CN107052362A - High-specific surface area ultrafine palladium powder and preparation method thereof - Google Patents
High-specific surface area ultrafine palladium powder and preparation method thereof Download PDFInfo
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- CN107052362A CN107052362A CN201710450372.8A CN201710450372A CN107052362A CN 107052362 A CN107052362 A CN 107052362A CN 201710450372 A CN201710450372 A CN 201710450372A CN 107052362 A CN107052362 A CN 107052362A
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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
- B22F9/24—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from liquid metal compounds, e.g. solutions
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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
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Abstract
It is an object of the invention to provide high-specific surface area ultrafine palladium powder and preparation method thereof, in the prior art, the technology for producing palladium powder is also relatively backward, and the preparation method research lifted particularly with palladium powder specific surface area is also fewer.The step of the present invention is into chlorine palladium acid solution by High Purity Palladium aqua regia dissolution；Then in chlorine palladium acid solution plus aqueous slkali adjustment system PH is 9~12, and add and dissolved PVP dispersant solutions and stir and control solution temperature；Reducing agent is configured to finite concentration and adds above-mentioned system, after charging is finished, continues to stir, obtains ultrafine palladium powder slurries；After after slurries clarification, supernatant liquor is drawn, deionized water washing, cyclic washing to electrical conductivity ﹤ 20us/cm, and vacuum drying is added, that is, is prepared into ultrafine palladium powder.Ultrafine palladium powder specific surface area height, the adsorption activity prepared is strong.
Description
Technical field
The invention belongs to high-molecular compound technical field, it is related to high-specific surface area ultrafine palladium powder and preparation method thereof.
Background technology
Ultrafine palladium powder is a kind of industrial chemicals, and because the mode of production is different, product quality is also each variant, and manufacturing cost has
Costliness has cheap, and the influence that environment is produced also is not quite similar.Domestic electronics industry develops later, the research to electronic material
Fall behind foreign countries' more than ten years, the especially research to palladium powder reports that seldom, the technology for producing palladium powder is also relatively backward, Domestic Palladium powder
Source relies primarily on import.
With the development of electronic information industry, metal blending property polymer conductor slurry has obtained fast development, ultra-fine palladium
Powder is in metal blending property conducting polymer slurry in improving the drought resisting material erosiveness of slurry and preventing silver ion migration
Excellent performance so as to the performance requirement more and more higher of palladium powder in industrial production.Wherein because high-specific surface area ultrafine palladium powder is super
Strong surface-active, adsorptivity and its excellent electrical property, industrially by largely as hydrogen purification material, thick film ink
Conductive phase, catalyst, purifying vehicle exhaust material etc. are applied.Some preparation sides for ultrafine palladium powder are had in the prior art
Method, but the preparation method research lifted for palladium powder specific surface area is also fewer.
The content of the invention
In view of this, it is a primary object of the present invention to provide high-specific surface area ultrafine palladium powder and preparation method thereof.
To reach above-mentioned purpose, the technical proposal of the invention is realized in this way：
The preparation method of high-specific surface area ultrafine palladium powder, it is characterised in that comprise the following steps：
（1）High Purity Palladium aqua regia dissolution is into chlorine palladium acid solution, and obtained solution is the first solution；
（2）Weigh polyvinylpyrrolidone and aqueous povidone solution is dissolved into deionized water, it is stand-by；In the first solution
It is PH=9~12 to plant and add aqueous slkali adjustment system, then adds the aqueous povidone solution dissolved and stirs,
Obtained solution is the second solution, and controls the temperature of the second solution；
（3）By reducing agent deionized water dissolved dilution, obtained solution is the 3rd solution, and the 3rd solution is slowly added into second
Solution is reduced, after addition is finished, and is continued to stir 30 minutes, is obtained ultrafine palladium powder slurries；
（4）After after the clarification of ultrafine palladium powder slurries, supernatant liquor is drawn, deionized water washing, cyclic washing to electrical conductivity ﹤ is added
20us/cm, and vacuum drying, that is, the product obtained are ultrafine palladium powder.
The step（1）In be into chlorine palladium acid solution, to add deionized water adjustment solution dense by High Purity Palladium aqua regia dissolution
Degree, solution concentration is calculated as 2.0%~4.0% using simple substance palladium.
The step（2）The consumption of middle polyvinylpyrrolidone is the 0.1%~0.5% of the mass parts of High Purity Palladium.
The step（2）In aqueous slkali be natrium carbonicum calcinatum or sodium hydroxide.
The step（2）The middle temperature for controlling the second solution is 30~50 DEG C.
The step（3）The reducing agent of middle selection is hydrazine hydrate, glucose.
The step（3）The middle adition process time that 3rd solution is slowly added to the second solution is 1~3min.
The step（4）Middle mode of washing washs for mashing.
The step（4）Middle vacuum drying is that 36~42h is dried under 80 DEG C of vacuum condition.
High-specific surface area ultrafine palladium powder made from the preparation method of described high-specific surface area ultrafine palladium powder.
Compared with prior art, beneficial effects of the present invention：
1. experimental provision, experimental condition and preparation process are simple, easy to operate, Product yields are high, with low cost, raw suitable for industry
Production；
2. controllability is good, the ultrafine palladium powder specific surface area prepared is 10~80m2/ g, specific surface area is high, adsorption activity is strong,
Particle diameter is 2~5um, moisture ＜ 0.5%；
3. products application extensively, can be used as hydrogen purification material, the conductive phase of thick film ink, catalyst, purifying vehicle exhaust material.
The ultrafine palladium powder specific surface area prepared after drying is 10~80m2/ g, particle diameter is 2~5um. moisture ＜ 0.5%.
Brief description of the drawings
Fig. 1 is the SEM figures for the high-specific surface area ultrafine palladium powder that the present invention is provided.
Embodiment
In order to make the purpose , technical scheme and advantage of the present invention be clearer, it is right below in conjunction with drawings and Examples
The present invention is further elaborated.It should be appreciated that the specific embodiments described herein are merely illustrative of the present invention, and
It is not used in the restriction present invention.
The present invention provides a kind of preparation method of high-specific surface area ultrafine palladium powder, comprises the following steps：
（1）High Purity Palladium aqua regia dissolution is into chlorine palladium acid solution, and obtained solution is the first solution；
（2）Weigh polyvinylpyrrolidone and aqueous povidone solution is dissolved into deionized water, it is stand-by；In the first solution
It is PH=9~12 to plant and add aqueous slkali adjustment system, then adds the aqueous povidone solution dissolved and stirs,
Obtained solution is the second solution, and controls the temperature of the second solution；Polyvinylpyrrolidone is PVP, main to play scattered make
With.
（3）By reducing agent deionized water dissolved dilution, obtained solution is the 3rd solution, and the 3rd solution is slowly added to
Second solution is reduced, after addition is finished, and is continued to stir 30 minutes, is obtained ultrafine palladium powder slurries；
（4）After after the clarification of ultrafine palladium powder slurries, supernatant liquor is drawn, deionized water washing, cyclic washing to electrical conductivity ﹤ is added
20us/cm, and vacuum drying, that is, the product obtained are ultrafine palladium powder.
The step（1）In be into chlorine palladium acid solution, to add deionized water adjustment solution dense by High Purity Palladium aqua regia dissolution
Degree, solution concentration is calculated as 2.0%~4.0% using simple substance palladium.It is mainly dissolving High Purity Palladium using the purpose of chloroazotic acid, can also be direct
Using finished product chlorine palladium acid solution, but it is more expensive.
The step（2）The consumption of middle polyvinylpyrrolidone is the 0.1%~0.5% of the mass parts of High Purity Palladium.
The step（2）In aqueous slkali be natrium carbonicum calcinatum or sodium hydroxide.
The step（2）The middle temperature for controlling the second solution is 30~50 DEG C.
The step（3）The reducing agent of middle selection is hydrazine hydrate, glucose.
The step（3）The middle adition process time that 3rd solution is slowly added to the second solution is 1~3min.Added
Gas, heat can be produced in a short time soon to cause danger；Added the ultrafine palladium powder surface area generated slowly not high.
The step（4）Middle mode of washing washs for mashing.
The step（4）Middle vacuum drying is that 36~42h is dried under 80 DEG C of vacuum condition.
High-specific surface area ultrafine palladium powder made from the preparation method of described high-specific surface area ultrafine palladium powder.
Embodiment 1
（1）By 50g High Purity Palladiums with 480mL aqua regia dissolutions into chlorine palladium acid solution, adding deionized water makes cumulative volume be 2000ml, dense
Spend for 2.4%（Calculated with simple substance palladium）.
（2）The aqueous solution that 0.1gPVP is dissolved into 0.1% with deionized water is weighed, it is stand-by.（1）Middle addition 150ml concentration
The alkaline solution that system is PH=11~12, water-bath are adjusted for 400g/L sodium hydroxide solution so that solution temperature is 35~45
DEG C, the PVP solution dissolved is added, is stirred.
（3）Measure 80% hydrazine hydrate（Mass concentration）Solution 50ml, adds 450ml deionized waters and is diluted, in stirring bar
The hydrazine hydrate solution diluted was added in 3 minutes under part above-mentioned（2）Solution in reduced, charging finish after, after
Continuous stirring 30 minutes.
（4）After after slurries clarification, supernatant liquor is drawn, deionized water washing is added, cyclic washing 11 times is to electrical conductivity
12us/cm, vacuum drying is 38h at 80 DEG C, and the ultrafine palladium powder specific surface area of preparation is 45.43m2/ g, average grain diameter is
2.5um。
Embodiment 2
（1）By 50g High Purity Palladiums with 480mL aqua regia dissolutions into chlorine palladium acid solution, adding deionized water makes cumulative volume be 2000ml, dense
Spend for 2.4%（Calculated with simple substance palladium）.
（2）The aqueous solution that 0.2gPVP is dissolved into 0.2% with deionized water is weighed, it is stand-by.（1）Middle addition 250ml concentration
It is PH=10~11, water-bath for 400g/L Carbon Dioxide sodium solution adjusting body system so that solution temperature is 35~45 DEG C, then is added
Enter the PVP solution dissolved, stir.
（3）Measure 80% hydrazine hydrate（Mass concentration）Solution 50ml, adds 450ml deionized waters and is diluted, in stirring bar
The hydrazine hydrate solution diluted was added in 3 minutes under part above-mentioned（2）Solution in reduced, charging finish after, after
Continuous stirring 30 minutes.
（4）After after slurries clarification, supernatant liquor is drawn, deionized water washing is added, cyclic washing 15 times to electrical conductivity is
18s/cm, vacuum drying is 38h at 80 DEG C, and the ultrafine palladium powder specific surface area of preparation is 75.8 m2/ g, average grain diameter is 4.6um.
Embodiment 3
（1）By 25g High Purity Palladiums with 250mL aqua regia dissolutions into chlorine palladium acid solution, adding deionized water makes cumulative volume be 1000ml, dense
Spend for 2.4%（Calculated with simple substance palladium）
（2）The aqueous solution that 0.05gPVP is dissolved into 0.2% with deionized water is weighed, it is stand-by.（1）Middle addition 500ml concentration is
400g/L sodium hydroxide solution adjustment system is PH=10~11, water-bath so that solution temperature is 30~40 DEG C.
（3）Weigh 50g and analyze pure glucose, plus 500ml deionized waters are dissolved, will dissolve under agitation
Glucose solution was added to above-mentioned in 3 minutes（2）Solution in reduced, charging finish after, continue stir 30 minutes.Treat
After slurries clarification, supernatant liquor is drawn, deionized water washing is added, cyclic washing 15 times to electrical conductivity is 18s/cm, and vacuum is dried
Do as 38h at 80 DEG C, the ultrafine palladium powder specific surface area of preparation is 25.3 m2/ g, average grain diameter is 4.2um.
The foregoing is only a preferred embodiment of the present invention, is not intended to limit the scope of the present invention.
Claims (10)
1. the preparation method of high-specific surface area ultrafine palladium powder, it is characterised in that comprise the following steps：
（1）High Purity Palladium aqua regia dissolution is into chlorine palladium acid solution, and obtained solution is the first solution；
（2）Weigh polyvinylpyrrolidone and aqueous povidone solution is dissolved into deionized water, it is stand-by；In the first solution
It is PH=9~12 to plant and add aqueous slkali adjustment system, then adds the aqueous povidone solution dissolved and stirs,
Obtained solution is the second solution, and controls the temperature of the second solution；
（3）By reducing agent deionized water dissolved dilution, obtained solution is the 3rd solution, and the 3rd solution is slowly added into second
Solution is reduced, after addition is finished, and is continued to stir 30 minutes, is obtained ultrafine palladium powder slurries；
（4）After after the clarification of ultrafine palladium powder slurries, supernatant liquor is drawn, deionized water washing, cyclic washing to electrical conductivity ﹤ is added
20us/cm, and vacuum drying, that is, the product obtained are ultrafine palladium powder.
2. the preparation method of high-specific surface area ultrafine palladium powder according to claim 1, it is characterised in that：The step（1）
In be into chlorine palladium acid solution, to add High Purity Palladium aqua regia dissolution deionized water adjustment solution concentration, solution is calculated with simple substance palladium
Concentration is 2.0%~4.0%.
3. the preparation method of high-specific surface area ultrafine palladium powder according to claim 1, it is characterised in that：The step（2）
The consumption of middle polyvinylpyrrolidone is the 0.1%~0.5% of the mass parts of High Purity Palladium.
4. the preparation method of high-specific surface area ultrafine palladium powder according to claim 1, it is characterised in that：The step（2）
In aqueous slkali be natrium carbonicum calcinatum or sodium hydroxide.
5. the preparation method of high-specific surface area ultrafine palladium powder according to claim 1, it is characterised in that：The step（2）
The middle temperature for controlling the second solution is 30~50 DEG C.
6. the preparation method of high-specific surface area ultrafine palladium powder according to claim 1, it is characterised in that：The step（3）
The reducing agent of middle selection is hydrazine hydrate, glucose.
7. the preparation method of high-specific surface area ultrafine palladium powder according to claim 1, it is characterised in that：The step（3）
The middle adition process time that 3rd solution is slowly added to the second solution is 1~3min.
8. the preparation method of high-specific surface area ultrafine palladium powder according to claim 1, it is characterised in that：The step（4）
Middle mode of washing washs for mashing.
9. the preparation method of high-specific surface area ultrafine palladium powder according to claim 1, it is characterised in that：The step（4）
Middle vacuum drying is that 36~42h is dried under 80 DEG C of vacuum condition.
10. the ultra-fine palladium of high-specific surface area made from the preparation method of high-specific surface area ultrafine palladium powder according to claim 1
Powder.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109865845A (en) * | 2019-03-29 | 2019-06-11 | 无锡英特派金属制品有限公司 | The preparation method of high-density palladium powder |
| CN115070058A (en) * | 2022-08-16 | 2022-09-20 | 西安锐创微米科技有限公司 | Preparation method of high-crystallinity and high-sphericity palladium powder with strong oxidation resistance |
| CN115889799A (en) * | 2022-10-28 | 2023-04-04 | 广东微容电子科技有限公司 | Preparation method of spherical nano palladium powder for high-end MLCC inner electrode slurry |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109865845A (en) * | 2019-03-29 | 2019-06-11 | 无锡英特派金属制品有限公司 | The preparation method of high-density palladium powder |
| CN115070058A (en) * | 2022-08-16 | 2022-09-20 | 西安锐创微米科技有限公司 | Preparation method of high-crystallinity and high-sphericity palladium powder with strong oxidation resistance |
| CN115070058B (en) * | 2022-08-16 | 2022-11-01 | 西安锐创微米科技有限公司 | Preparation method of high-crystallinity and high-sphericity palladium powder with strong oxidation resistance |
| CN115889799A (en) * | 2022-10-28 | 2023-04-04 | 广东微容电子科技有限公司 | Preparation method of spherical nano palladium powder for high-end MLCC inner electrode slurry |
| CN115889799B (en) * | 2022-10-28 | 2023-10-20 | 广东微容电子科技有限公司 | Preparation method of spherical nano palladium powder for high-end MLCC inner electrode slurry |
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