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A kind of acidic ionic liquid@cof material and its preparation method and application

An acidic ionic liquid, ionic liquid technology, applied in chemical instruments and methods, catalytic reactions, physical/chemical process catalysts, etc., can solve the problems of difficult catalyst separation and recovery, complex pore structure, complicated experimental operation, etc., and achieve easy recovery. Separation, high catalytic efficiency, overcoming the effect of recycling

Active Publication Date: 2020-08-21
INST OF PROCESS ENG CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] Ionic liquids are not only safe and environmentally friendly green solvents, patent CN 106694035A discloses a method for synthesizing isosorbide using sulfonic acid functionalized ionic liquids as catalysts, and patent CN 107722033A reduces the viscosity of the reaction mixture by adding hydrophobic ionic liquids and improves the dehydration of sugar alcohols The rectification yield and purity of the product, but the preparation of isosorbide by ionic liquid catalysis is usually under the condition of vacuum distillation, the cost is high, the separation and recovery of the catalyst are also difficult, and the carbonization is serious at high temperature
Patent CN 108126749A discloses a porous alkaline polyionic liquid as a catalyst to prepare isosorbide, but there are problems such as complicated experimental operation, small specific surface area, complex pore structure and slow mass transfer

Method used

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  • A kind of acidic ionic liquid@cof material and its preparation method and application
  • A kind of acidic ionic liquid@cof material and its preparation method and application
  • A kind of acidic ionic liquid@cof material and its preparation method and application

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Experimental program
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Effect test

Embodiment 2

[0056] Implementation method: Add 28.1g TAPB and 23.3g DMTA into a pressure-resistant tube (10mL, length 20cm, neck length 15cm), add 10mg 1-methyl-3-sulfopropylimidazolium bisulfate ionic liquid ([MSPI] [HSO 4 ]) (dissolved in 0.1mL water), 1mL mixed solvent (1,2-dichlorobenzene / n-butanol=1 / 1, v / v), sonication for 5min, freezing the solvent with liquid nitrogen, connecting a vacuum pump, the pressure in the tube When the temperature is lowered to 20Pa, seal the tube with a flame vacuum, wait until it returns to room temperature, put it in an oven, and react at 120°C for 3 days. After the reaction, cool to room temperature, break the pressure bottle, centrifuge to obtain a solid, wash with THF (3×10mL) and methanol (3×10mL), extract with THF for 1 day, and dry under vacuum at 120°C for 12h Catalyst B is obtained.

Embodiment 3

[0058] Implementation method: with embodiment 2, add 30mg ionic liquid [MSPI] [HSO 4 ] (dissolved in 0.1mL water), other constant, obtain catalyst C.

[0059] The prepared acidic ionic liquid @COF material was characterized by XRD, as shown in figure 1 shown. Depend on figure 1 The test results shown show that it is a highly crystalline porous material.

[0060] The prepared acidic ionic liquid @COF material was subjected to nitrogen adsorption and desorption tests, and the following results were obtained: figure 2 as shown. Depend on figure 2 The test results shown show that the catalyst has a micro- and mesoporous structure, which further demonstrates that it has a rich pore structure and a large specific surface area.

[0061] The prepared acidic ionic liquid @COF material was tested by infrared spectroscopy, and the results were as follows image 3 shown. Depend on image 3 The test results shown show that the catalyst was successfully synthesized and the acidic...

Embodiment 4

[0064] Implementation method: with embodiment 2, add 50mg ionic liquid [MSPI] [HSO 4 ] (dissolved in 0.1mL water), other constant, obtain catalyst D.

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Abstract

The invention provides an acidic ionic liquid@COF hybrid material by a one-pot in situ reaction. The material is used for catalyzing the intramolecular dehydration reaction of a polyhydric sugar alcohol to prepare a corresponding dehydrated compound. The acidic ionic liquid@COF hybrid material provided by the invention is a solid powder macroscopically, and has a large specific surface area and arich pore structure, and the solid acid catalyst with different pore sizes, pore volumes and active sites can be obtained by adjusting the kind and the mole of an added acidic ionic liquid. Compared with existing preparation methods, a method for preparing the corresponding dehydration compound from the polyhydric sugar alcohol by the solid acid catalysis system of the invention has the advantagesof high raw material conversion rate, high product selectivity, high catalytic activity, easy recovery and good cycle use performances of the catalyst, no device corrosion problem and high application potential.

Description

technical field [0001] The invention relates to the preparation and application of an acidic ionic liquid loaded onto a regular porous COF (covalent organic framework) material catalyst through a one-pot in-situ reaction, and belongs to the technical field of heterogeneous catalysis. Background technique [0002] The dehydrated compounds prepared by dehydration of polysaccharide alcohols are widely used in food, medicine, cosmetics, polymers and other fields due to their special chiral characteristics. Among them, the most typical is the dehydration of sorbitol to prepare isosorbide. Isosorbide is the only sugar diol that has been mass-produced industrially, and is an important bio-based chemical material. At present, the traditional method for preparing isosorbide adopts inorganic acid as catalyst, and HCl, H 3 PO 4 , HF, H 2 SO 4 and other inorganic acids as sorbitol dehydration catalysts. Although the catalytic activity of liquid acid is high, there are problems suc...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J31/06C07D487/04
CPCB01J31/06B01J2231/4288C07D487/04
Inventor 徐宝华杜一然何宏艳王耀锋潘嘉晟张锁江
Owner INST OF PROCESS ENG CHINESE ACAD OF SCI
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