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A kind of preparation SO from wollastonite as raw material 4 2- /tio 2 -sio 2 Method for solid superacid

A technology of solid superacid and wollastonite, which is applied in the field of preparing SO42-/TiO2-SiO2 solid superacid, and can solve the problems of catalysts that have not been reported yet.

Inactive Publication Date: 2016-09-07
ENERGY RES INST CO LTD HENAN ACADEMY OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, using wollastonite as raw material to prepare SO 4 2- / TiO 2 -SiO 2 Catalyst research has not been reported yet

Method used

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  • A kind of preparation SO from wollastonite as raw material <sub>4</sub> <sup>2-</sup> /tio <sub>2</sub> -sio <sub>2</sub> Method for solid superacid
  • A kind of preparation SO from wollastonite as raw material <sub>4</sub> <sup>2-</sup> /tio <sub>2</sub> -sio <sub>2</sub> Method for solid superacid
  • A kind of preparation SO from wollastonite as raw material <sub>4</sub> <sup>2-</sup> /tio <sub>2</sub> -sio <sub>2</sub> Method for solid superacid

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] Weigh 0.01mol of 325 mesh wollastonite powder and place it in 100 ml of 0.05mol / L Ti (SO 4 ) 2 In the solution, stirring for 24h, 0.5mol / L ammonia water was added dropwise to the system at a rate of 1mL / min to adjust the pH of the system to 2; the system was placed at a temperature of 80 o In the water bath of C, and continuously stirred for 2h, the reaction solution was washed by centrifugation until no SO was detected by barium dichloride. 4 2- ions, the washed precipitate was placed in an oven at 80 o Anatase TiO was obtained by drying at C 2 -SiO 2 Complex. The resulting TiO 2 -SiO 2 The complex was impregnated and stirred with 0.5mol / L sulfuric acid at a ratio of 20ml / g, filtered and dried to obtain SO 4 2- / TiO 2 -SiO 2 Solid superacids such as figure 1 As shown, the solid acid has good crystallinity, and the XRD peaks of anatase are obvious; such as figure 2 As shown, the acidity of the solid acid meets the standard.

Embodiment 2

[0025] Weigh 0.01mol of 325 mesh wollastonite powder and place it in 150 ml of 0.05mol / L Ti (SO 4 ) 2 In the solution, stir for 26h, add 0.5mol / L ammonia water to the system dropwise at a speed of 2mL / min to adjust the pH of the system to 3; place the system at a temperature of 85 o In the water bath of C, and continuously stirred for 3h, the reaction solution was washed by centrifugation until no SO was detected by barium dichloride. 4 2- ions, the washed precipitate was placed in an oven at 80 o Anatase TiO was obtained by drying at C 2 -SiO 2 Complex. The resulting TiO 2 -SiO 2 The complex was impregnated and stirred with 0.5mol / L sulfuric acid at a ratio of 20ml / g, filtered and dried to obtain SO 4 2- / TiO 2 -SiO 2 Solid super acid, the XRD pattern and TPD spectrum of the product are the same as those in Example 1.

Embodiment 3

[0027] Weigh 0.01mol 325 mesh wollastonite powder and place it in 200ml 0.05mol / L Ti(SO 4 ) 2 In the solution, stirring for 28h, 0.5mol / L ammonia water was added dropwise to the system at a speed of 3mL / min to adjust the pH of the system to 4; the system was placed at a temperature of 85 o In the water bath of C, and continuously stirred for 4h, the reaction solution was washed by centrifugation until no SO was detected by barium dichloride. 4 2- ions, the washed precipitate was placed in an oven at 80 o Anatase TiO was obtained by drying at C 2 -SiO 2 Complex. The resulting TiO 2 -SiO 2 The complex was impregnated and stirred with 0.5mol / L sulfuric acid at a ratio of 20ml / g, filtered and dried to obtain SO 4 2- / TiO 2 -SiO 2 Solid super acid, the XRD pattern and TPD spectrum of the product are the same as those in Example 1.

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Abstract

The invention belongs to the field of preparation technologies of solid superacid and in particular relates to a method for preparing SO4<2-> / TiO2-SiO2 solid superacid by taking wollastonite as a raw material. The method comprises the following steps: (1) adding the wollastonite into a Ti(SO4)2 solution, stirring, dropwise adding ammonia water and adjusting the pH to 1.5-4 so as to obtain a system; (2) subsequently putting the system in a water bath, continuously stirring for completing crystallization process, filtering a reactant, washing and drying to obtain a compound; (3) finally dipping the compound in sulfuric acid, stirring, filtering and drying to obtain the SO4<2-> / TiO2-SiO2 solid superacid. The raw material of the SO4<2-> / TiO2-SiO2 solid superacid is low in cost and easily available; the synthesis process and the crystallization process are simultaneously completed in the water bath with the temperature being more than 80 DEG C, so that the method is easy to operate and easy to control.

Description

technical field [0001] The invention belongs to the technical field of solid super acid preparation, and in particular relates to a kind of preparation of SO by using wollastonite as a raw material 4 2- / TiO 2 -SiO 2 Method for solid superacids. Background technique [0002] Solid super acid has the advantages of high catalytic activity, no corrosion of reaction equipment, no "three wastes" pollution, convenient preparation, and simple separation of regenerated and reused catalysts and products. Its research and application have become a hot field of seeking new green and environmentally friendly catalysts, which are of great significance to promoting the development of the chemical industry in the direction of environmental protection, and have become one of the hot spots of current catalysis research. of which SO promoted by sulfate 4 2- / W x O y Inorganic solid superacids exhibit high reactivity and good product selectivity for almost all acid-catalyzed reactions....

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J27/053
Inventor 任素霞常霞雷廷宙徐海燕耿锋何晓峰朱金陵
Owner ENERGY RES INST CO LTD HENAN ACADEMY OF SCI
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