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Preparation method and application of WO3/ZrO2 solid super acidic catalyst

A solid superacid and catalyst technology, which is applied in the direction of catalyst activation/preparation, physical/chemical process catalyst, metal/metal oxide/metal hydroxide catalyst, etc. Reuse and other issues to achieve good effect, high selectivity, high catalytic activity and selectivity

Inactive Publication Date: 2010-09-15
FUDAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In past studies, acid-washed layered clay, zeolite molecular sieve, layered zirconium phosphate, and SO 4 2- / ZrO 2 Materials such as solid superacids have been tried to catalyze the isomerization of α-pinene, but these catalysts have the following defects and deficiencies: low activity, low selectivity of target products, high reaction temperature, difficult to reuse, etc.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] 17.105 g of ZrO(NO 3 ) 2 2H 2 O was dissolved in 320mL of water, and concentrated ammonia water was slowly added dropwise under stirring until the pH = 9-10, and aged at room temperature for 24 hours. The aged sample was hydrothermally treated at 100°C for 24 hours, and the precipitate was filtered and washed until the filtrate Does not contain Cl - ion, the resulting Zr(OH) 4 The filter cake was dried at 100°C for 24 hours, then soaked and ground with 0.02mol / L ammonium metatungstate aqueous solution for 1 hour, the liquid-solid ratio was 3.05mL / g, evaporated to dryness by heating, and dried at 100°C for 12 hours, in the air atmosphere Calcined at 800°C for 3 hours to obtain Catalyst-1, in which WO 3 The content is 18wt%, and its specific surface is 70m 2 / g.

Embodiment 2

[0021] 41.248 g of ZrOCl 2 ·8H 2 O was dissolved in 320mL of water, and concentrated ammonia water was slowly added dropwise under stirring until the pH = 9-10, aged at room temperature for 36 hours, and the aged sample was hydrothermally treated at 100°C for 12 hours, and the precipitate was filtered and washed until the filtrate Does not contain Cl - ion, the resulting Zr(OH) 4 The filter cake was dried at 110°C for 12 hours, then soaked and ground with 0.01mol / L ammonium metatungstate aqueous solution for 2 hours, the liquid-solid ratio was 4.91mL / g, heated and evaporated to dryness, dried at 90°C for 24 hours, in air atmosphere Calcined at 800°C for 3 hours to obtain Catalyst-2, in which WO 3 The content is 15wt%, and its specific surface is 63m 2 / g.

Embodiment 3

[0023] 22.371 g of ZrCl 4 Dissolve in 320mL of water, slowly add concentrated ammonia water dropwise under stirring conditions until pH = 9-10, age at room temperature for 12 hours, the aged sample is hydrothermally treated at 100°C for 36 hours, the precipitate is filtered and washed until it is in the filtrate Does not contain Cl - ion, the resulting Zr(OH) 4 The filter cake was dried at 90°C for 36 hours, then soaked and ground with 0.03mol / L ammonium metatungstate aqueous solution for 0.6 hours, the liquid-solid ratio was 2.47mL / g, evaporated to dryness by heating, dried at 120°C for 6 hours, and placed in an air atmosphere Calcined at 800°C for 3 hours to obtain Catalyst-3, in which WO 3 The content is 21wt%, and its specific surface is 67m 2 / g.

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Abstract

The invention belongs to the technical field of catalysts, and particularly relates to a preparation method and application of a WO3 / ZrO2 solid super acidic catalyst. The preparation method comprises the following steps of: preparing a zirconium hydroxide precursor by adopting a precipitation method, carrying out hydro-thermal treatment on the precursor, soaking the precursor in ammonium meta-tungstate and roasting at high temperature to obtain the solid super acidic catalyst with larger specific surface. When applying the catalyst to Alpha-pinene isomerization reaction, a favorable effect can be obtained, Alpha-pinene conversion ratio and selectivity to target products of camphene and limonene are high and the catalyst still keeps high activity and high selectivity after multiple regeneration and repeated use.

Description

technical field [0001] The invention belongs to the technical field of catalysts, in particular to a WO 3 / ZrO 2 Preparation method and application of solid superacid catalyst. Background technique [0002] The prior art discloses that acid catalysis is a very important class of reactions. In recent years, with the improvement of environmental protection requirements, in order to realize green production, people are eager to replace the environmentally unfriendly catalysts used in some important industrial reactions, such as: HF, H 2 SO 4 、H 3 PO 4 and AlCl 3 Wait. WO 3 / ZrO 2 Solid superacid catalysts have both the reproducibility of heterogeneous catalysts and the high activity and high selectivity of liquid superacids, and are environmentally friendly. They are likely to replace liquid acids and become a new generation of catalysts under the current sustainable development background. , Create a batch of clean processes without environmental pollution. How to i...

Claims

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Application Information

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IPC IPC(8): B01J23/28B01J21/06B01J37/08C07C13/42C07C5/25C07C5/31
Inventor 涂兴珺华伟明乐英红翟德伟高滋
Owner FUDAN UNIV
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