Preparation method of amido bridged regular mesoporous organic base heterogeneous catalyst

A heterogeneous catalyst and organic base technology, applied in the preparation of organic compounds, organic compound/hydride/coordination complex catalysts, organic chemistry, etc., can solve difficult separation and recycling, limited industrial application prospects, Increased production costs and other issues, to achieve the effect of simple preparation process, uniform distribution of active sites, and cost savings

Inactive Publication Date: 2010-09-08
SHANGHAI NORMAL UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0002] Homogeneous organic base catalysts have good catalytic effects in chemical reactions, but due to the limitation of solubility, they are difficult to sep

Method used

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  • Preparation method of amido bridged regular mesoporous organic base heterogeneous catalyst
  • Preparation method of amido bridged regular mesoporous organic base heterogeneous catalyst
  • Preparation method of amido bridged regular mesoporous organic base heterogeneous catalyst

Examples

Experimental program
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Effect test

Embodiment 1

[0041] According to the following steps, the amino-bridged ordered mesoporous organic base heterogeneous catalyst is prepared.

[0042] 2.0g P123 (EO 20 PO 70 EO 20 ) (0.034mmol), 8.0g KCl (0.11mol) and 62mL 0.5M HCl solution were mixed and stirred for 3.5h at 40°C in a jacketed jacket; then 5.0mmol1,2-bistriethoxysilylethane ( BTES), after BTES prepolymerization for 120min, add 5.0mmol bis[3-(trimethoxysilyl)propyl]amine (BTMA), continue to stir for 24h, age at 100°C for 28h, filter and wash, 80°C A white solid was obtained after drying in vacuo. Grind the above materials with an agate mortar, and then use HCl / C 2 h 5OH mixed solution extracts and removes surfactant, and the mass volume ratio of solid and liquid is 1.0g: 900mL; In the described mixed solution of hydrochloric acid and ethanol, the content of hydrochloric acid is 1.0mol / L, and the content of ethanol is 800g / L. Then alkali washing: add the obtained product to saturated Na at 30°C 2 CO 3 After the solutio...

Embodiment 2

[0046] The amino-bridged ordered mesoporous organic base heterogeneous catalyst was prepared according to the following steps.

[0047] 1.9g P123 (EO 20 PO 70 EO 20 ) (0.33mmol), 8.2g KCl (0.11mol) and 30mL 0.5M HCl solution were mixed, stirred at 40°C for 3h in a jacketed jacket, and then 4.5mmol 1,2-bistriethoxysilylethane ( BTES), after BTES prepolymerization for 130min, add 5.5mmol bis[3-(trimethoxysilyl)propyl]amine (BTMA), continue to stir for 24h, age at 100°C for 28h, filter, wash, and vacuum dry After obtaining a white solid;

[0048] Grind the above materials with an agate mortar, and finally with HCl / C 2 h 5 OH carries out extraction except surfactant, and the mass volume ratio of solid and liquid is 1g: 1000mL; In the described mixed solution of hydrochloric acid and ethanol, hydrochloric acid content is 1.2mol / L, and the content of ethanol is 780g / L. The resulting product was added to saturated Na at 25°C 2 CO 3 After the solution was stirred for 18 hours,...

Embodiment 3

[0050] Prepare the ordered mesoporous organic base heterogeneous catalyst of amino bridge, the steps are as follows:

[0051] 2.1g P123 (EO 20 PO 70 EO 20 ) (0.36mmol), 8.6g KCl (0.12mmol) and 66mL 0.50M HCl solution were mixed, stirred at 38°C for 3h in a jacketed jacket, and then added 6.0mmol 1,2-bistriethoxysilylethane (BTES ), after BTES prepolymerization for 130min, add 4.0mmol bis[3-(trimethoxysilyl)propyl]amine (BTMA), continue to stir for 24h, age at 110°C for 26h, filter, wash and vacuum dry A white solid was obtained;

[0052] Grind the above materials with an agate mortar, and finally with HCl / C 2 h 5 OH is extracted to remove surfactant, the mass volume ratio of solid and liquid is 1g:900mL; in the mixed solution of hydrochloric acid and ethanol, the content of hydrochloric acid is 0.9mol / L, and the content of ethanol is 600g / L. The resulting product was added to saturated Na at 25°C 2 CO 3 After the solution was stirred for 15 hours, it was suction-filter...

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Abstract

The invention belongs to an organic base heterogeneous catalyst, in particular to a preparation method of an amido bridged regular mesoporous organic base heterogeneous catalyst. A homogeneous organic base catalyst in the prior art is separated and recycled difficultly from a reaction system, so that the production cost is increased, and environmental pollution is brought. The method comprises the following steps of: mixing P123, KCl, NaF or NaCl and HCl with water to prepare a surfactant; adding 1,2-bis(triethoxy silicon)ethane and amido bridged silicane; aging at the temperature of 90-110 DEG C for 26-36 hours and getting a deposit; grinding the deposit; adding a mixed solution of hydrochloric acid and ethanol and extracting at the temperature of 70-80 DEG C for 24-48 hours; washing a product with base; carrying out extraction filtration and vacuum dying at the temperature of 80 DEG C to obtain the amido bridged regular mesoporous organic base heterogeneous catalyst. The invention has the advantages of high catalytic activity, simple preparation process, catalyst recycle, cost saving and environmental pollution reduction.

Description

technical field [0001] The invention relates to an organic base heterogeneous catalyst, in particular to a preparation method of an amino-bridged ordered mesoporous organic base heterogeneous catalyst. Background technique [0002] Homogeneous organic base catalysts have good catalytic effects in chemical reactions, but due to the limitation of solubility, they are difficult to separate and recycle from the reaction system, resulting in increased production costs and environmental pollution, making industrial application prospects limited. Designing an immobilized organic base catalyst is beneficial to overcome the above defects. In order to obtain the same catalytic efficiency as the corresponding homogeneous catalyst, the immobilized organic base catalyst must not only retain the chemical environment of the original compound, but also have a high degree of dispersion activity. bit. Therefore, it is necessary to find an excellent carrier. The ordered mesoporous PMO materia...

Claims

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Application Information

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IPC IPC(8): B01J31/06B01J35/10C07C205/04C07C201/12
CPCY02P20/584
Inventor 杨迪迪朱凤霞杨旭石黄建林李和兴张昉
Owner SHANGHAI NORMAL UNIVERSITY
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