CN113134623B - Water-soluble amorphous noble metal nano particle and preparation method thereof - Google Patents
Water-soluble amorphous noble metal nano particle and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a water-soluble amorphous noble metal nano particle and a preparation method thereof, relating to the technical field of noble metal nano materials. The method comprises the following steps: and (2) uniformly dispersing a noble metal source and a reducing agent in a water solvent, then adjusting the pH value of the reaction solution to 2-8, and carrying out hydrothermal reaction at 120-200 ℃ for 10-20 h to obtain the water-soluble amorphous noble metal nano particles. The method for preparing the noble metal nanoparticles provided by the invention is simple and controllable, can be used for mass preparation, and is easy for industrialization.
Description
Technical Field
The invention relates to the technical field of precious metal nano materials, in particular to a water-soluble amorphous precious metal nano particle and a preparation method thereof.
Background
The water solubility can improve the application range of the metal nanoparticles, so that the metal nanoparticles can be widely applied to the aspects of catalysis, biology, medical treatment, fine chemical engineering and the like. In the field of catalysis, amorphous metal nanoparticle materials are used as catalysts to improve catalytic activity and selectivity. Compared with crystals, the amorphous metal particles are more flexible in application, amorphous phase atoms are randomly arranged, more randomly oriented unsaturated bonds are possessed, and the adsorption of reactants is facilitated. Meanwhile, a large number of flexibly changeable local structures exist in the amorphous phase, so that charge transfer between the active sites and intermediates can be accelerated.
At present, in the method for synthesizing water-soluble nanoparticles, whether the method is a direct reduction method or a post-synthesis surface modification method, a template or a surfactant is required to be added to modify or adsorb long-chain hydrophilic groups on the metal surface. Some modifying groups are difficult to remove, practical application is limited, controllability is poor, and the prepared particles are wide in size distribution and easy to precipitate in water. In the prior art, the realization of one-step metal reduction and surface hydrophilic modification processes during the preparation of water-soluble amorphous noble metal nanoparticles is only reported, so that the amorphous noble metal nanoparticles with high dispersion in a water solvent are prepared without additionally adding long-chain hydrophilic groups, and a foundation is laid for widening the application of the metal nanoparticles.
Disclosure of Invention
The present invention has been made to solve the above-mentioned problems occurring in the prior art, and an object of the present invention is to provide a method for preparing water-soluble amorphous noble metal nanoparticles, which can directly obtain water-soluble noble metal nanomaterials having different degrees of crystallinity and different compositions and modified with hydrophilic phosphate groups as required, by reacting a reducing inorganic acid such as sodium hypophosphite with a noble metal salt. And the special coordination environment on the surface of the metal particles enables the metal particles to be well dispersed on various substrates. The obtained carbon composite material is applied to electrocatalytic water decomposition.
The first object of the present invention is to provide a method for preparing water-soluble amorphous noble metal nanoparticles, comprising the steps of:
and (2) uniformly dispersing a noble metal source and a reducing agent in a water solvent, then adjusting the pH value of the reaction solution to 2-8, and carrying out hydrothermal reaction at 120-200 ℃ for 10-20 h to obtain the water-soluble amorphous noble metal nano particles.
Preferably, the noble metal source comprises one or more of a platinum source, a rhodium source, an iridium source, a ruthenium source, an osmium source.
Preferably, the platinum source is platinum chloride, chloroplatinic acid or chloroplatinic acid salt;
the iridium source is iridium chloride, chloroiridate, iridium acetate, iridium sulfate or chloroiridate;
the ruthenium source is ruthenium chloride, chlorine ruthenic acid, ruthenium acetate or chlorine ruthenate;
the rhodium source is rhodium chloride, chlororhodic acid, rhodium acetate or chlororhodate;
the iridium source is osmium chloride, osmium chloride tetroxide, osmium acetate or osmium chloride tetroxide.
Preferably, the reducing agent is hypophosphorous acid, hypophosphite, phosphorous acid, phosphite or phosphoric acid.
Preferably, the pH value of the reaction solution is adjusted by using an alkali liquor, wherein the alkali liquor is sodium hydroxide, potassium hydroxide or ammonia water.
Preferably, the molar ratio of the reducing agent to the noble metal source is 1:0.01 to 0.1.
The second purpose of the invention is to provide water-soluble amorphous noble metal nanoparticles, wherein the particle size of the nanoparticles is 1-2 nm.
The third object of the present invention is to provide a water-soluble amorphous noble metal nanoparticle dispersion prepared by uniformly dispersing the above nanoparticles in an aqueous solvent, which dispersion is stable in a solution having a pH ranging from 1 to 14.
The fourth purpose of the invention is to provide a composite, which comprises a carbon-based carrier and the noble metal nanoparticles loaded on the carbon-based carrier.
A fifth object of the present invention is to provide a method for preparing a complex, comprising the steps of: uniformly dispersing the carbon-based carrier and the noble metal nanoparticles in an aqueous solvent in an ultrasonic mode, and carrying out centrifugal washing for multiple times to obtain the compound.
Compared with the prior art, the invention has the beneficial effects that:
according to the method for preparing the noble metal nanoparticles, metal ions are rapidly reduced by hypophosphite under a hydrothermal condition, meanwhile, the pH value in a reaction system is adjusted, the reduction rate is controlled, phosphate species are adsorbed on the surface of a metal crystal nucleus, and the crystal nucleus is inhibited from growing by electrostatic repulsion force so as to be maintained in a low-crystallization and high-dispersion state; because the generated metal particles have low size (less than or equal to 1nm) and the surface is coated by polar groups, the metal particles can be efficiently dispersed in a high-polarity solvent (such as H)2O) in (A).
The method for preparing the noble metal nanoparticles provided by the invention is simple and controllable, can be used for mass preparation, and is easy for industrialization.
The invention can prepare amorphous water-soluble single/multi-metal nano particles by regulating and controlling the types of the added metal salts.
The method provided by the invention does not need to additionally add long-chain hydrophilic groups, and realizes metal reduction and surface hydrophilic modification in one step.
The noble metal nanoparticles provided by the invention have uniform particle size of 1-5 nm, and can be well dispersed in water and ethanol.
The dispersion provided by the invention has good stability in a wide pH range (1-14).
The present invention provides a dispersion that can achieve high dispersion on various types of substrates such as carbon materials, metal oxides, and the like.
Drawings
Figure 1 TEM image of noble metal nanoparticles provided in example 1.
Fig. 2 is a TEM image of a composite of amorphous platinum nanoparticles supported on carbon nanotubes as provided in example 6.
FIG. 3 is a TEM image of a composite of amorphous platinum nanoparticles supported on carbon black as provided in example 7.
Fig. 4 is an XRD pattern of the composite of amorphous platinum nanoparticles supported on carbon black provided in example 7.
FIG. 5 is an XPS plot of composites of example 7 with amorphous platinum nanoparticles supported on carbon black.
Fig. 6 is a TEM image of a composite of amorphous platinum nanoparticles supported on graphene provided in example 8.
FIG. 7 is a TEM image of a composite of amorphous iridium nanoparticles supported on carbon black as provided in example 9.
Detailed Description
In order to make the technical solutions of the present invention better understood and enable one skilled in the art to practice the present invention, the present invention is further described below with reference to specific examples and drawings, but the examples are not intended to limit the present invention.
It should be noted that the experimental methods described in the following examples are all conventional methods unless otherwise specified; the reagents and materials used are commercially available, unless otherwise specified.
The technical solution of the present invention is further described with reference to the following specific examples.
Example 1
A preparation method of water-soluble amorphous noble metal nanoparticle dispersion liquid comprises the following steps:
(1) weighing 400mg of sodium hypophosphite according to the proportion and dissolving in 7mL of deionized water; adding 1ml of prepared chloroplatinic acid solution (10mg/ml), and uniformly stirring; continuously adding 2ml of sodium hydroxide solution (8mg/ml), and stirring at normal temperature for 30min to obtain light yellow clear liquid; the mixed solution is put into a reaction kettle, and the hydrothermal condition is as follows: 180 ℃ for 12 h.
(2) Cooling to normal temperature, taking out the hydrothermal product, and then carrying out centrifugal treatment at the centrifugal speed of 8000r.p.m for 5 min; and dispersing the precipitated noble metal nano particles into water to obtain a noble metal nano particle dispersion liquid with a certain concentration.
Example 2
A preparation method of water-soluble amorphous noble metal nanoparticles comprises the following steps:
(1) weighing 400mg of sodium hypophosphite according to the proportion and dissolving in 7mL of deionized water; adding 1ml of prepared iridium chloride solution (10mg/ml), and uniformly stirring; continuously adding 1.7ml of sodium hydroxide solution (8mg/ml), and stirring at normal temperature for 30 min; the mixed solution is put into a reaction kettle, and the hydrothermal condition is as follows: 180 ℃ for 12 h.
(2) Cooling to normal temperature, taking out the hydrothermal product, and then carrying out centrifugal treatment at the centrifugal rotation speed of 10000r.p.m for 7 min; and dispersing the precipitated noble metal nano particles into water to obtain a noble metal nano particle dispersion liquid with a certain concentration.
Example 3
A method for preparing water-soluble amorphous noble metal nanoparticles, which is different from the above-mentioned examples in that two metal precursors are introduced, comprising the following steps:
(1) weighing 400mg of sodium hypophosphite according to the proportion and dissolving in 7mL of deionized water; adding 0.5ml of chloroplatinic acid solution (10mg/ml) and 0.5ml of iridium chloride solution (10mg/ml), and uniformly stirring; continuously adding 2ml of sodium hydroxide solution (8mg/ml), stirring at normal temperature for 30min, and filling into a reaction kettle under the hydrothermal condition: at 180 ℃ for 12 h;
(2) cooling to normal temperature, taking out the hydrothermal product, and then carrying out centrifugal treatment at the centrifugal rotation speed of 10000r.p.m for 6 min; and dispersing the precipitated noble metal nano particles into water to obtain a noble metal nano particle dispersion liquid with a certain concentration. .
Example 4
A method for preparing water-soluble amorphous noble metal nanoparticles, which is different from the above-mentioned examples in that two metal precursors are introduced, comprising the following steps:
(1) weighing 400mg of sodium hypophosphite according to the proportion and dissolving in 7mL of deionized water; adding 0.5ml of chloroplatinic acid solution (10mg/ml) and 0.5ml of rhodium chloride solution (10mg/ml), and uniformly stirring; continuously adding 2ml of sodium hydroxide solution (8mg/ml), stirring at normal temperature for 30min, and filling into a reaction kettle, wherein the hydrothermal conditions are as follows: at 180 ℃ for 12 h;
(2) cooling to normal temperature, taking out the hydrothermal product, and then carrying out centrifugal treatment at a centrifugal speed of 8000r.p.m for 7 min; and dispersing the precipitated noble metal nano particles into water to obtain a noble metal nano particle dispersion liquid with a certain concentration.
Example 5
A method for preparing water-soluble amorphous noble metal nanoparticles, which is different from the above-mentioned examples in that three metal precursors are introduced, comprising the following steps:
(1) weighing 400mg of sodium hypophosphite according to the proportion and dissolving in 7mL of deionized water; adding 0.5ml of chloroplatinic acid solution (10mg/ml), 0.5ml of iridium chloride solution (10mg/ml) and 0.5ml of rhodium chloride solution (10mg/ml), and uniformly stirring; continuously adding 2ml of sodium hydroxide solution (8mg/ml), stirring at normal temperature for 30min, and filling into a reaction kettle, wherein the hydrothermal conditions are as follows: at 180 ℃ for 12 h;
(2) cooling to normal temperature, taking out the hydrothermal product, and then carrying out centrifugal treatment at the centrifugal rotation speed of 10000r.p.m for 5 min; and dispersing the precipitated noble metal nano particles into water to obtain a noble metal nano particle dispersion liquid with a certain concentration.
Example 6
A method of preparing a composite comprising the steps of:
(1) dispersing 20mg of carbon nano tubes in 20ml of water, and carrying out ultrasonic treatment for 1 h; adding a certain amount of the noble metal dispersion liquid with fixed concentration provided in the embodiment 1, and continuing to perform ultrasonic treatment for 1 h;
(2) then carrying out centrifugal washing treatment, wherein the centrifugal rotating speed is 8000r.p.m, and the time is 5-7 min; washed twice with water and then 1 time with ethanol, platinum/carbon complex.
Example 7
A method of preparing a composite comprising the steps of:
(1) dispersing 20mg of carbon black in 20ml of water, and carrying out ultrasonic treatment for 1 h; adding a certain amount of the precious metal dispersion liquid with fixed concentration provided by the embodiment 1, and continuing to perform ultrasonic treatment for 1 h;
(2) then carrying out centrifugal washing treatment, wherein the centrifugal rotating speed is 10000r.p.m, and the time is 5-7 min; washed twice with water and then 1 time with ethanol, platinum/carbon complex.
Example 8
A method of preparing a composite comprising the steps of:
(1) dispersing 20mg of graphene in 20ml of water, and carrying out ultrasonic treatment for 1 h; adding a certain amount of the precious metal dispersion liquid with fixed concentration provided by the embodiment 1, and continuing to perform ultrasonic treatment for 1 h;
(2) then carrying out centrifugal washing treatment, wherein the centrifugal rotating speed is 8000-10000r.p.m, and the time is 5-7 min; washed twice with water and then 1 time with ethanol, platinum/carbon complex.
Example 9
A method of preparing a composite comprising the steps of:
(1) dispersing 20mg of carbon black in 20ml of water, and carrying out ultrasonic treatment for 1 h; adding a certain amount of the precious metal dispersion liquid with fixed concentration provided by the embodiment 2, and continuing to perform ultrasonic treatment for 1 h;
(2) then carrying out centrifugal washing treatment, wherein the centrifugal rotating speed is 8000-10000r.p.m, and the time is 5-7 min; washed twice with water and then 1 time with ethanol, iridium/carbon complex.
In order to illustrate the relevant performance of the composite material prepared by the preparation method provided by the invention, the precious metal nanoparticles provided in example 1 and the composites provided in examples 6 to 9 are tested for the relevant performance, which is specifically shown in fig. 1 to 5.
Figure 1 TEM image of noble metal nanoparticles provided in example 1.
As can be seen from FIG. 1, the prepared platinum nanoparticles are highly uniformly dispersed, have a particle size of about 1-2nm, and have an amorphous structure.
Fig. 2 is a TEM image of a composite of amorphous platinum nanoparticles supported on carbon nanotubes as provided in example 6.
As can be seen from FIG. 2, the prepared platinum nanoparticles can be well dispersed on the surface of the carbon nanotubes by simple mechanical mixing, and the particle size is maintained at 1-2 nm. The carrier not only helps to disperse the platinum nanoparticles, but also is expected to reduce nanoparticle agglomeration in the actual catalytic process.
FIG. 3 is a TEM image of a composite of amorphous platinum nanoparticles supported on carbon black as provided in example 7.
As can be seen from fig. 3, platinum nanoparticles can be supported on the surface of the porous carbon black in the same supporting manner as in example 6. The metal particles are uniformly dispersed, the size is between 1 and 2nm, and the metal loading can be regulated and controlled between 0 and 50 weight percent.
Fig. 4 is an XRD pattern of the composite of amorphous platinum nanoparticles supported on carbon black provided in example 7.
As shown in the XRD spectrum of fig. 4, the amorphous platinum nanoparticles supported only the peak of the carrier carbon in the crystal structure of the carbon black composite, showing that the prepared platinum nanoparticles are mainly in an amorphous state, corresponding to the TEM result.
FIG. 5 is an XPS survey of composites of example 7 with amorphous platinum nanoparticles supported on carbon black.
From the XPS survey spectrum of FIG. 5, it can be seen that the constituent elements of the carbon black composite supported by amorphous platinum nanoparticles are Pt, P, O and C.
Fig. 6 is a TEM image of a composite of amorphous metal platinum nanoparticles supported on graphene provided in example 8.
As can be seen from fig. 6, platinum nanoparticles can be supported on the surface of graphene in the same supporting manner as in example 6. The particles are uniformly dispersed and have a size of 1-2 nm. The type of support may be selected according to the reaction requirements.
FIG. 7 is a TEM image of a composite of amorphous iridium nanoparticles supported on carbon black as provided in example 9.
As can be seen from fig. 7, the iridium nanoparticles can be supported on the surface of the graphene in the same supporting manner as in example 6. The particles are uniformly dispersed and have a size of 1-2 nm. The type of support may be selected according to the reaction requirements.
In conclusion, in the method for preparing the noble metal nanoparticles, metal ions are rapidly reduced by hypophosphite under the hydrothermal condition, meanwhile, the pH value in a reaction system is adjusted, the reduction rate is controlled, phosphate species are adsorbed on the surface of a metal crystal nucleus, and the crystal nucleus is inhibited from growing by electrostatic repulsion, so that the crystal nucleus is maintained in a low-crystallization and high-dispersion state; because the size of the generated metal particles is low (less than or equal to 1nm), the surface of the metal particles is coated by polar groups, and thus the metal particles can be efficiently dispersed in a high-polarity solvent (such as H)2O) in (A).
The method for preparing the noble metal nanoparticles provided by the invention is simple and controllable, can be used for mass preparation, and is easy for industrialization.
The invention can prepare amorphous water-soluble single/multi-metal nano particles by regulating and controlling the types of the added metal salts.
The method provided by the invention does not need to additionally add long-chain hydrophilic groups, and realizes metal reduction and surface hydrophilic modification in one step.
The noble metal nanoparticles provided by the invention have uniform particle size of 1-5 nm, and can be well dispersed in water and ethanol.
The dispersion provided by the invention has good stability in a wide pH range (1-14).
The present invention provides a dispersion that can achieve high dispersion on various types of substrates such as carbon materials, metal oxides, and the like.
The present invention describes preferred embodiments and effects thereof. Additional variations and modifications in those embodiments may occur to those skilled in the art once they learn of the basic inventive concepts. Therefore, it is intended that the appended claims be interpreted as including preferred embodiments and all such alterations and modifications as fall within the scope of the invention.
Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.
Claims (7)
1. A preparation method of water-soluble amorphous noble metal nanoparticles is characterized by comprising the following steps:
uniformly dispersing a noble metal source and a reducing agent in a water solvent, then adjusting the pH value of a reaction solution to 2-8, and carrying out hydrothermal reaction at 120-200 ℃ for 10-20 h to obtain the water-soluble amorphous noble metal nanoparticles;
the particle size of the nano particles is 1-2 nm;
the noble metal source comprises one or more of a platinum source, a rhodium source, an iridium source, a ruthenium source and an osmium source; the reducing agent is hypophosphorous acid, hypophosphite, phosphorous acid, phosphite or phosphoric acid; the molar ratio of the reducing agent to the noble metal source is 1: 0.01-0.1.
2. The method of claim 1, wherein the source of platinum is platinic chloride, chloroplatinic acid, or chloroplatinate;
the iridium source is iridium chloride, chloroiridate, iridium acetate, iridium sulfate or chloroiridate;
the ruthenium source is ruthenium chloride, chlorine ruthenic acid, ruthenium acetate or chlorine ruthenate;
the rhodium source is rhodium chloride, chlororhodic acid, rhodium acetate or chlororhodate;
the osmium source is osmium chloride, osmium chloride tetroxide, osmium acetate or osmium chloride tetroxide.
3. The method of claim 1, wherein the pH of the reaction solution is adjusted by using an alkali solution, and the alkali solution is sodium hydroxide, potassium hydroxide or ammonia water.
4. A water-soluble amorphous noble metal nanoparticle obtained by the method of any one of claims 1 to 3.
5. A water-soluble amorphous noble metal nanoparticle dispersion, which is obtained by uniformly dispersing the nanoparticles according to claim 4 in an aqueous solvent, wherein the dispersion is stable in a solution having a pH in the range of 1 to 14.
6. A composite comprising a carbon-based support and the noble metal nanoparticles according to claim 4 supported on the carbon-based support.
7. A method for preparing the compound of claim 6, comprising the steps of: uniformly dispersing a carbon-based carrier and the noble metal nanoparticles as claimed in claim 4 in an aqueous solvent in an ultrasonic mode, and carrying out centrifugal washing for multiple times to obtain the compound.
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