CN103273074A - Process method of continuously producing ultra-fine nickel powder - Google Patents
Process method of continuously producing ultra-fine nickel powder Download PDFInfo
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- CN103273074A CN103273074A CN2013101017541A CN201310101754A CN103273074A CN 103273074 A CN103273074 A CN 103273074A CN 2013101017541 A CN2013101017541 A CN 2013101017541A CN 201310101754 A CN201310101754 A CN 201310101754A CN 103273074 A CN103273074 A CN 103273074A
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Abstract
The invention provides a process method of continuously producing ultra-fine nickel powder. The process method comprises the working procedures of preparation of raw materials, material conveying, ultrasound enhancement tubular reaction, rapid cleaning of pipelines, ultrasonic agitation stabilizing treatment, continuous cleaning and collection of the powder, vacuum drying, ball-milling dispersion and the like. By means of the technologies, in a preparation course, the process method has the advantages that continuous industrial production can be achieved, equipment investment is small, product quality is stable, and the shapes and the particle sizes of products are controllable.
Description
Technical field
The present invention relates to a kind of method of producing extra-fine nickel powder, relate in particular to a kind of pipe reaction of being convenient to pipeline cleaning and product collection and produce the extra-fine nickel powder method continuously.
Background technology
Granularity is tiny owing to having, specific area big for extra-fine nickel powder, surface energy advantages of higher, and have broad application prospects in fields such as electronics, electric power, metallurgy, chemical industry, can be used as different field such as electrocondution slurry, secondary cell, catalyst, carbide alloy, electrical alloy.
Domestic extra-fine nickel powder comparison common used in industry production method mainly contains carbonyl nickel thermal decomposition method, using vaporization condensation process, electrolysis, argon shield machinery ball-milling method, liquid phase reduction; the employing diverse ways can make sub-micron and the micron-class superfine nickel powder from 0.1 micron to 3 microns, but the product of different processes preparation presents different powder morphology feature and particle size distribution.The present invention generally speaking should belong to a kind of improvement to existing liquid phase reduction, has solved some practical problems that exist in the existing technology.
Existing extra-fine nickel powder industrialized preparing process has the following problem defective in other words: such as: 1. carbonyl nickel thermal decomposition method: have strong toxicity, therefore production process requires high to equipment, the industrialization investment is very big, and domestic production line instability, security incident also took place in the production of relevant producer; 2. using vaporization condensation process: domestic industryization do extra-fine nickel powder production technology preferably, but owing to nickel will be heated to more than the boiling point, therefore to equipment require highly, production cost also is difficult to reduce; 3. electrolysis: energy consumption is big, and the powder size of preparation is bigger than normal.Argon shield machinery ball-milling method: size distribution is inhomogeneous, and powder shape is irregular; 4. traditional liquid phase reduction: generally adopt still reaction, the powder size lack of homogeneity, and be difficult to realize serialization production, otherness is big between the product batches.
The main technique method of domestic production sub-micron and nano level superfine nickel powder is plasma or laser atomization process at present, and high but this technology requires production equipment, equipment has high input, thereby production cost is very high.Adopt liquid chemical method to prepare extra-fine nickel powder because production equipment is general, technical process is simple, is a process that can effectively reduce the extra-fine nickel powder production cost.But adopt conventional reaction still reaction, again because problems such as concentration gradient exist the resultants in reaction process granularity to be difficult to shortcomings such as control is even, the inconvenient dispersion of product.
Summary of the invention
In order to solve above technical problem, the present invention adopts pipe reaction, mainly be to have made the improved technology method at the production of popular response still formula, adopting the method powder to be created in the pipeline finishes fast, follow-up under dispersant and ultrasonic compound action, reduced the tendency that powder particle is reunited and grown up.In the pipe reaction process because the activity of superfines is very high, have the reacting pipe wall gather may, when serious even the phenomenon of pipeline blockage may occur.
The invention provides a kind of process of continuous production extra-fine nickel powder, it is characterized in that, comprise following step:
Steps A: nickel sulfate hexahydrate is dissolved in the deionized water, adds dispersant again, fully heating is preserved after the stirring and dissolving, obtains solution A, is stored in first storage tank and the 3rd storage tank; Dissolution of sodium hydroxide in deionized water, is fully stirred back heating and insulation, add hydrazine hydrate and NaBH again
4, fully heat after the stirring and dissolving, obtain mixed solution B and be stored in second storage tank and the 4th storage tank.
Step B: adopt flow pump respectively solution A and solution B to be delivered to ultrasonic intensified response entrance, open supersonic generator, with hybrid reaction in the reaction raw materials input channel mixing reactor, mixed solution outputed in the agitator after reaction was finished.
Step C: the solution that contains nickel powder that has reacted the back generation flows in the buffer storge vat, starts ultrasonic and the unlatching stirring, adds lauryl sodium sulfate, stabilization processes.
Step D: the mixed solution that will finish ultrasonic stabilization processes flows through and has the adsorbing conveyer belt of magnetic force, finishes collection, the powder of collecting is carried out drying handle in vacuum drying chamber, carries out the ball milling dispersion treatment again, obtains the extra-fine nickel powder product.
Wherein, first storage tank, second storage tank, the 3rd storage tank and the 4th storage tank are the identical storage tanks of same capacity, and two cover aggregate-storing systems are used alternatingly, and guarantee the continuity of producing.Have the adsorbing conveyer belt of magnetic force and adopt belt magnetic separator.
The present invention adopts a kind of improved liquid phase reduction to realize the serialization production of extra-fine nickel powder, and main process comprises operations such as the continuous wash collection, vacuum drying, ball milling dispersion of raw material preparation, mass transport, ultrasonic enhancing pipe reaction, pipeline Rapid Cleaning, ultrasonic agitation stabilization processes, powder.Its advantage is, realizes control to final products pattern, granularity by the adjusting to the proportioning of material composition and mass transport speed.Adopt ultrasonically enhanced pipe reaction to finish the reduction of nickel powder, and guarantee the uniformity consistency of powder size.Adopt the method for pipeline Rapid Cleaning to come the unimpeded of realization response pipeline, guarantee the industrial efficient of serialization.The adding of ultrasonically enhanced quick stirring and an amount of dispersant can effectively prevent the reunion between the powder particle.Magnetic conveyor type continuous wash is collected can improve production efficiency of products, and reduces powder in water and the dew of air is put the time, reduces the degree of oxidation of superfine powder.Adopt vacuum drying and ball milling to disperse to realize dehydration fully and the dispersion of product at last, reach the quality control requirement of corresponding product.
Preferably, in the described steps A, nickel sulfate hexahydrate is dissolved in the deionized water, adds dispersant again, fully be heated to 60-90 ℃ of preservation after the stirring and dissolving, obtain solution A, be stored in first storage tank and the 3rd storage tank; Dissolution of sodium hydroxide in deionized water, is heated to 60-90 ℃ of insulation after fully stirring, adds hydrazine hydrate and NaBH4, fully be heated to 60 ℃-90 ℃ after the stirring and dissolving, obtain mixed solution B and be stored in second storage tank and the 4th storage tank.
Preferably, in the described steps A, the mass ratio of described hydrazine hydrate and NaBH4 is 1:5-5:1, and described dispersant adopts PVP.
Preferably, among the described step B, the supersonic frequency of described supersonic generator is 30-50KHz, and power is 550-650W.
Preferably, among the described step B, the environment temperature of pipeline is 60-90 ℃.
Preferably, among the described step B, the flow velocity of solution A and solution B is 0.5-5.0L/min.
Preferably, among the described step C, ultrasonic frequency is 25-30KHz, and mixing speed is 200-1000 rev/min, and the time of stabilization processes is 1-3 hour.
Preferably, before the described step C, if when pipeline blockage or flow velocity occurring and reducing, adopt acid solution and deionized water that pipeline is carried out circulation flushing.
Preferably, described acid solution adopts at least a in hydrochloric acid and the nitric acid.
Preferably, among the described step D, for eliminating the situation that pipeline blockage appears in course of reaction, adopt deionized water and absolute ethyl alcohol to clean.
Preferably, among the described step D, the vacuum during vacuum drying is not higher than 100Pa, and temperature is 40-60 ℃, heat preservation and dryness 10-12 hour.
The present invention adopts special flushing of pipeline mechanism to its actual service efficiency of cleaning to guarantee this reaction pipeline, is conducive to the realization of the course of industrialization of this process.In the conveyor type mechanism of following adopted band magnetic force absorption powder is collected continuously simultaneously and has also been improved production efficiency of products widely, improved in the extra-fine nickel powder wet production cleaning process be exposed in the water for a long time or in the air and the oxidation situation that produces.And the preparation process of technology that the present invention adopts can realize advantages such as serialization industrial production, equipment investment are little, constant product quality, shape of product controllable granularity.
Description of drawings
Fig. 1 is implementing process flow chart of the present invention
Fig. 2 is the globular powdered nickel ESEM picture of the embodiment of the invention 1 preparation
Fig. 3 is the thorn shape nickel powder ESEM picture of the embodiment of the invention 2 preparations
The specific embodiment
Below in conjunction with accompanying drawing, more excellent embodiment of the present invention is described in further detail:
Embodiment 1
As shown in Figure 1, this method comprises following flow process:
1) raw material is prepared: with 13Kg NiSO
4 . 6H
2O is dissolved in the 100L deionized water, adds 225g PVP again, fully is heated to 60 ℃ after the stirring and dissolving, obtains solution A, is stored in first storage tank and the 3rd storage tank; 5.2KgNaOH is dissolved in the 96L deionized water, fully stirs the back heating, when 60 ℃ of water temperatures, add 4L concentration and be 50% hydrazine hydrate and 1.85Kg NaBH
4, fully be heated to 60 ℃ after the stirring and dissolving, obtain mixed solution B and be stored in second storage tank and the 4th storage tank.
2) mass transport: by measuring pump A and B two solution are pumped in the reacting pipe, control the flow velocity of two solution respectively at 0.5L/min.
3) ultrasonic enhancing pipeline hybrid reaction: before the reaction reacting pipe environment temperature is warmed up to 60 ℃, keeps constant temperature, before the reaction beginning, open ultrasonic wave, the control ultrasonic frequency is 40KHz, and power is 600W, makes the fully reaction in pipeline of A and B two solution.
4) the not timing pipeline is got express developed: observe the situation of change of flow pump, in time switch pipe valve when pipeline blockage or flow obviously reduce, stop mass transport, with circulation acid solution and deionized water rinsing pipeline, guarantee the unimpeded of pipeline.
5) ultrasonic agitation stabilization processes: the solution that contains nickel powder that has reacted the back generation flows in the buffer storge vat, start ultrasonic and the unlatching stirring, the control ultrasonic frequency is 28KHz, and mixing speed is 300 rev/mins, add lauryl sodium sulfate (SDS) 100g, stabilization processes 2 hours.
6) the attached powder of the continuous magnetic of conveyor type cleans and collects: the mixing material that will finish stabilization processes slowly imports on the belt magnetic separator, nickel powder is transmitted the band traction and upwards breaks away from deionized water solution under the magnetic force suction-operated, deionized water then under the gravity effect, enters in the waste liquid pool.To receive then nickel powder clean in deionized water for stirring again, magnetic force absorption, triplicate like this, to the pH value of mixed solution be 7.And then will receive the nickel powder absorption of stirring and washing, magnetic force, so triplicate in absolute ethyl alcohol again.
7) vacuum drying: will collect to such an extent that nickel powder carries out vacuum drying in vacuum drying chamber, vacuum is 100Pa, and temperature is 50 ℃, heat preservation and dryness 12 hours.
8) ball milling disperses: present powder fragmentation, the dispersion of slight reunion after adopting the low speed ball milling with vacuum drying, prepare corresponding superfine spherical nickel powder.
Embodiment 2
1) raw material is prepared: with 13Kg NiSO
4 . 6H
2O is dissolved in the 100L deionized water, adds 225g PVP again, fully is heated to 80 ℃ after the stirring and dissolving, obtain solution A, is stored in first storage tank and the 3rd storage tank; 5.2Kg NaOH is dissolved in the 77.5L deionized water, fully stir the back heating, during soon near 80 ℃, adding 22.5L concentration is 50% hydrazine hydrate in water temperature, fully be heated to 80 ℃ after the stirring and dissolving, obtain mixed solution B and be stored in second storage tank and the 4th storage tank.
2) mass transport: by measuring pump A and B two solution are pumped in the reacting pipe, control the flow velocity of two solution respectively at 1.5L/min.
3) ultrasonic enhancing pipeline hybrid reaction: before the reaction reacting pipe environment temperature is warmed up to 80 ℃, keeps constant temperature, before the reaction beginning, open ultrasonic wave, the control ultrasonic frequency is 50KHz, and power is 650W, makes the fully reaction in pipeline of A and B two solution.
4) the not timing pipeline is got express developed: observe the situation of change of flow pump, in time switch pipe valve when pipeline blockage or flow obviously reduce, stop mass transport, with circulation acid solution and deionized water rinsing pipeline, guarantee the unimpeded of pipeline.
5) ultrasonic agitation stabilization processes: the solution that contains nickel powder that has reacted the back generation flows in the buffer storge vat, start ultrasonic and the unlatching stirring, the control ultrasonic frequency is 30KHz, and mixing speed is 250 rev/mins, add lauryl sodium sulfate (SDS) 100g, stabilization processes 3 hours.
6) the attached powder of the continuous magnetic of conveyor type cleans and collects: the mixing material that will finish stabilization processes slowly imports on the belt magnetic separator, nickel powder is transmitted the band traction at magneticaction and upwards breaks away from deionized water solution, deionized water then under the gravity effect, enters in the waste liquid pool.To receive then nickel powder clean in deionized water for stirring again, magnetic force absorption, triplicate like this, to the pH value of mixed solution be 7.And then will receive the nickel powder absorption of stirring and washing, magnetic force, so triplicate in absolute ethyl alcohol again.
7) vacuum drying: will collect to such an extent that nickel powder carries out vacuum drying in vacuum drying chamber, vacuum 80Pa, temperature is 60 ℃, heat preservation and dryness 10 hours.
8) ball milling disperses: present powder fragmentation, the dispersion of slight reunion after adopting the low speed ball milling with vacuum drying, prepare corresponding ultra-fine thorn shape nickel powder.
By Fig. 2 and 3 as can be known, the particle diameter of embodiment 1 and embodiment 2 resulting nickel powders is respectively 150 nanometers and 500 nanometers, and particle diameter is little, can reach even particle size distribution, and the powder shape rule.
Above content be in conjunction with concrete preferred embodiment to further describing that the present invention does, can not assert that concrete enforcement of the present invention is confined to these explanations.For the general technical staff of the technical field of the invention, without departing from the inventive concept of the premise, can also make some simple deduction or replace, all should be considered as belonging to protection scope of the present invention.
Claims (10)
1. a process of producing extra-fine nickel powder continuously is characterized in that, comprises following step:
Steps A: nickel sulfate hexahydrate is dissolved in the deionized water, adds dispersant again, fully heating is preserved after the stirring and dissolving, obtains solution A, is stored in first storage tank and the 3rd storage tank; Dissolution of sodium hydroxide in deionized water, is fully stirred back heating and insulation, add hydrazine hydrate again or/and NaBH
4, fully heat after the stirring and dissolving, obtain mixed solution B and be stored in second storage tank and the 4th storage tank;
Step B: adopt flow pump respectively solution A and solution B to be delivered to ultrasonic intensified response entrance, open supersonic generator, with hybrid reaction in the reaction raw materials input channel mixing reactor, mixed solution outputed in the agitator after reaction was finished;
Step C: the solution that contains nickel powder that has reacted the back generation flows in the buffer storge vat, starts ultrasonic and the unlatching stirring, adds stabilizing agent, carries out stabilization processes;
Step D: the mixed solution that will finish ultrasonic stabilization processes flows through and has the adsorbing conveyer belt of magnetic force, finishes collection, and the powder of collecting is carried out the ball milling dispersion treatment after the drying in vacuum drying chamber, obtains the extra-fine nickel powder product.
2. the process of continuous production extra-fine nickel powder as claimed in claim 1, it is characterized in that, in the described steps A, nickel sulfate hexahydrate is dissolved in the deionized water, add dispersant again, fully be heated to 60-90 ℃ of preservation after the stirring and dissolving, obtain solution A, be stored in first storage tank and the 3rd storage tank; Dissolution of sodium hydroxide in deionized water, is heated to 60-90 ℃ of insulation after fully stirring, adds hydrazine hydrate and NaBH
4, fully be heated to 60 ℃-90 ℃ after the stirring and dissolving, obtain mixed solution B and be stored in second storage tank and the 4th storage tank.
3. the process of continuous production extra-fine nickel powder as claimed in claim 1 is characterized in that, in the described steps A, described dispersant adopts PVP.
4. the process of continuous production extra-fine nickel powder as claimed in claim 1 is characterized in that, among the described step D, described stabilizing agent adopts lauryl sodium sulfate.
5. the process of continuous production extra-fine nickel powder as claimed in claim 1 is characterized in that, among the described step B, the supersonic frequency of described supersonic generator is 30-50KHz, and power is 550-650W.
6. the process of continuous production extra-fine nickel powder as claimed in claim 1 is characterized in that, among the described step B, the environment temperature of pipeline is 60-90 ℃.
7. the process of continuous production extra-fine nickel powder as claimed in claim 1 is characterized in that, among the described step B, the flow velocity of solution A and solution B is 0.5-5.0L/min.
8. the process of continuous production extra-fine nickel powder as claimed in claim 1 is characterized in that, among the described step C, ultrasonic frequency is 25-30KHz, and mixing speed is 200-1000 rev/min, and the time of stabilization processes is 1-3 hour.
9. the process of continuous production extra-fine nickel powder as claimed in claim 1 is characterized in that, before the described step C, if when pipeline blockage or flow velocity occurring and reducing, adopts acid solution and deionized water that pipeline is carried out circulation flushing.
10. the process of continuous production extra-fine nickel powder as claimed in claim 1 is characterized in that, among the described step D, the vacuum during vacuum drying is not higher than 100Pa, and temperature is 40-60 ℃, heat preservation and dryness 10-12 hour.
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| CN103894623A (en) * | 2014-03-19 | 2014-07-02 | 深圳航天科技创新研究院 | Preparing method of antioxidant super-fine nickel powder |
| CN108247077A (en) * | 2018-01-25 | 2018-07-06 | 深圳市中金岭南科技有限公司 | A kind of method that micro- reaction prepares copper powder |
| CN108778577A (en) * | 2016-03-04 | 2018-11-09 | 住友金属矿山株式会社 | The manufacturing method of nickel powder |
| CN109311094A (en) * | 2016-06-21 | 2019-02-05 | 住友金属矿山株式会社 | Manufacturing method, the manufacturing device of nickel powder of nickel powder |
| CN109663929A (en) * | 2019-01-24 | 2019-04-23 | 兰州石化职业技术学院 | A kind of preparation method of rule nanogold particle |
| CN112358737A (en) * | 2020-11-05 | 2021-02-12 | 浙江迪邦化工有限公司 | Continuous production process of azo disperse dye with ester group |
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| CN112358737A (en) * | 2020-11-05 | 2021-02-12 | 浙江迪邦化工有限公司 | Continuous production process of azo disperse dye with ester group |
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