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Ordered mesoporous KIT-6 loaded zirconium sulfate-aluminum composite oxide solid acid material, and preparation and application thereof

A KIT-6, aluminum composite technology, applied in the direction of catalyst activation/preparation, biofuel, fatty acid esterification, etc., can solve the problems of low acid content, poor structural thermal stability, and small pore size of solid acid materials, and achieve the preparation method Easy to implement, adjustable coating degree, and controllable surface acidity

Active Publication Date: 2021-10-22
TAIYUAN UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] However, the mesoporous zirconia supports prepared by traditional methods not only exhibit poor porosity, low specific surface area, and small pore size, but also are prone to crystal phase transformation during the heating process, resulting in SO 4 2- The resulting solid acid materials generally have disadvantages such as low acid content, poor structural thermal stability, difficult to control the type and distribution of acid centers, and the active components are easily lost and deactivated during the catalytic process, which severely limits its application in many catalytic reactions. practical application

Method used

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  • Ordered mesoporous KIT-6 loaded zirconium sulfate-aluminum composite oxide solid acid material, and preparation and application thereof
  • Ordered mesoporous KIT-6 loaded zirconium sulfate-aluminum composite oxide solid acid material, and preparation and application thereof
  • Ordered mesoporous KIT-6 loaded zirconium sulfate-aluminum composite oxide solid acid material, and preparation and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0048] Slowly add 2.0g of n-butanol dropwise into 80mL of 0.5mol / L hydrochloric acid solution dissolved with 3.26g of glacial acetic acid and 2.0g of P123, and after vigorous stirring at 35°C for 6h, add 4.3g of ethyl orthosilicate to the reaction solution , and keep stirring at this temperature for 24h.

[0049] Put the white solid suspension obtained by the above self-assembly in a closed high-pressure reactor, heat it to 140°C for hydrothermal polymerization treatment for 24 hours, take out the reaction product, filter it with suction, wash it, and dry it to prepare the coated surfactant gel A bundle of ordered mesoporous KIT-6 materials is a white solid.

[0050] in N 2 Under the atmosphere, the white solid obtained above was heated to 550° C. for 2 h at high temperature to promote the partial carbonization and shrinkage of the surfactant micelles existing in the KIT-6 mesoporous channels.

[0051] Next, place the carbonized material in 20 mL of an aqueous solution disso...

Embodiment 2

[0067] Slowly add 2.5g of n-butanol dropwise to 65mL of 1.0mol / L hydrochloric acid solution dissolved with 3.0g of glacial acetic acid and 2.5g of P123, and after vigorous stirring at 35°C for 10h, add 3.02g of methyl orthosilicate to the reaction solution , and keep stirring at this temperature for 24h.

[0068]Put the white solid suspension obtained by the above self-assembly in a closed high-pressure reactor, heat it to 120°C for hydrothermal polymerization treatment for 24 hours, take out the reaction product, filter it with suction, wash it, and dry it to prepare the coated surfactant gel A bundle of ordered mesoporous KIT-6 materials is a white solid.

[0069] in N 2 Under the atmosphere, the white solid obtained above was heated to 450° C. for 2 h at a high temperature, and the surfactant micelles existing in the KIT-6 mesoporous channels were partially carbonized and shrunk.

[0070] Next, place the carbonized material in 15 mL of an aqueous solution in which 0.3 mol...

Embodiment 3

[0077] Slowly add 2.0 g of n-butanol dropwise into 80 mL of 2.0 mol / L hydrochloric acid solution in which 0.84 g of citric acid and 2.2 g of P123 are dissolved, stir vigorously at 35°C for 8 hours, then add 0.96 g of white carbon black to the reaction solution, and Stirring was continued at this temperature for 24h.

[0078] Put the white solid suspension obtained by the above self-assembly in a closed high-pressure reactor, heat it to 120°C for hydrothermal polymerization treatment for 24 hours, take out the reaction product, filter it with suction, wash it, and dry it to prepare the coated surfactant gel A bundle of ordered mesoporous KIT-6 materials is a white solid.

[0079] in N 2 Under the atmosphere, the white solid obtained above was heated to 550° C. for 2 h at high temperature to promote the partial carbonization and shrinkage of the surfactant micelles existing in the KIT-6 mesoporous channels.

[0080] Next, the carbonized material was placed in 15 mL of an aqueo...

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Abstract

The invention discloses an ordered mesoporous KIT-6 loaded zirconium sulfate-aluminum composite oxide solid acid materia. The material is obtained by taking a KIT-6 material with a three-dimensional cubic ordered mesoporous pore structure as a carrier, uniformly coating the surface of the carrier with a layer of zirconium-aluminum composite oxide and stably immobilizing a large number of sulfuric acid groups. The solid acid material prepared by the invention has a highly regular and ordered three-dimensional cubic mesoporous channel structure, large specific surface area and pore volume, uniform mesoporous aperture, and adjustable mesoporous wall surface acid amount, acid center type, acid density and acid strength, and shows excellent biodiesel yield, catalytic stability and regeneration and reuse performance in catalysis of transesterification of biodiesel synthesized from soybean oil and methanol.

Description

technical field [0001] The invention belongs to the technical field of preparation of inorganic porous solid acid catalytic materials, and relates to a sulfated zirconia-based composite metal oxide solid acid material and a preparation method thereof. The composite metal oxide solid acid material of the present invention has a highly regular and ordered three-dimensional cubic mesoporous channel structure, high specific surface area and pore volume, and uniform mesoporous pore diameter, and the acid content, acid density, and acid center type on the surface of the pore wall And the acid strength is adjustable, which can be used to catalyze the transesterification reaction of soybean oil and methanol to synthesize biodiesel. Background technique [0002] In the field of acid catalysis, compared with traditional liquid acid catalysts (such as H 2 SO 4 , HF and H 3 PO 4 ), solid acid catalysts have the advantages of no corrosion, no pollution, easy separation, reusability, ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J29/03B01J35/10B01J37/10B01J37/08B01J37/02C11C3/10C10L1/02
CPCB01J29/0308B01J37/10B01J37/082B01J37/0205B01J37/0207C11C3/10C10L1/02B01J2229/40B01J2229/37B01J2229/186B01J2229/20B01J35/615B01J35/617B01J35/633B01J35/635B01J35/647Y02E50/10
Inventor 于峰张豆豆潘大海任所财闫晓亮刘同慧陈树伟褚格闫贝贝王恒燕李瑞丰
Owner TAIYUAN UNIV OF TECH
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