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Preparation method of silicotungstic heteropoly acid loaded catalyst

A technology of silicotungstic acid and catalyst, which is applied in the field of preparation of silicotungstic heteropolyacid supported catalysts, can solve the problems of poor activity of silicotungstic heteropolyacid supported catalysts, and achieves increased pore size, good selectivity, and good internal the effect of diffusion

Active Publication Date: 2015-01-07
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The technical problem to be solved by the present invention is the problem of poor activity of silicotungstic heteropoly acid supported catalysts in the prior art, and a new preparation method of silicotungstic heteropoly acid supported catalysts is provided

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
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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

technical field [0001] The invention relates to a preparation method of a silicotungstic heteropolyacid supported catalyst. Background technique [0002] Heteropoly acid has strong acidity. In organic medium, the molar catalytic activity of heteropoly acid is 100-1000 times that of sulfuric acid. Heteropoly acids are relatively stable, non-toxic and easy to handle, and do not produce side reactions such as sulfidation, chlorination and nitration. As a new type of catalytic material, it has shown broad application prospects in the fields of oil refining and chemical industry, and has been successfully applied in olefin hydration, alkylation and isomerization reactions. The specific surface area of ​​heteropoly acid (<10m 2 / g) is very small, and it needs to be loaded as a solid catalyst to increase its specific surface area so that the active components can be fully utilized. Document CN200710118426.7 introduces a silicotungsten, phosphotungstic heteropolyacid supported...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J23/30B01J21/08C07C69/14C07C67/08
Inventor 杨洪云高焕新金国杰丁琳陈璐康陈军
Owner CHINA PETROLEUM & CHEM CORP
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