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Preparation method of catalytic material of nitrogen-doped mesoporous carbon-silicon dioxide-based strongly-acidic multi-phase ion liquid

A technology of silica and ionic liquids, applied in the field of material science, can solve the problems of complex preparation process, high cost, and low catalytic efficiency, and achieve the effect of increasing specific surface area, simple and effective method, and excellent catalytic performance

Inactive Publication Date: 2013-12-25
SHAOXING UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0006] However, the current traditional mesoporous carbonized nitrogen materials have disadvantages such as complex preparation process, low catalytic efficiency, poor catalyst regeneration performance, and high cost, which limit the application of this type of catalyst in industrial production.

Method used

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  • Preparation method of catalytic material of nitrogen-doped mesoporous carbon-silicon dioxide-based strongly-acidic multi-phase ion liquid
  • Preparation method of catalytic material of nitrogen-doped mesoporous carbon-silicon dioxide-based strongly-acidic multi-phase ion liquid
  • Preparation method of catalytic material of nitrogen-doped mesoporous carbon-silicon dioxide-based strongly-acidic multi-phase ion liquid

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0039] Firstly, using ethanol as solvent and F127 as template to synthesize nitrogen-doped mesoporous carbon-silica nanocomposite heterogeneous ionic liquid catalytic material, changing the nitrogen content.

[0040] Add 20g of absolute ethanol to 2.4g of F127 to dissolve, then add 20.4g (50%) of cyanamide aqueous solution, adjust the pH to about 2.0 with 1:1 hydrochloric acid, stir for 30 minutes, add 2.25mL of ethyl orthosilicate, and continue stirring After 3 hours, the solvent was evaporated at room temperature to obtain a white film, and baked at 100 degrees Celsius for 24 hours to obtain the primary product of nitrogen-doped mesoporous carbon-silica. The primary product obtained above is calcined at 600° C. for 3 hours under the protection of an inert gas to obtain a nitrogen-doped mesoporous carbon-silicon dioxide nanocomposite with open pores.

[0041] Functionalized ionic liquid: add 1 g of the material obtained above to 20 ml of toluene solution containing 1.0 g of 1,3...

Embodiment 2

[0046] Nitrogen-doped mesoporous carbon-silica nanocomposite heterogeneous ionic liquid catalytic materials were synthesized with methanol as solvent and F127 as template.

[0047] Add 10g of anhydrous methanol to dissolve 1.6g of F127, then add 10.2g (50%) of cyanamide aqueous solution, adjust the pH to about 2.0 with 1:1 hydrochloric acid, stir for 30 minutes, add 2.25mL of ethyl orthosilicate, and continue stirring After 3 hours, the solvent was evaporated at room temperature to obtain a white film, and baked at 140 degrees Celsius for 24 hours to obtain the primary product of nitrogen-doped mesoporous carbon-silica. The primary product obtained above is calcined at 800° C. for 3 hours under inert gas protection conditions to obtain carbonized nitrogen-silicon dioxide nanocomposites with open pores.

[0048] Functionalized ionic liquid: add 1 g of the material obtained above to 20 ml of toluene solution containing 0.8 g of 1,3-propane sultone, reflux at 100 degrees Celsius ...

Embodiment 3

[0050] Nitrogen-doped mesoporous carbon-silica nanocomposite heterogeneous ionic liquid catalytic materials were synthesized by using ethanol as solvent, P123 as template, and changing the synthesis temperature.

[0051] Add 10g of absolute ethanol to 2.0g P123 to dissolve, then add 10.2g (50%) cyanamide aqueous solution, adjust the pH to about 2.0 with 1:1 hydrochloric acid, stir for 30 minutes, add 2.25mL orthosilicate ethyl ester, continue stirring After 3 hours, the solvent was evaporated at room temperature to obtain a white film, and baked at 80 degrees Celsius for 24 hours to obtain the primary product of nitrogen-doped mesoporous carbon-silica. The primary product obtained above is calcined at 550° C. for 3 hours under the protection of an inert gas to obtain a nitrogen-doped mesoporous carbon-silicon dioxide nanocomposite with open pores.

[0052] Functionalized ionic liquid: add 1 g of the material obtained above to 20 ml of toluene solution containing 0.8 g of 1,3-p...

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Abstract

The invention provides a preparation method of a catalytic material of nitrogen-doped mesoporous carbon-silicon dioxide-based strongly-acidic multi-phase ion liquid. The preparation method comprises the steps of taking P123 or F127 as a template agent, cyanamide as a carbon source and tetraethoxysilane as an inorganic source, and obtaining a primary product by volatilized self assembly under the condition of acidic room temperature and heat treatment; then under the protective condition of inert gases, baking at the high temperature to obtain a nanocomposite with open hole channels; and then carrying out quaternized reaction, and obtaining the catalytic material of the nitrogen-doped mesoporous carbon-silicon dioxide-based strongly-acidic multi-phase ion liquid by further acid exchange. The preparation method provided by the invention has the advantages that tested by catalytic reaction, the catalytic activity in reaction for preparing biodiesel by catalyzing biomass to carry out conversion-ester exchange is very excellent, and the regenerating capability of the catalyst is strong, so that the preparation method has certain industrial significance for improving the preparation efficiency of the biological material on large scale.

Description

technical field [0001] The invention belongs to the technical field of material science, in particular to a method for preparing a strongly acidic heterogeneous ionic liquid catalytic material with a large specific surface area and rich mesoporous structure. Background technique [0002] In recent years, with the rapid development of industry, the demand for energy in various countries is also constantly increasing. Traditional fossil energy cannot meet the growing demand for energy in various countries due to its shortcomings such as limited reserves and non-renewability. In addition, the environmental problems caused by pollutants such as sulfur and nitrogen produced during the combustion of fossil energy have also received widespread attention from the world. Energy problems have become a global problem that needs to be solved urgently. The development of new clean and renewable Energy is the key to solving energy problems. Among all kinds of new energy, bioenergy is a k...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J31/02B01J35/10C11C3/10
Inventor 孔维萍刘福建
Owner SHAOXING UNIVERSITY
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