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Ordered mesoporous Al-SBA-15 loaded sulfated zirconium oxide solid acid material, and preparation and application thereof

A technology of al-sba-15 and zirconia, applied in catalyst activation/preparation, fatty acid esterification, liquid carbon-containing fuel, etc., can solve problems such as low specific surface area, low acid content of solid acid materials, and limitations in practical applications , to achieve high catalytic activity

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

[0006] However, the mesoporous zirconia supports prepared by traditional methods often have a disordered "worm-like pore" structure, which exhibits disadvantages such as poor porosity, low specific surface area, small pore size, and easy crystal phase transition when heated, which leads to its 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 their use in many catalytic reactions. practical application of

Method used

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  • Ordered mesoporous Al-SBA-15 loaded sulfated zirconium oxide solid acid material, and preparation and application thereof
  • Ordered mesoporous Al-SBA-15 loaded sulfated zirconium oxide solid acid material, and preparation and application thereof
  • Ordered mesoporous Al-SBA-15 loaded sulfated zirconium oxide solid acid material, and preparation and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0053] Under vigorous stirring at 38°C, add 3.25g of ethyl orthosilicate to 50mL of 2.0mol / L hydrochloric acid solution dissolved with 1.6g of P123 and 0.82g of citric acid, and maintain the temperature to continue stirring for 24 hours, then filter the reaction solution with suction , washing, and preparing a white solid of the ordered mesoporous SBA-15 material that encapsulates surfactant micelles and whose pore walls are rich in Si-OH species.

[0054] Add the white solid obtained from the above self-assembly into 30 mL of 0.5 mol / L aluminum isopropoxide aqueous solution, adjust the pH of the reaction mixture to 2.0 with dilute hydrochloric acid, stir at room temperature for 30 min, and place the reaction mixture in a closed autoclave Inside, heated to 180°C for hydrothermal treatment for 24 hours, the reaction product was taken out, filtered, washed, and dried to prepare an ordered mesoporous Al-SBA-15 material wrapped with surfactant micelles and uniformly grafted with Al...

Embodiment 2

[0072] Under strong stirring at 32°C, add 3.02g of methyl orthosilicate to 45mL of 2.0mol / L hydrochloric acid solution dissolved with 2.0g of P123 and 1.65g of glacial acetic acid, and maintain the temperature for 12h with stirring, and filter the reaction solution with suction , washing, and preparing a white solid of the ordered mesoporous SBA-15 material that encapsulates surfactant micelles and whose pore walls are rich in Si-OH species.

[0073] Add the white solid obtained from the above self-assembly into 25 mL of 1.0 mol / L aluminum nitrate aqueous solution, adjust the pH value of the reaction mixture to 2.4 with dilute hydrochloric acid, stir at room temperature for 30 min, and place the reaction mixture in a closed autoclave. Heating to 150°C for hydrothermal treatment for 24 hours, taking out the reaction product, suction filtration, washing, and drying to prepare a white solid of ordered mesoporous Al-SBA-15 material wrapped with surfactant micelles and uniformly gra...

Embodiment 3

[0082] Under strong stirring at 40°C, add 0.72g of white carbon black to 40mL of 1.0mol / L hydrochloric acid solution dissolved with 2.1g of P123 and 0.62g of tartaric acid, and maintain the temperature to continue stirring for 24h, then filter and wash the reaction solution. A white solid of ordered mesoporous SBA-15 material was prepared which encapsulated surfactant micelles and the pore walls were rich in Si-OH species.

[0083] Add the white solid obtained from the above self-assembly into 30 mL of 1.5 mol / L aluminum tert-butoxide aqueous solution, adjust the pH of the reaction mixture to 2.5 with dilute hydrochloric acid, stir at room temperature for 30 min, and place the reaction mixture in a closed autoclave Inside, heated to 160°C for hydrothermal treatment for 24 hours, the reaction product was taken out, filtered, washed, and dried to prepare an ordered mesoporous Al-SBA-15 material wrapped with surfactant micelles and uniformly grafted with Al atoms on the pore wall ...

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Abstract

The invention discloses an ordered mesoporous Al-SBA-15 loaded sulfated zirconium oxide solid acid material. The material is obtained by taking an ordered mesoporous Al-SBA-15 material rich in surface Al-OH species obtained by grafting Al on the pore wall surface of the ordered mesoporous SBA-15 material as a carrier and immobilizing sulfated zirconium oxide. The solid acid material prepared by the invention has a highly regular and ordered mesoporous channel structure, larger specific surface area and pore volume, higher structural stability and adjustable mesopore wall surface acid amount, acid center type, acid density and acid strength, and the solid acid material shows excellent biodiesel yield, catalytic stability and reproducible reusability in catalyzing 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 solid acid material and a preparation method thereof. The solid acid material of the present invention has a highly regular and orderly mesoporous channel structure, high specific surface area and pore volume, and large mesoporous pore diameter, and the acid content, acid density, acid center type and acid strength on the surface of the pore wall are adjustable. , 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 acids (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, and recyclability, and have broad application prospects in catalytic cracking, alkylation, isomerizatio...

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
CPCB01J29/0308B01J37/10B01J37/082B01J37/0205B01J37/0207C11C3/10C10L1/02B01J2229/40B01J2229/37B01J2229/186B01J2229/20B01J35/615B01J35/617B01J35/635B01J35/638B01J35/647Y02E50/10
Inventor 潘大海闫贝贝于峰任所财陈树伟闫晓亮李瑞丰王琰王恒燕史秀锋
Owner TAIYUAN UNIV OF TECH