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Activated charcoal carried silver phosphotungstomolybdate heteroployacid catalyzer and method for preparing the same and application thereof

A technology of heteropolyacids and catalysts, applied in chemical instruments and methods, preparation of organic compounds, physical/chemical process catalysts, etc., can solve problems such as low solubility, difficulty in ensuring catalyst quality and stability, and achieve easy handling and high activity high effect

Inactive Publication Date: 2009-02-25
LIAOCHENG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0013] In summary, in the prior art so far, the heteropolyacid catalyst with activated carbon as the carrier is obtained by impregnating the heteropolyacid solution with the carrier, but generally the solubility of heteropolyacid salts in polar solvents is small, so The method of impregnating a heteropolyacid salt solution with a carrier is difficult to regulate the loading range when preparing a heteropolyacid salt catalyst supported by a carrier, which makes it difficult to guarantee the quality and stability of the prepared catalyst

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] Preparation of activated carbon-supported molybdenum phosphotungstic acid silver salt catalyst

[0035] A certain amount of 200-400 micron activated carbon is added with 10% HNO 3 Heat and reflux for 1.5 hours in the solution until the activated carbon is just submerged, then wash the activated carbon particles with cooling water until the pH is neutral, filter with suction, dry at 120°C for 3 hours, and cool in a desiccator. Add 3 g of activated carbon to 10 ml of 10% H 3 PW 6 Mo 6 o 40 Stir in the solution (95% ethanol and water are mixed in equal volume as solvent), slowly add 20ml concentration of 10% AgNO 3 solution, let it stand, and the precipitated phosphomolybdenum tungsten heteropolyacid silver salt to be formed is supported by activated carbon particles, and the loaded activated carbon particles are placed in a drying oven, dried at 90°C for 3 hours, and then cooled in a desiccator to obtain activated carbon-supported phosphorus Molybdenum tungsten heter...

Embodiment 2

[0037] Preparation of activated carbon-supported molybdenum phosphotungstic acid silver salt catalyst

[0038] A certain amount of 300-400 micron activated carbon is added with 10% HNO 3 The solution was heated to reflux for 1.5 hours until the solution was just submerged in activated carbon, washed with cooling water until the pH was neutral, filtered with suction, dried at 120°C for 3 hours, and cooled in a desiccator. Add 3 g of activated carbon to 10 ml of 15% H 3 PW6 Mo 6 o 40 Stir in the solution (95% ethanol and water are mixed in equal volume as solvent), slowly add 30ml concentration of 10% AgNO 3 The solution was left to stand, dried in a drying oven at 90° C. for 3 hours, and cooled in a desiccator to obtain a silver phosphomolybdenum tungsten heteropolyacid catalyst supported on activated carbon.

Embodiment 3

[0046] Catalytic Activity of Various Catalysts for the Reaction of Cyclohexanone and Ethylene Glycol

[0047] With the activated carbon supported phosphomolybdenum tungstic acid silver salt catalyst prepared by embodiment 1 and 2 and the phosphomolybdenum tungstoheteropoly acid silver salt catalyst prepared by comparative examples 1 and 2, evaluate its reaction to cyclohexanone and ethylene glycol by the following method Catalytic activity for alcohol reactions.

[0048] Add cyclohexanone, ethylene glycol, 10ml water-carrying agent cyclohexane and a certain amount of catalyst into a 100mL three-necked bottle at a ratio of 1:1.8, install a thermometer, a water separator and a reflux condenser, and heat the reflux fraction. water until almost no water comes out. Cool slightly and drain the water layer. The organic layers were combined and washed successively with saturated brine and secondary water until neutral, and then washed with anhydrous MgSO 4 Dry and distill, collect ...

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PUM

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Abstract

The present invention discloses an activated carbon supported phosphomolybdic tungsten heteropoly acid silver salt catalyst, and the preparation method and application in ketal synthesis. The catalyst is obtained by treating activated carbon via HNO3, adding the activated carbon into phosphomolybdic tungsten heteropoly acid solution, stirring, adding with AgNO3 solution drip by drip, standing for precipitation adsorption and then drying. The catalyst of the present invention consists of the activated carbon particles with the particle diameter of 75-800 nm loading the phosphomolybdic tungsten heteropoly acid silver salt with the weight occupying 1-50 percent, and is characterized in manageability after reaction, high activity, wide loading range and uniform activated distribution, which is suitable for the generation ketol reaction of ketone and alcohol.

Description

technical field [0001] The invention relates to a solid acid catalyst and its preparation and application, in particular to an activated carbon-supported phosphomolybdenum tungsten heteropolyacid silver salt catalyst, its preparation method and its application in ketal synthesis. Background technique [0002] Ketals are important intermediates in the chemical industry, often used in the protection of ketones, and even as special reaction solvents. Ketals have better floral and fruity aromas than parent carbonyl compounds, and most of them have special aromas. They have been widely used as new fragrances in daily chemical and food industries for more than ten years. [0003] The traditional method for synthesizing ketals is to synthesize ketones and alcohols by direct dehydration under the catalysis of inorganic acids (such as sulfuric acid, hydrochloric acid, phosphoric acid). The rate is high, but they all have strong corrosiveness, severely corrode equipment, produce a se...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J27/19B01J23/50C07C41/56
Inventor 龚树文尹汉东刘丽君李考真魏西莲
Owner LIAOCHENG UNIV
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