Magnesium-aluminum hydrotalcite loaded-type superfine nano-palladium catalyst and preparation method thereof

A magnesium-aluminum hydrotalcite, ultra-fine nanotechnology, applied in the direction of catalyst activation/preparation, chemical instruments and methods, physical/chemical process catalysts, etc., can solve the problem of affecting the phase state and morphology of palladium nanoparticles, and environmental pollution of stabilizers , nano-palladium loss and other problems, to achieve good catalytic performance and reusable performance, narrow particle size distribution, and small average particle size

Active Publication Date: 2019-04-16
INST OF PETROCHEM HEILONGJIANG ACADEMY OF SCI
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  • Abstract
  • Description
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Problems solved by technology

[0004] In order to solve the problems of environmental pollution caused by the use of stabilizers in the preparation process of nano-palladium catalysts, the loss of nano-palladium and the influence on the phase state and morphology of palladium nanoparticles, the invention provides a magnesium-aluminum hydrotalcite-supported ultrafine nano-palladium catalyst and its preparation method

Method used

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  • Magnesium-aluminum hydrotalcite loaded-type superfine nano-palladium catalyst and preparation method thereof
  • Magnesium-aluminum hydrotalcite loaded-type superfine nano-palladium catalyst and preparation method thereof
  • Magnesium-aluminum hydrotalcite loaded-type superfine nano-palladium catalyst and preparation method thereof

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Embodiment 1

[0029] A preparation method of magnesium-aluminum hydrotalcite-supported ultrafine nano-palladium catalyst, the steps are as follows: according to a certain weight ratio, magnesium-aluminum hydrotalcite is mixed with water; Ultrasonic power is used to ultrasonically treat the mixed solution, so that the magnesium aluminum hydrotalcite is evenly dispersed in the mixed solution; according to a certain Pd 2+ The weight ratio of magnesium-aluminum hydrotalcite to the above-mentioned mixed solution is added to the above-mentioned mixed solution, and the resulting mixed solution is ultrasonically treated with the second ultrasonic power. After a certain period of ultrasound, the upper liquid is removed by centrifugation, and the obtained precipitate is magnesium-aluminum hydrotalcite. type ultrafine nano-palladium catalyst.

Embodiment 2

[0031] A preparation method of magnesium-aluminum hydrotalcite-supported ultrafine nano-palladium catalyst, the steps are as follows:

[0032] According to a certain Mg 2+ with Al 3+ Dissolve magnesium salt and aluminum salt in deionized water at a molar ratio to obtain solution A; according to a certain OH - / (Mg 2+ +Al 3+ ) and CO 3 2- / Al 3+ The molar ratio of NaOH and Na 2 CO 3 Dissolve in deionized water to obtain solution B; at room temperature, add solution B dropwise to solution A, adjust the pH value after stirring for a certain period of time to obtain magnesium aluminum hydrotalcite jelly; place the magnesium aluminum hydrotalcite jelly Carry out crystallization treatment at a certain temperature, wash, dry and grind after cooling to obtain powdered magnesium aluminum hydrotalcite.

[0033] Mix magnesium-aluminum hydrotalcite with water according to a certain weight ratio, pass nitrogen into the obtained mixed solution to replace the air as a protective gas...

Embodiment 3

[0035] A preparation method of magnesium-aluminum hydrotalcite-supported ultrafine nano-palladium catalyst, the steps are as follows:

[0036] by Mg 2+ with Al3+ The molar ratio is 1~4:1. Dissolve magnesium salt and aluminum salt in deionized water to obtain solution A; press OH - / (Mg 2+ +Al 3+ ) and CO 3 2- / Al 3+ The molar ratio of NaOH and Na is 1-4:1 2 CO 3 dissolved in deionized water to obtain solution B; at room temperature, slowly add solution B dropwise to solution A, and after stirring for 2 hours, adjust the pH value to 10-11 to obtain magnesium-aluminum hydrotalcite jelly; the magnesium-aluminum hydrotalcite The jelly was placed in a polytetrafluoroethylene autoclave, and crystallized at 80°C for 18 hours. After natural cooling, the white jelly was separated and washed 3 times with deionized water, and placed in a 60°C drying oven overnight. Grind in a bowl to obtain white powder, and obtain powdered magnesium aluminum hydrotalcite.

[0037] According to ...

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Abstract

The invention relates to a magnesium-aluminum hydrotalcite loaded-type superfine nano-palladium catalyst and a preparation method thereof, and belongs to the technical field of palladium catalysts. Inorder to solve the problem that environmental pollution is generated due to the fact that a stabilizer is used in the nano-palladium catalyst preparation process, the invention provides the preparation method of the magnesium-aluminum hydrotalcite loaded-type superfine nano-palladium catalyst. The method comprises the steps that magnesium-aluminum hydrotalcite is mixed with water, nitrogen is introduced, mixed liquid is subjected to ultrasonic treatment at first ultrasonic power, the magnesium-aluminum hydrotalcite is uniformly dispersed in the mixed liquid; a palladium brine solution is added according to the certain weight ratio of Pd<2+> to magnesium-aluminum hydrotalcite, and precipitate obtained through centrifugation is the magnesium-aluminum hydrotalcite loaded-type superfine nano-palladium catalyst. Accordingly, the stabilizer and a reducing agent are not used, the particle size of superfine nano-palladium particles is only 1.85-3.45 nm, the catalyst is applied to a Suzuki coupling reaction, and good catalytic performance and reusability are shown.

Description

technical field [0001] The invention belongs to the technical field of palladium catalysts, in particular to a magnesium-aluminum hydrotalcite-supported ultrafine nano-palladium catalyst and a preparation method thereof. Background technique [0002] Palladium-catalyzed Suzuki coupling reaction is the main method to construct carbon-carbon bonds, and has been widely used in the synthesis of natural products, pharmaceutical intermediates and advanced functional materials. The palladium catalyst is the core of the whole reaction and also the focus of research. In the Suzuki coupling reaction, the homogeneous palladium complex catalyst is generally used, which can be uniformly dispersed in the reaction solution, and has high catalytic efficiency and product yield, but the homogeneous palladium complex cannot be recycled and reused. Residual palladium will pollute the product, increasing the difficulty of product separation and purification; and although the supported palladium...

Claims

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Application Information

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IPC IPC(8): B01J23/56B01J37/34
CPCB01J23/007B01J23/58B01J37/343B01J35/393
Inventor 白雪峰李佳哲吕宏飞刘洋胡永玲李晓鹏
Owner INST OF PETROCHEM HEILONGJIANG ACADEMY OF SCI
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