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Preparation method for modified palladium-carbon catalyst for Suzuki coupling reaction

A palladium-carbon catalyst and catalyst technology, applied in chemical instruments and methods, physical/chemical process catalysts, metal/metal oxide/metal hydroxide catalysts, etc., can solve the problem of poor catalytic effect of chlorinated aromatics and cannot be recycled and reused , increase cost and other issues, to achieve the effect of improving catalyst activity, improving reusable performance, and increasing metal dispersion

Active Publication Date: 2015-06-10
XIAN CATALYST NEW MATERIALS CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] For a long time, the catalyst of the Suzuki coupling reaction is mainly a homogeneous palladium catalyst. Palladium usually forms a homogeneous catalyst with an organic ligand (such as a palladium-phosphine complex, etc.), and the catalyst activity is often high, the selectivity is good, and the reaction conditions are relatively Mild, but there are problems such as high price: ①Most phosphine ligands are sensitive to air and moisture, and need to be in an inert gas atmosphere to effectively catalyze the reaction; ②The homogeneous catalyst is difficult to separate from the reaction mixture, and cannot be recycled and reused. ③ Trace metal residues will contaminate the product, which is a fatal shortcoming especially for pharmaceuticals and some fine chemicals with high requirements
[0006] At present, compared with homogeneous palladium catalysts, Pd / C catalysts still have problems such as low activity and poor catalytic effect on chlorinated aromatics, which need to be improved.

Method used

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  • Preparation method for modified palladium-carbon catalyst for Suzuki coupling reaction
  • Preparation method for modified palladium-carbon catalyst for Suzuki coupling reaction
  • Preparation method for modified palladium-carbon catalyst for Suzuki coupling reaction

Examples

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Embodiment 1

[0031] The modified palladium carbon catalyst for the Suzuki coupling reaction in this embodiment consists of an activated carbon carrier and an active component loaded on the activated carbon carrier, wherein the active component is palladium and nickel; the mass percentage of palladium in the catalyst is 5%. , the mass percentage of nickel is 0.5%;

[0032] The preparation method of present embodiment catalyst comprises the following steps:

[0033] Step 1. Under the condition of 60°C and continuous stirring, firstly mix 4gNiCl 2 ·6H 2 A mixture of O and 0.67g polyvinylpyrrolidone (PVP) was dissolved in 80mL of distilled water to obtain solution A, then 80mL of absolute ethanol was added to obtain solution B, and then 3mL of hydrazine hydrate was slowly added dropwise to solution B to obtain nano-nickel sol , and its TEM photo is shown in figure 1 ,Depend on figure 1 It can be seen that nickel does exist in nanoscale sol state;

[0034] Step 2, the particle size is 38μm...

Embodiment 2

[0040] The modified palladium carbon catalyst for the Suzuki coupling reaction in this embodiment consists of an activated carbon carrier and an active component loaded on the activated carbon carrier, wherein the active component is palladium and nickel; the mass percentage of palladium in the catalyst is 5%. , the mass percentage of nickel is 1%;

[0041] The preparation method of present embodiment catalyst comprises the following steps:

[0042] Step 1. Under the condition of 40°C and continuous stirring, firstly mix 4.2gNi(OAc) 2 4H 2 A mixture of O and 1.4g polyvinylpyrrolidone (PVP) was dissolved in 55mL of distilled water to obtain solution A, then 55mL of absolute ethanol was added to obtain solution B, and then 6.5mL of hydrazine hydrate was slowly added dropwise to solution B to obtain nano-nickel Sol;

[0043] Step 2, the particle size is 38μm ~ 74μm, the specific surface area is 1000m 2 The gac / g is placed in boiling mass percent concentration of 5% sodium car...

Embodiment 3

[0049] The modified palladium-carbon catalyst for the Suzuki coupling reaction in this embodiment consists of an activated carbon carrier and an active component loaded on the activated carbon carrier, wherein the active component is palladium and nickel; the mass percentage of palladium in the catalyst is 7.5% , the mass percentage of nickel is 2%;

[0050] The preparation method of present embodiment catalyst comprises the following steps:

[0051] Step 1. Under the condition of 50°C and continuous stirring, first mix 5.0gNi(NO 3 ) 2 ·6H 2 A mixture of O and 2.5g of polyvinylpyrrolidone (PVP) was dissolved in 50mL of distilled water to obtain solution A, then 50mL of absolute ethanol was added to obtain solution B, and then 8.0mL of hydrazine hydrate was slowly added dropwise to solution B to obtain nano-nickel Sol;

[0052] Step 2, the particle size is 38μm ~ 74μm, the specific surface area is 1200m 2 The activated carbon per g is placed in boiling mass percent concent...

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Abstract

The invention discloses a preparation method for modified palladium-carbon catalyst for Suzuki coupling reaction. The catalyst is composed of active carbon, and palladium and nickel loaded on the active carbon, wherein the mass percent of the palladium is 5-10%, and the mass percent of the nickel is 0.5-3%. The preparation method for the modified palladium-carbon catalyst for the Suzuki coupling reaction includes steps that 1, preparing nano-nickel sol; 2, preparing active carbon carrier; 3, preparing nickel-containing size; 4, preparing palladium-containing solution; 5, adding the palladium-containing solution to the nickel-containing size, preserving the heat, dipping and filtering to obtain a piece of filter cake; 6, performing reduction treatment, and washing to obtain the modified palladium-carbon catalyst. The modified palladium-carbon catalyst prepared by the method can be used for the Suzuki coupling reaction, and the modified palladium-carbon catalyst has advantages of high reaction activity, high selectivity, good stability and the like; the catalyst is easy to be separated from the product, the catalyst preparation technique is simple, the catalyst can be used repeatedly, the precious metal-palladium is easy to recycle, the pollution and energy consumption are reduced, and the economical benefit and environment significance are important.

Description

technical field [0001] The invention belongs to the technical field of preparation of supported noble metal catalysts, and in particular relates to a preparation method of a modified palladium carbon catalyst for Suzuki coupling reaction. Background technique [0002] Since Miyaura et al. reported in 1979 that under the catalysis of palladium, the coupling reaction of organoboron compounds and halogenated hydrocarbons under mild conditions to prepare asymmetric biaryls, the Suzuki coupling reaction has formed a new era in the selective construction of carbon-carbon bonds. a new field of research. Carbon-carbon bond coupling can transform simple molecules into complex ones, and plays an extremely important role in chemical synthesis. This key step is included in the synthesis of many organic chemicals such as drugs, dyes and pesticides. In recent years, it has been a research hotspot in catalytic chemistry and organic chemistry. The research and development of Suzuki couplin...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J23/89
Inventor 闫江梅曾利辉曾永康张之翔
Owner XIAN CATALYST NEW MATERIALS CO LTD
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