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Magnetic composite microsphere for catalyzing CO2 and epoxy compound cycloaddition reaction as well as preparation method and application thereof

A technology of magnetic composite microspheres and microspheres, applied in chemical instruments and methods, organic compound/hydride/coordination complex catalysts, chemical/physical processes, etc., can solve the problems of mild reaction conditions, limited prospects, etc. The effect of controllable process, low cost and simple operation

Inactive Publication Date: 2014-04-09
FUDAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] Most of the heterogeneous catalysts currently studied cannot meet the following conditions at the same time: high catalytic activity, mild reaction conditions, no need to add additional solvents or / and co-catalysts, stable Good performance, recyclability, etc., which limits their prospects for industrial application

Method used

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  • Magnetic composite microsphere for catalyzing CO2 and epoxy compound cycloaddition reaction as well as preparation method and application thereof
  • Magnetic composite microsphere for catalyzing CO2 and epoxy compound cycloaddition reaction as well as preparation method and application thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0039] Example 1: Core-shell Fe with a magnetic core of about 180nm, a carbon layer thickness of about 20nm, and a coordination polymer shell of about 5nm 3 o 4 Preparation of CSalen-Al Microspheres

[0040] 1. Fe 3 o4 Preparation of C

[0041] Dissolve 0.5g of ferrocene in 35mL of acetone, add 2.0mL of hydrogen peroxide while stirring magnetically, and then place it in a stainless steel autoclave with Teflon lining, and place the autoclave in an oven at 220°C for 24h. Take it out and cool it to room temperature with tap water; separate the product by magnetic separation, wash with acetone and absolute ethanol to remove unreacted reactants, and finally disperse the product in absolute ethanol for later use.

[0042] 2. Preparation of Salen-metal complex (I)

[0043] Add 2mmol of salicylaldehyde derivative (IV) to the reactor, after dissolving toluene, add 2mmol of p-pyridinebenzoic acid, then heat and reflux for 4 days, stop the reaction, filter, rinse the filter cake with...

Embodiment 2

[0048] Example 2: Core-shell Fe with a magnetic core of about 90nm, a carbon layer thickness of about 20nm, and a coordination polymer shell of about 10nm 3 o 4 Preparation of CSalen-Al Microspheres

[0049] 1. Fe 3 o 4 The preparation of C is as described in Example 1-1. The difference is that the amount of ferrocene added is changed from 0.5g to 0.2g.

[0050] 2. Preparation of Salen-metal complex (I)

[0051] Add 3mmol salicylaldehyde derivative (IV) to the reactor, after dissolving toluene, add 3mmol p-pyridine benzoic acid, then heat and reflux for 4 days, stop the reaction, filter, rinse the filter cake with toluene and vacuum dry to obtain water Salicylic aldehyde derivatives (III);

[0052] Add 4mmol of salicylaldehyde derivative (III) to the reactor, dissolve in ethanol, add 4mmol of 1,2-position disubstituted diamine, then add 16mL of potassium carbonate aqueous solution, heat to reflux under nitrogen atmosphere 2 hour, stop the reaction, filter, and vacuum-dr...

Embodiment 3

[0055] Example 3: The core-shell type Fe with a magnetic core of about 180nm, a carbon layer thickness of about 10nm, and a coordination polymer shell of about 10nm 3 o 4 Preparation of CSalen-Al Microspheres

[0056] 1. Fe 3 o 4 The preparation of C is as described in Example 1-1. The difference is that the amount of hydrogen peroxide is changed from 2.0mL to 1.0mL.

[0057] 2. Preparation of Salen-metal complex (I)

[0058] Add 3mmol salicylaldehyde derivative (IV) to the reactor, after dissolving toluene, add 3mmol p-pyridine benzoic acid, then heat and reflux for 4 days, stop the reaction, filter, rinse the filter cake with toluene and vacuum dry to obtain water Salicylic aldehyde derivatives (III);

[0059] Add 4mmol of salicylaldehyde derivative (III) to the reactor, dissolve in ethanol, add 4mmol of 1,2-position disubstituted diamine, then add 16mL of potassium carbonate aqueous solution, heat to reflux under nitrogen atmosphere 8 hour, stop the reaction, filter,...

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Abstract

The invention belongs to the technical field of a functional material, and particularly relates to a preparation method and application of a magnetic composite microsphere for catalyzing CO2 and expoxy cycloaddition reaction. The kernel of the nuclear-shell composite microsphere is magnetic ferroferric oxide / carbon composite microsphere, and the shell is a coordination polymer with catalytic activity. The preparation method comprises the following steps of synthesizing the magnetic ferroferric oxide / carbon composite microsphere in one step through a solvothermal method, and catalyzing the polymerization of active molecule Salen-metal coordinate through the induction of metal ions through a coordination chemical method so as to obtain the ferroferric oxide / carbon / coordination polymer composite microsphere with catalytic activity. The composite microsphere has the characteristics of high magnetic responsiveness, high stability, high catalytic activity and high yield. The method is simple to operate and controllable in process, the prepared composite microsphere can be used for catalyzing the CO2 and epoxy compound cycloaddition reaction and is promising in industrial application prospect.

Description

technical field [0001] The invention belongs to the technical field of functional materials, and in particular relates to a solid-supported catalyst for catalyzing CO 2 Magnetic composite microspheres for cycloaddition reaction with epoxy compounds, preparation method and application thereof. Background technique [0002] carbon dioxide (CO 2 ) is currently the most important greenhouse gas on the earth, and it is also the cheapest and most abundant resource in the C1 family. Globally, CO 2 The carbon content is ten times that of oil, coal and natural gas. Based on the dual consideration of environmental protection and energy, human beings have been exploring CO 2 scientific transformation and utilization. In the past ten years, about CO 2 There is a lot of research on resource utilization of CO, but there are not many ways to use it in industrial production. CO 2 Cycloaddition with epoxides to prepare cyclic carbonates is a typical reaction. The reaction has the adv...

Claims

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Application Information

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IPC IPC(8): B01J31/28B01J31/40B01J35/08C07D317/36C07D317/46
CPCY02P20/584
Inventor 郭佳安乔
Owner FUDAN UNIV
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