CN112023977A - Y-type molecular sieve packaged platinum group noble metal nanoparticle catalyst and preparation method thereof - Google Patents
Y-type molecular sieve packaged platinum group noble metal nanoparticle catalyst and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a Y-type molecular sieve packaged platinum group noble metal nanoparticle catalyst and a preparation method thereof, wherein the preparation method comprises the following steps: dispersing a Y-type molecular sieve in an ethanol solvent, adding a platinum group precursor of platinum group elements in a cation form, carrying out in-hole adsorption on the platinum group precursor by the Y-type molecular sieve, and reducing the adsorbed sample in the ethanol solvent under a hydrogen atmosphere to prepare the Y-type molecular sieve packaged platinum group noble metal nanoparticle catalyst. The invention is based on the capillary action force and the electrostatic adsorption action force of micropores of the Y-shaped molecular sieve, utilizes the characteristic of electronegativity of a framework of the Y-shaped molecular sieve, and realizes the uniform packaging of the Y-shaped molecular sieve on platinum group noble metal nano particles in a normal pressure hydrogen atmosphere under a liquid phase condition by selecting a precursor of platinum group elements in a cation form.
Description
Technical Field
The invention belongs to the field of heterogeneous catalyst preparation, and particularly relates to a preparation method of a Y-type molecular sieve packaged platinum group noble metal nanoparticle catalyst.
Background
The noble metal nano catalyst has smaller particle size and higher specific surface area, so the noble metal nano catalyst shows good catalytic activity and has good application prospect in the fields of fine chemical production, medicine preparation and the like. In contrast, the noble metal nano-catalyst is easily agglomerated or sintered in the catalytic process due to the influence of particle size and specific surface area, thereby causing the reduction of catalytic activity. How to improve the stability of the noble metal nano-catalyst has become a key problem to be solved urgently in the field.
The molecular sieve is a crystalline silicate or aluminosilicate and is formed by connecting silicon-oxygen tetrahedron or aluminum-oxygen tetrahedron through oxygen bridge bonds, has a plurality of pore passages with uniform pore diameters and regularly arranged pores in the structure, and has excellent thermal stability and hydrothermal stability. By utilizing the limited domain effect of the molecular sieve pore channel, the noble metal nanoparticles encapsulated in the molecular sieve crystal can show very good stability, and are not easy to agglomerate and grow under the high-temperature condition.
At present, the method for encapsulating noble metal in a molecular sieve pore channel is mainly an in-situ encapsulation method, and the principle of the method is that a noble metal precursor is encapsulated into a molecular sieve crystal through a self-assembly process in the synthesis of the molecular sieve by utilizing the interaction of a primary/secondary structure unit and the noble metal precursor (mainly relating to ligand containing amino), and then the required molecular sieve encapsulated noble metal nano-particles are prepared through the steps of high-temperature roasting, reduction and the like. Typically, the Enrique Iglesia group uses SOD type molecular sieve, GIS type molecular sieve and ANA type molecular sieve as carriers, and selects Pt (NH)3)4(NO3)2For the precursor, platinum nanoparticles are successfully encapsulated into the molecular sieve crystal by an in-situ synthesis method (J.Am.chem.Soc.2012,134,17688), and the encapsulated platinum particles show good thermal stability. But such a preparation methodThe latter stages involve high temperature firing processes during which the encapsulated particles have a slightly longer potential.
The impregnation method is a traditional method for loading noble metal on a molecular sieve, for example, chloroplatinic acid or chloropalladic acid is loaded on various molecular sieve carriers by an impregnation method, and then steps of drying, calcining and the like are carried out to finally obtain the molecular sieve loaded noble metal type catalyst. However, the noble metal precursor inevitable in the impregnation process may be adsorbed on the outer surface of the molecular sieve, thereby causing the noble metal agglomeration or deactivation of the supported catalyst when used at high temperature. How to optimize the traditional impregnation method and prevent the noble metal precursor salt from being adsorbed and diffused on the outer surface of the molecular sieve, but diffused into the pore canal of the molecular sieve as much as possible is an effective way for solving the problem that the noble metal supported catalyst is easy to agglomerate and deactivate.
Disclosure of Invention
The invention aims to provide a Y-type molecular sieve packaged platinum group noble metal nanoparticle catalyst and a preparation method thereof, which are used for improving the thermal stability of platinum group noble metal nanoparticles. The Y molecular sieve has good high-temperature stability, precious metal particles are packaged into a Y molecular sieve pore channel, and the high-temperature agglomeration of the precious metal particles can be inhibited by utilizing the confinement effect of the Y molecular sieve pore channel.
In order to achieve the purpose, the invention adopts the technical scheme that:
a preparation method of platinum group nanoparticles encapsulated by Y-type molecular sieve comprises the following steps:
dispersing a Y-type molecular sieve in an ethanol solvent, adding a platinum group precursor of platinum group elements in a cation form, carrying out pore adsorption on the platinum group precursor by using the Y-type molecular sieve, and reducing the adsorbed sample in the ethanol solvent under a hydrogen atmosphere to obtain the Y-type molecular sieve encapsulated platinum group nanoparticles.
Further, the concentration of the Y-type molecular sieve in an ethanol solvent is 4-10 mg/ml, the platinum group precursor is calculated according to the platinum group elements, and the mass ratio of the platinum group elements to the Y-type molecular sieve is as follows: 0.5-4.0: 100, respectively; the platinum group precursor is obtained by dissolving platinum group precursor salt in ethanol; the platinum group precursor is added dropwise.
Further, the dispersion of the Y-type molecular sieve in ethanol and the addition of the platinum group precursor are carried out at room temperature; and adding the platinum group precursor, and stirring for 4-24 hours for adsorption.
Furthermore, the temperature condition of reducing the adsorbed sample in a hydrogen atmosphere is 40-70 ℃, the hydrogen pressure is 1-2.5 atmospheric pressure, and the reduction time is 24-36 hours.
Further, washing and vacuum drying the sample after reduction to obtain the Y-type molecular sieve encapsulated platinum group nanoparticles.
Furthermore, the molar ratio of silicon to aluminum of the Y-type molecular sieve is 2-7.
Furthermore, the molar ratio of silicon to aluminum of the Y-type molecular sieve is 2-5.
Further, the platinum group precursor salt is platinum acetylacetonate or palladium acetylacetonate.
A Y-type molecular sieve packaged platinum group noble metal nano-particle catalyst.
The invention relates to a preparation method of a Y-type molecular sieve packaged platinum group noble metal nanoparticle catalyst, which comprises the following steps:
using ethanol as a solvent, under the condition of 20-30 ℃, adsorbing and diffusing a platinum group noble metal precursor into a Y-type molecular sieve pore channel by using electrostatic adsorption force and capillary force of a molecular sieve on the precursor of a platinum group element in a cation form, and reducing the precursor diffused into the molecular sieve pore channel into corresponding nano particles in a hydrogen atmosphere after adsorption.
Compared with the prior art, the invention has the following beneficial effects:
according to the invention, by utilizing the negative charge characteristic of a framework of the Y molecular sieve, a precursor of platinum group elements in a cation form is selected for adsorption and diffusion, the framework of the Y molecular sieve is negative, the dissolved precursor dissociates platinum group element cations (with positive charges), the platinum group elements can be diffused into the pore channels of the molecular sieve as much as possible by combining the electrostatic adsorption effect with the capillary effect of the pore channels of the molecular sieve, the platinum group elements are prevented from being adsorbed on the outer surface of the molecular sieve to the maximum extent, and then the platinum group nanoparticles packaged by the Y molecular sieve can be obtained by the processes of hydrogen reduction, washing, drying and the like. The high temperature roasting shows that the platinum group particles do not obviously agglomerate and grow after the roasting at the high temperature of 500 ℃, 600 ℃ and 700 ℃.
Drawings
The accompanying drawings, which are incorporated in and constitute a part of this application, illustrate embodiments of the invention and, together with the description, serve to explain the invention and not to limit the invention. In the drawings:
FIG. 1 is an XRD pattern of a Y molecular sieve encapsulating Pd particles;
FIG. 2 is a TEM image of the Pd particles encapsulated by the Y molecular sieve;
FIG. 3 is a TEM image of the Pd particles encapsulated by the Y molecular sieve after being calcined at 500 ℃;
FIG. 4 is a TEM image of the Pd particles encapsulated by the Y molecular sieve after being roasted at 600 ℃;
FIG. 5 is a TEM image of the Pd particles encapsulated by the Y molecular sieve after being calcined at 700 ℃;
FIG. 6 is a TEM image of Y molecular sieve encapsulated Pd particles with sodium chloropalladate as a precursor.
Detailed Description
The present invention will be described in detail below with reference to the embodiments with reference to the attached drawings. It should be noted that the embodiments and features of the embodiments in the present application may be combined with each other without conflict.
The following detailed description is exemplary in nature and is intended to provide further details of the invention. Unless otherwise defined, all technical terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this application belongs. The terminology used herein is for the purpose of describing particular embodiments only and is not intended to be limiting of exemplary embodiments according to the invention.
Example 1
Taking dried HY molecular sieve 50mg, and the Si/Al ratio (SiO) of HY molecular sieve2/Al2O3) Is 3: 1, adding 10mL of absolute ethyl alcohol, and uniformly mixing by ultrasonic waves. Weighing 2.74mg palladium acetylacetonate, dissolving in 1.12mL absolute ethyl alcohol, performing ultrasonic treatment until palladium acetylacetonate powder is completely dissolved, and dissolving the dissolved solutionSlowly and dropwise adding the mixture into an HY molecular sieve ethanol solution, and stirring for 10 hours at room temperature or in a water bath (25-30 ℃).
Taking a sample after stirring overnight, centrifuging, removing supernate, adding 10mL of absolute ethyl alcohol to wash the sample, repeating for three times, then adding 10mL of absolute ethyl alcohol, ultrasonically dispersing, slowly stirring in a water bath at 60 ℃, and carrying out 0.1MPa H2Reducing for 24h under the condition. Taking a reduced sample, centrifuging, removing supernatant, adding 5mL of absolute ethyl alcohol and deionized water respectively, then ultrasonically washing, repeating the washing step for three times, and placing the sample in a vacuum drying oven to dry overnight. Obtaining the HY molecular sieve Pd @ HY encapsulating the palladium nano particles.
It can be obtained from the XRD data of fig. 2 that the self-structure of the Y-type molecular sieve subjected to the catalyst encapsulation process is not significantly affected, and no significant characteristic peak of palladium element is observed in the XRD data of the loaded molecular sieve, indicating that the nanoparticle supported by the molecular sieve has a small particle size and is not significantly agglomerated. From the TEM data in fig. 2, it can be seen that the palladium nanoparticles are reduced and loaded on the HY molecular sieve, and the particle size distribution of the reduced nanoparticles is relatively uniform, the average particle size is 1.6nm, and no obvious agglomeration phenomenon occurs on the molecular sieve support.
FIG. 4 is a TEM image of the Pd particles encapsulated by the Y molecular sieve and then calcined at 500 ℃, which shows that the particle size distribution of the calcined nano particles is still uniform and no obvious agglomeration phenomenon occurs on the molecular sieve carrier.
FIG. 4 is a TEM image of the molecular sieve Y after being calcined at 600 ℃ after encapsulating Pd particles, and it can be seen that no Pd particles are significantly agglomerated on the molecular sieve carrier after calcination.
Fig. 5 is a TEM image of the Y molecular sieve after encapsulating Pd particles and then calcining at 700 ℃, and also no agglomeration and size growth of the Pd particles were observed.
Example 2
And adding 10mL of absolute ethyl alcohol into the dry HY molecular sieve of 45mg with the silicon-aluminum ratio of 3, and ultrasonically mixing uniformly. Weighing 2.74mg of palladium acetylacetonate, dissolving the palladium acetylacetonate in 1.12mL of absolute ethanol, performing ultrasonic treatment until palladium acetylacetonate powder is completely dissolved, slowly dropwise adding the dissolved solution into an HY molecular sieve ethanol solution, and stirring for 15 hours at room temperature or in water bath (25-30 ℃).
Taking a sample after stirring overnight, centrifuging, removing supernate, adding 8mL of absolute ethyl alcohol to wash the sample, repeating for three times, then adding 10mL of absolute ethyl alcohol, ultrasonically dispersing, slowly stirring in a water bath at 63 ℃, and carrying out 0.1MPa H2Reducing for 26h under the condition. Taking a reduced sample, centrifuging, removing supernatant, adding 5mL of absolute ethyl alcohol and deionized water respectively, then ultrasonically washing, repeating the washing step for three times, and placing the sample in a vacuum drying oven to dry overnight. Obtaining the HY molecular sieve Pd @ HY encapsulating the palladium nano particles.
Example 3
Taking dried HY molecular sieve 50mg with the silica-alumina ratio of HY molecular sieve of 4, adding 10mL of absolute ethanol, and ultrasonically mixing uniformly. Weighing 2.74mg of palladium acetylacetonate, dissolving the palladium acetylacetonate in 1.12mL of absolute ethanol, performing ultrasonic treatment until palladium acetylacetonate powder is completely dissolved, slowly dropwise adding the dissolved solution into an HY molecular sieve ethanol solution, and stirring for 10 hours at room temperature or in water bath (25-30 ℃).
Taking a sample after stirring overnight, centrifuging, removing supernate, adding 10mL of absolute ethyl alcohol to wash the sample, repeating for three times, then adding 10mL of absolute ethyl alcohol, ultrasonically dispersing, slowly stirring in a water bath at 60 ℃, and carrying out 0.1MPa H2Reducing for 24h under the condition. Taking a reduced sample, centrifuging, removing supernatant, adding 5mL of absolute ethyl alcohol and deionized water respectively, then ultrasonically washing, repeating the washing step for three times, and placing the sample in a vacuum drying oven to dry overnight. Obtaining the HY molecular sieve Pd @ HY encapsulating the palladium nano particles.
Example 4
Taking dried HY molecular sieve 50mg with the silica-alumina ratio of HY molecular sieve 5, adding 10mL of absolute ethanol, and ultrasonically mixing. Weighing 2.74mg of palladium acetylacetonate, dissolving the palladium acetylacetonate in 1.12mL of absolute ethanol, performing ultrasonic treatment until palladium acetylacetonate powder is completely dissolved, slowly dropwise adding the dissolved solution into an HY molecular sieve ethanol solution, and stirring for 10 hours at room temperature or in water bath (25-30 ℃).
Taking a sample after stirring overnight, centrifuging, removing supernate, adding 10mL of absolute ethyl alcohol to wash the sample, repeating for three times, then adding 10mL of absolute ethyl alcohol, ultrasonically dispersing, slowly stirring in a water bath at 60 ℃, and carrying out 0.1MPa H2Reducing for 24h under the condition. Taking a reduced sample, centrifuging, removing supernate, adding 5mL of absolute ethyl alcohol and deionized water respectively, then ultrasonically washing,this washing step was repeated three times and the samples were placed in a vacuum oven to dry overnight. Obtaining the HY molecular sieve Pd @ HY encapsulating the palladium nano particles.
Example 5
Taking dried HY molecular sieve 50mg with the silica-alumina ratio of HY molecular sieve of 3, adding 10mL of absolute ethanol, and ultrasonically mixing uniformly. Weighing 3.00mg of platinum acetylacetonate, dissolving the platinum acetylacetonate in 1.12mL of absolute ethyl alcohol, performing ultrasonic treatment until platinum acetylacetonate powder is completely dissolved, slowly dropwise adding the dissolved solution into an HY molecular sieve ethanol solution, and stirring for 10 hours at room temperature or in water bath (25-30 ℃).
Taking a sample after stirring overnight, centrifuging, removing supernate, adding 10mL of absolute ethyl alcohol to wash the sample, repeating for three times, then adding 10mL of absolute ethyl alcohol, ultrasonically dispersing, slowly stirring in a water bath at 60 ℃, and carrying out 0.1MPa H2Reducing for 24h under the condition. Taking a reduced sample, centrifuging, removing supernatant, adding 5mL of absolute ethyl alcohol and deionized water respectively, then ultrasonically washing, repeating the washing step for three times, and placing the sample in a vacuum drying oven to dry overnight. Obtaining the HY molecular sieve Pt @ HY encapsulating the platinum nano particles.
Comparative example 1
Sodium chloropalladate is used as a precursor, and a traditional immersion method is used for preparation to serve as a comparative example. Weighing 1.18mg of sodium chloropalladate powder, dissolving in 300ul of deionized water, performing ultrasonic dispersion, after complete dissolution, dropwise adding the powder into a 100mg HY molecular sieve to ensure that the molecular sieve is completely and uniformly immersed in a sodium chloropalladate solution to achieve a wet state, standing overnight, then placing the sample in an oven, drying in an air environment at 100 ℃ for 4 hours, and raising and reducing the temperature for 30 min. And after the sample is cooled, placing the dried sample in a muffle furnace, roasting for 4 hours at 300 ℃ in an air environment, wherein the heating rate is 0.5 ℃/min. And roasting to obtain a sample prepared by an impregnation method. As can be seen from fig. 6TEM, the particle size of the Y molecular sieve supported Pd using sodium chloropalladate as a precursor is large, and the particle size distribution is not uniform.
It will be appreciated by those skilled in the art that the invention may be embodied in other specific forms without departing from the spirit or essential characteristics thereof. The embodiments disclosed above are therefore to be considered in all respects as illustrative and not restrictive. All changes which come within the scope of or equivalence to the invention are intended to be embraced therein.
Claims (9)
1. A preparation method of a Y-type molecular sieve encapsulated platinum group noble metal nanoparticle catalyst is characterized by comprising the following steps:
dispersing a Y-type molecular sieve in an ethanol solvent, adding a platinum group precursor of platinum group elements in a cation form, carrying out in-hole adsorption on the platinum group precursor by the Y-type molecular sieve, and reducing the adsorbed sample in the ethanol solvent under a hydrogen atmosphere to prepare the Y-type molecular sieve packaged platinum group noble metal nanoparticle catalyst.
2. The preparation method of claim 1, wherein the concentration of the Y-type molecular sieve in the ethanol solvent is 4-10 mg/ml, the mass ratio of the platinum group elements to the Y-type molecular sieve is calculated according to the platinum group elements in the platinum group precursor: 0.5-4.0: 100, respectively; the platinum group precursor is obtained by dissolving platinum group precursor salt in ethanol; the platinum group precursor is added dropwise.
3. The preparation method according to claim 2, wherein the dispersion of the Y-type molecular sieve in ethanol and the addition of the platinum group precursor are carried out at room temperature; and adding the platinum group precursor, and stirring for 4-24 hours for adsorption.
4. The method according to claim 1, wherein the temperature for reducing the adsorbed sample in a hydrogen atmosphere is 40 to 70 ℃, the hydrogen pressure is 1 to 2.5 atm, and the reduction time is 24 to 36 hours.
5. The preparation method of claim 4, wherein the sample after the reduction is washed and vacuum-dried to obtain Y-type molecular sieve encapsulated platinum group nanoparticles.
6. The preparation method of claim 1, wherein the molar silica-alumina ratio of the Y-type molecular sieve is 2-7.
7. The preparation method of claim 1, wherein the molar silica-alumina ratio of the Y-type molecular sieve is 2-5.
8. The method according to claim 2, wherein the platinum group precursor salt is platinum acetylacetonate or palladium acetylacetonate.
9. A Y-type molecular sieve encapsulated platinum group noble metal nanoparticle catalyst, characterized by being prepared by the preparation method of any one of claims 1 to 8.
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| CN113368885A (en) * | 2021-05-12 | 2021-09-10 | 天津大学 | HY molecular sieve supported palladium catalyst and preparation method and application thereof |
| CN113875775A (en) * | 2021-10-08 | 2022-01-04 | 中山大学 | Preparation method of all-silicon molecular sieve packaged nano-silver bactericide |
| CN114558610A (en) * | 2022-03-15 | 2022-05-31 | 南京大学 | Limited-area Pd-based catalyst and preparation method and application thereof |
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| CN113875775A (en) * | 2021-10-08 | 2022-01-04 | 中山大学 | Preparation method of all-silicon molecular sieve packaged nano-silver bactericide |
| CN114558610A (en) * | 2022-03-15 | 2022-05-31 | 南京大学 | Limited-area Pd-based catalyst and preparation method and application thereof |
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Application publication date: 20201204 |