CN114378298B - Preparation method of superfine platinum powder - Google Patents
Preparation method of superfine platinum powder Download PDFInfo
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- CN114378298B CN114378298B CN202111570770.6A CN202111570770A CN114378298B CN 114378298 B CN114378298 B CN 114378298B CN 202111570770 A CN202111570770 A CN 202111570770A CN 114378298 B CN114378298 B CN 114378298B
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- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 title claims abstract description 140
- 238000002360 preparation method Methods 0.000 title claims abstract description 12
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 claims abstract description 62
- 229910052697 platinum Inorganic materials 0.000 claims abstract description 45
- 239000002244 precipitate Substances 0.000 claims abstract description 33
- 229910001961 silver nitrate Inorganic materials 0.000 claims abstract description 31
- 239000008367 deionised water Substances 0.000 claims abstract description 21
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 21
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 21
- 238000010438 heat treatment Methods 0.000 claims abstract description 17
- 238000001914 filtration Methods 0.000 claims abstract description 16
- 238000003756 stirring Methods 0.000 claims abstract description 14
- 239000003638 chemical reducing agent Substances 0.000 claims abstract description 12
- 239000000126 substance Substances 0.000 claims abstract description 12
- 238000006243 chemical reaction Methods 0.000 claims abstract description 10
- 229910021607 Silver chloride Inorganic materials 0.000 claims abstract description 7
- HKZLPVFGJNLROG-UHFFFAOYSA-M silver monochloride Chemical compound [Cl-].[Ag+] HKZLPVFGJNLROG-UHFFFAOYSA-M 0.000 claims abstract description 7
- 238000005406 washing Methods 0.000 claims abstract description 7
- QCDFRRQWKKLIKV-UHFFFAOYSA-M chloroplatinum Chemical class [Pt]Cl QCDFRRQWKKLIKV-UHFFFAOYSA-M 0.000 claims abstract 2
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 claims description 12
- 238000000034 method Methods 0.000 claims description 11
- YRKCREAYFQTBPV-UHFFFAOYSA-N acetylacetone Chemical compound CC(=O)CC(C)=O YRKCREAYFQTBPV-UHFFFAOYSA-N 0.000 claims description 10
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 8
- 239000002253 acid Substances 0.000 claims description 8
- BDAGIHXWWSANSR-UHFFFAOYSA-N methanoic acid Natural products OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 0.000 claims description 8
- 238000001035 drying Methods 0.000 claims description 6
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims description 5
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 claims description 5
- 229910052700 potassium Inorganic materials 0.000 claims description 5
- 239000011591 potassium Substances 0.000 claims description 5
- 229910052708 sodium Inorganic materials 0.000 claims description 5
- 239000011734 sodium Substances 0.000 claims description 5
- OSWFIVFLDKOXQC-UHFFFAOYSA-N 4-(3-methoxyphenyl)aniline Chemical compound COC1=CC=CC(C=2C=CC(N)=CC=2)=C1 OSWFIVFLDKOXQC-UHFFFAOYSA-N 0.000 claims description 4
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims description 4
- 229910021529 ammonia Inorganic materials 0.000 claims description 4
- 235000019253 formic acid Nutrition 0.000 claims description 4
- 230000035484 reaction time Effects 0.000 claims description 3
- 238000001514 detection method Methods 0.000 claims description 2
- CLSUSRZJUQMOHH-UHFFFAOYSA-L platinum dichloride Chemical class Cl[Pt]Cl CLSUSRZJUQMOHH-UHFFFAOYSA-L 0.000 claims description 2
- 239000011780 sodium chloride Substances 0.000 claims description 2
- 239000000706 filtrate Substances 0.000 claims 1
- 239000002245 particle Substances 0.000 abstract description 8
- 239000002270 dispersing agent Substances 0.000 abstract description 5
- 238000004519 manufacturing process Methods 0.000 abstract description 5
- 239000000376 reactant Substances 0.000 abstract description 4
- 238000001291 vacuum drying Methods 0.000 abstract 1
- 239000000843 powder Substances 0.000 description 6
- 238000001000 micrograph Methods 0.000 description 4
- 230000003197 catalytic effect Effects 0.000 description 3
- KIDPOJWGQRZHFM-UHFFFAOYSA-N platinum;hydrate Chemical compound O.[Pt] KIDPOJWGQRZHFM-UHFFFAOYSA-N 0.000 description 3
- 238000005054 agglomeration Methods 0.000 description 2
- 230000002776 aggregation Effects 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 229920000036 polyvinylpyrrolidone Polymers 0.000 description 2
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 description 2
- 239000001267 polyvinylpyrrolidone Substances 0.000 description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 description 1
- 239000002202 Polyethylene glycol Substances 0.000 description 1
- 235000010489 acacia gum Nutrition 0.000 description 1
- 239000001785 acacia senegal l. willd gum Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 229910000510 noble metal Inorganic materials 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 229920001223 polyethylene glycol Polymers 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 239000002861 polymer material Substances 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
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
- B22F9/24—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from liquid metal compounds, e.g. solutions
Landscapes
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Manufacture Of Metal Powder And Suspensions Thereof (AREA)
Abstract
The invention discloses a preparation method of superfine platinum powder, which comprises the following steps: dissolving chloro-platinum salt in deionized water at normal temperature to obtain clear platinum-containing solution for later use; dissolving silver nitrate in deionized water at normal temperature to obtain a clear silver nitrate solution for later use; heating platinum-containing solution to a certain temperature under stirring, adding silver nitrate solution dropwise according to chemical weight, and detecting no free Ag after reaction + 、Cl ‑ Filtering the generated silver chloride precipitate, and collecting a platinum-containing solution; transferring the collected platinum-containing solution into a container, adding a reducing agent, stirring uniformly, heating to react, generating black precipitate in the system, filtering the precipitate, collecting the precipitate, washing the precipitate with deionized water for multiple times, and vacuum drying to obtain superfine platinum powder with the particle size ranging from 0.5 mu m to 1.0 mu m. The invention does not need strict control of pH value, temperature, reactant concentration and other technological conditions, does not need to add a high molecular dispersing agent, and is easy to realize the industrialized production of superfine platinum powder.
Description
Technical Field
The invention relates to a preparation method of superfine platinum powder, belonging to the field of powder material preparation.
Background
Platinum is widely used because of its special physical properties and better chemical stability and catalytic activity, and platinum powder is an important way for noble metal platinum to be used in a saving way, especially ultrafine platinum powder, and because of the reduced particle size, the use amount of platinum can be greatly reduced, and meanwhile, the special optical, electrical, magnetic and catalytic properties caused by the small-size effect lead the platinum to be widely applied in industry.
The superfine platinum powder is an important derivative product of platinum, and according to different application fields, the superfine platinum powder with different morphologies needs to be developed, wherein the superfine platinum powder comprises spherical powder, flaky powder, rod-shaped powder, dendritic powder and the like, and a solution chemical method is a main method for preparing the morphology-controllable superfine platinum powder.
A great deal of literature reports a method for preparing superfine platinum powder through solution chemical reaction, but in order to control morphology and reduce agglomeration, high polymer materials such as polyvinylpyrrolidone (PVP), polyethylene glycol, arabic gum and the like are generally required to be added as dispersing agents, and the concentration of platinum in a reaction solution is required to be controlled at a lower level so as to avoid agglomeration of platinum particles. However, in the industrial mass production process of ultrafine platinum powder, the polymer dispersant is extremely liable to remain on the surface of the powder, so that the usability such as the catalytic activity of the platinum powder is lowered. In addition, since the concentration of platinum in the reaction solution is low, the production lot of ultrafine platinum powder is hardly expanded.
Disclosure of Invention
The technical problem to be solved by the invention is to overcome the defects, and provide the preparation method of the superfine platinum powder, which does not need strict control of technological conditions such as pH value, temperature, reactant concentration and the like, does not need to add a high molecular dispersing agent, and is easy to realize industrialized production of the superfine platinum powder.
The method of the invention can be realized by the following technical scheme:
the preparation method of the superfine platinum powder comprises the following steps:
(1) Dissolving a certain amount of chloro-compound platinum salt into deionized water at normal temperature to obtain a clear platinum-containing solution for later use;
(2) Dissolving a certain amount of silver nitrate into deionized water at normal temperature to obtain a clarified silver nitrate solution for later use;
(3) Heating platinum-containing solution to a certain temperature under stirring, adding silver nitrate solution dropwise according to chemical metering, reacting for a certain time, and detecting no free Ag + 、Cl - Filtering the generated silver chloride precipitate, and collecting a platinum-containing solution;
(4) Transferring the collected platinum-containing solution into a container, adding a reducing agent, stirring uniformly, heating and reacting for a certain time to generate black precipitate in the system, filtering and collecting the obtained precipitate, washing the precipitate with deionized water for multiple times, and then drying in vacuum to obtain black superfine platinum powder with the particle size range of 0.5-1.0 mu m.
Preferably, the platinum chloride in the step (1) is potassium chloroplatinite, sodium chloroplatinite, chloroplatinic acid and ammonia chloroplatinic acid, and the concentration of platinum in the platinum-containing solution is 0.1mol/L to 0.8mol/L.
Preferably, the concentration of silver nitrate in the step (2) is 0.1mol/L to 0.8mol/L.
Preferably, the heating temperature in the step (3) ranges from 40 ℃ to 90 ℃ and the reaction time ranges from 7 hours to 12 hours.
Preferably, the free Ag in step (3) + 、Cl - The detection method comprises collecting reaction system solution, filtering to remove precipitate, dividing the obtained solution into two parts, dripping silver nitrate solution into one part, dripping sodium chloride solution into the other part, observing that no white precipitate is generated, and judging that no free Ag exists + 、Cl - 。
Preferably, the reducing agent added in the step (4) is formic acid, formaldehyde or acetylacetone.
Preferably, the reducing agent is used in step (4) in an amount of 1.5 to 3 times the theoretical amount.
Preferably, the heating reaction temperature in the step (4) ranges from 40 ℃ to 90 ℃ and the reaction time ranges from 6 hours to 9 hours.
The mechanism and the beneficial effects of the invention are as follows:
(1) In the invention, potassium chloroplatinite, sodium chloroplatinite, chloroplatinic acid or ammonia chloroplatinic acid react with silver nitrate to generate platinum hydrate, the hydrate is easy to reduce, and the platinum hydrate is used as a reactant to be beneficial to the generation of ultrafine platinum powder tending to flake;
(2) Because platinum hydrate is easy to reduce, formic acid, formaldehyde and acetylacetone with weak reducing capability are selected as reducing agents, and the reducing conditions are mild, so that the reduction of the size of platinum grains is facilitated;
(3) The method does not need strict control of process conditions such as pH value, temperature, reactant concentration and the like, does not need to add a high molecular dispersing agent, and is easy to realize industrialized production of superfine platinum powder.
Drawings
FIG. 1 is a scanning electron microscope image of the ultra-fine platinum powder prepared in example 1.
FIG. 2 is a scanning electron microscope image of the ultra-fine platinum powder prepared in example 2.
FIG. 3 is a scanning electron microscope image of the ultra-fine platinum powder prepared in example 3.
FIG. 4 is a scanning electron microscope image of the ultra-fine platinum powder prepared in example 4.
Detailed Description
For ease of understanding, the present invention will be further described with reference to the drawings and examples, in which specific descriptions are provided. It should be particularly pointed out that these descriptions are merely exemplary descriptions and do not constitute limitations on the scope of the invention. Many variations and modifications of the invention will be apparent to those skilled in the art in light of the teachings of this specification.
Example 1 (chloroplatinic acid)
The preparation method of the superfine platinum powder comprises the following steps:
(1) Dissolving a certain amount of chloroplatinic acid into deionized water at normal temperature to obtain a clear platinum-containing solution for standby, wherein the platinum-containing concentration of the solution is 0.5mol/L;
(2) Dissolving a certain amount of silver nitrate into deionized water at normal temperature to obtain a clarified silver nitrate solution for standby, wherein the concentration of the silver nitrate solution is 0.5mol/L;
(3) Heating the platinum-containing solution to 50 ℃ under stirring, then dropwise adding a silver nitrate solution according to the chemical weight, reacting for 8 hours, and detecting that no free Ag exists + 、Cl - Filtering the generated silver chloride precipitate, and collecting a platinum-containing solution;
(4) Transferring the collected platinum-containing solution into a container, adding acetylacetone serving as a reducing agent with the stoichiometric amount of 1.5 times, uniformly stirring, heating to 80 ℃ for reacting for 5 hours, generating black precipitate in the system, filtering the precipitate obtained by collection, washing the precipitate with deionized water for multiple times, and then drying in vacuum to obtain black platinum powder.
As shown in FIG. 1, the scanning electron microscope of the ultra-fine platinum powder of this example shows that the particle size of the prepared platinum powder is 0.5 μm to 1.0. Mu.m.
Example 2 (Potassium chloroplatinite)
The preparation method of the superfine platinum powder comprises the following steps:
(1) Dissolving a certain amount of potassium chloroplatinite into deionized water at normal temperature to obtain a clear platinum-containing solution for standby, wherein the platinum-containing concentration of the solution is 0.8mol/L;
(2) Dissolving a certain amount of silver nitrate into deionized water at normal temperature to obtain a clarified silver nitrate solution for standby, wherein the concentration of the silver nitrate solution is 0.8mol/L;
(3) Heating the platinum-containing solution to 70 ℃ under stirring, then dropwise adding silver nitrate solution according to the chemical weight, reacting for 7 hours, and detecting that no free Ag exists + 、Cl - Filtering the generated silver chloride precipitate, and collecting a platinum-containing solution;
(4) Transferring the collected platinum-containing solution into a container, adding formic acid serving as a reducing agent with the chemical dose being 2.0 times, uniformly stirring, heating to 90 ℃ for reaction for 4 hours, generating black precipitate in the system, filtering the precipitate obtained by collection, washing the precipitate with deionized water for multiple times, and then drying in vacuum to obtain black platinum powder.
As shown in FIG. 2, the scanning electron microscope of the ultra-fine platinum powder of this example shows that the particle size of the prepared platinum powder is 0.5 μm to 1.0. Mu.m.
Example 3 (sodium chloroplatinite)
The preparation method of the superfine platinum powder comprises the following steps:
(1) Dissolving a certain amount of sodium chloroplatinite into deionized water at normal temperature to obtain a clear platinum-containing solution for standby, wherein the platinum-containing concentration of the solution is 0.6mol/L;
(2) Dissolving a certain amount of silver nitrate into deionized water at normal temperature to obtain a clarified silver nitrate solution for standby, wherein the concentration of the silver nitrate solution is 0.6mol/L;
(3) Heating the platinum-containing solution to 80 ℃ under stirring, then dropwise adding a silver nitrate solution according to the chemical weight, reacting for 10 hours, and detecting that no free Ag exists + 、Cl - Filtering the generated silver chloride precipitate, and collecting a platinum-containing solution;
(4) Transferring the collected platinum-containing solution into a container, adding a reducing agent formaldehyde with the chemical dose being 3.0 times, uniformly stirring, heating to 60 ℃ for reaction for 4 hours, generating black precipitate in the system, filtering the precipitate obtained by collection, washing the precipitate with deionized water for multiple times, and then drying in vacuum to obtain black platinum powder.
As shown in FIG. 3, the scanning electron microscope of the ultra-fine platinum powder of this example shows that the particle size of the prepared platinum powder is 0.5 μm to 1.0. Mu.m, as can be seen from FIG. 3.
Example 4 (ammonium chloroplatinite)
The preparation method of the superfine platinum powder comprises the following steps:
(1) Dissolving a certain amount of chloroplatinic acid ammonia into deionized water at normal temperature to obtain a clear platinum-containing solution for standby, wherein the platinum-containing concentration of the solution is 0.3mol/L;
(2) Dissolving a certain amount of silver nitrate into deionized water at normal temperature to obtain a clarified silver nitrate solution for standby, wherein the concentration of the silver nitrate solution is 0.3mol/L;
(3) Heating the platinum-containing solution to 90 ℃ under stirring, then dropwise adding a silver nitrate solution according to the chemical weight, reacting for 4 hours, and detecting that no free Ag exists + 、Cl - Filtering the generated silver chloride precipitate, and collecting a platinum-containing solution;
(4) Transferring the collected platinum-containing solution into a container, adding acetylacetone serving as a reducing agent with the chemical dosage being 3.0 times, uniformly stirring, heating to 50 ℃ for reacting for 9 hours, generating black precipitate in the system, filtering, collecting the obtained precipitate, washing the precipitate with deionized water for multiple times, and then drying in vacuum to obtain black platinum powder.
As shown in FIG. 4, the scanning electron microscope of the ultra-fine platinum powder of this example shows that the particle size of the prepared platinum powder is 0.5 μm to 1.0. Mu.m, as can be seen from FIG. 4.
Claims (6)
1. The preparation method of the superfine platinum powder is characterized by comprising the following steps of:
(1) Dissolving a chloro-platinum salt in deionized water to obtain a clear platinum-containing solution for standby, wherein the concentration of platinum in the platinum-containing solution is 0.1 mol/L-0.8 mol/L;
(2) Dissolving silver nitrate into deionized water to obtain a clear silver nitrate solution for standby, wherein the concentration of the silver nitrate in the silver nitrate solution is 0.1 mol/L-0.8 mol/L;
(3) Heating the platinum-containing solution to 40-90 ℃ under the stirring condition, then dropwise adding a silver nitrate solution according to the chemical metering, reacting for 7-12 hours, and detecting that no free Ag exists + 、Cl - Filtering the generated silver chloride precipitate, and collecting a platinum-containing solution;
(4) Transferring the collected platinum-containing solution into a container, adding a reducing agent, uniformly stirring, heating and reacting for a certain time to generate black precipitate in the system, filtering and collecting the obtained precipitate, washing the precipitate with deionized water for multiple times, and then drying in vacuum to obtain superfine platinum powder;
the grain diameter of the superfine platinum powder is 0.5-1.0 mu m.
2. The method for preparing ultrafine platinum powder according to claim 1, wherein the platinum chloride salt in the step (1) is potassium chloroplatinate, sodium chloroplatinate, chloroplatinic acid or ammonia chloroplatinate.
3. The method for preparing ultrafine platinum powder according to claim 1, wherein the free Ag in the step (3) + 、Cl - The detection method comprises the following steps: filtering the reaction system solution to remove precipitate, dividing the obtained filtrate into two parts, dripping silver nitrate solution into one part, dripping sodium chloride solution into the other part, and judging that no free Ag is generated when no white precipitate is formed in observation + 、Cl - 。
4. The method for preparing ultrafine platinum powder according to claim 1, wherein the reducing agent added in the step (4) is formic acid, formaldehyde or acetylacetone.
5. The method for preparing ultrafine platinum powder according to claim 4, wherein the amount of the reducing agent is 1.5 to 3 times the theoretical amount.
6. The method for preparing ultrafine platinum powder according to any one of claims 1 to 5, wherein the heating reaction temperature in the step (4) is 40 ℃ to 90 ℃ and the reaction time is 6 to 9 hours.
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| CN202111570770.6A CN114378298B (en) | 2021-12-21 | 2021-12-21 | Preparation method of superfine platinum powder |
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| CN114378298B true CN114378298B (en) | 2024-04-02 |
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2021
- 2021-12-21 CN CN202111570770.6A patent/CN114378298B/en active Active
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|---|---|---|---|---|
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| US4396588A (en) * | 1981-03-09 | 1983-08-02 | Mpd Technology Corporation | Preparation of cis-diamminediaquaplatinum(II) nitrate |
| JPH03131533A (en) * | 1989-10-14 | 1991-06-05 | Tanaka Kikinzoku Kogyo Kk | Production of ruthenium nitrate solution |
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