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High-efficient iron-series catalyst and its preparation method

A catalyst and catalyst carrier technology, applied in the field of iron-based catalysts and their preparation, can solve the problems of reducing the specific surface area and activity of iron-based catalysts, particle growth, secondary agglomeration, etc., and achieve easy industrial production, simple preparation process, good stability effect

Inactive Publication Date: 2010-04-21
JIANGSU TIANYI ULTRA FINE METAL POWDER
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] The recent research results of my country's 863 program show that the synthesis of nano-scale particles using divalent iron salt as the basic raw material can play a very good catalytic effect, but the precursor of the nano-catalyst generated during the preparation process is a metastable solid, such as If it is not dispersed in time, secondary agglomeration will occur; when the precursor is oxidized to form a catalyst product, the particle growth will also occur, reducing the specific surface area and activity of the iron-based catalyst

Method used

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Examples

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Effect test

preparation example Construction

[0020] The preparation method of efficient iron-based catalyst of the present invention consists of the following steps:

[0021] ① Add a solid catalyst carrier to the autoclave, vacuumize or replace the air in the autoclave with high-purity nitrogen or inert gas, and add iron pentacarbonyl liquid;

[0022] ②Start the heating device, heat it to the temperature and keep it warm, so that the iron pentacarbonyl evaporates into steam in the reactor and fully expands, and penetrates into the micropores of the catalyst carrier;

[0023] ③ Continue to raise the temperature or pass high-temperature and high-pressure high-purity nitrogen or other inert gases into the reactor to decompose the iron pentacarbonyl adsorbed in the micropores of the carrier in situ to obtain nano-sized iron particles;

[0024] ④ Cooling, discharge the gas to the tail gas treatment system, put the finished nano-iron-based catalyst into a package filled with high-purity nitrogen or other inert gas, and keep it...

Embodiment 1

[0029] Add zeolite to a 2L high-pressure reaction kettle, blow nitrogen to replace the residual air in the kettle and the pipeline, add 200ml of pentacarbonyl iron liquid, heat to 60°C for 2h, continue heating to 200°C, hold for 1h, cool down, and open the exhaust valve The gas in the kettle is discharged to obtain the nano-iron-based catalyst, which is taken out and put into a packaging bag filled with high-purity nitrogen for airtight storage.

[0030] The above-mentioned nano-iron-based catalyst was applied to the direct coal liquefaction experiment: Huolinhe lignite was used, hydrogenated residual oil was used as a solvent, the reaction temperature was 350°C, the initial pressure of hydrogen was 6MPa, the amount of catalyst added was 3%, and the mass ratio of Fe:S was 2 : 3 add sulfur powder, the reaction time is 1.5 hours, the coal conversion rate is 84.3%, and the oil recovery rate is 56.2%.

Embodiment 2

[0032] The same preparation method as in Example 1 was used to produce nanometer iron-based catalysts, wherein the solid catalyst was activated carbon, 800ml of iron pentacarbonyl liquid, the heating temperature was 103°C, the temperature was kept for 1.2h, and the temperature was continued to 250°C for half an hour. The coal type was changed to Shenhua Dongsheng lignite for coal liquefaction experiment, the coal conversion rate was 83.2%, and the oil recovery rate was 58.7%.

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Abstract

The present invention discloses one kind of nanometer iron catalyst and its preparation process and apparatus. The nanometer iron catalyst is prepared through the following steps: adding liquid iron pentacarbonyl; heating iron pentacarbonyl in a reactor for the iron pentacarbonyl to infiltrate into the pores of catalyst carrier; further heating or introducing high temperature pressurized high purity nitrogen or other inert gas to decompose iron pentacarbonyl to obtain nanometer level iron particle; cooling, filling the prepared nanometer iron catalyst into package filled with high purity nitrogen and sealing for preserving. The present invention utilizes solid carrier to block the aggregation of iron particle for obtain nanometer iron particle. The nanometer iron catalyst has high activity, high dispersivity, high stability and simple preparation process, and is suitable for industrial production.

Description

technical field [0001] The invention relates to an iron-based catalyst and a preparation method thereof, in particular to an in-situ decomposition of iron pentacarbonyl on a solid catalyst carrier to produce a uniformly dispersed and highly efficient iron-based catalyst and a preparation method thereof. Background technique [0002] The transition group element iron has a special d electron orbital, and the H 2 , N 2 , NH 3 、C 2 h 2 、C 2 h 4 It can produce chemical adsorption, generate intermediate species on the surface, activate and dissociate the adsorbed molecules into atoms, and provide reactants for various chemical reactions, so it is an excellent chemical catalyst. Iron-based catalysts have been widely used in the fields of coal chemical industry, petroleum refining, ammonia synthesis and decomposition catalysis. [0003] At present, the commonly used iron-based catalysts mainly include natural pyrite, pyrite and various smelting waste residues. Its particles...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J23/745
Inventor 高为鑫柯尊斌张蓉艳
Owner JIANGSU TIANYI ULTRA FINE METAL POWDER
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