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Preparation method for supported type palladium catalyst

A supported palladium and catalyst technology, which is applied in chemical instruments and methods, physical/chemical process catalysts, metal/metal oxide/metal hydroxide catalysts, etc., can solve the problem of lack of modification means, expensive equipment and operating costs, and operation High cost and other issues, to achieve good scale production and industrial application, reduce operating costs, and good stability

Inactive Publication Date: 2014-07-23
CHINA UNIV OF PETROLEUM (EAST CHINA)
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0011] c. There are specific requirements for the type of catalyst support, which limits the broad application of the method;
[0012] d, the preparation method requires expensive equipment, and the operating cost is too high;
[0013] e. After the palladium component is loaded on the carrier, there is a lack of other beneficial modification means except simple roasting; or due to reason (d), the post-treatment also requires expensive equipment and operating costs
[0014] f. When used under high temperature conditions, its palladium components are always easy to aggregate;
[0015] g. The stability of use under high temperature and different atmosphere conditions is not clear

Method used

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  • Preparation method for supported type palladium catalyst

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preparation example Construction

[0058] The preparation method of supported palladium catalyst adopts the above-mentioned supported palladium catalyst preparation device, and the concrete steps are as follows:

[0059] Step 1, catalyst carrier loading, the specific method is as follows:

[0060] The catalyst carrier is Al 2 o 3 , SiO 2 , aluminosilicate, zeolite molecular sieve, MgO or ZrO 2 One or a mixture of several of them; the catalyst carrier is granular, and the particle size is within the range of 10 to 100 mesh; the catalyst carrier is filled in the main pipeline 1, and the catalyst carrier fills the cross section of the main pipeline 1 to form a catalyst carrier bed Layer 4: Catalyst carrier bed layer 4 is fixed with metal mesh, glass wool or quartz wool; make sure that all gas sources connected to the supported palladium catalyst preparation device are closed.

[0061] Step 2, the gas phase deposition of palladium acetylacetonate; Concrete method is as follows:

[0062] Open the first containe...

Embodiment 1

[0079] Preparation device such as figure 1 As shown, the catalyst carrier is 5.0g 20-50 mesh Al 2 o 3 Carrier particles;

[0080] 4g palladium acetylacetonate is housed in the first container 9;

[0081] The bipyridine in the second container 13 is 2,2-bipyridine, and its mass is 4g;

[0082] The quality of methyl orthosilicate in the third container 17 is 4g;

[0083] The quality of saturated ammonia water in the fourth container 21 is 133g;

[0084] The gas provided by the inert gas source 6 is pure N 2 gas;

[0085] The gas provided by the oxygen gas source 7 is O 2 with N 2 mixture, where O 2 The mole fraction of is 10.2%;

[0086] The gas provided by the hydrogen gas source 8 is pure hydrogen;

[0087] The gas provided by the first container gas source 10 is pure N 2 gas;

[0088] The gas provided by the second container gas source 14 is pure N 2 gas;

[0089] The gas provided by the third container gas source 18 is pure N 2 gas;

[0090] The gas provided...

Embodiment 2

[0128] The difference from Example 1 is:

[0129] Catalyst carrier is made of the Al in example one 2 o 3 Replaced with SiO 2 ; SiO 2 The particles are 20-50 mesh.

[0130] Step 2, the temperature of the second container is changed to 95°C.

[0131] Step 6: Change the temperature of the catalyst carrier bed 4 to 100° C., and change the holding time to 0.6 h.

[0132] Step 7: Change the temperature of the catalyst carrier bed 4 to 100° C., and change the holding time to 2 hours.

[0133] In order to verify the positive effect of the product in Example 2, 3 parts of the product in Example 2 were weighed, each 0.5g, numbered #11, #12, #13. These three samples were used according to the usage methods of #1, #2, and #3 samples in Example 1, respectively.

[0134] Then, a TEM experiment was carried out to measure the microscopic size of the above-mentioned supported palladium catalyst, and CO-chemisorpotion was carried out to measure the percentage of bare palladium atoms on ...

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Abstract

The invention belongs to the field of catalyst preparation and relates to a preparation device and a preparation method for a supported type palladium catalyst. The preparation device comprises a main pipeline, wherein a catalyst support is filled in the main pipeline to form a catalyst support bed layer; an inert gas source, an oxygen gas source and a hydrogen gas source enter the main pipeline through a gas inlet respectively, separately and directly; gas from a first container gas source, a second container gas source, a third container gas source and a fourth container gas source enters the main pipeline; the gas flowing into the main pipeline passes through the catalyst support bed layer and then flows out from a gas outlet. The preparation method comprises the following steps: filling the catalyst support; performing vapor deposition on palladium acetylacetonate; performing primary hydrogen reduction; adsorbing dipyridyl; selectively desorbing the dipyridyl; forming a tetramethyl orthosilicate coverage layer; solidifying tetramethyl orthosilicate; performing oxygen roasting; performing secondary hydrogen reduction. The preparation method is low in equipment cost and low in operation cost; a catalyst product which contains high-dispersion palladium components and is ultra-stable under the high-temperature using condition can be obtained.

Description

technical field [0001] The invention belongs to the field of catalyst preparation, and in particular relates to a preparation method of a supported palladium catalyst, which is used for preparing a supported palladium catalyst with high dispersion of palladium metal components and superstable at high temperature. Background technique [0002] Supported catalysts with metal palladium (Pd) as the active component are often used in industrial production and laboratory research or research and development in the field of heterogeneous catalysis, and play an especially important role in the catalytic production process of the petrochemical industry. From the basic principle of surface chemistry, the smaller the microscopic size of the active metal aggregates on the carrier, the higher its dispersion, and the better the catalytic effect may be. At present, there are many methods to realize the preparation of supported small-sized metal palladium catalysts. These preparation method...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J23/44
Inventor 林旭锋席燕燕严魏宁许路遥火玉龙
Owner CHINA UNIV OF PETROLEUM (EAST CHINA)