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Magnetic superfine solid acid catalyst in double-shell structure and its prepn process

A solid acid catalyst, solid acid technology, applied in catalyst activation/preparation, chemical instruments and methods, physical/chemical process catalysts, etc.

Inactive Publication Date: 2003-11-05
BEIJING UNIV OF CHEM TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The purpose of the present invention is to overcome the above shortcomings that the active center of the catalyst cannot fully function, and prepare a magnetic solid acid catalyst with a double-shell structure, that is, select a carrier with a large surface area as the transition layer, and first wrap the magnetic core coating, and then let the active components be monodispersed on its surface, greatly increasing the number of acid centers, and preparing a magnetic solid acid catalyst with a double-layer coating structure

Method used

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  • Magnetic superfine solid acid catalyst in double-shell structure and its prepn process

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] FeCl 2 4H 2 O solution (0.1mol / l) and FeCl 3 ·6H 2 Add O solution (0.1mol / l) into a three-necked flask at a ratio of 5:1, place it in a constant temperature water bath at 65°C, add 0.1mol / l NaOH dropwise while stirring, until the pH value of the solution reaches 12, and continue to age with constant temperature stirring 30min. Use a magnetic field to separate the magnetic substrate from the supernatant. Wash with deionized water until the pH value of the solution is close to 7, and the black magnetic core Fe can be obtained. 3 o 4 .

[0022] Take the Fe that is made into 0.0025mol suspension 3 o 4 Add 50ml into a three-necked flask, place it in a constant temperature water bath at 50±1°C and stir, add 1mol / l NaOH dropwise to make the pH of the solution reach 9. 0.025mol ethanol solution of tetraethyl orthosilicate (1.9mol / l) was added dropwise, and 1mol / l NaOH was added dropwise at the same time to keep the pH of the reaction solution at 9 all the time. After ...

Embodiment 2

[0026] According to the method of embodiment 1, with 50ml Fe 3 o 4 (0.0025mol) with 100ml ZrOCl 2 .8H 2 O (0.0125mol) can be used as raw material to prepare ZrO 2 with Fe 3 o 4 ZrO with a molar ratio of 5:1 2 / Fe 3 o 4 Carrier with magnetic, according to 25%wt loading capacity, use Zr(SO 4 ) 2 4H 2 O solution was impregnated at room temperature for 6 h, filtered and dried to obtain Zr(SO 2 ) 2 / ZrO 2 / Fe 3 o 4 catalyst.

[0027] 0.6 g of the above catalyst was weighed and put into the reaction system as in Example 1, and the esterification conversion activity of the catalyst was measured to be 98%.

Embodiment 3

[0029] According to the method of Example 1, finally press 25%wt loading capacity, use SO 4 2- -ZrO 2 impregnated SiO 2 / Fe 3 o 4 , to get SiO 2 with Fe 3 o 4 SO with a molar ratio of 10:1 4 2- -ZrO 2 / SiO 2 / Fe 3 o 4 Magnetic solid acid catalyst.

[0030] 0.6 g of the above catalyst was weighed and put into the reaction system as in Example 1, and the esterification conversion activity of the catalyst was measured to be 98%.

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Abstract

The catalyst features that magnetic nucleus is coated with high-specific surface area carrier to form carrier with magnetic nucleus and the carrier with magnetic nucleus is further coated with one layer of strong solid acid. The catalyst is prepared through sol-gel process, in which magnetic nucleus Fe3O4, Co-Fe3O4, Mn-Fe3O4 or Ni-Fe3O4 is coated with high-specific surface area carrier SiO2, ZrO2, Al2O3, TiO2, etc. to form carrier with magnetic nucleus; and subsequent soaking process, in which strong solid acid Zr(SO4)2, SO42--ZrO2, F-ZrO2, etc. is dispersed to the surface of the carrier with magnetic nucleus. This kind of solid acid catalyst in double-shell structure is mainly used in acid catalytic reaction, and features magnetism and high catalytic activity.

Description

Technical field: [0001] The invention relates to a double shell structure magnetic solid acid catalyst and a preparation method thereof. Background technique: [0002] At present, when studying solid acid catalysts at home and abroad, we often encounter the problem that ultrafine catalyst particles are difficult to separate and recycle. In view of this situation, our laboratory and Harbin Engineering University jointly proposed the idea of ​​endowing the catalyst with magnetism and using an external magnetic field to separate it. In the patent application 00133474.3, the ZrO 2 Coated in Fe 3 o 4 Externally prepared ZrO 2 / Fe 3 o 4 Magnetic solid acid catalyst, Zr(SO 4 ) 2 4H 2 O and Fe 3 o 4 Zr(SO 4 ) 2 / Fe 3 o 4 Magnetic solid acid catalyst, but these two preparation methods are to directly coat the active component on the surface of the magnetic core, the disadvantage is that the surface active component is affected by the influence of the magnetic core and d...

Claims

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Application Information

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IPC IPC(8): B01J27/053B01J35/00B01J35/08B01J37/02
CPCB01J27/053B01J37/0221B01J35/33B01J35/51
Inventor 段雪常铮
Owner BEIJING UNIV OF CHEM TECH
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