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Gas-phase synthesis method for small-scale high-dispersion Pd/C catalyst

A gas-phase synthesis and catalyst technology, applied in chemical instruments and methods, preparation of amino compounds, preparation of organic compounds, etc., can solve problems such as uneven distribution of catalytic species, difficult synthesis process, wide metal particle size distribution, etc., to avoid synthesis The process is not easy to control, the effect of reducing production steps, saving production time and energy consumption

Inactive Publication Date: 2015-03-25
XIAN MODERN CHEM RES INST
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] The purpose of the present invention is to propose a Pd / C catalyst gas-phase Preparation

Method used

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  • Gas-phase synthesis method for small-scale high-dispersion Pd/C catalyst
  • Gas-phase synthesis method for small-scale high-dispersion Pd/C catalyst
  • Gas-phase synthesis method for small-scale high-dispersion Pd/C catalyst

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Embodiment 1

[0023] This embodiment provides a kind of gas phase synthesis method of small-scale, highly dispersed Pd / C catalyst, and the concrete steps of this method are:

[0024] Step 1: Place 1 g of activated carbon carrier in a fixed-bed reactor, seal the reactor, feed nitrogen gas and adjust the reactor pressure to 130 Pa, heat the activated carbon to 200°C, and heat palladium hexafluoroacetylacetonate to 60°C;

[0025] Step 2, palladium hexafluoroacetylacetonate steam enters the reactor and reacts with the surface groups of the activated carbon to undergo a gas-solid interface reaction. The time of the gas-solid interface reaction is 2 minutes. The Pd element is fixed on the surface of the activated carbon, and then a reducing gas is introduced into the reactor Formaldehyde reduces the Pd element fixed on the surface, and the reduction reaction time is 2 minutes. The above process is cycled once to generate 0.5% Pd / C catalyst.

[0026] Take by weighing 218.1 mg of the catalyst prep...

Embodiment 2

[0028] This embodiment provides a kind of gas phase synthesis method of small-scale, highly dispersed Pd / C catalyst, and the concrete steps of this method are:

[0029] Step 1: Place 1 g of activated carbon carrier in a fixed-bed reactor, seal the reactor, feed nitrogen gas and adjust the reactor pressure to 130 Pa, heat the activated carbon to 200°C, and heat palladium hexafluoroacetylacetonate to 60°C;

[0030] Step 2, palladium hexafluoroacetylacetonate steam enters the reactor and reacts with the surface groups of the activated carbon to undergo a gas-solid interface reaction. The time of the gas-solid interface reaction is 5 minutes. The Pd element is fixed on the surface of the activated carbon, and then the reducing gas is introduced into the reactor Formaldehyde reduces the Pd element fixed on the surface, and the reduction reaction time is 5 minutes. The above process is cycled once to generate 1.4% Pd / C catalyst.

[0031] Weigh 77.9 mg of the catalyst prepared in Ex...

Embodiment 3

[0033] This embodiment provides a kind of gas phase synthesis method of small-scale, highly dispersed Pd / C catalyst, and the concrete steps of this method are:

[0034] Step 1: Place 1 g of activated carbon carrier in a fixed-bed reactor, seal the reactor, feed nitrogen gas and adjust the reactor pressure to 130 Pa, heat the activated carbon to 200°C, and heat palladium hexafluoroacetylacetonate to 60°C;

[0035] Step 2: Palladium hexafluoroacetylacetonate vapor enters the reactor to react with the surface groups of the activated carbon to undergo a gas-solid interface reaction. The time for the gas-solid interface reaction is 20 minutes. The Pd element is fixed on the surface of the activated carbon, and then a reducing gas is introduced into the reactor Formaldehyde reduces the Pd element fixed on the surface, and the reduction reaction time is 20 minutes. The above process is cycled once to generate a 5.0% Pd / C catalyst.

[0036] When the gas-solid interface reaction time ...

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Abstract

The invention provides a gas-phase synthesis method for a small-scale high-dispersion Pd / C catalyst. According to the method, immobilization of Pd element on the carrier surface is realized by utilizing gas-solid interface reaction between Pd-containing metallo-organic compound steam and a special group on the carrier surface, and the Pd element fixed on the surface is reduced by using reducing gas. The process can be repeatedly performed according to actual demands until the Pd / C catalyst of the needed metal particle size and loading quantity is generated. The Pd nanoparticle catalyst synthesized based on a vapor phase method has the advantages of high dispersity, uniform distribution, accurately controlled particle size, dimensional stability and the like and has excellent activity, selectivity and stability in the catalytic reaction. According to the method, the defects that the synthetic process is difficult to control, the size distribution of metal particles is wide and the catalytic species is non-uniform in distribution in the traditional liquid phase impregnation-reduction method are overcome. In addition, the method is high in automation degree and simple in operating steps, the raw materials and energy consumption are saved, and large-scale production of the product is easily realized.

Description

technical field [0001] The invention relates to a catalyst synthesis method, in particular to a gas phase synthesis method of a Pd / C catalyst. Background technique [0002] Pd / C catalyst has high activity and specific reaction selectivity, and is widely used in various hydrogenation, dehydrogenation and oxidation reactions in the fields of petrochemical, fine chemical, pharmaceutical, dyestuff, pesticide, rubber additives and other fields. In recent years, many scholars at home and abroad have studied how to prepare small-scale Pd / C catalysts. On the one hand, small-scale Pd grains can significantly improve catalytic activity. On the other hand, the noble metal element Pd is an expensive and scarce resource. Smaller-sized Pd particles It helps to make full use of catalytic components and reduce catalyst costs. There are many ways to prepare palladium-carbon catalysts. Generally, the conventional liquid phase reduction method is used to uniformly load the active component Pd...

Claims

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Application Information

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IPC IPC(8): B01J23/44C07C211/46C07C209/36
Inventor 冯昊龚婷万洪张伟秦利军
Owner XIAN MODERN CHEM RES INST
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