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Preparation method and application of ionic liquid functionalized Al-MCM-41 mesoporous material

A technology of al-mcm-41 and mesoporous materials, which is applied in the fields of carbon dioxide or inorganic carbonate preparation, educts, organic chemistry, etc., can solve problems such as the limitation of the application of homogeneous catalysts and the difficulty of separating homogeneous catalysts from products, etc. Achieve the effect of simple preparation process and high catalytic activity

Inactive Publication Date: 2011-09-21
TIANJIN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] Homogeneous catalysts for the reaction of propylene oxide and carbon dioxide to generate propylene carbonate mainly include organic bases, metal complexes, ionic liquids, etc., although homogeneous catalysts have high catalytic activity for this reaction, but due to the Separation is difficult, which limits the application of homogeneous catalysts

Method used

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  • Preparation method and application of ionic liquid functionalized Al-MCM-41 mesoporous material
  • Preparation method and application of ionic liquid functionalized Al-MCM-41 mesoporous material
  • Preparation method and application of ionic liquid functionalized Al-MCM-41 mesoporous material

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] Dissolve 0.213g of aluminum nitrate and 2.4g of cetyltrimethylammonium bromide in 100mL of deionized water (Si:Al molar ratio is 80), add 3mL of ethylenediamine, stir well at room temperature, dropwise add 10mL of Ethyl silicate, after stirring vigorously at room temperature for 4 hours, placed it in a water bath at 80°C for 1 hour, moved it to a 100mL hydrothermal reaction kettle, hydrothermally crystallized at 100°C for 72h, filtered, washed with 300mL deionized water, and placed in Dry at 100°C for 8h, and finally raise the temperature to 550°C at a rate of 1°C / min in a muffle furnace, and bake at 550°C for 6h to obtain a skeleton-doped aluminum-doped mesoporous material Al-MCM-41 (80).

[0025] Take 5.0g of the prepared Al-MCM-41(80), add 100mL of toluene, add 5.0mL of 3-chloropropyltrimethoxysilane, add 0.5mL of triethylamine, and reflux at a temperature of 112°C for 48h. After the end, cool to room temperature, carry out vacuum suction filtration, then successivel...

Embodiment 2

[0028] The preparation method is the same as in Example 1, only changing the aluminum salt precursor sodium metaaluminate (NaAlO 2 ), that is, take 0.122g sodium metaaluminate (NaAlO 2 ) and 2.4g of cetyltrimethylammonium bromide were dissolved in 100mL of deionized water (Si:Al molar ratio was 30), 4mL of ethylenediamine was added, fully stirred at room temperature, and 10mL of ethyl orthosilicate was added dropwise , after stirring vigorously at room temperature for 4 hours, put it in a water bath at 80°C for 1 hour, move it to a 100mL hydrothermal reaction kettle, conduct hydrothermal crystallization at 100°C for 72h, filter, wash with 300mL deionized water, and dry at 100°C After 8 hours, the temperature was raised to 550°C at a speed of 1°C / min in a muffle furnace, and then fired at 550°C for 6 hours to obtain a skeleton-doped aluminum mesoporous material Al-MCM-41 (30).

[0029] Take 5.0g of the prepared Al-MCM-41(30), add 100mL of toluene, add 5.0mL of 3-chloropropyltr...

Embodiment 3

[0032] The reaction of propylene oxide and carbon dioxide to generate propylene carbonate was carried out in a 50mL stainless steel autoclave and heated by electromagnetic stirring. Add 5g of propylene oxide into the reaction kettle, add 0.4g of the prepared ionic liquid functionalized Al-MCM-41 mesoporous material catalyst, then pass in carbon dioxide gas to evacuate, close the outlet valve, and close the inlet after the pressure shows 3MPa valve. Stir and heat up to a reaction temperature of 130° C., and react at a constant temperature for 6 hours. After the reaction, the reactor was placed in an ice-water bath for 3 hours, and then unreacted carbon dioxide gas was released, and the solid catalyst was separated by centrifugation.

[0033] The product is analyzed by gas chromatography: hydrogen flame ionization detector, nitrogen as carrier gas, gasification chamber temperature 260 °C, detector temperature 260 °C, sample volume 0.2 μL, analysis conditions are initial column ...

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Abstract

The invention relates to a preparation method and application of an ionic liquid functionalized Al-MCM-41 mesoporous material. The preparation method comprises the following steps of: preparing a solution by taking CTAB (Cetyltrimethyl Ammonium Bromide) as a template agent, TEOS (Tetraethyl Orthosilicate) as a silicone source and aluminum nitrate or sodium metaaluminate as a precursor according to a molar ratio, and crystallizing, filtering, washing, drying and roasting the solution to obtain Al-MCM-41; obtaining Al-MCM-41-Cl through coupling; reacting the Al-MCM-41-Cl with N-methylimidazole,and carrying out cooling, suction filtering, washing and drying to obtain the ionic liquid functionalized mesoporous material Al-MCM-41-Im. The invention has the advantages that the method has simpleprocess, and the ionic liquid functionalized Al-MCM-41 mesoporous material has ordered and uniformly distributed pore structure and acid-situ surface and can be used as a catalyst for a reaction between epoxypropane and carbon dioxide to produce propylene carbonate.

Description

technical field [0001] The invention relates to the preparation and application of an ionic liquid functionalized Al-MCM-41 mesoporous material, which belongs to the technology of functionalizing the ionic liquid of the mesoporous material. Background technique [0002] Mesoporous materials have a highly ordered pore structure, a single distribution of pore size, and can be adjusted within 2-50nm, have good hydrothermal and thermal stability, particles have a regular and controllable shape, and a large specific surface area, so they have a wide range of applications Prospects, such as macromolecular catalysis, selective adsorption, functional materials, etc. However, due to its lack of active centers, its catalytic activity is not high, which greatly limits its application in the field of catalysis. In order to improve the catalytic activity of mesoporous materials, the modification of mesoporous materials has become the main research topic now. [0003] There are mainly t...

Claims

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Application Information

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IPC IPC(8): B01J31/26C07C69/96C07C68/04
CPCY02P20/141
Inventor 韩金玉王华蔡超常贺英
Owner TIANJIN UNIV
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