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Vapor-phase deposition preparation method of load type iron catalyst

An iron catalyst, vapor deposition technology, applied in catalyst activation/preparation, molecular sieve catalysts, chemical instruments and methods, etc., can solve the problems of high safety cost, strong toxicity and explosive capacity, etc. Strong control effect

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

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Problems solved by technology

However, as we all know, Fe(CO)5 has strong toxicity and explosive ability, and its operation process must bear extremely high safety costs
[0007] In summary, in the field of preparation of supported iron catalysts, there is still a lack of a method that does not require liquid, has no (low) toxicity of raw materials, is environmentally friendly, and is safe to operate. A preparation method with simple steps, low cost, and small (<15 nm) iron component particles on the catalyst

Method used

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  • Vapor-phase deposition preparation method of load type iron catalyst

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preparation example Construction

[0026] The preparation method of the supported iron catalyst comprises the following steps.

[0027] Step 1, filling of the catalyst carrier; the specific method is as follows:

[0028] 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 reaction tube, and the catalyst carrier fills the cross section of the reaction tube to form a catalyst carrier bed 3; The catalyst carrier bed 3 is fixed by metal mesh, glass wool or quartz wool.

[0029] Step 2, place the ferrocene heap; the specific method is as follows:

[0030] A ferrocene stack is placed near the inlet end in the reaction tube; the mass ratio of the ferrocene to the catalyst carrier is 1:30 to 20:1; the center distance between the ferrocene stack and the catalyst carrier bed 3 is 0 to 50 cm;

[0031] St...

Embodiment 1

[0040] The preparation device of supported iron catalyst such as figure 1 As shown, the material of the reaction tube is quartz; the first thermocouple and the second thermocouple are K-type thermocouples; the stop valve and gas pipeline are made of stainless steel; the gas source is high-purity N 2 and compressed air; the flow rate of the source gas is controlled and displayed by a flow meter.

[0041] The preparation method of supported iron catalyst, the preparation steps are as follows:

[0042] Step (1), weigh 1.0 g γ-Al 2 o 3 Carrier, particle size is 20~50 mesh, according to figure 1 Place in a quartz reaction tube and fix it with wire mesh.

[0043] Step (2), take by weighing 0.8 g ferrocene solid, press figure 1 The way to put into the reaction tube, ferrocene pile and the center distance of the carrier layer is 10 cm.

[0044] Step (3), with N 2 As the air source, open the shut-off valve to make N 2 Into the inlet end of the reaction tube, N 2 The flow rate ...

Embodiment 2

[0048] Embodiment two, The difference with Example 1 is: step (1) uses γ-Al 2 o 3 The particle size of the carrier is 40-80 mesh. Step (3) The temperatures measured by the two thermocouples are both 130°C; N 2 The flow rate is 40 mL / min. Step (5) The second thermocouple shows a temperature of 400 o C; the time is 6h.

[0049] After the preparation, the iron content in the catalyst was analyzed to be 5.5 wt%, and the size of the nano-iron was analyzed by transmission electron microscope to be 2-7nm.

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Abstract

The invention belongs to the preparation field of industrial catalysts, and specifically relates to a vapor-phase deposition preparation method of a load type iron catalyst. The preparation method of the load type iron catalyst adopts a vapor-phase deposition preparation device of the load type iron catalyst, and comprises the following steps: step I, filling a catalyst carrier; step II, placing a ferrocene heap; step III, depositing an iron component; step IV, roasting at a low temperature; and step V, roasting at a high temperature. The vapor-phase deposition preparation method disclosed by the invention can be used for obtaining the load type iron catalyst with a high-dispersion iron component; the preparation method is simple and convenient to operate, strong in controllability, high in preparation efficiency, strong in universality for different carrier types, and convenient to popularize; the preparation method does not involve liquid, and therefore, waste liquid treatment is not needed; the safety of a preparation process is greatly improved; the iron catalyst obtained by the preparation method disclosed by the invention can be directly applied to chemical industry production of a fixed-bed reactor.

Description

technical field [0001] The invention belongs to the field of industrial catalyst preparation, and in particular relates to a method for preparing a supported iron catalyst by vapor deposition. The supported iron catalyst is prepared by a metal organic compound vapor deposition method. Background technique [0002] Supported iron (Fe)-based catalysts are catalysts for many important industrial catalytic production processes, such as the catalytic oxidation of alkanes, and the process of obtaining hydrocarbons from synthesis gas through Fischer-Tropsch reaction. From the perspective of microscopic principles, the catalytic performance of a catalyst for a certain reaction is largely determined by the microscopic distribution and chemical state of the active components of the catalyst, and these two factors are closely related to how the catalyst is prepared. Therefore, it is of great significance to explore different preparation processes of catalysts for the improvement of cat...

Claims

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Application Information

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IPC IPC(8): B01J37/03B01J23/745B01J29/035
Inventor 林旭锋席燕燕许路遥严魏宁
Owner CHINA UNIV OF PETROLEUM (EAST CHINA)
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