Preparation method of tungstenic heteropolyacid catalyst

A technology of heteropoly acid and catalyst, which is applied in the field of preparation of tungsten-containing heteropoly acid catalyst, can solve the problems of not mentioning the water removal method and the name of the desiccant, and the type and amount of the desiccant are not clearly written, so as to save water and remove water. Raw materials, convenient for industrial production, and the effect of improving yield

Inactive Publication Date: 2013-05-01
SOUTH CHINA UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Other articles on the preparation of heteropolyacid-type catalysts also mostly use organic solvents instead, without clearly stating the type and amount, nor mentioning the method of water removal and the name of the desiccant

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] Weigh 12.5 g of tungstic acid, add 50 mL of 30% (mass fraction) hydrogen peroxide, raise the temperature to 60°C, and stir for 1 h until the solution is colorless. Filter, and cool the solution to room temperature. Weigh 1.6 g of phosphoric acid (85%, mass fraction), add 1.5 mL of water to dilute and add to the reaction solution, dilute the system to 150 mL with water, and stir for 30 min. Then, 400 mL of dichloromethane solution dissolved with 9.42 g of cetylpyridinium chloride was added dropwise to the reaction solution, and the stirring was continued for 1 h. The solution was allowed to stand, the organic phase was separated, and dichloromethane was distilled off in a water bath at 60°C to obtain a pale yellow solid catalyst [π-C 5 h 5 NC 16 h 33 ] 3 [ PO 4 ( WO 3 ) 4 ], the yield is calculated according to cetylpyridine chloride, and the yield is above 90%.

Embodiment 2

[0029] Weigh 12.5 g of tungstic acid, add 50 mL of 30% hydrogen peroxide, raise the temperature to 60°C, and stir for 1 h until the solution is colorless. Filter, and cool the solution to room temperature. Weigh 1.6 g of phosphoric acid (85%, mass fraction), add 1.5 mL of water to dilute and add to the reaction solution, dilute the system to 150 mL with water, and stir for 60 min. Then, 600 mL of dichloromethane solution dissolved with 9.42 g of cetylpyridinium chloride was added dropwise to the reaction solution, and the stirring was continued for 2 h. The solution was allowed to stand still, the organic phase was separated, and dichloromethane was distilled off in a water bath at 60°C to obtain a pale yellow solid catalyst [π-C 5 h 5 NC 16 h 33 ] 3 [ PO 4 ( WO 3 ) 4], the yield is calculated according to cetylpyridine chloride, and the yield is more than 95%.

Embodiment 3

[0031] Weigh 12.5 g of tungstic acid, add 50 mL of 40% hydrogen peroxide, raise the temperature to 65°C, and stir for 2 h until the solution is colorless. Filter, and cool the solution to room temperature. Weigh 1.6 g of phosphoric acid (85%, mass fraction), add 1.5 mL of water to dilute and add to the reaction solution, dilute the system to 150 mL with water, and stir for 90 min. Then, 600 mL of dichloromethane solution dissolved with 9.42 g of cetylpyridinium chloride was added dropwise to the reaction solution, and the stirring was continued for 3 h. The solution was allowed to stand, the organic phase was separated, and dichloromethane was distilled off in a water bath at 60°C to obtain a pale yellow solid catalyst [π-C 5 h 5 NC 16 h 33 ] 3 [ PO 4 ( WO 3 ) 4 ], the yield is calculated according to cetylpyridine chloride, and the yield is above 95%.

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Abstract

The invention relates to a preparation method of a tungstenic heteropolyacid catalyst. The method comprises the following steps that (1) an appropriate amount of tungstic acid and an oxidant are contacted, heated and stirred until a solution is colourless; filtering is conducted; the solution is cooled to a room temperature for use; (2) phosphoric acid is weighed, diluted and then added to reaction liquid; a system is diluted by water; stirring is conducted for reaction; (3) hexadecylpyridinium chloride is dissolved in methylene chloride and dropwise added to a final solution obtained in Step (2); stirring is continued for reaction; and (4) the solution stands; an organic phase is separated; methylene chloride is distilled off in a water bath at 50-60 DEG C; and a light-yellow solid catalyst is obtained. The preparation method has a creative improvement based on the original preparation method, so that the yield is increased, the cost is lowered, the flow is simplified, and industrial production is easy to realize.

Description

technical field [0001] The invention relates to a catalyst mainly used in an epoxidation reaction system, in particular to a preparation method of a tungsten-containing heteropolyacid catalyst. Background technique [0002] Heteropoly acid is a general term for oxygen-containing polyacids formed by central atoms (such as P, Ge, etc.) and coordination atoms (such as Mo, W, V, etc.) in a certain structure through the coordination bridge of oxygen atoms. Heteropolyacid catalysts, including heteropolyacid and heteropolyacid salt catalysts, are a class of acidic and redox catalysts with great development potential, and have developed rapidly in applied research and development in recent years. Because heteropolyacid is composed of two groups with different polarities, it can be dissolved in the system where water and other polar organic substances exist. It is a homogeneous catalyst with mild reaction conditions, high catalytic efficiency, and can be recycled. It is a green and ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J31/18
Inventor 刘国琴荆璐刘新旗于龙肖俊华
Owner SOUTH CHINA UNIV OF TECH
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