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Preparation method of heptanuclear manganese-substituted silicon tungsten oxide catalyst and application thereof

A technology of manganese substitution and catalyst, which is applied in the field of preparation of heptanuclear manganese substitution silicotungsten oxygen cluster catalysts, can solve the problems of undiscovered patent documents and achieve the effect of simple preparation method

Active Publication Date: 2018-05-25
LIAOCHENG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, transition metal substituted silicotungsten oxide clusters have not been reported as catalysts for this reaction.
[0004] Through searching, no published patent documents related to the application of the present invention have been found

Method used

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  • Preparation method of heptanuclear manganese-substituted silicon tungsten oxide catalyst and application thereof
  • Preparation method of heptanuclear manganese-substituted silicon tungsten oxide catalyst and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] Example 1: Compound K 10 (H 2 O) 26 mn 7 (H 2 O) 9 Si 4 W 40 o 140 preparation of

[0027] Add sodium tungstate (0.5mmol), water (10 mL), manganese chloride (0.1mmol), sodium silicate (0.1mmol), potassium chloride (0.8mmol) in a clean reaction kettle The pH of the solution was adjusted to 4 with hydrochloric acid, stirred for 12 hours, and reacted at 150 degrees Celsius for 5 days. After the reaction was completed, it was cooled to room temperature and filtered to obtain black crystals. The yield is about 31%.

Embodiment 2

[0028] Example 2: Compound K 10 (H 2 O) 26 mn 7 (H 2 O) 9 Si 4 W 40 o 140 preparation of

[0029] Add sodium tungstate (0.6mmol), water (15 mL), manganese chloride (0.1mmol), sodium silicate (0.1mmol), potassium chloride (0.8mmol) in a clean reaction kettle The pH of the solution was adjusted to 4 with hydrochloric acid, stirred for 12 hours, and reacted at 150 degrees Celsius for 5 days. After the reaction was completed, it was cooled to room temperature and filtered to obtain black crystals. The yield is about 35%.

Embodiment 3

[0030] Example 3: Compound K 10 (H 2 O) 26 mn 7 (H 2 O) 9 Si 4 W 40 o 140 preparation of

[0031] Add sodium tungstate (0.7mmol), water (20 mL), manganese nitrate (0.5mmol), sodium silicate (0.1mmol), potassium chloride (0.8mmol) in a clean reaction kettle in turn The pH of the solution was adjusted to 6, stirred for 24 hours, and reacted at 160 degrees Celsius for 7 days. After the reaction was completed, it was cooled to room temperature and filtered to obtain black crystals. The yield is about 43%.

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Abstract

The invention discloses a preparation method of a heptanuclear manganese-substituted silicon tungsten oxide catalyst and application thereof. The preparation method comprises the following steps: placing sodium tungstate, water, manganese salt, sodium silicate and potassium chloride in a reaction kettle, adjusting the pH, carrying out a reaction, cooling to room temperature after the reaction, andfiltering to obtain black crystals. When the catalyst is applied to the process of synthesizing TBiTD by an oxygen method, the high yield is as high as 86%, a reaction process is simple, the obtainedproduct is high in purity, and post-treatment is simple.

Description

technical field [0001] The invention belongs to the technical field of catalyst material preparation, and relates to a preparation method and application of a heptanuclear manganese substituted silicon tungsten oxygen cluster catalyst. technical background [0002] Polyoxometalates (abbreviated as POMs) are a class of clusters containing Mo, W, V and other elements. The research on catalysis is becoming more and more extensive, and the research focus has shifted from structure to catalysis. At present, Japan has successively realized industrialization projects such as POMs catalyzed propylene hydration to prepare isopropanol, POMs gas-phase oxidation of 2-methacrolein to prepare methacrylic acid, and POMs to oxidize ethylene to prepare acetic acid and other industrial projects. These major achievements have had extensive influence in the international chemical community. , bringing huge economic benefits. Among them, silicon tungsten oxygen clusters are a common and very im...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J31/16B01J27/188B01J23/30B01J23/34C07C333/32C01G45/00
CPCB01J23/30B01J23/34B01J27/188B01J31/1608C01G45/006C01P2002/72C07C333/32
Inventor 李春霞武福燕李文玲崔传生黄现强
Owner LIAOCHENG UNIV
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