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High-activity and high-stability solid super acid and preparation method thereof

A solid super acid, high stability technology, used in the preparation of carboxylate, catalyst activation/preparation, chemical instruments and methods, etc., to achieve the effects of simple operation, high activity and high stability

Active Publication Date: 2017-10-17
NANJING FORESTRY UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, the methods for improving the stability of solid superacids still mainly follow the previous research ideas, however, there is no research on SO 4 2- / M x o y The large-scale industrial application of solid superacid has been reported, and its stability is still a research hotspot

Method used

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  • High-activity and high-stability solid super acid and preparation method thereof
  • High-activity and high-stability solid super acid and preparation method thereof
  • High-activity and high-stability solid super acid and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] Weigh 10g 0.1% SO 4 2- / Al 2 o 3 -ZrO 2 (The preparation method refers to [Fang Jianhua, Chen Boshui, Wang Jiu, Wu Jiang.SO 4 2- / Al 2 o 3 -ZrO 2 Research on preparation of biodiesel from waste animal and vegetable oils catalyzed by solid acid[J].], the same below) was dispersed in toluene solvent, added silane modifier, stirred at -20°C for 1 min, then cooled, filtered and washed. Collect the filter cake, dry it in an oven at 20°C, and grind it at room temperature to obtain a solid superacid sample containing 0.01% modifier, recorded as 0.01% silane-0.1% - / Al 2 o 3 -ZrO 2 .

[0021] 0.1% SO prepared above 4 2- / Al 2 o 3 -ZrO 2 Catalyst and 0.01% monosilane-0.1% SO 4 2- / Al 2 o 3 -ZrO 2 The catalyst was treated with water (the method is the same as [Qian Qi, Wang Danya, Wang Lei, Zhang Xue, Hu Di, Zhao Xuejuan, Li Xiaobao, Li Licheng. Comparison of the stability of sulfuric acid-promoted solid superacid under water pretreatment conditions[J]. Chem...

Embodiment 2

[0029]Weigh 10g 0.5% SO 4 2- / Al 2 o 3 -ZrO 2 (The preparation method refers to [Fang Jianhua, Chen Boshui, Wang Jiu, Wu Jiang.SO 4 2- / Al 2 o 3 -ZrO 2 Research on the preparation of biodiesel from waste animal and vegetable oils catalyzed by solid acid[J].]) dispersed in acetone solvent, added trimethylchlorosilane modifier, stirred at 100°C for 240min, then cooled, filtered and washed. Collect the filter cake and dry it in an oven at 150°C, and grind it at room temperature to obtain a solid superacid sample containing 0.1% modifier, recorded as 0.1% trimethylchlorosilane-0.5% SO 4 2- / Al 2 o 3 -ZrO 2 .

[0030] 0.5% SO prepared above 4 2- / Al 2 o 3 -ZrO 2 Catalyst and 0.1% Trimethylchlorosilane-0.5% SO 4 2- / Al 2 o 3 -ZrO 2 The catalyst was treated with water (the method is the same as [Qian Qi, Wang Danya, Wang Lei, Zhang Xue, Hu Di, Zhao Xuejuan, Li Xiaobao, Li Licheng. Comparison of the stability of sulfuric acid-promoted solid superacid under water...

Embodiment 3

[0037] Weigh 10g 1%SO 4 2- / Al 2 o 3 -ZrO 2 (The preparation method refers to [Fang Jianhua, Chen Boshui, Wang Jiu, Wu Jiang.SO 4 2- / Al 2 o 3 -ZrO 2 Preparation of biodiesel from waste animal and vegetable oils catalyzed by solid acid[J].]) dispersed in cyclohexane solvent, added octadecyltrichlorosilane modifier, stirred at 250°C for 2160min, then cooled and filtered , wash, collect the filter cake and put it into an oven for drying at 250°C, grind at room temperature to obtain a solid superacid sample containing 1% modifier, record 1% octadecyl trichlorosilane-1% SO 4 2- / Al 2 o 3 -ZrO 2 .

[0038] 1% SO prepared above 4 2- / Al 2 o 3 -ZrO 2 Catalyst and 1% Octadecyltrichlorosilane - 1% SO 4 2- / Al 2 o 3 -ZrO 2 After the catalyst is treated with water, the solid acid and water are at a solid-to-liquid ratio of 1:50, stirred at room temperature for 3 hours, filtered, and dried to obtain water-treated samples, which are recorded as 1% SO 4 2- / Al 2 o ...

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PUM

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Abstract

The invention discloses a high-activity and high-stability solid super acid and a preparation method thereof. The solid super acid consists of two parts, namely a sulfuric acid promoted type solid super acid and a modification group, wherein the mass content of sulfate radicals in the sulfuric acid promoted type solid super acid is 0.1-10%; the modification group is a C1-C20 organic matter with a silicon group or ester group; the mass content ratio of the modification group to the solid acid is 0.01-10%. The solid super acid disclosed by the invention has both high activity and high stability, and can still have the catalysis activity equivalent to that of a fresh solid acid after being soaked in water. The preparation method of the novel solid super acid, which is disclosed by the invention, has the advantages of being simple and convenient to operate, possible in industrial application and the like.

Description

technical field [0001] The invention relates to the technical field of material preparation, in particular to a high-activity and high-stability solid superacid and a preparation method thereof. Background technique [0002] Immobilizing sulfuric acid onto certain metal oxides can make a sulfuric acid-promoted solid superacid (SO 4 2- / M x o y , M is a metal element, and x and y are the coordination numbers of the metal element and oxygen), this type of material has attracted widespread attention. Currently, SO 4 2- / M x o y Types of solid superacids are: SO 4 2- / ZrO 2 , SO 4 2- / TiO 2 , SO 4 2- / Fe 2 o 3 , SO 4 2- / SnO 2 Wait. Compared with traditional liquid acid and other types of solid acid catalytic materials, SO 4 2- / M x o y It has the advantages of high catalytic efficiency, simple preparation method, low cost, easy recovery, non-corrosion and environmental protection, and shows good catalytic activity and selectivity for almost all acid-cat...

Claims

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Application Information

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IPC IPC(8): B01J27/053B01J37/00C07C67/08C07C69/14
CPCB01J27/053B01J37/00C07C67/08C07C69/14
Inventor 李力成岳海芹钱祺李小保王磊花泽林赵学娟
Owner NANJING FORESTRY UNIV