CN111496270B - Method for preparing nano metal platinum particles - Google Patents
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- CN111496270B CN111496270B CN202010527444.6A CN202010527444A CN111496270B CN 111496270 B CN111496270 B CN 111496270B CN 202010527444 A CN202010527444 A CN 202010527444A CN 111496270 B CN111496270 B CN 111496270B
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- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 title claims abstract description 116
- 229910052697 platinum Inorganic materials 0.000 title claims abstract description 57
- 239000002245 particle Substances 0.000 title claims abstract description 54
- 238000000034 method Methods 0.000 title claims abstract description 32
- 229910052751 metal Inorganic materials 0.000 title claims abstract description 22
- 239000002184 metal Substances 0.000 title claims abstract description 22
- 150000001875 compounds Chemical class 0.000 claims abstract description 30
- 239000003638 chemical reducing agent Substances 0.000 claims abstract description 17
- 239000002243 precursor Substances 0.000 claims abstract description 16
- 238000001035 drying Methods 0.000 claims abstract description 8
- 229910017053 inorganic salt Inorganic materials 0.000 claims abstract description 8
- 239000008139 complexing agent Substances 0.000 claims abstract description 7
- 238000001914 filtration Methods 0.000 claims abstract description 6
- 238000005406 washing Methods 0.000 claims abstract description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 6
- 229910052783 alkali metal Inorganic materials 0.000 claims description 10
- 238000006243 chemical reaction Methods 0.000 claims description 9
- IKHGUXGNUITLKF-UHFFFAOYSA-N Acetaldehyde Chemical compound CC=O IKHGUXGNUITLKF-UHFFFAOYSA-N 0.000 claims description 8
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 6
- CIWBSHSKHKDKBQ-JLAZNSOCSA-N Ascorbic acid Chemical compound OC[C@H](O)[C@H]1OC(=O)C(O)=C1O CIWBSHSKHKDKBQ-JLAZNSOCSA-N 0.000 claims description 6
- -1 alkali metal formate Chemical class 0.000 claims description 6
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 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
- 150000001340 alkali metals Chemical class 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
- BDAGIHXWWSANSR-UHFFFAOYSA-N methanoic acid Natural products OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 0.000 claims description 4
- 239000001509 sodium citrate Substances 0.000 claims description 4
- NLJMYIDDQXHKNR-UHFFFAOYSA-K sodium citrate Chemical compound O.O.[Na+].[Na+].[Na+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O NLJMYIDDQXHKNR-UHFFFAOYSA-K 0.000 claims description 4
- 239000002253 acid Substances 0.000 claims description 3
- 235000010323 ascorbic acid Nutrition 0.000 claims description 3
- 239000011668 ascorbic acid Substances 0.000 claims description 3
- 229960005070 ascorbic acid Drugs 0.000 claims description 3
- 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 2
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 2
- IKHGUXGNUITLKF-XPULMUKRSA-N acetaldehyde Chemical compound [14CH]([14CH3])=O IKHGUXGNUITLKF-XPULMUKRSA-N 0.000 claims description 2
- 235000011054 acetic acid Nutrition 0.000 claims description 2
- 235000019253 formic acid Nutrition 0.000 claims description 2
- 150000004820 halides Chemical class 0.000 claims description 2
- WSFSSNUMVMOOMR-NJFSPNSNSA-N methanone Chemical compound O=[14CH2] WSFSSNUMVMOOMR-NJFSPNSNSA-N 0.000 claims description 2
- 229910017604 nitric acid Inorganic materials 0.000 claims description 2
- 238000002360 preparation method Methods 0.000 abstract description 8
- 238000005054 agglomeration Methods 0.000 abstract description 7
- 230000002776 aggregation Effects 0.000 abstract description 7
- 239000002105 nanoparticle Substances 0.000 abstract description 2
- 238000006722 reduction reaction Methods 0.000 description 10
- 229910000510 noble metal Inorganic materials 0.000 description 8
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 6
- 239000000706 filtrate Substances 0.000 description 6
- 229920005862 polyol Polymers 0.000 description 5
- 150000003077 polyols Chemical class 0.000 description 5
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 4
- 238000005265 energy consumption Methods 0.000 description 4
- 230000007935 neutral effect Effects 0.000 description 4
- VWDWKYIASSYTQR-UHFFFAOYSA-N sodium nitrate Chemical compound [Na+].[O-][N+]([O-])=O VWDWKYIASSYTQR-UHFFFAOYSA-N 0.000 description 4
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 description 3
- 230000005540 biological transmission Effects 0.000 description 3
- 239000003054 catalyst Substances 0.000 description 3
- 238000007598 dipping method Methods 0.000 description 3
- 239000010411 electrocatalyst Substances 0.000 description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- WCUXLLCKKVVCTQ-UHFFFAOYSA-M Potassium chloride Chemical compound [Cl-].[K+] WCUXLLCKKVVCTQ-UHFFFAOYSA-M 0.000 description 2
- 238000003917 TEM image Methods 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 239000000446 fuel Substances 0.000 description 2
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 description 2
- 239000004317 sodium nitrate Substances 0.000 description 2
- 235000010344 sodium nitrate Nutrition 0.000 description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 239000004280 Sodium formate Substances 0.000 description 1
- UBZYWIKLAYTIOV-UHFFFAOYSA-N [Na].CC=O Chemical compound [Na].CC=O UBZYWIKLAYTIOV-UHFFFAOYSA-N 0.000 description 1
- 239000011149 active material Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 239000008187 granular material Substances 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 239000002923 metal particle Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000001103 potassium chloride Substances 0.000 description 1
- 235000011164 potassium chloride Nutrition 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 239000003223 protective agent Substances 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- HLBBKKJFGFRGMU-UHFFFAOYSA-M sodium formate Chemical compound [Na+].[O-]C=O HLBBKKJFGFRGMU-UHFFFAOYSA-M 0.000 description 1
- 235000019254 sodium formate Nutrition 0.000 description 1
- 239000007790 solid phase Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
Images
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
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
Abstract
The invention provides a method for preparing nano metal platinum particles, which comprises the steps of dissolving a platinum precursor compound, a complexing agent and an auxiliary inorganic salt compound in water to form a solution, standing for a certain time, adding a reducing agent compound into the solution, reacting for a certain time, and finally carrying out subsequent treatment of filtering, washing and drying on the reacted system to obtain the metal platinum particles. The preparation method of the invention can stably react newly generated platinum nanoparticles, effectively avoid the agglomeration of the generated platinum particles, and prepare the metal platinum particles with excellent isotropic performance and uniform particle size distribution.
Description
Technical Field
The invention relates to a preparation method of granular noble metal, in particular to a preparation method of nano-metal platinum granules.
Background
At present, the platinum noble metal is a core active material of the fuel cell in the fields of catalysts and the like which are generally applied to the fuel cell. The preparation of platinum particles for catalysts by chemical reduction is the most common method at present. Including dip reduction and polyol reduction. The solid-phase dipping reduction method comprises the steps of dipping a platinum noble metal precursor and a carrier, drying and grinding the platinum noble metal precursor and the carrier, and introducing hydrogen into a tubular furnace for reduction at high temperature (generally more than 200 ℃), wherein the method has high energy consumption and the noble metal is unevenly distributed on the carbon carrier; the liquid phase dipping reduction method is that firstly, a noble metal precursor and a carbon carrier are dipped, and then a strong reducing agent is added for room temperature reduction, although the method is simple, rapid and has no energy consumption, the prepared electro-catalyst has large grain diameter and uneven grain diameter distribution. The most common polyol reduction method is that glycol and other polyols are used as a solvent and a reducing agent at the same time, the noble metal precursor is reduced into the electrocatalyst by heating (120-160 ℃) for 3-8 hours, and the electrocatalyst prepared by the method has small particle size and uniform dispersion because the polyols play a role of a protective agent at the same time, and has the defects of high energy consumption, incapability of recycling and high cost due to the oxidation of the glycol and other polyols in the reaction process. In addition, the platinum particles prepared by the chemical reduction methods have anisotropy and large particle size, are easy to age and grow in the using process and have poor stability.
Disclosure of Invention
The invention aims to provide a method for preparing nanoscale metal platinum particles with uniform particle size distribution, small particle size and isotropic performance. The method is realized through the following scheme.
A method for preparing nano metal platinum particles is implemented according to the following steps in sequence:
dissolving a platinum precursor compound, a complexing agent and an auxiliary inorganic salt compound in water to form a solution, keeping the pH value of the solution at 3-8, and standing for 24-72 hours at 10-40 ℃; the platinum precursor compound is selected from one or more of chloroplatinic acid, potassium chloroplatinate, sodium chloroplatinate, potassium chloroplatinate or sodium chloroplatinate, the complexing agent is selected from one or more of formaldehyde, acetaldehyde, citric acid and sodium citrate, and the auxiliary inorganic salt compound is selected from one or more of nitric acid of alkali metal and halide of alkali metal;
(II) adding a reducing agent compound into the solution after standing in the step I, and reacting for 30-180 minutes at 20-50 ℃; the reducing agent compound is selected from one or more of ascorbic acid, formic acid, acetic acid, alkali metal formate, alkali metal acetate, acetaldehyde and alkali metal acetaldehyde compound.
In order to obtain a finished product with high purity, the solution obtained after the reaction in the step II is subjected to subsequent treatment comprising filtration, washing and drying, and the step II can be carried out by adopting the same method in the prior art and then is subjected to drying treatment when the solution is washed to be neutral.
In the step I, the molar ratio of platinum of the platinum precursor compound to the complexing agent is 1 (1-20), and the reaction is more complete.
In the step I, the molar ratio of platinum of the platinum precursor compound to the auxiliary inorganic salt compound is 1 (5-30), so that granular agglomeration can be effectively prevented in the subsequent reduction reaction.
And in the second step, adding the reducing agent compound according to the molar ratio of the reducing agent compound to platinum of the platinum precursor compound of (10-50) to 1, so that the reaction is more complete.
In the step II, when the molar concentration of the reducing agent compound is 0.001-0.05 mol/L, the reaction of reducing platinum is more moderate, and the particles are favorably not agglomerated.
Compared with the existing method for preparing the noble metal platinum particles, the method has the following advantages:
1. in the preparation method, because the auxiliary inorganic salt compound is added in the step I, the newly generated platinum nano particles can be stably reacted, the agglomeration of the generated platinum particles is effectively avoided, and the utilization rate of platinum can be improved.
2. The preparation method adopts a two-step method, namely the reducing agent is added after the solution in the step I is kept still for a certain time, so that the metal platinum particles with excellent isotropy and uniform particle size distribution can be prepared, the average particle size is 1.0-2.5 nm, the platinum particles prepared by the existing one-step method are in a crotch shape, the average particle size is about 3.0-7.0 nm, and the platinum particles are anisotropic.
3. The preparation method has mild conditions, easily controlled process and lower energy consumption during batch preparation.
Drawings
FIG. 1 Transmission Electron micrograph of platinum particles of example 1
FIG. 2 Transmission Electron micrograph of platinum particles of comparative example 1
FIG. 3 particle size distribution diagram of platinum particles obtained in example 1
Detailed Description
Example 1
A method for preparing nano metal platinum particles is implemented according to the following steps in sequence:
dissolving 0.01mmol of chloroplatinic acid, 0.1mmol of sodium citrate and 0.05mmol of sodium nitrate in water to form a solution, adjusting and maintaining the pH value of the solution to be 3-5 by using sodium hydroxide, and standing at 10 ℃ for 72 hours;
(II) adding 100ml of ascorbic acid with the concentration of 0.001mol/L into the solution after standing in the step I, and reacting for 180 minutes at 20 ℃.
(III) filtering the solution obtained after the reaction in the step II, washing until the pH value of the filtrate is neutral, and drying the washed filtrate.
The metal platinum particles prepared by the steps are taken as a comparative example 1, the transmission electron microscope adopting the reducing agent and the precursor of the prior art and the like prepared by one step method is shown as figures 1 and 2 respectively under the same conditions, the figure 1 shows the metal platinum particles of the embodiment 1, the figure 2 shows the metal platinum of the comparative example 1, and the comparison of the two figures shows that the metal platinum particles of the embodiment 1 basically have no agglomeration, while the metal platinum of the comparative example 1 is in an obvious tree branch shape, which shows that certain agglomeration exists. The metallic platinum particles of example 1, however, are substantially isotropic, and are advantageous in terms of the utilization efficiency of platinum when used as a catalyst.
The particle size distribution of the platinum metal particles of example 1 is shown in FIG. 3, which shows that the average particle size is 1.7nm and the particle size distribution is uniform.
Example 2
A method for preparing nano metal platinum particles is implemented according to the following steps in sequence:
dissolving 0.01mmol of potassium chloroplatinite, 0.2mmol of acetaldehyde and 0.3mmol of potassium chloride in water to form a solution, adjusting and maintaining the pH value of the solution to be 4-8 by using potassium hydroxide, and standing for 50 hours at 30 ℃; (II) adding 10ml of sodium formate with the concentration of 0.05mol/L into the solution after standing in the step I, and reacting for 30 minutes at 50 ℃.
(III) filtering the solution obtained after the reaction in the step II, washing until the pH value of the filtrate is neutral, and drying the washed filtrate.
The metal platinum particles prepared by the steps are observed by a transmission electron microscope, and basically have no agglomeration, and the average particle size of the metal platinum particles in the embodiment is 2.4nm and uniform in particle size distribution through a particle size test.
Example 3
A method for preparing nano metal platinum particles is implemented according to the following steps in sequence:
dissolving 0.01mmol of sodium chloroplatinate, 0.01mmol of sodium citrate and 0.15mmol of sodium nitrate in water to form a solution, adjusting and maintaining the pH value of the solution to be 3-7 by using sodium hydroxide, and standing for 24 hours at 40 ℃;
(II) adding 60ml of 0.005mol/L acetaldehyde sodium into the solution after standing in the step I, and reacting at 30 ℃ for 120 minutes.
(III) filtering the solution obtained after the reaction in the step II, washing until the pH value of the filtrate is neutral, and drying the washed filtrate.
The metal platinum particles prepared by the steps are observed by a transmission electron microscope, and basically have no agglomeration, and the average particle size of the metal platinum particles in the embodiment is 1.2nm and uniform in particle size distribution through a particle size test.
Claims (6)
1. A method for preparing nano metal platinum particles is characterized by comprising the following steps: the method is implemented according to the following steps in sequence,
dissolving a platinum precursor compound, a complexing agent and an auxiliary inorganic salt compound in water to form a solution, keeping the pH value of the solution at 3-8, and standing for 24-72 hours at 10-40 ℃; the platinum precursor compound is selected from one or more of chloroplatinic acid, potassium chloroplatinate, sodium chloroplatinate, potassium chloroplatinate or sodium chloroplatinate, the complexing agent is selected from one or more of formaldehyde, acetaldehyde, citric acid and sodium citrate, and the auxiliary inorganic salt compound is selected from one or more of nitric acid of alkali metal and halide of alkali metal;
(II) adding a reducing agent compound into the solution after standing in the step I, and reacting for 30-180 minutes at 20-50 ℃; the reducing agent compound is selected from one or more of ascorbic acid, formic acid, acetic acid, alkali metal formate, alkali metal acetate, acetaldehyde and alkali metal acetaldehyde compound.
2. The method of preparing nano-metallic platinum particles according to claim 1, wherein: and (3) carrying out subsequent treatment comprising filtration, washing and drying on the solution after the reaction in the step II.
3. The method for preparing nano-metallic platinum particles as set forth in claim 1 or 2, wherein: in the step I, the molar ratio of platinum of the platinum precursor compound to the complexing agent is 1 (1-20).
4. The method for preparing nano-metallic platinum particles as set forth in claim 1 or 2, wherein: in the step I, the molar ratio of platinum of the platinum precursor compound to the auxiliary inorganic salt compound is 1 (5-30).
5. The method for preparing nano-metallic platinum particles as set forth in claim 1 or 2, wherein: and in the second step, adding a reducing agent compound according to the molar ratio of the reducing agent compound to platinum of the platinum precursor compound of (10-50) to 1.
6. The method of preparing nano-metallic platinum particles according to claim 5, wherein: and in the step II, adding a reducing agent compound with the molar concentration of 0.05-0.001 mol/L.
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| CN115194171B (en) * | 2022-05-27 | 2023-09-26 | 氢电中科（广州）新能源设备有限公司 | Highly dispersed platinum nanoparticle solution and preparation method thereof |
| CN115365509B (en) * | 2022-08-19 | 2023-12-22 | 中钢集团南京新材料研究院有限公司 | Preparation method of platinum nanocrystalline, platinum nanocrystalline and catalyst |
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