CN102649161B - Nickel powder with large furnace safety supervision system (FSSS) particle size and preparation method thereof - Google Patents
Nickel powder with large furnace safety supervision system (FSSS) particle size and preparation method thereof Download PDFInfo
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- CN102649161B CN102649161B CN201110043426.1A CN201110043426A CN102649161B CN 102649161 B CN102649161 B CN 102649161B CN 201110043426 A CN201110043426 A CN 201110043426A CN 102649161 B CN102649161 B CN 102649161B
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C19/00—Alloys based on nickel or cobalt
- C22C19/03—Alloys based on nickel or cobalt based on nickel
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/05—Metallic powder characterised by the size or surface area of the particles
- B22F1/052—Metallic powder characterised by the size or surface area of the particles characterised by a mixture of particles of different sizes or by the particle size distribution
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/10—Sintering only
- B22F3/11—Making porous workpieces or articles
- B22F3/1143—Making porous workpieces or articles involving an oxidation, reduction or reaction step
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/16—Making metallic powder or suspensions thereof using chemical processes
- B22F9/18—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
- B22F9/20—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from solid metal compounds
- B22F9/22—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from solid metal compounds using gaseous reductors
Abstract
The invention is suitable for the technical field of metallurgy and provides nickel powder with large furnace safety supervision system (FSSS) particle size and a preparation method thereof. The preparation method of the nickel powder comprises the following steps that: ammonium oxalate and nickel chloride react for 10 to 30 minutes under the conditions that the temperature is 50 to 60 DEG C and the pH value is 1.5 to 3.0 so as to obtain nickel-oxalate precipitates; the operations of flashing, drying and crushing are carried out on the nickel-oxalate precipitates so as to obtain a nickel-oxalate precursor; the treatment of reducing is carried out on the nickel-oxalate precursor under the condition that the temperature is 450 to 550 DEG C so as to obtain a nickel powder precursor; and the operation of turbine crushing is carried out on the nickel powder precursor, and then the operation of airflow crushing is carried out so as to obtain the nickel powder. The nickel powder prepared by the preparation method provided by the invention has large FSSS particle size, small D50 particle size, narrow particle-size distribution and high purity and is in a porous class spherical pattern, the performance approaches to the T123 carboxylic nickel powder of the INCO company, and the requirement of performance of powder metallurgy and the like can be met. The nickel powder has extensive application field. The preparation method provided by the invention is simple to operate, has low requirement to equipment and high production benefit, is friendly to the environment and is very suitable for industrialized production.
Description
Technical field
The invention belongs to metallurgical technology field, relate in particular to a kind of large FSSS particle diameter nickel powder preparation method and nickel powder.
Background technology
At present, alloy material, powder metallurgy require the FSSS particle diameter of nickel powder large, and D50 particle diameter is little, narrowly distributing.The general T123 carboxyl nickel powder that adopts INCO company to produce, but carboxyl method is poisonous.Though the nickel powder particle diameter that electrolysis is produced is large, the large cost of power consumption is high.Someone prepares the method for nickel powder with pyrolysis reduction, the nickel powder FSSS of preparation is large, but D50 particle diameter is too large, and distribution neither be very even.
Summary of the invention
In view of this, the embodiment of the present invention provides a kind of large FSSS particle diameter, little D50 particle diameter, is evenly distributed and environmental friendliness, nickel powder preparation method with low cost.
The present invention is achieved in that
A large FSSS nickel powder preparation method, comprises the steps:
In temperature, be 50-60 ℃, pH value is under 1.5-3.0 condition, by ammonium oxalate and nickel chloride reaction 10-30 minute, obtains nickel oxalate precipitation;
This nickel oxalate precipitation is carried out to expansion drying fragmentation, obtain nickel oxalate precursor;
By this nickel oxalate precursor, in temperature, be that under 450-550 ℃ of condition, reduction is processed, obtain nickel powder precursor;
This nickel powder precursor is carried out to turbine fragmentation, then carry out airflow crash, obtain nickel powder.
The embodiment of the present invention further provides above-mentioned preparation method prepared nickel powder, and FSSS particle diameter is 3-8 micron, and D50 is 8-18 micron.
Nickel powder prepared by embodiment of the present invention preparation method, FSSS particle diameter is large, D50 particle diameter is little, narrow diameter distribution, purity is high, and performance approaches the T123 carboxyl nickel powder of INCO company, can meet the performance requirements such as powder metallurgy, has wide application.Embodiment of the present invention preparation method, simple to operate, low for equipment requirements, with low cost, productivity effect is high, and environmental friendliness is very suitable for suitability for industrialized production.
Accompanying drawing explanation
Fig. 1 is nickel powder electron-microscope scanning figure prepared by embodiment of the present invention preparation method.
The specific embodiment
In order to make object of the present invention, technical scheme and advantage clearer, below in conjunction with embodiment, the present invention is further elaborated.Should be appreciated that specific embodiment described herein, only in order to explain the present invention, is not intended to limit the present invention.
The embodiment of the present invention provides a kind of large FSSS nickel powder preparation method, comprises the steps:
Step S01, is 50-60 ℃ in temperature, and pH value is under 1.5-3.0 condition, by ammonium oxalate and nickel chloride reaction 10-30 minute, obtains nickel oxalate precipitation;
Step S02, carries out expansion drying fragmentation by this nickel oxalate precipitation, obtains nickel oxalate precursor;
Step S03, is that under 450-550 ℃ of condition, reduction is processed by this nickel oxalate precursor in temperature, obtains powdered nickel precursor body;
Step S04, carries out turbine fragmentation by this nickel powder precursor, then carries out airflow crash, obtains nickel powder.
Particularly, in the embodiment of the present invention, the large FSSS particle diameter of indication refers to that FSSS particle diameter is greater than more than 3 microns.
Particularly, in step S01, the ammonium oxalate of use is restriction not, can be also homemade ammonium oxalate for commercially available, and preparation method is as follows:
The oxalic acid solution (being preferably 150g/L) of preparation 100-200g/L, passes into ammoniacal liquor this oxalic acid solution pH value is adjusted to 4.0-4.5, is preferably 4.3, obtains ammonium oxalate solution, adjusts oxalic acid solution temperature 60-85 ℃ simultaneously, is preferably 70-75 ℃.
The nickel chloride using in step S01 is restriction not, can be for commercially available, also can be for homemade, and preparation method is as follows:
Nickeliferous waste material is through Ore Leaching, purification by liquid extraction, then with hydrochloric acid back extraction, obtain the nickel chloride solution of concentration 60-100g/L.
In step S01, ammonium oxalate and nickel chloride are 50-65 ℃ in temperature, preferably 50-60 ℃, pH value is 1.5-3.0, is preferably 1.5-2.5, reaction 10-30 minute, preferred 10-15 minute, obtain nickel oxalate precipitation, this step reaction is preferably carried out under stirring condition, and mixing speed 200-800r/min is preferably 400-800r/min, when reaction finishes, the pH value of reaction solution is adjusted to 1.8-2.3, continues reaction 5-30 minute, make the nickel content of supernatant in reacted solution be less than 100mg/L.
Particle diameter and ammonium oxalate temperature and the pH value of the nickel oxalate precipitation of preparing in step S01, reaction temperature and pH value, mixing speeds etc. are relevant.The nickel oxalate particle diameter that the high precipitation of ammonium oxalate temperature generates is large; In ammonium oxalate solution, ammonium radical ion and nickel play complexing, be conducive to form the uniform nickel oxalate precipitation of particle diameter, but ammonium oxalate pH value are too high, and ammonia excess coefficient is large, causes waste and increases subsequent wastewater treatment difficulty; Reaction temperature is high, and nickel oxalate particle is easily grown up; PH value in reaction is high, and nickel oxalate nucleation rate is greater than germination speed, easily forms fine particle, and pH value in reaction is low, and the nickel oxalate speed of growth is accelerated, and easily causes nickel oxalate particle to become large; Mixing speed is fast, is conducive to generate fine grained nickel oxalate; Parameter when step S01 passes through to select above-mentioned reaction, has guaranteed that the grain diameter of prepared nickel oxalate precipitation is moderate.
This reaction equation is expressed as:
(NH
4)
2C
2O
4+NiCl
2＝NiC
2O
4↓+2NH
4Cl。
Further, before step S02, also comprise the step of the washing and filtering of above-mentioned nickel oxalate, be specially, the nickel oxalate precipitation obtaining in step S01, through filter centrifugal, is washed with 70-90 ℃ of pure water, be preferably the pure water of 80 ℃.
Particularly, in step S02, this expansion drying break process refers to:
Nickel oxalate is deposited in and in flash dryer treatment facility, has experienced pulverizing, gas-solid contact, dry, classification four-stage, its expansion drying operation principle is: after material enters drying machine, be stirred immediately paddle and air-flow crushing, to increase the decentralization of material and the surface area of unit volume wet stock, because agitator is crushing material and produce dispersion, enter the hot-air of hothouse also in turbulence state highly simultaneously, reach very soon gas-solid mixing, lump material is surrounded by hot-air in good fluidized state.Between material and hot-air, carry out in the dry run of mass-and heat-transfer, most of moisture is fallen in this phase evaporation.Material is subject to after pulverizing and moisture evaporation, and buoyancy is greater than gravity, and material moves upward, and enters clasfficiator.Material is spiral under the carrying secretly of gas, under the effect of centrifugal force, material particular diameter little at interior ring, large wet at outer shroud, granule is taken out of from hothouse center by gas when moisture reaches requirement, compared with wet granular, continue pulverizing more greatly dry, thereby guarantee water content and the epigranular of product.Qualified nickel oxalate is caught dirt collection through multistage cloth bag and is obtained nickel oxalate finished product.Most of nickel oxalate is collected in first order collector, and a small amount of tiny nickel oxalate particle is brought in the second level and third level collector by hot blast tail gas, by cloth bag, is collected.The second level and third level nickel oxalate ratio generally account for the 10-20% of nickel oxalate total amount, and its particle diameter and apparent density are little, separated thereby the nickel oxalate that realization is collected with the first order obtains, and make nickel oxalate particle diameter more even.
The broken equipment integrating of expansion drying using in this step S02 has sorting function, and other are restriction not, is preferably expansion drying crushing all-in-one machine, and in this step, the parameter of the broken one of expansion drying is:
When nickel oxalate precipitation enters expansion drying disintegrating apparatus, water content is controlled at 20-40%, 180 ℃-200 ℃ of hot blast inlet temperatures, and 80 ℃-90 ℃ of hot-blast outlet temperature, main frame frequency 30-50HZ, rotating speed is 1800-3000r/min, air-introduced machine air quantity 1-3 meter per second.
The nickel oxalate precipitation that step S01 obtains, through the expansion drying break process of step S02, obtains nickel oxalate presoma, and the D50 particle diameter of this nickel oxalate presoma is 8-25 micron.
Particularly, in step S03, by this nickel oxalate precursor, in temperature, be under 450-550 ℃ of condition, to reduce to process 90-150 minute, obtain powdered nickel precursor body.In this step, the reducing agent using is gaseous reducing agent, for example, and hydrogen, carbon monoxide; Or the mist of the mist of hydrogen, carbon monoxide and inert gas such as hydrogen and nitrogen etc.In this step, the equipment of use is restriction not, preferably push boat type reduction furnace and steel belt type reducing furnace.Nickel oxalate presoma in step S02 is processed through the reduction of this step, obtains powdered nickel precursor body.
Particularly, in step S04, this powdered nickel precursor body is carried out to turbine break process, then carry out airflow crash processing.
This turbine break process refers to utilizes turbine disintegrating apparatus, and material to be broken smashes by the turbine vibration being produced by powerful air-flow between blade and abrading block, through impacting, shear, grinding, realizes broken.Turbine break process effect in this step, on the one hand powdered nickel precursor body is carried out to preliminary fragmentation, on the other hand, due to the ultrafine powder that can produce in this break process, but this turbine disintegrating apparatus can carry out dust removal process, superfines enters and in bagroom, realizes a small amount of classification with tail gas; The turbine disintegrating apparatus using in this step is restriction not, as long as it is broken to realize above-mentioned turbine, and turbine disintegrating machine for example, in turbine break process step, the main frame frequency of turbine disintegrating machine is 30-35HZ, rotating speed is 1500-2500r/min; Further, the turbine fragmentation of this step is carried out in inert environments, and this inert environments is restriction not, such as helium atmosphere, nitrogen atmosphere, neon atmosphere etc.
The equipment that in this step, airflow crash processing is used is airslide disintegrating mill, is a kind of equipment of realizing the pulverizing of dry type material fining with high velocity air, and it forms by pulverizing nozzle, grading rotor, screw feeder etc.
This airflow crash is processed and is referred to: pass through airslide disintegrating mill, material enters pulverizing chamber by screw feeder, compressed air passes through the superonic flow nozzzle of particular arrangement to pulverizing chamber high velocity jet, material accelerates in supersonic jet, the repeated stock of Bing nozzle intersection, collision, reach pulverizing, by comminuting matter, with ascending air pulverizer, entered grading room, due to the rotation of classification particle high speed, particle had both been subject to the centrifugal force that grading rotor produces, be subject to again the centripetal force that air-flow viscous effect produces, when being subject to centrifugal force, particle is greater than centripetal force, be that more than classification footpath corase particles returns to pulverizing chamber and continues impact comminution, fine particle below classification footpath enters cyclone separator with air-flow, trap is collected, gas is got rid of by air-introduced machine.
The main frame frequency of the airflow crash machine that in this step, airflow crash processing is used is 30-40HZ, and rotating speed is 2500-3500r/min;
This airflow crash is processed the aforementioned powdered nickel precursor body through turbine break process is strengthened to fragmentation, further breaks up the aggregate in powdered nickel precursor body, makes nickel powder particle diameter more even.This airflow crash is processed and is carried out under inert atmosphere, and this inert atmosphere is restriction not, and for example, purity is more than 99% nitrogen atmosphere, helium atmosphere, argon gas atmosphere, neon atmosphere etc.
The technical indicator of the nickel powder that embodiment of the present invention nickel powder preparation method is prepared is as follows:
Nickel powder index: FSSS particle diameter 3-8 μ m, average grain diameter D508-12 μ m, D10 > 5 μ m, D90 < 25 μ m, apparent density 1.2-2.5g/cm
3;
Refer to Fig. 1, Fig. 1 shows nickel powder Electronic Speculum figure prepared by said method, and as can be seen from the figure, its concrete dynamic modulus surface and class spherical morphology, be easy to mix with other metal dust, forms closely and uniformly and distribute.
Nickel powder prepared by embodiment of the present invention preparation method, FSSS particle diameter is large, D50 particle diameter is little, narrow diameter distribution, performance approaches the carboxyl nickel powder of INCO T123, can meet powder metallurgy performance requirement, has wide application.Embodiment of the present invention preparation method, simple to operate, low for equipment requirements, productivity effect is high, and environmental friendliness is very suitable for suitability for industrialized production.
Below in conjunction with specific embodiment, above-mentioned nickel powder preparation method is described in detail.
Example
The oxalic acid solution of preparation 150g/L, passes into liquefied ammonia, and regulating pH value is 4.3, obtains ammonium oxalate solution, and heating-up temperature is stabilized in 70 ℃;
This ammonium oxalate solution is reacted in reactor with the nickel chloride solution of 90g/L, and controlling nickel chloride flow is 1000-1500L/min, and ammonium oxalate flow is 2500-3500L/min.Regulating pH value in reaction is 2.0, and the reaction time is 12 minutes, and ageing 10 minutes is filtered with centrifuge, 80 ℃ of hot pure water washings;
Nickel oxalate precipitation after this washing is carried out to expansion drying break process, and expansion drying disintegrating machine can by parts of fine grain sorting out, obtain the uniform nickel oxalate presoma of particle diameter.
Change pH value in reaction and temperature, reaction time, obtain different-grain diameter nickel oxalate presoma, specific as follows:
From upper table, can draw, the D50 particle diameter of the nickel oxalate presoma preparing in example, between 8.8-19.1 micron, has larger particle diameter.
By above-mentioned nickel oxalate presoma, in push boat type reduction furnace, in temperature, be reductase 12 hour in the hydrogen of 520 ℃, obtain powdered nickel precursor body;
Powdered nickel precursor body is carried out to turbine break process, then carry out airflow crash machine and process and to obtain evengranular nickel powder.
Particle diameter is the above-mentioned processing of nickel oxalate precursor process of 10.6 μ m, and the nickel powder parameter finally obtaining is as follows: FSSS particle diameter 3.15 μ m, D10 particle diameter 5.4 μ m, D50 particle diameter 8.7 μ m, D90 particle diameter 21.3 μ m, apparent density 1.48g/cm
3.
Change nickel oxalate powder stock and reduction temperature, obtain the nickel powder of different-grain diameter, specific as follows:
From upper table, can draw, the FSSS particle diameter of the resulting nickel powder of example is between 3.2-4.3 micron, and D50 particle diameter is between 9-14 micron, from these data, can draw, the prepared nickel powder particle size range of example is narrow, and particle diameter is less.
Attached: nickel powder prepared by use the present invention and the performance parameter of INCO T123 carboxyl nickel powder.
The reduced parameter of the T123 carboxyl nickel powder of nickel powder performance prepared by the present invention and INCO company:
INCO T123 carboxyl nickel powder
1) physical property:
FSSS granularity 3.0～7.0 (μ m) apparent density 1.6～2.6g/cm
3
2) chemical analysis:
Carbon≤0.10% iron≤0.01% sulphur≤0.001% oxygen≤0.15%
Nickel powder of the present invention
1) physical property:
FSSS particle diameter 3.0～8.0 (μ m) apparent density 1.2～2.5g/cm
3
2) chemical analysis:
Other element≤0.005% of carbon≤0.05% iron≤0.005% sulphur≤0.005% oxygen≤0.25%
The foregoing is only preferred embodiment of the present invention, not in order to limit the present invention, all any modifications of doing within the spirit and principles in the present invention, be equal to and replace and improvement etc., within all should being included in protection scope of the present invention.
Claims (7)
1. a large FSSS particle diameter nickel powder preparation method, comprises the steps:
In temperature, be 50-60 ℃, pH value is under 1.5-3.0 condition, by ammonium oxalate and nickel chloride reaction 10-30 minute, obtains nickel oxalate precipitation;
Described nickel oxalate precipitation is carried out to expansion drying fragmentation, obtain nickel oxalate presoma, described expansion drying break process step medium speed is 1800-3000r/min;
By described nickel oxalate presoma, in temperature, be that under 450-550 ℃ of condition, reduction is processed, obtain powdered nickel precursor body;
Described powdered nickel precursor body is carried out to turbine fragmentation, then carry out airflow crash, obtain nickel powder, wherein, described turbine break process step medium speed is 1500-2500r/min and carries out in inert environments, and described airflow crash treatment step medium speed is 2500-3500r/min; The FSSS particle diameter of nickel powder prepared by described nickel powder preparation method is 3-8 micron, and D50 is 8-18 micron.
2. nickel powder preparation method as claimed in claim 1, is characterized in that: described nickel powder preparation method also comprises the preparation process of following ammonium oxalate:
The oxalic acid solution of preparation 100-200g/L, adds ammoniacal liquor or liquefied ammonia that this oxalic acid solution pH value is adjusted to 4.0-4.5, obtains ammonium oxalate solution.
3. nickel powder preparation method as claimed in claim 2, is characterized in that: the temperature of described ammonium oxalate solution is 60-85 ℃.
4. nickel powder preparation method as claimed in claim 1, is characterized in that: when described ammonium oxalate and nickel chloride reaction finish, adjust the pH value of reaction solution to 1.8-2.3, make nickel content in supernatant be less than 100mg/L.
5. nickel powder preparation method as claimed in claim 1, is characterized in that: the time that described reduction is processed is 90-150 minute.
6. nickel powder preparation method as claimed in claim 1, is characterized in that: described nickel oxalate precipitation is carried out also comprising the step that described nickel oxalate precipitation is washed with 70-90 ℃ of pure water before expansion drying break process.
7. nickel powder preparation method as claimed in claim 1, is characterized in that: the D50 particle diameter of described nickel oxalate presoma is 8-25 micron.
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| CN201110043426.1A CN102649161B (en) | 2011-02-23 | 2011-02-23 | Nickel powder with large furnace safety supervision system (FSSS) particle size and preparation method thereof |
| PCT/CN2011/079133 WO2012113217A1 (en) | 2011-02-23 | 2011-08-30 | Nickel powder having high fsss particle size, and preparation method therefor |
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| CN105728741B (en) * | 2014-12-09 | 2017-12-15 | 荆门市格林美新材料有限公司 | The application of the preparation method of nickel powder and its nickel powder of preparation |
| CN104588660B (en) * | 2015-01-07 | 2016-12-07 | 中南大学 | A kind of solid phase combustion synthetic method preparing porous metals integral section |
| CN104827036A (en) * | 2015-05-11 | 2015-08-12 | 东睦新材料集团股份有限公司 | Preparation method of iron-based powder metallurgical part |
| CN104988344B (en) * | 2015-06-23 | 2017-07-28 | 辽宁石化职业技术学院 | The preparation method of composite hydrogen storage material |
| CN105921762B (en) * | 2016-06-17 | 2017-11-03 | 陕西理工学院 | The Co-based alloy powder preparation method of shaping can be densified |
| CN110318072A (en) * | 2018-03-29 | 2019-10-11 | 荆门市格林美新材料有限公司 | The extracting method of tough cathode is extracted in a kind of cobalt concentrate |
| CN110625131A (en) * | 2018-06-25 | 2019-12-31 | 荆门市格林美新材料有限公司 | Basic nickel powder precursor and preparation method thereof |
| CN110961658A (en) * | 2018-09-28 | 2020-04-07 | 荆门市格林美新材料有限公司 | Preparation method of iron-doped superfine nickel powder |
| CN110983142B (en) * | 2019-11-25 | 2021-10-19 | 河海大学 | Preparation method of tungsten carbide-nickel hard alloy |
| CN112355318B (en) * | 2020-10-21 | 2023-05-19 | 荆楚理工学院 | Large-particle-size porous spherical nickel powder and preparation method thereof |
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| US20060107792A1 (en) * | 2004-11-19 | 2006-05-25 | Michael Collins | Method for producing fine, low bulk density, metallic nickel powder |
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