Heterogenous organic metal catalyst with three-dimensional mesoporous structure, preparation method and application thereof

An organometallic, three-dimensional mesoporous technology, applied in the direction of isomerization preparation, organic compound/hydride/coordination complex catalysts, chemical instruments and methods, etc., can solve the problem that the activity and selectivity remain unchanged and the catalyst cannot be recycled Utilization, heavy metal ion pollution and other problems, to achieve the effect of high selectivity and acquisition rate

Inactive Publication Date: 2007-05-16
SHANGHAI NORMAL UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The purpose of the present invention is to overcome the shortcomings of the existing homogeneous catalysts in the aqueous phase homo-allylic alcohol isomerization reaction that expensive catalysts cannot be recycled and heavy metal ions will pollute the environment, and provide a catalyst that can be recycled many times with high activity. Three-dimensional mesoporous structure heterogeneous organometallic catalysts with almost constant selectivity;

Method used

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  • Heterogenous organic metal catalyst with three-dimensional mesoporous structure, preparation method and application thereof
  • Heterogenous organic metal catalyst with three-dimensional mesoporous structure, preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] Step 1: At 30°C, mix 0.5g F127, 30g 2M hydrochloric acid, 2.5g and 0.69mL 1,3,5-trimethylbenzene, stir at 30°C until all surfactants are dissolved, then add 2.0mL TEOS and continue stirring 1h, 0.41mL of 2-(diphenylsulfone)ethyltriethoxysilane was added, and stirring was continued at the same temperature for 24 hours. The obtained mixed solution was transferred to a polytetrafluoroethylene hydrothermal bottle, and hydrothermally reacted in an oven at 100°C for 1 day. After cooling, a white powder was obtained after suction filtration, washing, and natural drying at room temperature.

[0031] Step 2: Put 0.5g of the sample without extracting surfactant and 30g of 2M hydrochloric acid into a polytetrafluoroethylene water thermos bottle, and age them at 100°C for 48 hours, then filter, wash and dry them, and finally extract the samples The obtained white powder was extracted to remove the organic structure directing agent.

[0032] Step 3: Dissolve 95.86 mg RuCl at room t...

Embodiment 2

[0036] Step 1: Same as Step 1 in Example 1.

[0037] Step 2: Put 0.5g of the sample without extracting surfactant and 30g of 2M hydrochloric acid into a polytetrafluoroethylene water thermos bottle, age them at 120°C for 48 hours, filter them with suction, wash them, and dry them. The obtained white powder was extracted to remove the organic structure directing agent.

[0038] Step 3: Same as Step 3 in Example 1.

[0039] Step 4: with step 4 in embodiment 1, obtain the immobilized organometallic catalyst (Ru-PPh 2 - FDU-12-2) Catalyst.

[0040] Step 5: Same as Step 5 in Example 1.

Embodiment 3

[0042] Step 1: Same as Step 1 in Example 1.

[0043] Step 2: Put 0.5g of the sample without extracting surfactant and 30g of 2M hydrochloric acid into a polytetrafluoroethylene water thermos bottle, age them at 130°C for 48 hours, filter them with suction, wash them, and dry them. The obtained white powder was extracted to remove the organic structure directing agent.

[0044] Step 3: Same as Step 3 in Example 1.

[0045] Step 4: with step 4 in embodiment 1, obtain the immobilized organometallic catalyst (Ru-PPh 2 - FDU-12-3) Catalyst.

[0046] Step 5: Same as Step 5 in Example 1.

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Abstract

The invention relates to a method for preparing three-dimension non-uniform organic metal catalyst, wherein it comprises preparing carrier; reacting the toluene solution of organic metal with carrier under argon gas for 12-48h, filtering and drying; adding catalyst into extractor to be extracted and using non-water toluene to wash until the solution is transparent, to obtain the product, whose specific area is 150-500cm3 / g, aperture is 2-10nm, and capacitor is 0.4-1.0cm3 / g. The invention has high activity and high selectivity.

Description

technical field [0001] The invention relates to a catalyst and a preparation method thereof, in particular to a three-dimensional mesoporous structure heterogeneous organometallic catalyst and a preparation method thereof, which are mainly used for the isomerization reaction of homoallylic alcohol in an aqueous medium. Background technique [0002] Allyl alcohol isomerization is not only widely used in organic synthesis, but also a key step in the preparation of many natural products with biological functions. The traditional allyl alcohol isomerization reaction needs to be carried out in an organic solvent, and the volatilization and emission of organic solvents are important factors that constitute environmental pollution, while H 2 O instead of organic solvents is one of the keys to clean organic synthesis in environmentally friendly media to achieve green chemistry. However, due to the limitation of solubility, all the reported isomerization reactions of allyl alcohol i...

Claims

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Application Information

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IPC IPC(8): B01J31/24B01J31/28B01J35/10C07C29/56
CPCY02P20/50
Inventor 李和兴张昉
Owner SHANGHAI NORMAL UNIVERSITY
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