N-(4-toluenesulfonyl)-1,2-diphenyl ethylenediamine functionalized hollow PMO (Periodic Mesoporous Organosilica) catalyst preparation method

A technology of p-toluenesulfonyl and diphenylethylenediamine, which is applied in the field of preparation technology of hollow PMO catalysts, can solve the problems of limited catalytic activity, inability to uniformly disperse catalysts and reaction systems, etc.

Inactive Publication Date: 2013-12-11
SHANGHAI NORMAL UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the organic framework mesoporous silicon-based materials reported in the literature have a relatively large molecular weight, and the smallest particle diameter is greater than 300 nanometers. Therefore, when it is used in a chemical reaction, the catalyst cannot be uniformly dispersed in the reaction system, and its catalytic activity is greatly reduced. degree of limitation

Method used

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  • N-(4-toluenesulfonyl)-1,2-diphenyl ethylenediamine functionalized hollow PMO (Periodic Mesoporous Organosilica) catalyst preparation method
  • N-(4-toluenesulfonyl)-1,2-diphenyl ethylenediamine functionalized hollow PMO (Periodic Mesoporous Organosilica) catalyst preparation method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] Embodiment 1: Preparation of hollow PMO type catalyst carrier

[0030] Dissolve 0.318 g (1.5 mmol) of (1S,2S)-(+)-N-p-toluenesulfonyl-1,2-diphenylethylenediamine (DPEN) in 10 mL of dichloromethane and keep its temperature at -5~0℃;

[0031] Then, 0.46mL (1.5mmol) (2-triethoxysilyl) ethylbenzenesulfonyl chloride was added dropwise to the dichloromethane solution of DPEN at a rate of 5-8 drops / min;

[0032] After reacting for 6 hours, the solvent was spin-dried to obtain (1S,2S)-(+)-N-p-p-(2-triethoxysilyl)ethylbenzenesulfonyl-1,2-diphenylethylenediamine, referred to as Ts-DPEN functionalized silicon source;

[0033] Dissolve 0.5g of F127 in 30mL of 2.0M hydrochloric acid solution, keep stirring at 15°C for 30min, and rotate at 1200r / min.

[0034] Then 0.5 g (4.17 mmol) of mesitylene and 2.5 g (33.6 mmol) of potassium chloride were added. After mechanical stirring at 1200r / min for two hours, 0.4g (0.82mmol) Ts-DPEN functionalized silicon source and 2.61g (7.38mmol) bi...

Embodiment 2

[0038] Embodiment 2: Preparation of hollow PMO type catalyst carrier

[0039] The preparation of the Ts-DPEN functionalized silicon source is the same as in Example 1.

[0040] Dissolve 0.6g of F127 in 30mL of 2.0M hydrochloric acid solution, keep stirring at 15°C for 30min, and rotate at 1200r / min.

[0041]Then 0.5 g (5.04 mmol) of mesitylene and 2.5 g (33.6 mmol) of potassium chloride were added. After mechanical stirring at 1200r / min for two hours, 0.4g (0.82mmol) Ts-DPEN functionalized silicon source and 2.61g (7.38mmol) bistriethoxysilylethane were added dropwise at a rate of 90-95 drops per minute. The Ts-DPEN functionalized silicon source was diluted with 0.5mL of dichloromethane.

[0042] Continue mechanical stirring for 24 hours, then sink at 100°C for 24 hours, perform suction filtration after the precipitation, and put the obtained white solid in a vacuum drying oven at 60-65°C to dry overnight.

[0043] Finally, it was subjected to Soxhlet extraction with ethano...

Embodiment 3

[0044] Embodiment 3: Preparation of hollow PMO type catalyst carrier

[0045] The preparation of the Ts-DPEN functionalized silicon source is the same as in Example 1.

[0046] Dissolve 0.5g of F127 in 30mL of 2.0M hydrochloric acid solution, keep stirring at 15°C for 30min, and rotate at 1200r / min.

[0047] Then 0.5 g (4.17 mmol) of mesitylene and 3.0 g (40.32 mmol) of potassium chloride were added. After mechanical stirring at 1200r / min for two hours, 0.4g (0.82mmol) Ts-DPEN functionalized silicon source and 2.61g (7.38mmol) bistriethoxysilylethane were added dropwise at a rate of 90-95 drops per minute. The Ts-DPEN functionalized silicon source was diluted with 0.5mL of dichloromethane.

[0048] Continue mechanical stirring for 24 hours, then sink at 100°C for 24 hours, perform suction filtration after the precipitation, and put the obtained white solid in a vacuum drying oven at 60-65°C to dry overnight.

[0049] Finally, it was subjected to Soxhlet extraction with etha...

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Abstract

The invention discloses a preparation method of an N-(4-toluenesulfonyl)-1,2-diphenyl ethylenediamine functionalized hollow PMO (Periodic Mesoporous Organosilica) catalyst. The hollow PMO catalyst can be better dispersed into an organic or inorganic solvent, as a result, compared with a traditional PMO material, the hollow PMO catalyst can remarkably increase the reaction speed on the basis of the speed of the traditional PMO catalyst. The catalyst prepared by the preparation method has the following advantages: (1) the reaction speed is further increased; (2) a series of catalysts can be synthesized through coordinating different metals with the catalyst; (3) the catalyst can be better dispersed into a reaction system.

Description

technical field [0001] The invention belongs to the technical field of catalysts, and in particular relates to a preparation process of a hollow PMO catalyst functionalized with N-p-toluenesulfonyl-1,2-diphenylethylenediamine. Background technique [0002] Since C.T.Kresge first reported ordered mesoporous silicon-based materials in 1992, mesoporous silicon-based materials (PMO) have been one of the hotspots of scientific research because of their excellent performance. According to reports, its field of application has also been continuously expanded. Compared with SBA-15 and MCM-41 series compounds, organic framework silicon-based mesoporous materials can greatly reduce the number of hydroxyl groups on the surface of materials, so they have great potential in the modification of materials. (C.T.Kresge.et al., Nature, 1992,359,710-712.M.Jaroniec.et al.,J.Am.Chem.Soc.2005,127,60-61.S.Minakata.et al.,Chem. Rev.2009,109,711–724.H.X.Li.et al.J.Am.Chem.Soc.2010,132,1492–1493.M...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J31/22B01J31/02B01J32/00
Inventor 刘国华刘锐程探宇孔令玉陈忱徐向明
Owner SHANGHAI NORMAL UNIVERSITY
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