CN107030293A - A kind of preparation method of utilization secondary reduction high-purity nickel powder - Google Patents
A kind of preparation method of utilization secondary reduction high-purity nickel powder Download PDFInfo
- Publication number
- CN107030293A CN107030293A CN201611065526.3A CN201611065526A CN107030293A CN 107030293 A CN107030293 A CN 107030293A CN 201611065526 A CN201611065526 A CN 201611065526A CN 107030293 A CN107030293 A CN 107030293A
- Authority
- CN
- China
- Prior art keywords
- nickel powder
- secondary reduction
- preparation
- temperature
- reduction
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Classifications
-
- 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 discloses a kind of preparation method of utilization secondary reduction high-purity nickel powder, following steps are specifically included：Step 1, ball-shape nickel hydroxide is reduced, a reduced nickel powder is obtained；Step 2, pulping and washing is carried out to the nickel powder of the step 1；Step 3, the nickel powder after being washed to the step 2 carries out secondary reduction；Step 4, the nickel powder after being reduced to the step 3 carries out broken sieving, obtains high-purity globular powdered nickel.The setting that the present invention passes through parameter when secondary reduction, reduction and washing, the content of the sodium in nickel powder is set to control in below 50ppm, and the pattern of nickel powder is spherical, controllable with the index such as preferable dispersiveness, AD, FSSS, can make satisfactory nickel powder according to different demands adjusting process in addition.
Description
Technical field
The invention belongs to metal-powder fabricating technology field, and in particular to one kind utilizes secondary reduction high-purity nickel powder
Preparation method.
Background technology
Nickel powder is mainly used in coating and plastics make conducting pigment shielding electromagnetic interference and radio frequency interference, makees various high glaze dresses
Decorations paint and plastics, make anti-corrosive paint etc., fine grained globular powdered nickel can be used for electrically conductive ink, purposes ratio instead of aluminium powder in water-based system
It is wide.The mode of production of existing globular powdered nickel, sodium impurity is difficult to remove by way of directly washing, and causes nickel powder after reduction
Sodium content it is higher.
The content of the invention
It is an object of the invention to provide a kind of preparation method of utilization secondary reduction high-purity nickel powder, dropped by secondary reduction
The content of sodium in low nickel powder.
The technical solution adopted in the present invention is, a kind of preparation method of utilization secondary reduction high-purity nickel powder：
Step 1, ball-shape nickel hydroxide is reduced, a reduced nickel powder is obtained；
Step 2, pulping and washing is carried out to the nickel powder of the step 1；
Step 3, the nickel powder after being washed to the step 2 carries out secondary reduction；
Step 4, the nickel powder after being reduced to the step 3 carries out broken sieving, obtains high-purity globular powdered nickel.
The features of the present invention is also resided in,
Reduce ball-shape nickel hydroxide in the step 1 to carry out in reduction furnace, the recovery time is 3~6h.
The reduction furnace is four-temperature region push boat type hydrogen reduction furnace, and warm area temperature setting is trapezoidal warm area, and two ends temperature is low, in
Between main warm area temperature it is high.
The two ends temperature differs 10~30 DEG C with medium temperature.
The main warm area temperature is 350~550 DEG C.
The boat size is 540mm*540mm*80mm, and boat charge is 5~8kg.
The nickel powder after reduction is washed with pure water in the step 2, washing water temperature is 60~90 DEG C, and water consumption is nickel
8~10 times of powder weight, stirring pulping and washing 3 times, filter after washing, are dried at 70 DEG C.
Secondary reduction temperature is set as 300~400 DEG C in the step 3, and the recovery time is 1~3h, 5~8kg of boat charge.
The step 4 carries out crossing 200 eye mesh screens after Mechanical Crushing to nickel powder after secondary reduction.
The beneficial effects of the invention are as follows a kind of preparation method of utilization secondary reduction high-purity nickel powder of the invention passes through two
The setting of parameter when secondary reduction, reduction and washing, makes the content of the sodium in nickel powder control in below 50ppm, and the pattern of nickel powder
To be spherical, controllable with the index such as preferable dispersiveness, AD, FSSS, it can be made meeting according to different demands adjusting process in addition
It is required that nickel powder.
Brief description of the drawings
Fig. 1 provides the electron microscope of the nickel powder prepared in embodiment 1 for the present invention；
Fig. 2 provides the electron microscope of the nickel powder prepared in embodiment 2 for the present invention；
Fig. 3 provides the electron microscope of the nickel powder prepared in embodiment 3 for the present invention；
Fig. 4 provides the electron microscope of the nickel powder prepared in embodiment 4 for the present invention；
Fig. 5 provides the electron microscope of the nickel powder prepared in embodiment 5 for the present invention.
Embodiment
In order to make the purpose , technical scheme and advantage of the present invention be clearer, with reference to embodiments, to the present invention
It is further elaborated.It should be appreciated that the specific embodiments described herein are merely illustrative of the present invention, it is not used to
Limit the present invention.
The embodiment of the present invention provides a kind of preparation method of utilization secondary reduction high-purity nickel powder, specifically includes following step
Suddenly：
Step 1, ball-shape nickel hydroxide is reduced, a reduced nickel powder is obtained；
Reduced in the push boat type hydrogen reduction furnace of four-temperature region, the recovery time is 3~6h, warm area temperature setting is trapezoidal temperature
Area, two ends temperature is low, and middle main warm area temperature is high, and two ends temperature differs 10~30 DEG C with medium temperature, and main warm area temperature is 350
~550 DEG C, boat size is 540mm*540mm*80mm, and boat charge is 5~8kg.
Step 2, pulping and washing is carried out to the nickel powder of the step 1；
The nickel powder after reduction is washed with pure water, washing water temperature be 60~90 DEG C, water consumption for nickel powder weight 8~
10 times, stirring pulping and washing 3 times is filtered after washing, dried at 70 DEG C；
Step 3, the nickel powder after being washed to the step 2 carries out secondary reduction；
Secondary reduction temperature is set as 300~400 DEG C, and the recovery time is 1~3h, 5~8kg of boat charge；
Step 4, the nickel powder after being reduced to the step 3 carries out crossing 200 eye mesh screens after Mechanical Crushing, obtains high-purity spherical
Nickel powder.
Compared compared with preparation method, the present invention mainly has following technical advantage：Join during by secondary reduction and reduction
Several settings, makes the content control of the sodium in nickel powder be spherical, disperse with preferable in below 50ppm, and the pattern of nickel powder
The index such as property, AD, FSSS is controllable, can make satisfactory nickel powder according to different demands adjusting process in addition.
Embodiment 1
Ball-shape nickel hydroxide is once reduced first：The temperature of reduction is 450 DEG C, and boat charge is 8kg, recovery time
For 4h；Secondly pulping and washing is carried out：It is 60 DEG C to wash water temperature, and water consumption is 10 times of nickel powder weight；Then secondary reduction is carried out：
The temperature of reduction is 350 DEG C, and boat charge is 8kg, and the recovery time is 2h；Finally carry out crossing 200 eye mesh screens after Mechanical Crushing.Obtain
Nickel powder amount containing sodium be 39ppm, nickel powder AD be 2.45g/cm3, nickel powder FSSS is 3.44 μm (as shown in Figure 1).Same process bar
Under part, unwashed nickel powder amount containing sodium is up to 103ppm.
Embodiment 2
Ball-shape nickel hydroxide is once reduced first：The temperature of reduction is 550 DEG C, and boat charge is 8kg, recovery time
For 3h；Secondly pulping and washing is carried out：It is 90 DEG C to wash water temperature, and water consumption is 8 times of nickel powder weight；Then secondary reduction is carried out：
The temperature of reduction is 300 DEG C, and boat charge is 8kg, and the recovery time is 3h；Finally carry out crossing 200 eye mesh screens after Mechanical Crushing.Obtain
Nickel powder amount containing sodium be 45ppm, nickel powder AD be 2.15g/cm3, nickel powder FSSS is 2.84 μm (as shown in Figure 2).Same process bar
Under part, unwashed nickel powder amount containing sodium is up to 112ppm.
Embodiment 3
Ball-shape nickel hydroxide is once reduced first：The temperature of reduction is 350 DEG C, and boat charge is 5kg, recovery time
For 5h；Secondly pulping and washing is carried out：It is 70 DEG C to wash water temperature, and water consumption is 9 times of nickel powder weight；Then secondary reduction is carried out：
The temperature of reduction is 400 DEG C, and boat charge is 7kg, and the recovery time is 1h；Finally carry out crossing 200 eye mesh screens after Mechanical Crushing.Obtain
Nickel powder amount containing sodium be 46ppm, nickel powder AD be 2.05g/cm3, nickel powder FSSS is 2.71 μm (as shown in Figure 3).Same process bar
Under part, unwashed nickel powder amount containing sodium is up to 121ppm.
Embodiment 4
Ball-shape nickel hydroxide is once reduced first：The temperature of reduction is 500 DEG C, and boat charge is 7kg, recovery time
For 3h；Secondly pulping and washing is carried out：It is 80 DEG C to wash water temperature, and water consumption is 9 times of nickel powder weight；Then secondary reduction is carried out：
The temperature of reduction is 320 DEG C, and boat charge is 5kg, and the recovery time is 2h；Finally carry out crossing 200 eye mesh screens after Mechanical Crushing.Obtain
Nickel powder amount containing sodium be 43ppm, nickel powder AD be 2.41g/cm3, nickel powder FSSS is 3.56 μm (as shown in Figure 4).Same process bar
Under part, unwashed nickel powder amount containing sodium is up to 123ppm.
Embodiment 5
Ball-shape nickel hydroxide is once reduced first：The temperature of reduction is 400 DEG C, and boat charge is 6kg, recovery time
For 4h；Secondly pulping and washing is carried out：It is 80 DEG C to wash water temperature, and water consumption is 10 times of nickel powder weight；Then secondary reduction is carried out：
The temperature of reduction is 380 DEG C, and boat charge is 6kg, and the recovery time is 2h；Finally carry out crossing 200 eye mesh screens after Mechanical Crushing.Obtain
Nickel powder amount containing sodium be 38ppm, nickel powder AD be 2.77g/cm3, nickel powder FSSS is 3.01 μm (as shown in Figure 5).Same process bar
Under part, the unwashed high 136ppm of nickel powder amount containing sodium.
The foregoing is only a preferred embodiment of the present invention, is not intended to limit the scope of the present invention.
Claims (8)
1. a kind of preparation method of utilization secondary reduction high-purity nickel powder, it is characterised in that specifically include following steps：
Step 1, ball-shape nickel hydroxide is reduced, a reduced nickel powder is obtained；
Step 2, pulping and washing is carried out to the nickel powder of the step 1；
Step 3, the nickel powder after being washed to the step 2 carries out secondary reduction；
Step 4, the nickel powder after being reduced to the step 3 carries out broken sieving, obtains high-purity globular powdered nickel.
2. the preparation method of a kind of utilization secondary reduction high-purity nickel powder according to claim 1, it is characterised in that described
Reduce ball-shape nickel hydroxide in step 1 to carry out in reduction furnace, reduction temperature is 350~550 DEG C, the recovery time is 3~6h.
3. the preparation method of a kind of utilization secondary reduction high-purity nickel powder according to claim 2, it is characterised in that described
Reduction furnace is four-temperature region push boat type hydrogen reduction furnace, and warm area temperature setting is trapezoidal warm area, and two ends temperature is low, middle main warm area temperature
It is high.
4. the preparation method of a kind of utilization secondary reduction high-purity nickel powder according to claim 3, it is characterised in that described
Two ends temperature differs 10~30 DEG C with medium temperature.
5. the preparation method of a kind of utilization secondary reduction high-purity nickel powder according to claim 4, it is characterised in that described
Boat size is 540mm*540mm*80mm, and boat charge is 5~8kg.
6. the preparation method of a kind of utilization secondary reduction high-purity nickel powder according to claim 1, it is characterised in that described
The nickel powder after reduction is washed with pure water in step 2, washing water temperature be 60~90 DEG C, water consumption for nickel powder weight 8~
10 times, stirring pulping and washing 3 times is filtered after washing, dried at 70 DEG C.
7. the preparation method of a kind of utilization secondary reduction high-purity nickel powder according to claim 1, it is characterised in that described
Secondary reduction temperature is set as 300~400 DEG C in step 3, and the recovery time is 1~3h, 5~8kg of boat charge.
8. the preparation method of a kind of utilization secondary reduction high-purity nickel powder according to claim 1, it is characterised in that described
Step 4 carries out crossing 200 eye mesh screens after Mechanical Crushing to nickel powder after secondary reduction.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611065526.3A CN107030293A (en) | 2016-11-28 | 2016-11-28 | A kind of preparation method of utilization secondary reduction high-purity nickel powder |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611065526.3A CN107030293A (en) | 2016-11-28 | 2016-11-28 | A kind of preparation method of utilization secondary reduction high-purity nickel powder |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN107030293A true CN107030293A (en) | 2017-08-11 |
Family
ID=59530617
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201611065526.3A Pending CN107030293A (en) | 2016-11-28 | 2016-11-28 | A kind of preparation method of utilization secondary reduction high-purity nickel powder |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN107030293A (en) |
Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR20040094096A (en) * | 2003-05-01 | 2004-11-09 | 김광호 | Preparation of spherical ultrafine nickel powders by wet reduction process |
| CN101797650A (en) * | 2010-04-22 | 2010-08-11 | 昆明贵金属研究所 | Method for producing surface-activated superfine nickel powder |
| CN101837463A (en) * | 2009-03-20 | 2010-09-22 | 中国科学院过程工程研究所 | Method preparing superfine metallic nickel powder with high frequency plasma |
| CN102909383A (en) * | 2011-08-03 | 2013-02-06 | 深圳市格林美高新技术股份有限公司 | Method for preparing ultrafine nickel powder or cobalt powder |
| CN103334017A (en) * | 2013-07-01 | 2013-10-02 | 贵研铂业股份有限公司 | Method for preparing high-purity nickel powder from waste high-temperature alloy |
| CN103624251A (en) * | 2013-12-02 | 2014-03-12 | 深圳市格林美高新技术股份有限公司 | Half-micron cobalt powder, preparation method thereof, cobalt hydroxide powder and preparation method thereof |
| CN104227012A (en) * | 2013-06-14 | 2014-12-24 | 中国振华集团云科电子有限公司 | Preparation method for ultra-fine copper powder |
-
2016
- 2016-11-28 CN CN201611065526.3A patent/CN107030293A/en active Pending
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR20040094096A (en) * | 2003-05-01 | 2004-11-09 | 김광호 | Preparation of spherical ultrafine nickel powders by wet reduction process |
| CN101837463A (en) * | 2009-03-20 | 2010-09-22 | 中国科学院过程工程研究所 | Method preparing superfine metallic nickel powder with high frequency plasma |
| CN101797650A (en) * | 2010-04-22 | 2010-08-11 | 昆明贵金属研究所 | Method for producing surface-activated superfine nickel powder |
| CN102909383A (en) * | 2011-08-03 | 2013-02-06 | 深圳市格林美高新技术股份有限公司 | Method for preparing ultrafine nickel powder or cobalt powder |
| CN104227012A (en) * | 2013-06-14 | 2014-12-24 | 中国振华集团云科电子有限公司 | Preparation method for ultra-fine copper powder |
| CN103334017A (en) * | 2013-07-01 | 2013-10-02 | 贵研铂业股份有限公司 | Method for preparing high-purity nickel powder from waste high-temperature alloy |
| CN103624251A (en) * | 2013-12-02 | 2014-03-12 | 深圳市格林美高新技术股份有限公司 | Half-micron cobalt powder, preparation method thereof, cobalt hydroxide powder and preparation method thereof |
Non-Patent Citations (1)
| Title |
|---|
| 赵家春等: "利用硫酸镍制备超细球形镍粉的实验研究", 《无机盐工业》 * |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN103540786B (en) | Preparation method of graphene/copper-nickel nano composite material | |
| JP5981049B2 (en) | Method for preparing nickel-cobalt-manganese hydroxide | |
| CN109014239A (en) | A kind of preparation method of touch screen laser ablation silver paste silver powder | |
| CN109365830A (en) | A kind of preparation method of the spherical super fine silver powder of high jolt ramming | |
| US11426795B2 (en) | Silver particles and manufacturing method therefor | |
| CN107661986A (en) | A kind of method for being prepared on a large scale the high sphericity super fine silver powder of high dispersive | |
| CN113292106A (en) | Three-time calcination preparation method of large-particle-size aluminum-doped cobaltosic oxide | |
| CN111790918A (en) | Preparation method of silver powder with low thermal shrinkage | |
| CN102683050A (en) | Preparation method of nano Ag-SnO2 electric contact composite | |
| Su et al. | A review of 1D magnetic nanomaterials in microwave absorption | |
| CN102941351B (en) | A kind of preparation method of superfine cupper powder | |
| CN103878389B (en) | A kind of production method of coarse granule cobalt powder | |
| CN107030293A (en) | A kind of preparation method of utilization secondary reduction high-purity nickel powder | |
| CN113172233A (en) | Nano spherical close-packed hexagonal cobalt powder and preparation method thereof | |
| CN106670489A (en) | Preparing method for spherical high-purity nickel powder | |
| CN111235695A (en) | Preparation method of porous carbon fiber electromagnetic wave absorbing agent | |
| CN106623961A (en) | Preparation method of nickel powder with small FSSS | |
| CN106799498A (en) | A kind of preparation method of globular powdered nickel | |
| CN104056646B (en) | The preparation method of a kind of Co/Ni and aluminum pyrophosphate composite hollow microballoon and application thereof | |
| CN103028736B (en) | Silver-coated cobalt powder and preparation method thereof | |
| CN113488330B (en) | Preparation method of functional magnetic slurry and magnetic device | |
| CN114361448A (en) | Lithium iron phosphate, preparation method thereof and lithium ion battery | |
| CN110426924B (en) | Ceramic powdered ink with high pigment content and preparation method thereof | |
| CN105081343A (en) | Manufacturing method for conductive silver powder used for touch screen UV-type laser engraving silver paste | |
| CN107350479A (en) | A kind of preparation method of superfine ferro-nickel alloyed powder |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20170811 |
|
| RJ01 | Rejection of invention patent application after publication |