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Supported palladium-based catalyst and preparation method and application thereof

A supported palladium and catalyst technology, which is applied in the field of materials, can solve the problems of difficult maintenance of catalyst reactivity, unstable palladium metal, and poor stability, and achieve excellent catalytic activity and catalytic stability. The preparation method is simple and easy, and the particle size evenly distributed effect

Inactive Publication Date: 2021-08-06
UNIV OF SCI & TECH OF CHINA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the preparation process of palladium-based metal catalysts often requires a high temperature environment. Palladium metal itself is very unstable due to its inherent thermodynamics at high temperatures, and is particularly prone to surface migration and aggregation. Compound catalysts still have great challenges
On the other hand, also due to the instability of palladium metal, the prepared palladium-based metal catalysts are usually very poor in stability, and the reactivity of the prepared catalysts is difficult to maintain, so they cannot be applied on a large scale in actual production.

Method used

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  • Supported palladium-based catalyst and preparation method and application thereof
  • Supported palladium-based catalyst and preparation method and application thereof
  • Supported palladium-based catalyst and preparation method and application thereof

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preparation example Construction

[0042] The invention provides a preparation method of supported palladium-based catalyst, comprising the following steps:

[0043] a) Al salt, K2 SO 4 and CO(NH 2 ) 2 mixing in water, heating and reacting, filtering, drying, and calcining to obtain an alumina carrier; the microscopic appearance of the alumina carrier is a three-dimensional flower cluster;

[0044] b) mixing the alumina carrier and Pd salt in water, removing water, and calcining to obtain calcined powder;

[0045] c1) The calcined powder and non-noble metal salt are mixed in water, and the water is removed to obtain a dry powder mixture; the non-noble metal salt is Pb salt, Fe salt, In salt, Ga salt or Cu salt; after that, the dry powder is The mixture is heated and reduced in a reducing gas atmosphere to obtain a supported palladium-based catalyst;

[0046] or,

[0047] c2) heating and reducing the calcined powder and Zn powder in a reducing atmosphere to obtain a supported palladium-based catalyst.

[0...

Embodiment 1

[0067] 1) Synthesis of carrier materials:

[0068] 7.55g Al(NO 3 ) 3 9H 2 O, 3.50g K 2 SO 4 and 2.50g CO(NH 2 ) 2 Dissolve in 400 mL deionized water; then transfer the resulting mixture into a 500 mL tetrafluoroethylene-lined stainless steel autoclave and heat at 180 °C for 3 h; when cooled to room temperature, collect the white precipitate by filtration and dry at 80 °C for 12 h ; Finally, in a muffle furnace, the alumina carrier is obtained by heating to 500° C. for 2 hours at a heating rate of 1° C. / min.

[0069] 2) Preparation of supported palladium-based catalyst:

[0070] Get 100mg of alumina carrier prepared in 1) and 16.04mg of PdCl 2 2H 2 O was co-dispersed in a 100mL flask containing 50mL of deionized water, added a magnet, and stirred magnetically at room temperature for 6-24 hours at a speed of 1000r / min; took out the magnet, and evaporated the above mixture to dryness by rotary evaporation; after that Put the above-mentioned evaporated sample into a muff...

Embodiment 2

[0082] 1) Preparation of supported palladium-based catalyst:

[0083] Get 100mg of alumina carrier prepared in 1) and 10.02mg of PdCl 2 2H 2 O was co-dispersed in a 100mL flask containing 50mL of deionized water, added a magnet, and stirred magnetically at room temperature for 6-24 hours at a speed of 1000r / min; took out the magnet, and evaporated the above mixture to dryness by rotary evaporation; after that Put the above-mentioned evaporated sample into a muffle furnace, heat it to 500°C at a heating rate of 1°C / min and calcinate for 2 hours to obtain a brown-yellow powder;

[0084] According to the Pd / Fe molar ratio of 3:1, that is, 1 times the Pd-Fe intermetallic compound (Pd 3 The stoichiometric ratio of Fe) is obtained by calcining the tan powder 50mg loaded with Pd and the required amount of FeCl 3 ·6H 2 O was co-dispersed in a 100mL flask containing 50mL of deionized water, added a magnet, and stirred magnetically at room temperature for 6-24 hours at a speed of 10...

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Abstract

The invention belongs to the field of materials, and particularly relates to a supported palladium-based catalyst and a preparation method and application thereof. The preparation method comprises the following steps: a) mixing Al salt, K2SO4 and CO (NH2) 2 in water, heating for reaction, filtering, drying and calcining to obtain an alumina carrier; b) mixing the alumina carrier and Pd salt in water, removing water, and calcining to obtain calcined powder; c1) mixing the calcined powder and a non-noble metal salt in water, and removing water to obtain a dry powder mixture; then, heating and reducing the dry powder mixture in a reducing gas atmosphere to obtain a supported palladium-based catalyst; or c2) heating and reducing the calcined powder and Zn powder in a reducing atmosphere to obtain the supported palladium-based catalyst. The palladium-based intermetallic compound in the supported palladium-based catalyst prepared by the method is small in particle size and uniform in particle size distribution, and has excellent catalytic activity and catalytic stability for selective hydrogenation reaction of phenylacetylene.

Description

technical field [0001] The invention belongs to the field of materials, in particular to a supported palladium-based catalyst and its preparation method and application. Background technique [0002] In the field of heterogeneous catalysis, supported palladium-based metal catalysts have always maintained great interest and attention in the industry. Over the past decades, studies have found that supported palladium-based metal catalysts have unique catalytic properties in different important molecular reactions, such as hydrogenation and dehydrogenation, electrocatalytic reactions, methane oxidation, CO oxidation, C-H activation, and organic coupling. reaction. However, the monometallic palladium catalyst is a double-edged sword for the selective hydrogenation reaction. It brings high activity to the reaction but also causes the reaction selectivity to be greatly reduced. Therefore, by alloying Pd with foreign non-noble metal atoms , the electronic properties of performanc...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J23/62B01J23/89B01J23/60B01J37/02B01J37/08B01J37/18C07C5/09C07C15/46
CPCB01J23/628B01J23/8906B01J23/62B01J23/8926B01J23/60B01J37/0207B01J37/088B01J37/18C07C5/09C07C2523/62C07C2523/89C07C2523/60B01J35/393B01J35/23C07C15/46
Inventor 梁海伟焦文中
Owner UNIV OF SCI & TECH OF CHINA
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