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Preparing method of high working temperature magnetic carrier

A technology of magnetic carrier and working temperature, applied in catalyst carriers, chemical instruments and methods, catalyst activation/preparation, etc., can solve the problems of weakened magnetism, no way to work normally, etc., and achieve the effect of high magnetic performance

Inactive Publication Date: 2010-02-17
CHINA UNIV OF PETROLEUM (EAST CHINA)
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, it should also be noted that the temperature of most catalytic reactions will exceed 100 ° C, and the original magnetic catalysts will be greatly weakened at high temperatures, and there is no way to work normally. Therefore, the preparation of magnetic catalysts that can work at high temperatures The catalyst carrier is very important

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] a. FeSO with a mass fraction of 8% 4 Add NaOH solution with a mass fraction of 5% in the salt solution, adjust the pH value of the solution to 10, control the reaction temperature at 40°C, stir evenly, and pass in air to oxidize, the gas flow rate is controlled at 50L / h, when Fe 2+ When fully oxidized, the solution is left to stand, then suction filtered and washed, and the washed product is dehydrated at 200°C, and reduced by passing hydrogen at 300°C for 3 hours to obtain Fe 3 o 4 , and then oxidized in air at 250°C for 3h to obtain needle-like γ-Fe 2 o 3 ;

[0022] b. Add γ-Fe in step a 2 o 3 Disperse in 0.5mol / l NaOH solution, disperse and stir at 60°C for 0.5h, stir and dropwise add 0.2mol / l cobalt sulfate solution under nitrogen protection, and add dropwise 0.5 h, and then take out the cobalt-coated acicular γ-Fe 2 o 3 Wash with water until neutral, and dry in a desiccator at 60°C for 24 hours;

[0023] c. Prepare a 0.5 mol / l silicate solution at a temper...

Embodiment 2

[0034] The acicular gamma-Fe obtained in embodiment 1 2 o 3 Disperse in 0.5mol / l NaOH solution, disperse and stir at 60°C for 0.5h, stir and dropwise add 0.2mol / l cobalt sulfate solution under nitrogen protection, and add dropwise for 1h at a molar ratio of Fe:Co=1:0.5 , and then take out the cobalt-coated acicular γ-Fe 2 o 3 Wash with water until neutral, and dry in a desiccator at 60°C for 24 hours;

[0035] a. Prepare a 0.5mol / l silicate solution at a temperature of 20°C, add 0.5mol / l acid under stirring conditions, adjust the pH of the solution to 8, and prepare the cobalt-coated γ-Fe 2 o 3 Ultrasonic dispersion in the above silicate solution, the molar ratio is Si:Fe=1:3, then add 0.2mol / l acid to adjust the pH value of the solution to 4, stir for 3h, then centrifuge the product, wash to obtain the package Coated SiO 2 magnetic powder;

[0036] b. Coating SiO in step a 2 The magnetic powder is ultrasonically dispersed in deionized water, and then mixed evenly with...

Embodiment 3

[0045] The acicular gamma-Fe obtained in embodiment 1 2 o 3 Disperse in 0.5mol / l NaOH solution, disperse and stir at 60°C for 0.5h, stir and dropwise add 0.2mol / l cobalt sulfate solution under nitrogen protection, add 0.5 h, and then take out the cobalt-coated acicular γ-Fe 2 o 3 Wash with water until neutral, and dry in a desiccator at 60°C for 24 hours;

[0046] a. Prepare a 0.5mol / l silicate solution at a temperature of 40°C, add 0.5mol / l acid under stirring conditions, adjust the pH of the solution to 9, and prepare the cobalt-coated γ-Fe 2 o 3 Ultrasonic dispersion in the above silicate solution, the molar ratio is Si:Fe=1:5, then add 0.2mol / l acid to adjust the pH value of the solution to 3, stir for 3h, then centrifuge the product, wash to obtain the package Coated SiO 2 magnetic powder;

[0047] b. Coating SiO in step a 2 The magnetic powder is ultrasonically dispersed in deionized water, and then mixed evenly with 0.5mol / l aluminum sol and 0.5mol / l organic ami...

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Abstract

The invention discloses a preparing method of a high working temperature magnetic carrier, comprising the following steps: 1) preparing needle-like gamma-Fe2O3; 2) coating cobalt on the surface of gamma-Fe2O3; 3) coating a transition layer SiO2 on the surface of gamma-Fe2O3 or barium ferrite; and 4) after dispersing magnetic powder coated with SiO2, mixing the magnetic powder, alumina based sol and organic amine solution, and shaping oil posts to obtain a magnetic nuclear shell structure alumina carrier composed of an inner nuclear layer, a transition layer and an outer shell layer. The magnetic carrier prepared with the method of the invention still has high magnetic performance at the working temperature of 30-300 DEG C; at the working temperature of 100 DEG C, the coercive force is greater than 10kA / m which is 5Am<2> / kg greater than the specific saturation magnetization; after loading various catalysis active substances, the magnetic carrier can satisfy the catalysis selective hydrogenation reaction of high reaction system temperature fluidized beds and magnetically stabilized beds.

Description

technical field [0001] The invention relates to a preparation method of a high working temperature magnetic carrier. Background technique [0002] Magnetic catalysts are a class of catalysts with magnetic response characteristics. The composition of the magnetic catalyst includes a magnetic core and a coating layer, and then a layer of active components is loaded on the magnetic core or carrier to make it have catalytic activity. The magnetic core material is mainly made of iron oxide, and the cladding layer is mainly made of Al 2 o 3 , SiO 2 , ZrO 2 , to protect the core and load the active agent. Magnetic catalyst not only combines the advantages of high catalytic activity in homogeneous catalysis, but also avoids the characteristics of diffusion limitation in heterogeneous catalysis, and at the same time endows the catalyst with unique magnetic separation characteristics, which simplifies the operation process and reduces the operation cost. [0003] Magnetically st...

Claims

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Application Information

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IPC IPC(8): B01J32/00B01J23/78B01J23/75B01J35/02B01J37/12B01J37/18B01J37/34C10G45/00
Inventor 于濂清刘晨光付庆涛
Owner CHINA UNIV OF PETROLEUM (EAST CHINA)
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