Preparation method of load type nano catalyst for catalyzing Suzuki coupling reaction

A nano-catalyst and supported palladium technology, which is applied in the field of catalyst preparation, can solve the problems of particle redistribution and agglomeration, and achieve the effects of small size, avoiding particle redistribution, and not easy to agglomerate

Inactive Publication Date: 2015-11-11
INST OF PETROCHEM HEILONGJIANG ACADEMY OF SCI
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Problems solved by technology

[0003] The purpose of the present invention is to solve the problem that the palladium nano-particles formed in the reduction preparation process of existing chemical reagents are prone to particle redistribution and agglomeration in the liquid phase system, and a kind of supported palladium nano-catalyst for catalyzing Suzuki coupling reaction is provided Preparation

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  • Preparation method of load type nano catalyst for catalyzing Suzuki coupling reaction
  • Preparation method of load type nano catalyst for catalyzing Suzuki coupling reaction
  • Preparation method of load type nano catalyst for catalyzing Suzuki coupling reaction

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specific Embodiment approach 1

[0014] Specific embodiment one: the preparation method of the loaded palladium nano-catalyst of catalytic Suzuki coupling reaction in the present embodiment is carried out according to the following steps:

[0015] 1. Mix 1g of activated carbon carrier with 2-10ml of 0.0470mol / L Na at room temperature 2 PdCl 4 The solutions were mixed, stirred and impregnated for 12 hours, then centrifuged, and dried at 110°C for 12 hours to obtain a sample;

[0016] 2. Take 0.1g sample evenly spread on the carrier boat, place it in the discharge tube, use the vacuum pump to vacuum the inside of the plasma discharger, and pass it into the N 2 Plasma discharge gas, by adjusting the fine-tuning valve, the gas pressure is kept at 60-120Pa, and high-voltage direct current is applied at both ends of the electrodes, the gas in the discharge tube is broken down, and glow discharge plasma is triggered. The discharge power is 330W-660W, and the discharge time for 5-60min, the Pd 2+ Reduction into a ...

specific Embodiment approach 2

[0018] Specific embodiment two: the difference between this embodiment and specific embodiment one is that in step one, at room temperature, 1 g of activated carbon carrier and 5 ml of 0.0470mol / L Na 2 PdCl 4 The solution is mixed. Others are the same as in the first embodiment.

specific Embodiment approach 3

[0019] Embodiment 3: This embodiment differs from Embodiment 1 or Embodiment 2 in that the gas pressure is kept at 70-110 Pa in step 2. Others are the same as those in the first or second embodiment.

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Abstract

The invention provides a preparation method of a load type nano catalyst for catalyzing a Suzuki coupling reaction, and relates to a preparation method of a catalyst. According to the preparation method, the problem that particle redistribution and aggregation are prone to occurring on palladium nanoparticles formed in the existing chemical reagent reducing preparation process in a liquid phase system is solved. The preparation method comprises the following steps that at room temperature, activated carbon and a Na2PdC14 solution are mixed, centrifuged and dried for 12 h, and a sample is obtained; the sample is taken, evenly laid on a bearing boat and placed in a discharge tube, vacuumizing is performed, N2 plasma discharge gas is pumped in, high-voltage direct currents are applied at the two ends of an electrode, the gas in the discharge tube is broken through, glow discharge plasma is initiated, and then the load type nano catalyst is obtained. According to the preparation method, the glow discharge plasma is used for preparing the load type nano catalyst in a reduction mode, particle redistribution caused by liquid phase system reduction is avoided, and the prepared Pd nanoparticles are not prone to aggregating, small in size and homogeneours in dispersion. The method belongs to the field of catalyst preparation.

Description

technical field [0001] The invention relates to a preparation method of a catalyst. Background technique [0002] The Suzuki coupling reaction is one of the important reactions for constructing C-C bonds, and the palladium catalysts used can be divided into homogeneous catalysts and heterogeneous catalysts. However, the palladium nanoparticles formed in the reduction preparation process of the existing chemical reagents are prone to the problems of particle redistribution and agglomeration in the liquid phase system. Homogeneous palladium catalysts are difficult to separate and recover. Supported heterogeneous catalysts can realize the recovery and utilization of catalysts. At present, the preparation of supported catalysts is mainly to realize Pd by chemical reduction. 2+ However, the reduction system usually needs to be carried out in the liquid phase or under high temperature conditions, which is prone to the problems of particle redistribution and agglomeration. Conte...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J23/44C07C15/14C07C1/32C07C49/784C07C45/68C07C43/205C07C41/30C07C205/06C07C201/12C07C255/50C07C253/30C07B37/00
Inventor 白雪峰刘洋吕宏飞李猛杨杰
Owner INST OF PETROCHEM HEILONGJIANG ACADEMY OF SCI
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