Preparation of Ti-MCM-41 mesoporous material with functionalized ionic liquid and application thereof

A technology of ti-mcm-41 and mesoporous materials, applied in organic chemistry, chemical instruments and methods, chemical/physical processes, etc., can solve problems such as the difficulty of separating homogeneous catalysts from products and the limitations of homogeneous catalyst applications, and achieve The effect of simple preparation process and high catalytic activity

Inactive Publication Date: 2011-09-14
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 of Ti-MCM-41 mesoporous material with functionalized ionic liquid and application thereof
  • Preparation of Ti-MCM-41 mesoporous material with functionalized ionic liquid and application thereof
  • Preparation of Ti-MCM-41 mesoporous material with functionalized ionic liquid and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] Dissolve 5.46g of cetyltrimethylammonium bromide (CTAB) in 180mL of deionized water, add 12mL of ethylenediamine, stir well, (according to Si:Ti molar ratio is 50), add dropwise 20.8g of Ethyl silicate (TEOS), then add 0.68g butyl titanate and 40mL H 2 o 2 and 10mL of isopropanol, stirred for 2h, placed in a water bath at 80°C for 1h, then moved to a hydrothermal reaction kettle, hydrothermally treated at 100°C for 72h, and finally, filtered and washed with 300mL of deionized water, The obtained solid was dried at 100°C for 8 hours, then heated to 550°C at a rate of 1°C / min, and calcined at 550°C for 6 hours to remove the surfactant to obtain Ti-MCM-41(50).

[0025] Take 5.0 g of prepared Ti-MCM-41 (50), add 100 mL of toluene, add 5.0 mL of 3-chloropropyltrimethoxysilane, add 0.5 mL of triethylamine, and reflux at a temperature of 110 ° C for 48 h. After the end, cool to room temperature, carry out vacuum suction filtration, then successively wash with 100mL toluene, ...

Embodiment 2

[0028] Dissolve 6.10g of cetyltrimethylammonium bromide (CTAB) in 180mL of deionized water, add 12mL of ethylenediamine, stir well, add 23.2g of tetraethyl orthosilicate (TEOS) dropwise, and then add 1.85g butyl titanate and 100mLH 2 o 2 and 28mL of isopropanol, stirred for 2h, placed in a water bath at 80°C for 1h, then moved to a hydrothermal reaction kettle, hydrothermally treated at 100°C for 72h, and finally, filtered and washed with 300mL of deionized water, The obtained solid was dried at 100°C for 8h, heated to 550°C at a speed of 1°C / min, and calcined at 550°C for 6h to remove the surfactant to obtain Ti-MCM-41(70).

[0029] Take 5.0 g of prepared Ti-MCM-41 (70), add 100 mL of toluene, add 5.0 mL of 3-chloropropyltrimethoxysilane, add 0.5 mL of triethylamine, and reflux at a temperature of 110 ° C for 48 h. After the end, cool to room temperature, carry out vacuum suction filtration, then successively wash with 100mL toluene, 100mL ethanol and water mixed solution (1:...

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. In reactor, add 5g propylene oxide, add 0.4gTi-MCM-41-Im (50) catalyzer, then pass into carbon dioxide gas and evacuate, close outlet valve, after pressure shows 3MPa, close inlet 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 reaction kettle 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 to obtain the product.

[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 temperature 40 °C, and then The temperature was raised...

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Abstract

The invention relates to the preparation of a Ti-MCM-41 mesoporous material with functionalized ionic liquid and an application thereof. The preparation method comprises the following steps of: adopting CTAB (Cetyltrimethyl Ammonium Bromide) as a template agent, adopting TEOS (tetraethyl orthosilicate) as silicon source, and adopting tetrabutyl titanate as a precursor; preparing solution according to mol ratio; crystallizing, filtering, washing, drying and roasting to obtain Ti-MCM-41; then coupling to obtain Ti-MCM-41-Cl; and adopting the Ti-MCM-41-Cl to react with N-methylimidazole; cooling, extracting, washing and drying to obtain the mesoporous material Ti-MCM-41-lm with functionalized ionic liquid. The preparation and the application have the following advantages: the method is simple in process; the mesoporous material Ti-MCM-41-lm with functionalized ionic liquid has orderly and uniformly distributed hole-channel structures; the surface of the mesoporous material has acid sites; and the mesoporous material is adopted as a catalyst for the reaction of epoxypropane with carbon dioxide to produce propylene carbonate.

Description

technical field [0001] The invention relates to the preparation and application of an ionic liquid functionalized Ti-MCM-41 mesoporous material, which belongs to the technology of mesoporous material ionic liquid functionalization. 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 two modifi...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J31/38C07D317/36
Inventor 韩金玉王华蔡超常贺英
Owner TIANJIN UNIV
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