Immobilized heteropoly acid ionic liquid catalyst and preparation method thereof

A technology of ionic liquid and catalyst, which is applied to graphene oxide immobilized heteropolyacid ionic liquid catalyst and its preparation. The application field of this catalyst in liquid-phase Beckmann reaction can solve the problem of easy loss and deactivation of catalytic active components, Unsatisfactory catalyst activity, poor support structure stability, etc., to achieve the effect of stable mechanical and chemical properties, simple and easy synthesis method, and stable catalytic performance

Active Publication Date: 2017-05-31
CHANGZHOU UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0008] In view of the shortcomings of the existing immobilized ionic liquid synthesis technology, such as the cost of raw and auxiliary materials is relatively expensive, the stability of the carrier structure is poor, the catalyst activity is not ideal, a

Method used

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  • Immobilized heteropoly acid ionic liquid catalyst and preparation method thereof
  • Immobilized heteropoly acid ionic liquid catalyst and preparation method thereof
  • Immobilized heteropoly acid ionic liquid catalyst and preparation method thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0028] GO was prepared by the improved Hummers method, and the specific process was as follows: 1 g of graphite powder and 0.5 g of NaNO were added to a 250 mL four-neck flask equipped with a mechanical stirring device under ice bath conditions. 3 and 23mL concentrated sulfuric acid. While vigorously stirring, a certain amount of KMnO was slowly added in batches 4 After that, react for 1.5h. Then the temperature of the water bath was raised to 30° C., and after slowly adding 100 mL of deionized water dropwise, the stirring was continued for 1.5 h. After the stirring was completed, the temperature of the water bath was raised to 95 °C, and after stirring for 30 min, it was cooled to room temperature. Add 300mL of deionized water and 0.6mL of hydrogen peroxide dropwise, stir well and filter with suction, wash with 5% hydrochloric acid first, and then wash the sample with deionized water until neutral. Dry at 80°C for 5h to obtain graphite oxide powder. Before use, wash with ...

Embodiment 2

[0031] Add 20 times of 3-chloropropyltrimethoxysilane to the GO suspension prepared in Example 1, transfer the flask to an oil bath, stir at 110° C. for 24 h under reflux, and cool to room temperature. After filtration, repeated washing with ethanol and deionized water, and drying at 80°C, the synthesized GO with silane chains was added to the flask, and then 6.8 times of imidazole and 900 times of toluene were added, and the mixture was stirred and refluxed at 110°C for 24 hours. After the reaction, cool to room temperature. GO with imidazole was obtained after filtration, washing and drying. The synthesized GO with imidazole, propyl sultone and toluene were mixed according to the ratio of 1:12:900, and the reaction was stirred at 80°C for 24h. After the reaction, GO with imidazole group of alkylsulfonic acid was obtained by filtering, washing and drying. The synthesized GO with imidazole group of alkylsulfonic acid, phosphotungstic acid and water were mixed according to th...

Embodiment 3

[0033]Add 30 times of 3-chloropropyltriethoxysilane to the GO suspension prepared in Example 1, transfer the flask to an oil bath, stir and reflux at 90°C for 24 hours, and cool to room temperature. After filtration, washing and drying, the synthesized GO with silyl group was added into the flask, then 10 times of imidazole and 400 times of toluene were added, and the mixture was stirred and refluxed at 110°C for 24 hours. After the reaction, cool to room temperature. GO with imidazole was obtained after filtration, washing and drying. The synthesized GO with imidazole, butyl sultone and toluene were mixed according to the ratio of 1:18:400, and the reaction was stirred at 80°C for 24h. After the reaction, GO with imidazole group of alkylsulfonic acid was obtained by filtering, washing and drying. The synthesized GO with imidazole group of alkylsulfonic acid, phosphotungstic acid and water were mixed according to the ratio of 1:18:500, and stirred and reacted at 60°C for 24h...

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Abstract

The invention provides an immobilized heteropoly acid ionic liquid catalyst for liquid phase Beckmann rearrangement reaction and a preparation method thereof. A carrier is graphene oxide (GO) powder prepared by a modified Hummers chemical method. The method comprises the following steps: firstly performing condensation reaction between GO and a silane coupling agent, then performing alkylation reaction with imidazole, successively sulfonating with alkyl sultone and finally performing disproportionated reaction through Keggin structure heteropolyacid. The immobilized heteropoly acid ionic liquid catalyst provided by the invention firstly utilizes GO as the carrier, and heteropoly acid ionic liquid with a sulfonic acid group is immobilized on the surface of the catalyst through a chemical grafting method. The preparation method provided by the invention has the benefits that raw materials are easy to obtain, the catalyst is simple to prepare, a solvent can be recycled after the catalyst is used, and almost no pollution is caused to the environment. The synthesized catalyst is applied to the liquid phase Beckmann rearrangement reaction; the catalyst is convenient for separation and recovery operation, and long in service life, so that the use cost is greatly reduced; therefore, the catalyst becomes a green chemical novel catalytic material with an application prospect.

Description

technical field [0001] The invention relates to the field of preparation of immobilized heteropolyacid ionic liquid, in particular to a graphene oxide immobilized heteropolyacid ionic liquid catalyst and a preparation method thereof, and also relates to the application of the catalyst in liquid-phase Beckmann reaction. Background technique [0002] In recent years, ionic liquids, as catalysts, have become the focus of organic synthesis and catalytic materials research due to their unique properties. Although ionic liquid catalysts, especially heteropolyanionic catalysts, have the advantages of "soft" (liquid) materials in liquid-phase Beckmann rearrangement reactions, such as good fluidity and uniform acid strength distribution, etc., thus exhibiting good catalytic activity and selectivity, etc., but the separation and reuse of liquid catalysts are not as convenient as solid catalysts, and the purity of the product is not high, which limits its application field. Therefore,...

Claims

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Application Information

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IPC IPC(8): B01J31/18B01J31/02B01J27/188B01J27/19B01J23/30C07D223/10C07C231/10C07C233/07
CPCB01J23/30B01J27/188B01J27/19B01J31/0295B01J2231/4277C07C231/10C07D223/10C07C233/07Y02P20/50Y02P20/584
Inventor 张卫红杜晨辉刘珊珊刘平李永昕
Owner CHANGZHOU UNIV
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