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Activated carbon immobilized ionic liquid catalyst and application thereof

A technology of ionic liquid and activated carbon, which is applied in activated carbon-supported ionic liquid catalyst and its application field, can solve the problems of weak adsorption, easy detachment of ionic liquid, and easy destruction of carrier structure, and achieve the effect of easy separation

Inactive Publication Date: 2015-04-29
ZHEJIANG UNIV OF TECH
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method of immobilizing ionic liquids with anions is easy to destroy the support structure during the preparation process, and the most critical thing is that the impregnation method is only suitable for AlCl 3 Immobilized imidazole-based ionic liquids, other types of ionic liquids can only be simply adsorbed on the surface of the carrier because they cannot form a specific covalent bond with the carrier, this adsorption is weak, and the ionic liquid is easy to fall off during the reaction

Method used

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  • Activated carbon immobilized ionic liquid catalyst and application thereof
  • Activated carbon immobilized ionic liquid catalyst and application thereof
  • Activated carbon immobilized ionic liquid catalyst and application thereof

Examples

Experimental program
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Effect test

Embodiment 1 4

[0030]Examples 1 to 4 focus on the effect of the type of oxidizing agent in the oxidation treatment on the performance of the activated carbon-immobilized ionic liquid catalyst. The preparation method of the catalyst is as follows: 2 g of activated carbon and 20 mL of water are made into a slurry at a ratio of 1 g: 10 ml, and an oxidizing agent (nitric acid, hydrogen peroxide, peracetic acid, potassium permanganate, details See Table 1), heat at 90°C for 4 hours, filter, wash with deionized water until neutral and dry at 110°C to obtain activated carbon after oxidation treatment. Then 80 mL of thionyl chloride and 2 g of oxidized activated carbon were mixed at a ratio of 40 ml: 1 g, heat-treated at 60 ° C for 12 hours, and the remaining thionyl chloride was removed by distillation under reduced pressure to obtain activated carbon after oxidation and chlorination. Further, 0.5 g of oxidized and chlorinated activated carbon, 0.01 mol of 1-(2-aminoethyl hydrobromide) 3-methylimid...

Embodiment 15 20

[0040] Examples 15 to 20 focus on the effects of the type and ratio of chlorination reagents in chlorination treatment on the performance of activated carbon-immobilized ionic liquid catalysts. The catalyst preparation method is as follows: make activated carbon and water into a slurry at a ratio of 1 g: 10 ml, add nitric acid with a molar ratio of 0.4: 1 to activated carbon, heat treatment at 90 ° C for 4 h, filter, wash with deionized water until neutral and place in Dry at 110°C to obtain activated carbon after oxidation treatment. Then different chlorination reagents (thionyl chloride, acetyl chloride, benzoyl chloride, oxalyl chloride, see Table 3 for details) and activated carbon after oxidation treatment were mixed in different proportions (see Table 3 for details), and heated at 60°C After 12 hours of treatment, the residual chlorination reagent was removed by distillation under reduced pressure to obtain activated carbon after oxidation and chlorination treatment. Fu...

Embodiment 21

[0044] Embodiments 21 to 26

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Abstract

The invention discloses an activated carbon immobilized ionic liquid catalyst and application thereof. The activated carbon immobilized ionic liquid catalyst is prepared from the following steps: performing oxidation treatment and chlorination on activated carbon sequentially, so as to obtain oxidized and chlorinated activated carbon; performing refluxing on the oxidized and chlorinated activated carbon, bromized 1-(2-amino ethyl hydrobromic acid)-3 methylimidazole onium salt ionic liquid and organic amine in tetrahydrofuran for 20-30 h, filtering, and washing and drying filter cakes B, so as to obtain solid products; adding the solid products into a potassium hydroxide solution, stirring for 20-30 h at the temperature of 0-5 DEG C, filtering, washing filter cakes C and drying, so as to obtain the activated carbon immobilized ionic liquid catalyst. The activated carbon immobilized ionic liquid catalyst provided by the invention can be used for catalyzing of knoevenagel condensation, during after-treatment, the activated carbon immobilized ionic liquid catalyst can be separated from reaction mixed liquor through simple centrifuging or filtering only, and the activated carbon immobilized ionic liquid catalyst can be used repeatedly.

Description

(1) Technical field [0001] The invention relates to an activated carbon immobilized ionic liquid catalyst and its application in Knoevenagel condensation reaction. (2) Background technology [0002] Ionic liquids have many physical and chemical properties such as wide liquid temperature range, strong solubility, low vapor pressure, good chemical and thermal stability, high ionic conductivity, and adjustable structure. It shows great application potential in many fields. In 2002, the German BASF company successfully used ionic liquid phase separation to realize large-scale application in the synthesis of fine chemicals. The new process increased the space-time yield of alkoxyphenylphosphine by 80,000 times. [0003] However, ionic liquids also have some disadvantages, such as high price, incomplete separation and purification of catalysts, etc., and it is very difficult to separate ionic liquids and reaction mixtures for reactants and products that are difficult to volatiliz...

Claims

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Application Information

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IPC IPC(8): B01J31/02C07C255/34C07C253/34
CPCY02P20/584
Inventor 王红马磊李小年崔露丹
Owner ZHEJIANG UNIV OF TECH
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