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Preparation method of sandwich nickel substituted silicon tungsten oxygen cluster catalyst

A sandwich-type, catalyst technology is applied in the oxidation preparation of carbonyl compounds, chemical instruments and methods, metal/metal oxide/metal hydroxide catalysts, etc. , the effect of good catalytic activity

Inactive Publication Date: 2019-09-17
聊城市技师学院
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0006] The purpose of the present invention is to solve the problem that the catalytic activity of simple polymetallic oxygen cluster catalysts needs to be improved in the selective oxidation process of alcohols, and to provide a preparation method for synthesizing sandwich-type nickel-substituted silicon-tungsten oxygen cluster catalysts, in order to improve the selection of alcohols. play a catalytic role in sexual oxidation

Method used

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  • Preparation method of sandwich nickel substituted silicon tungsten oxygen cluster catalyst
  • Preparation method of sandwich nickel substituted silicon tungsten oxygen cluster catalyst
  • Preparation method of sandwich nickel substituted silicon tungsten oxygen cluster catalyst

Examples

Experimental program
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Effect test

Embodiment 1

[0027] Example 1 Compound K 4 (H 2 O) 8 Na 8 (H 2 O) 8 Ni 4 Si 2 W 18 o 68 The preparation, its synthetic steps are as follows:

[0028] Add K successively to a clean beaker 8 [γ-SiW 10 o 36 ]·12H 2 O (1.5g) and 20mL sodium acetate-acetic acid buffer solution, stirred vigorously at 40°C for 15min, added nickel chloride (0.2g), reacted for 2h, after the reaction was completed, cooled to room temperature, filtered, and the filtrate slowly evaporated at room temperature , After 5-7 days, blocky single crystals were obtained. The yield is about 35%.

Embodiment 2

[0029] Example 2 Compound K 4 (H 2 O) 8 Na 8 (H 2 O) 8 Ni 4 Si 2 W 18 o 68 The preparation, its synthetic steps are as follows:

[0030] Add K successively to a clean beaker 8 [γ-SiW10 o 36 ]·12H 2 O (2g) and 20mL sodium acetate-acetic acid buffer solution, stirred vigorously at 40°C for 15min, added nickel chloride (0.2g), reacted for 2h, after the reaction was completed, cooled to room temperature, filtered, and the filtrate evaporated slowly at room temperature, After 5-7 days, bulk single crystals are obtained. The yield is about 37%.

Embodiment 3

[0031] Example 3 Compound K 4 (H 2 O) 8 Na 8 (H 2 O) 8 Ni 4 Si 2 W 18 o 68 The preparation, its synthetic steps are as follows:

[0032] Add K successively to a clean beaker 8 [γ-SiW 10 o 36 ]·12H 2 O (1.5g) and 30mL sodium acetate-acetic acid buffer solution, stirred vigorously at 40°C for 15min, added nickel chloride (0.25g), reacted for 2h, after the reaction was completed, cooled to room temperature, filtered, and the filtrate evaporated slowly at room temperature , After 5-7 days, blocky single crystals were obtained. The yield is about 38%.

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Abstract

The invention discloses a preparation method for a sandwich-type nickel-substituted silicon-tungsten oxygen cluster catalyst. This method combines K 8 [γ‑SiW 10 O 36 ]·12H 2 O, nickel chloride, and sodium acetate-acetic acid buffer solution are placed in a beaker to react. After the reaction is completed, filter and the filtrate slowly evaporates to obtain a crystal of a sandwich-type nickel-substituted silicon-tungsten oxygen cluster catalyst. The method of the invention has the characteristics of fast reaction speed, simple reaction process, high purity of the product obtained, and simple post-processing. In the selective oxidation of aromatic alcohols, the conversion rate is as high as 90.8% and the selectivity is as high as 95.1%.

Description

technical field [0001] The invention belongs to the technical field of catalyst material preparation, and relates to the preparation technology of a sandwich-type nickel-substituted silicon-tungsten-oxygen cluster catalyst. The novel sandwich-type nickel-substituted silicon-tungsten-oxygen cluster has better catalytic activity. Background technique [0002] Polyoxometalates (abbreviated as POMs) are a kind of metal-oxygen clusters (Metal-Oxygen Clusters) compounds rich in transition elements such as Mo, W, V, Nb and Ta in the skeleton structure. The composition and structure of POMs determine its strong acidity and strong oxidizing properties, so polymetallic oxygen clusters exhibit excellent catalytic properties in many types of organic synthesis reactions. Since the 1970s, many catalysis scientists have been involved in the field of POMs research, and have achieved world-renowned achievements in both basic theoretical research and industrial application development. At pr...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J23/888B01J27/188C07C47/54C07C47/542C07C47/55C07C47/575C07C45/29
CPCC07C45/294B01J23/002B01J23/888B01J27/188B01J2523/00B01J35/30B01J2523/12B01J2523/13B01J2523/41B01J2523/69B01J2523/847C07C47/54C07C47/542C07C47/55C07C47/575
Inventor 韩艳华宋成敏
Owner 聊城市技师学院