Preparation method of silicotungstic heteropoly acid loaded catalyst

A supported catalyst and silicotungstic heteropolyacid technology, which is applied in the preparation of organic compounds, the preparation of carboxylate, chemical instruments and methods, etc. Enlargement, good thermal stability, good selectivity

Active Publication Date: 2012-10-24
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Benefits of technology

This patented process involves preparing an alkaline treated (Si02) porous material that helps with mixing different types of molecules together for better results during chemical reactions like alcoholysis or esterification processes. It also improves its durability over time due to improved heat resistance compared to other materials commonly found on carriers such as zeolite powder. Overall this new type of catalyst provides more efficient ways to produce desired products from various sources than traditional methods.

Problems solved by technology

This patented describes different types of materials called heteropolymers or polyoxometalates with various structures like tetrahedral atoms connected by bonds between carbon atoms through covalent bonding. These compounds have unique properties due to their ability to form complex networks when combined together without losing any part of them themselves. They also exhibit excellent stability even at high temperatures over long periods of time.

Method used

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  • Preparation method of silicotungstic heteropoly acid loaded catalyst
  • Preparation method of silicotungstic heteropoly acid loaded catalyst
  • Preparation method of silicotungstic heteropoly acid loaded catalyst

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0016] Formed SiO 2 Immersed in 0.01 mol / L Na 2 CO 3 In the solution, the impregnation temperature is 40°C, the impregnation time is 16 hours, and then the impregnated SiO 2 Filter, wash with water until neutral, and dry for later use. Take Keggm structure silicotungstic acid H 3 SiW 12 o 40 · x H 2 Dissolve 20 grams of O(x=0-30) in 10 milliliters of deionized water. Get the SiO that the above-mentioned alkali handles standby 2 20 grams mixed with the above silicotungstic acid solution, deionized water and SiO 2 The liquid-solid ratio is 0.5 ml / g. In a rotary evaporator, the immersion temperature is 60°C, and the immersion is continuously rotated and immersed for 24 hours; then it is taken out and dried under a nitrogen flow for 6 hours at a drying temperature of 120°C; and then under a nitrogen flow, at 300°C 50 wt% silicotungstic acid / SiO was prepared by firing for 3 hours 2 catalyst. Table 1 shows the surface pore parameters of the prepared silicotungstic heterop...

Embodiment 2

[0021] Formed SiO 2 Immersed in 0.05 mol / L NaHCO 3 In the solution, the impregnation temperature is 30°C, the impregnation time is 18 hours, and then the impregnated SiO 2 Filter, wash with water until neutral, and dry for later use. Take the Keggin structure silicotungstic acid H 3 SiW 12 o 40 · x H 2 O (x = 0 ~ 30) 20 grams is dissolved in 40 milliliters of methanol, take the SiO 2 40 grams are mixed with the above silicotungstic acid solution, methanol and SiO 2 The liquid-solid ratio is 1.0 ml / g. In a rotary evaporator, the immersion temperature is 30°C, and the immersion is continuously rotated and immersed for 18 hours; then it is taken out and dried under nitrogen flow for 3 hours at a drying temperature of 140°C; and then under nitrogen flow, 350°C 44 wt% silicotungstic acid / SiO was prepared by firing for 4 hours 2 catalyst. Table 2 shows the surface pore parameters of the prepared silicotungstic heteropolyacid-supported catalyst.

[0022] Table 2

[0023] ...

Embodiment 3

[0026] Formed SiO 2 Immerse in 0.1 mol / L NaOH solution, the impregnation temperature is 50°C, and the impregnation time is 20 hours, and then the impregnated SiO 2 Filter, wash with water until neutral, and dry for later use. Take the Keggin structure silicotungstic acid H 3 SiW 12 o 40 · x H 2 O (x = 0 ~ 30) 30 grams is dissolved in 135 milliliters of ethanol, take the SiO 2 90g is mixed with the above silicotungstic acid solution, ethanol and SiO 2 The liquid-solid ratio is 1.5 ml / g. In a rotary evaporator, the immersion temperature is 40°C, and the immersion is continuously rotated and immersed for 20 hours; then it is taken out and dried under nitrogen flow for 9 hours at a drying temperature of 160°C; and then under nitrogen flow, 400°C 37.5% by weight silicotungstic acid / SiO was prepared by firing for 5 hours 2 catalyst. Table 3 shows the surface pore parameters of the prepared silicotungstic heteropolyacid-supported catalyst.

[0027] table 3

[0028]

[00...

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Abstract

The invention relates to a preparation method of a silicotungstic heteropoly acid loaded catalyst, and aims to mainly solve the problem of poor activity of silicotungstic heteropoly acid loaded catalysts in the prior art. The method of the invention includes the following steps of: a) steeping a molded SiO2 carrier in an alkaline solution with a concentration of 0.001-5 mol/L for 8-48 hours at a temperature of 10-100DEG C, and conducting filtration, washing, as well as drying for standby use; b) dissolving a Keggin structured silicotungstic heteropoly acid H3SiW12O40.x H2O in water or an organic solvent; c) mixing the SiO2 carrier treated by step a) with the silicotungstic heteropoly acid solution obtained in step b); and d) carrying out dynamic steeping on the liquid-solid mixture obtained in step c), then performing drying and roasting in an inert atmosphere, thus obtaining the silicotungstic heteropoly acid loaded catalyst. The technical scheme adopted by the method of the invention well solves the problem, and can be used in the industrial production of silicotungstic heteropoly acid loaded catalysts.

Description

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Claims

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Application Information

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Owner CHINA PETROLEUM & CHEM CORP
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