Preparation method of zirconium-containing solid super acid

A technology of solid super acid and zirconium source, applied in chemical instruments and methods, molecular sieve catalysts, physical/chemical process catalysts, etc., can solve the problems of sulfuric acid concentration limitation, poor hydrothermal stability, high temperature resistance, etc., to achieve acidity and The effect of uniformity improvement, good hydrothermal stability, and good hydrothermal stability

Inactive Publication Date: 2015-10-14
XIANGTAN UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] Although halogen-containing solid superacids have high catalytic activity, there are problems such as easy detachment of active components, high temperature resistance, poor hydrothermal stability, and environmental pollution, which limit their application; SO 4 2- / MxOy type solid superacid has the advantages of simple preparation and high activity, but the existing problems are relatively small specific surface, irregular pore structure, poor catalytic selectivity, SO 4 2- Groups are easily lost in water or other solvents, the concentration of sulfuric acid used for impregnation is limited
At present, there is no synthesis of MFI framework type superacid catalyst by template ion exchange in the disclosed solid superacids.

Method used

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  • Preparation method of zirconium-containing solid super acid
  • Preparation method of zirconium-containing solid super acid
  • Preparation method of zirconium-containing solid super acid

Examples

Experimental program
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Embodiment 1

[0055] Take 38g of tetrapropylammonium hydroxide solution with a mass fraction of 23.5% and mix it with 55g of water, stir at 60°C for about 0.5h, then add 39g of ethyl orthosilicate dropwise to the mixture; after the dropwise addition, set the temperature At 80°C, start timing from temperature adjustment, remove alcohol for 7 hours, add water to maintain the volume of the solution; pour out the liquid, add water to 114g, and then crystallize at 200°C for three days; centrifuge, wash, and Dry to obtain the pure silicon molecular sieve S-1 containing the template agent in the channel. Mix 5g of the above-mentioned S-1 molecular sieve with 13.0g of tetrapropylammonium hydroxide solution with a mass fraction of 23.5% and 80g of ethanol, stir and mix thoroughly at 40°C; then dissolve 2.8g of tetrabutyl zirconate in 50g of ethanol, slowly Add dropwise to the above mixed solution, carry out template ion exchange at 40°C for 10h; then filter out the solid, wash, dry, and roast at 500...

Embodiment 2

[0058] Take 38g of tetrapropylammonium hydroxide solution with a mass fraction of 23.5% and mix it with 55g of water, stir at 60°C for about 0.5h, then add 39g of ethyl orthosilicate dropwise to the mixture; after the dropwise addition, set the temperature At 80°C, start timing from temperature adjustment, remove alcohol for 7 hours, add water to maintain the volume of the solution; pour out the liquid, add water to 114g, and then crystallize at 200°C for three days; centrifuge, wash, and Dry to obtain the pure silicon molecular sieve S-1 containing the template agent in the channel. Mix 5g of the above S-1 molecular sieve with 9g of tetrapropylammonium hydroxide solution with a mass fraction of 23.5% and 150g of isopropanol, stir and mix thoroughly at 70°C; then dissolve 4g of tetrabutyl zirconate in 50g of isopropanol , slowly added dropwise to the above mixture, and carried out template ion exchange at 70°C for 20h; then filtered out the solid, washed, dried, and roasted at...

Embodiment 3

[0060] Take 38g of tetrapropylammonium hydroxide solution with a mass fraction of 23.5% and mix it with 55g of water, stir at 60°C for about 0.5h, then add 39g of ethyl orthosilicate dropwise to the mixture; after the dropwise addition, set the temperature At 80°C, start timing from temperature adjustment, remove alcohol for 7 hours, add water to maintain the volume of the solution; pour out the liquid, add water to 114g, and then crystallize at 200°C for three days; centrifuge, wash, and Dry to obtain the pure silicon molecular sieve S-1 containing the template agent in the channel. Mix 5g of the above S-1 molecular sieve with 15.8g of tetrapropylammonium bromide solution with a mass fraction of 23.5% and 200g of ethanol, stir and mix thoroughly at 70°C; then dissolve 6g of zirconium nitrate pentahydrate in 50g of ethanol, slowly drop In the above mixed solution, template ion exchange was carried out at 90°C for 30h; then the solid was filtered out, washed, dried, and calcine...

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Abstract

The invention discloses a preparation method of a zirconium-containing solid super acid. According to the preparation method, template ion exchange is adopted so as to introduce a certain amount of zirconium element into unroasted pure silicon molecular sieve; Zr-MFI is obtained via filtering, washing, and roasting; a solution with a certain SO4<2-> concentration is used for dipping the obtained molecular sieve; and the solid super acid is obtained via filtering, drying, and roasting. Compared with molecular sieves of other skeleton types, the MFI-type skeleton structure obtained via preparation catalysis possesses neat pore passage structures and relatively thick pore walls, and excellent hydrothermal stability; pore passage regularity can be maintained for a long time under mechanical action of flow such as high temperature high pressure flow, collapse is not induced, stability is high, acid strength is high, the zirconium-containing solid super acid possesses both excellent performance of solid molecular sieves, acidity of super acid, and uniformly distributed acid sites, is a novel acid catalytic material with enormous potential; and application prospect in reactions such as alkylation, isomerization, esterification, acylation, polymerization, and oxidation is promising.

Description

technical field [0001] The invention relates to a method for preparing a solid superacid, in particular to a method for preparing a molecular sieve solid superacid through a template ion exchange method. Background technique [0002] Acid catalysts are widely used catalysts in the chemical industry. Traditional acid catalysts include liquid catalysts such as concentrated sulfuric acid and hydrofluoric acid. These catalysts have sufficient contact with materials and high catalytic efficiency. However, these two types of catalysts have problems of polluting the environment and corroding equipment, and are facing elimination. Compared with liquid acids, the density of strong acid centers in general solid acids is much smaller than that of liquid acids, and the intensity distribution of acid centers is not uniform, so it is difficult to meet the demand for acid strength in many reactions, thus restricting its industrial application. Therefore, the development of solid superacid...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J29/89
Inventor 吴剑杜思思毛志铭吴照伟
Owner XIANGTAN UNIV
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