolves long-pending
3L;
When overflowing to agitated reactor 3 after 3) question response still 2 is filled it up with, and stream adding 40-60g/L sodium hydroxide solution, stirring, flow velocity is 2-5L/min, and agitated reactor 3 is filled it up with in the back overflow agitated reactor 4, and the molten long-pending of described agitated reactor 4 is 5 * 10
3L; Reaction temperature all remains on 80-100 ℃;
4) in agitated reactor 4, continue to stir, after stream is full, overflows in the inorganic salt precipitates continous way rinsing maching and wash;
5) behind the nickel hydroxide or cobalt pulp after will washing, the plate and frame filter press press filtration becomes filter cake;
6) filter cake is refrigerated to freeze all; The drying and crushing all-in-one is pulverized dry; Get high pure and ultra-fine nickel hydroxide or cobalt dust;
7) high pure and ultra-fine nickel hydroxide or cobalt dust are reduced to high pure and ultra-fine nickel or cobalt powder in hydrogen reduction furnace, or roasting in a kind of inorganic salt uniform calcination rotary kiln, high pure and ultra-fine nickel oxide or cobalt powder got.
The ultra-fine nickel hydroxide of high-purity hard aggregation-free or cobalt dust, the ultra-fine nickel of high-purity hard aggregation-free or cobalt powder, high pure and ultra-fine nickel oxide or cobalt powder that above-mentioned each embodiment produces do not have hard aggregation, and D50 is the 2-3 micron.
Claims (6)
1. the production method of high-purity hard aggregation-free extra-fine nickel powder or cobalt powder, this method comprises:
1) nickel nitrate adopts P204, P507 extraction, or cobalt nitrate extracts with P204, with highly purified nickel nitrate of 60g-100g/L or cobalt nitrate solution, heat 80-100 ℃, is added in the agitated reactor, presses per 1 * 10
3L nickel nitrate or cobalt nitrate solution, doping A 14-16 kilogram stirs, and described additive A is by by volume 1: 1: 1 ratio of acetone, hexylene glycol, alcohol, temperature 50-100 ℃ of preparation;
2) add 7-10 g/L additive B again; Addition is nickel nitrate or cobalt nitrate solution volume 2 times; Described additive B is by the ratio preparation in 1: 1: 1 by weight of urea, ammonium carbonate, ammoniacal liquor, and the concentration of ammoniacal liquor is 20-25%, stirs while adding; Added in 40-60 minute, the temperature of agitated reactor remains on 80-100 ℃;
3) add 40-60 g/L sodium hydroxide solution with the additive B equal volume again, stir while adding, added in 40-60 minute, keep 80-100 ℃ of temperature, continue to keep temperature to stir 3 hours;
4) washing, filtration get nickel hydroxide filter cake or cobalt hydroxide filter cake;
5) freezing nickel hydroxide filter cake of refrigerator or cobalt hydroxide filter cake are to icing the knot state;
6) drying and crushing gets high pure and ultra-fine nickel hydroxide powder or cobalt hydroxide powder;
7) high pure and ultra-fine nickel hydroxide powder or cobalt hydroxide powder are reduced to high-purity hard aggregation-free extra-fine nickel powder or cobalt powder in hydrogen reduction furnace.
2. the production method of ultra-fine nickel oxide powder of high-purity hard aggregation-free or cobalt oxide powder, this method comprises:
1) nickel nitrate adopts P204, P507 extraction, or cobalt nitrate extracts with P204, with highly purified nickel nitrate of 60g-100g/L or cobalt nitrate solution, heat 80-100 ℃, is added in the agitated reactor, presses per 1 * 10
3L nickel nitrate or cobalt nitrate solution, doping A 14-16 kilogram stirs, and described additive A is by by volume 1: 1: 1 ratio of acetone, hexylene glycol, alcohol, temperature 50-100 ℃ of preparation;
2) add 7-10 g/L additive B again; Addition is nickel nitrate or cobalt nitrate solution volume 2 times; Described additive B is by the ratio preparation in 1: 1: 1 by weight of urea, ammonium carbonate, ammoniacal liquor, and the concentration of ammoniacal liquor is 20-25%, stirs while adding; Added in 40-60 minute, the temperature of agitated reactor remains on 80-100 ℃;
3) add 40-60 g/L sodium hydroxide solution with the additive B equal volume again, stir while adding, added in 40-60 minute, keep 80-100 ℃ of temperature, continue to keep temperature to stir 3 hours;
4) washing, filtration get nickel hydroxide filter cake or cobalt hydroxide filter cake;
5) freezing nickel hydroxide filter cake of refrigerator or cobalt hydroxide filter cake are to icing the knot state;
6) drying and crushing gets high pure and ultra-fine nickel hydroxide powder or cobalt hydroxide powder;
7) high pure and ultra-fine nickel hydroxide powder or cobalt hydroxide powder are got ultra-fine nickel oxide powder of high-purity hard aggregation-free or cobalt oxide powder at the roasting roasting in kilns.
3. production method according to claim 1 and 2 is characterized in that: said highly purified nickel nitrate or cobalt nitrate solution are 70g-80g/L; Doping A 14-15 kilogram, additive B is 7-8 g/L.
4. production method according to claim 1 and 2 is characterized in that: said highly purified nickel nitrate or cobalt nitrate solution are 70g/L; 14 kilograms of doping A, additive B are 7 g/L; Sodium hydroxide solution is 40 g/L.
5. the continuous producing method of ultra-fine nickel oxide powder of high-purity hard aggregation-free or cobalt oxide powder, it comprises:
1) nickel nitrate adopts P204, P507 extraction, and after cobalt nitrate extracted with P204, compound concentration was 60g-100g/L, by per 1 * 10
3L nickel nitrate or cobalt nitrate solution; Doping A 14-16 kilogram; And in the continuous adding of the stream agitated reactor 1, stir while adding, overall flow rate is 1-2.5L/min; The temperature of agitated reactor remains on 80-100 ℃, and described additive A is by the ratio preparation in by volume 1: 1: 1 of acetone, hexylene glycol, alcohol;
When overflowing to agitated reactor 2 after 2) question response still 1 is filled it up with; And the stream adding 7-10 g/L additive B aqueous solution, flow velocity is 2-5L/min, stirs; Described additive B is by the ratio preparation in 1: 1: 1 by weight of urea, ammonium carbonate, ammoniacal liquor, and the concentration of ammoniacal liquor is 20-25%;
When overflowing to agitated reactor 3 after 3) question response still 2 is filled it up with, and stream adding 40-60 g/L sodium hydroxide solution, stirring, flow velocity is 2-5L/min, agitated reactor 3 is filled it up with in the back overflow agitated reactor 4;
The molten long-pending of described agitated reactor 1,2,3,4 is 5 * 10
3L; Reaction temperature all remains on 80-100 ℃;
4) in agitated reactor 4, continue to stir, after stream is full, overflows in the inorganic salt precipitates continous way rinsing maching and wash;
5) behind the nickel hydroxide or cobalt hydroxide pulp after will washing, the plate and frame filter press press filtration becomes filter cake;
6) filter cake is refrigerated to freeze all; The drying and crushing all-in-one is pulverized dry; Get high pure and ultra-fine nickel hydroxide powder or cobalt hydroxide powder;
7), get ultra-fine nickel oxide powder of high-purity hard aggregation-free or cobalt oxide powder with high pure and ultra-fine nickel hydroxide powder or the roasting in a kind of inorganic salt uniform calcination rotary kiln of cobalt hydroxide powder.
6. the continuous producing method of high-purity hard aggregation-free extra-fine nickel powder or cobalt powder, it comprises:
1) nickel nitrate adopts P204, P507 extraction, and after cobalt nitrate extracted with P204, compound concentration was 60g-100g/L, by per 1 * 10
3L nickel nitrate or cobalt nitrate solution; Doping A 14-16 kilogram; And in the continuous adding of the stream agitated reactor 1, stir while adding, overall flow rate is 1-2.5L/min; The temperature of agitated reactor remains on 80-100 ℃, and described additive A is by the ratio preparation in by volume 1: 1: 1 of acetone, hexylene glycol, alcohol;
When overflowing to agitated reactor 2 after 2) question response still 1 is filled it up with; And the stream adding 7-10 g/L additive B aqueous solution, flow velocity is 2-5L/min, stirs; Described additive B is by the ratio preparation in 1: 1: 1 by weight of urea, ammonium carbonate, ammoniacal liquor, and the concentration of ammoniacal liquor is 20-25%;
When overflowing to agitated reactor 3 after 3) question response still 2 is filled it up with, and stream adding 40-60 g/L sodium hydroxide solution, stirring, flow velocity is 2-5L/min, agitated reactor 3 is filled it up with in the back overflow agitated reactor 4;
The molten long-pending of described agitated reactor 1,2,3,4 is 5 * 10
3L; Reaction temperature all remains on 80-100 ℃;
4) in agitated reactor 4, continue to stir, after stream is full, overflows in the inorganic salt precipitates continous way rinsing maching and wash;
5) behind the nickel hydroxide or cobalt hydroxide pulp after will washing, the plate and frame filter press press filtration becomes filter cake;
6) filter cake is refrigerated to freeze all; The drying and crushing all-in-one is pulverized dry; Get high pure and ultra-fine nickel hydroxide powder or cobalt hydroxide powder;
7) high pure and ultra-fine nickel hydroxide powder or cobalt hydroxide powder are reduced to high-purity hard aggregation-free extra-fine nickel powder or cobalt powder in hydrogen reduction furnace.
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| CN2011100412031A CN102154549B (en) | 2011-02-21 | 2011-02-21 | Production method for high-purity hard-agglomeration-free superfine nickel oxide or cobalt and nickel or cobalt powder |
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