Loading type Pd base metal nanometer cluster catalyst, preparing method and applications thereof

A metal nanoparticle and base metal technology, which is applied to a supported Pd-based metal nanocluster catalyst and the field of preparation and application thereof, can solve the problems of decreased catalyst activity, difficult hydrogenation of intermediate products, and difficulty in product separation.

Active Publication Date: 2010-07-07
PEKING UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Add a lot of Sn 4+ Although the selectivity of p-CAN can be further improved, it will also lead to a significant decrease in catalyst activity, making it difficult to completely hydrogenate intermediate products, and a large amount of modifiers will also cause difficulties in product separation.

Method used

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  • Loading type Pd base metal nanometer cluster catalyst, preparing method and applications thereof
  • Loading type Pd base metal nanometer cluster catalyst, preparing method and applications thereof
  • Loading type Pd base metal nanometer cluster catalyst, preparing method and applications thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0066] Example 1: Preparation of γ-Fe by Pd nanoclusters and in a partially reduced state 2 o 3 Constituted catalyst (Pd: 3wt.%) and its catalytic performance test. (wt.% is mass percentage, the same below)

[0067] 1. Catalyst preparation

[0068] Get 10ml concentration and be that the sodium hydroxide aqueous solution of 0.20mol / L joins in the palladium chloride aqueous solution of 20ml (2.82 * 10 -2 mol / L), stirred at room temperature for 1min to obtain a palladium metal compound colloid, and the content of Pd in ​​the colloid was 2.00g / L. The electron micrograph of the palladium metal compound nanoparticle in the palladium metal compound colloid is as figure 1 shown. Transmission electron microscope (TEM) analysis shows that the average particle size of the palladium metal compound nanoparticles is 2nm, and the particle size distribution is 1-3nm.

[0069] 10% ammonia water and 4% ferric chloride (0.25mol / L) aqueous solutions were prepared respectively, and an approp...

Embodiment 2

[0087] Embodiment 2: Preparation is made of Pd nano-clusters and Fe in a partially reduced state 3 o 4 The constituted catalyst (Pd: 0.25wt.%) and its catalytic performance test.

[0088] 1. Catalyst preparation

[0089] Disperse 1g of palladium chloride in 300ml of ethylene glycol, add 1ml of hydrochloric acid (30wt.%), and prepare the ethylene glycol solution of palladium chloric acid (1.88×10 -2 mol / L). Cool the freshly prepared palladium chloride ethylene glycol solution and NaOH aqueous solution (0.25mol / L) to 263K. Take 4.5ml of fully cooled NaOH aqueous solution and add it to 12ml of palladium chloride in ethylene glycol solution under stirring, and continue to stir for 120min at a temperature of 273K to obtain a palladium metal compound colloid. The content of Pd in ​​the colloid is 1.45g / L.

[0090] Fe 3 o 4 The nanostructure material is prepared as follows: 10g of ferric chloride hexahydrate and 10g of urea are dissolved in 60ml of ethylene glycol, heated to 46...

Embodiment 3

[0103] Example 3: Preparation of γ-Fe by Pd nanoclusters and in a partially reduced state 2 o 3 Constituted catalyst (Pd: 15wt.%)

[0104] Prepare palladium metal compound colloid according to the method of step one in Example 1.

[0105] Prepare 2% (mass percentage) KOH aqueous solution and 0.17mol / L ferric nitrate aqueous solution respectively, take an appropriate amount of KOH aqueous solution and slowly add it dropwise to 150ml ferric nitrate solution under stirring, finally control the pH at about 4, and age for 10 minutes. Filtrate and wash the precipitated ferric hydroxide, beat the filter cake in 30ml of 1% dilute hydrochloric acid and slightly heat the slurry at 333K to obtain ferric hydroxide colloid, cool to room temperature for later use.

[0106] Add 176.6ml of the above-mentioned newly prepared palladium metal compound colloid dropwise to the above-mentioned ferric hydroxide colloid, then inject a mixed solution of 100ml of ethylene glycol and glycerol (ethylen...

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Abstract

The invention discloses a loading type Pd base metal nanometer cluster catalyst, a preparing method and applications thereof. The catalyst comprises Pd metal nanometer particles of 1-25nm, or bimetal or polymetal nanometer particles containing Pd, and ferric oxide nanometer particles, wherein the ferric oxide nanometer particle is used as the carrier, has the primary particle size of 5-200nm, and has the general formula of FeyOx; the bimetal or polymetal nanometer particles are selected from one or a plurality of Pt, Rh, Ru, Os, Ir and Re; when the metal nanometer particles are Pd nanometer particles, x/y is greater than 1, but is smaller than 4/3, or is greater than 4/3, but is smaller than 3/2; and when the metal nanometer particles are bimetal or polymetal nanometer particles containing Pd, x/y is greater than 1, but is smaller than or equal to 3/2. The catalyst has excellent activity, selectivity and stability on the selective hydrogenating synthesis chlorinated arylamine of the chlorinated aromatic compounds, solves the problems of hydrogenolysis and dechlorination of products in the process of the Pd catalyst catalyzing the chlorinated aromatic compounds to hydrogenate to prepare the chlorinated arylamine, and has important industrial application values.

Description

technical field [0001] The invention relates to a supported Pd-based metal nano-cluster catalyst, a preparation method and application thereof. Background technique [0002] Iron oxides, especially magnetic iron oxides (including γ-Fe 2 o 3 and Fe 3 o 4 ) have special electronic, magnetic and optical properties. Magnetic separation of catalysts can be achieved by loading metals on magnetic iron oxide or supports containing magnetic iron oxide. [0003] γ-Fe coated with hydroxyapatite by Hara et al. 2 o 3 As a carrier, Pd-hydroxyapatite-γ-Fe was prepared 2 o 3 catalyst. The catalyst can catalyze a series of chlorine-containing aromatic compounds such as chlorobenzene, chloroaniline, chloroacetophenone, etc. to hydrogenolysis dechlorination rapidly, and is a highly active dechlorination catalyst (T.Hara, et al., Green Chem. , 2007, 9, 1246-1251). In addition, the catalyst can be easily separated from the reaction system and reused by applying an external magnetic fi...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J23/89C07C209/36C07C211/43
CPCY02P20/582
Inventor 王远刘洪全肖超
Owner PEKING UNIV
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