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Preparation method of tetramer nickel substituted silicon tungsten oxygen cluster catalyst

A technology of catalyst and silicon tungsten, which is applied in the field of preparation of tetrapolynickel instead of silicon tungsten oxygen cluster catalyst, can solve the problems of catalytic activity to be improved, achieve good catalytic activity, simple preparation method, and easy separation

Inactive Publication Date: 2017-10-27
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

[0005] 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 thioether, and to provide a preparation method for synthesizing tetrapolynickel substituted silicotungsten oxygen cluster catalysts, in order to improve the catalytic performance of thioether play a catalytic role in the selective oxidation of

Method used

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

Examples

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Effect test

Embodiment 1

[0027] Example 1 Compound K 16 (H 2 O) 44 Ni 8 (H 2 O) 8 Si 4 W 40 o 144 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 (2mmol) and 50mL water, stir at 60°C for 15min, add nickel chloride (1mmol), adjust the pH value between 5 with dilute acetic acid, react for 10h, after the reaction is completed, cool to room temperature, filter, and the filtrate is at room temperature Evaporated slowly under the condition of 3~4 days to obtain bulk single crystal. The yield is about 30%.

Embodiment 2

[0029] Example 2 Compound K 16 (H 2 O) 44 Ni 8 (H 2 O) 8 Si 4 W 40 o 144 The preparation, its synthetic steps are as follows:

[0030] Add K successively to a clean beaker 8 [γ-SiW 10 o 36 ]·12H 2 O (3mmol) and 60mL water, stir at 60°C for 15min, add nickel chloride (1mmol), adjust the pH value between 5 with dilute acetic acid, react for 10h, after the reaction is completed, cool to room temperature, filter, and the filtrate is at room temperature Evaporate slowly under the condition of 3~4 days to obtain bulk single crystal. The yield is about 35%.

Embodiment 3

[0031] Example 3 Compound K 16 (H 2 O) 44 Ni 8 (H 2 O) 8 Si 4 W 40 o 144 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 (3mmol) and 70mL water, stirred at 60°C for 15min, added nickel salt (2mmol), adjusted the pH value between 6 with dilute acetic acid, reacted for 15h, after the reaction was completed, cooled to room temperature, filtered, and the filtrate was kept at room temperature Evaporate slowly, and block single crystals are obtained after 3-4 days. The yield is about 42%.

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Abstract

The invention discloses a preparation method of a tetramer nickel substituted silicon tungsten oxygen cluster catalyst. The method comprises the following steps: placing K8[gamma-SiW10O36].12H2O, nickel chloride and water into a beaker and reacting, and then filtering and slowly volatilizing the filtrate, thereby acquiring a crystal of the tetramer nickel substituted silicon tungsten oxygen cluster catalyst. The method has the characteristics of high reaction speed, simple reaction process, high-purity product, simple post-processing, and the like. In the selective oxidization of sulfur ether, the conversion rate is as high as 93.4% and the selectivity is as high as 99.3%.

Description

technical field [0001] The invention belongs to the technical field of catalyst material preparation, and relates to the preparation technology of tetrapolynickel substituted silicon tungsten oxide cluster catalyst. Background technique [0002] Inorganic-organic hybrid materials have recently become a hot research field for scientists, especially the hybrid materials obtained by combining metal-oxygen clusters with organic ligands. They not only have various structures, but also have potential applications in many fields. Prospects, such as catalysis, hydrogen storage, molecular adsorption, magnetism, and photochemistry. Polyoxometalates (POMs for short) have become a well-known inorganic building block due to their excellent catalytic performance and their chemical stability, including oxidation stability, thermal stability and hydrolytic stability. As an important branch of POMs, tungstate has become a very important option for constructing hybrid materials based on POMs...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J23/888C07C315/02C07C317/14C07C317/22
Inventor 韩艳华宋成敏
Owner 聊城市技师学院
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