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Hierarchical pore molecular sieve encapsulated platinum-nickel bimetallic nanocatalytic material and its preparation method and application

A bimetallic nanometer and catalytic material technology, which is applied in the direction of molecular sieve catalysts, chemical instruments and methods, physical/chemical process catalysts, etc., can solve the problems of lack of effective regulation of bimetallic distribution positions, easy aggregation and loss of bimetallic active centers, easy loss and Agglomeration and other problems, achieve high reactivity and selectivity, avoid sintering, improve mass transfer and heat transfer

Active Publication Date: 2022-03-08
SOUTHEAST UNIV
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Problems solved by technology

[0004] At present, there are many technologies for encapsulating bimetallic catalysts with molecular sieves. Chinese patent CN112044467A discloses a method of mixing and crystallizing molecular sieve seeds and nanometer metal sources to prepare any two metals in Cu, Ti, Ni, and Fe as active components. The preparation method of bimetallic MFI molecular sieves with molecular sieves as the carrier realizes the doping and encapsulation of bimetals in the molecular sieve framework, but the distribution position of the bimetals in the molecular sieve framework and cage lacks effective control, and the catalyst is easily caused by the bimetallic during the reaction process. Sintering and loss inactivation of active components; Chinese patent CN107661776A discloses a method for preparing SAPO molecular sieves containing Cu and Ag bimetals by ion exchange, and the prepared SAPO molecular sieves containing Cu and Ag bimetals have better hydrothermal stability However, during the high-temperature catalytic reaction, Cu and Ag bimetals are easy to lose and agglomerate
Most of the reported molecular sieve-supported bimetallic catalysts are prepared by the ion exchange method, which lacks the control of the distribution of the bimetallic on the molecular sieve, and the bimetallic active center is easy to agglomerate and lose, and the stability is poor.

Method used

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  • Hierarchical pore molecular sieve encapsulated platinum-nickel bimetallic nanocatalytic material and its preparation method and application
  • Hierarchical pore molecular sieve encapsulated platinum-nickel bimetallic nanocatalytic material and its preparation method and application
  • Hierarchical pore molecular sieve encapsulated platinum-nickel bimetallic nanocatalytic material and its preparation method and application

Examples

Experimental program
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Effect test

Embodiment 1

[0025] At 25°C, add 1.2g of nano-silica and 50g of deionized water into the reactor, react at 80°C for 1h, add 15g, 2wt.% methanol solution of methacryloxysilane, and continue the reaction for 6h. Filter, wash the filter cake with 100g of ethanol, and dry at 70°C for 12h to obtain the modified silicon source;

[0026] At 25°C, add 1g of ethylenediamine and 15g of deionized water into the reactor, react at 30°C for 0.5h, add 0.1g of platinum acetate, 0.5g of basic nickel carbonate, and continue the reaction for 1h to obtain the PtNi bimetallic precursor body;

[0027] At 25°C, add 5g of modified silicon source, 3g of sodium metaaluminate, 4g of tetrapropylammonium hydroxide, 2g of NaOH, 0.2g of PtNi bimetallic precursor, and 100g of deionized water into the reactor, and react at 150°C for 3 days. After cooling down to room temperature, filter; wash the filter cake with deionized water until the pH of the washing liquid reaches 7, dry at 80°C for 12h, and then bake at 600°C for...

Embodiment 2

[0033] At 25°C, add 1.5g of nano-silica and 50g of deionized water into the reactor, react at 70°C for 2h, add 18g, 2wt.% of 3-(2,3-glycidyloxy)propyltrimethoxy The methanol solution of base silane was continued to react for 8 hours, then filtered, and the filter cake was washed with 130 g of ethanol, and dried at 80°C for 12 hours to obtain a modified silicon source;

[0034] At 25°C, add 1.2g of diethylenetriamine and 18g of deionized water into the reactor, react at 50°C for 0.2h, add 0.1g of platinum acetate, 0.6g of hexaammine nickel chloride, and continue the reaction for 2h to obtain PtNi bimetallic precursor;

[0035] At 25°C, add 8g of modified silicon source, 1g of aluminum isopropoxide, 5g of tetrapropylammonium bromide, 1.5g of NaOH, 0.1g of PtNi bimetallic precursor, and 75g of deionized water into the reactor, and react at 140°C for 4d , after cooling down to room temperature, filter; wash the filter cake with deionized water until the pH of the washing solution...

Embodiment 3

[0038] At 25°C, add 2g of nano-silica and 60g of deionized water into the reactor, react at 90°C for 0.5h, add 25g, 3wt.% of 3-(2,3-epoxypropoxy)propyltrimethoxy The methanol solution of base silane was continued to react for 10 hours, then filtered, and the filter cake was washed with 200 g of ethanol, and dried at 60°C for 24 hours to obtain a modified silicon source;

[0039] At 25°C, add 0.8g of ethylenediamine and 20g of deionized water into the reactor, react at 30°C for 0.5h, add 0.15g of potassium chloroplatinate, 1g of basic nickel carbonate, and continue the reaction for 0.5h to obtain PtNi Bimetallic precursors;

[0040] At 25°C, add 15g of modified silicon source, 2g of sodium metaaluminate, 6g of tetrapropylammonium hydroxide, 1.5g of NaOH, 0.15g of PtNi bimetallic precursor, and 80g of deionized water into the reactor, and react at 170°C for 3 days. After cooling down to room temperature, filter; wash the filter cake with deionized water until the pH of the wash...

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Abstract

The invention discloses a multi-stage pore molecular sieve-encapsulated platinum-nickel bimetal nano-catalysis material and its preparation method and application. The modified silicon source is prepared by modifying nano-silica with a silane coupling agent, and the PtNi bimetallic precursor is obtained by electrostatic self-assembly of an amine structure-directing agent and a Pt and Ni source. Based on the total mass of the catalytic material, the mass percentage of nickel is 0.1-20 wt%, and the mass percentage of platinum is 0.1-5 wt%. Using a one-step method, in the process of synthesizing hierarchically porous molecular sieves, PtNi bimetallic precursors were introduced in situ to realize the selective encapsulation of PtNi bimetallic nanoclusters in the side cages of hierarchically porous molecular sieves. The catalytic material is used to catalyze the reaction of pyridine dehydrogenation coupling to 2,2'-bipyridine, which has the advantages of low dosage, less side reactions and short process, and has good performance in the fields of adsorption separation, petrochemical industry, fine chemical production and so on. Application prospect.

Description

technical field [0001] The invention belongs to an industrial catalytic material and a preparation method thereof, in particular to a platinum-nickel double-metal nano-catalysis material encapsulated by a multi-stage molecular sieve, a preparation method and an application thereof. Background technique [0002] Due to its high catalytic activity and selectivity, PtNi bimetallic nanocatalytic materials are widely used in reactions such as alkane dehydrogenation, automobile exhaust gas conversion, methane reforming, and electrocatalytic hydrogen evolution. The catalytic performance of bimetallic nanocatalytic materials has an important influence. The smaller the size and the higher the dispersion of PtNi bimetallic nanoparticles, the better the catalytic activity. However, due to the high surface energy of PtNi bimetallic nanoparticles, it is difficult for PtNi bimetallic particles to maintain their original structure and morphology during catalytic reactions, especially in hi...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J29/46B01J29/03C07D213/22
CPCB01J29/46B01J29/0333C07D213/22B01J2229/186
Inventor 周钰明鲍杰华王彦云卜小海张泽武张一卫盛晓莉
Owner SOUTHEAST UNIV
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