Method for preparing chitosan immobilized Lewis acidic ionic liquid and DCPP synthesized by using chitosan immobilized Lewis acidic ionic liquid in presence of high-efficient catalyst

A technology of Lewis acidic and ionic liquids, which is applied in the field of preparation of chitosan-immobilized Lewis acidic ionic liquids, can solve problems that have not been reported in the literature, and achieve the effects of low price, easy scale-up production, and easy availability

Inactive Publication Date: 2010-04-21
NANCHANG HANGKONG UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Chitosan is a renewable resource with very rich sources. It has not been reported in the literature at home and abroad to use it as an immobilization material for

Method used

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  • Method for preparing chitosan immobilized Lewis acidic ionic liquid and DCPP synthesized by using chitosan immobilized Lewis acidic ionic liquid in presence of high-efficient catalyst
  • Method for preparing chitosan immobilized Lewis acidic ionic liquid and DCPP synthesized by using chitosan immobilized Lewis acidic ionic liquid in presence of high-efficient catalyst
  • Method for preparing chitosan immobilized Lewis acidic ionic liquid and DCPP synthesized by using chitosan immobilized Lewis acidic ionic liquid in presence of high-efficient catalyst

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0014] Example 1: PmimCl-FeCl 3 -CS Catalytic Synthesis of DCPP

[0015] 1. Preparation of Lewis acid ionic liquid

[0016] 1-Methylimidazole and Y-chloropropyltrimethoxysilane were refluxed and reacted at 70°C for 70h, and then reacted at 70°C according to the molar ratio of Lewis acid anhydrous ferric chloride to the prepared product of 2:1 24h.

[0017] 2. Preparation of chitosan immobilized Lewis acid ionic liquid

[0018] Such as figure 1 As shown, the obtained ionic liquid containing chloroferric acid and 2 times the mass of chitosan were dispersed in acetonitrile and refluxed for 20 hours, and the solvent was removed by rotary evaporation. The obtained solid was Soxhlet extracted with dichloromethane for 30 hours to obtain a solid chitosan. Supported acidic ionic liquid catalyst PmimCl-FeCl 3 -CS.

[0019] 3. The prepared catalyst can efficiently synthesize DCPP

[0020] Add appropriate amount of catalyst PmimCl-FeCl in a round bottom flask equipped with reflux device 3 -CS, ph...

Embodiment 2

[0021] Example 2: PmimCl-AlCl 3 -CS Catalytic Synthesis of DCPP

[0022] 1. Preparation of Lewis acid ionic liquid

[0023] 1-Methylimidazole and Y-chloropropyltrimethoxysilane were refluxed and reacted at 70°C for 70h, and then reacted at 70°C according to the molar ratio of Lewis acid anhydrous aluminum chloride to the prepared product of 2:1 24h.

[0024] 2. Preparation of chitosan immobilized Lewis acid ionic liquid

[0025] Such as figure 1 As shown, the obtained chloroaluminate-containing ionic liquid and 2 times the mass of chitosan were dispersed in acetonitrile and refluxed for 20 hours, and the solvent was removed by rotary evaporation. The obtained solid was Soxhlet extracted with dichloromethane for 30 hours to obtain a chitosan solid Supported acidic ionic liquid catalyst PmimCl-AlCl 3 -CS.

[0026] 3. The prepared catalyst can efficiently synthesize DCPP

[0027] Add an appropriate amount of catalyst PmimCl-AlCl in a round bottom flask equipped with a reflux device. 3 -C...

Embodiment 3

[0028] Example 3: PmimCl-InCl 3 -CS Catalytic Synthesis of DCPP

[0029] 1. Preparation of Lewis acid ionic liquid

[0030] 1-Methylimidazole and Y-chloropropyltrimethoxysilane were refluxed and reacted at 70°C for 70h, and then reacted at 70°C for 24h according to the molar ratio of Lewis acid indium chloride to the prepared product of 2:1.

[0031] 2. Preparation of chitosan immobilized Lewis acid ionic liquid

[0032] Such as figure 1 As shown, the obtained ionic liquid containing chloroindium acid and 2 times the mass of chitosan were dispersed in acetonitrile and refluxed for 20 hours, and the solvent was removed by rotary evaporation. The obtained solid was Soxhlet extracted with dichloromethane for 30 hours to obtain a solid chitosan. Supported acidic ionic liquid catalyst PmimCl-InCl 3 -CS.

[0033] 3. The prepared catalyst can efficiently synthesize DCPP

[0034] Add appropriate amount of catalyst PmimCl-InCl in a round bottom flask equipped with reflux device 3 -CS, phosphoru...

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Abstract

The invention relates to a method for preparing chitosan immobilized Lewis acidic ionic liquid and DCPP synthesized by using chitosan immobilized Lewis acidic ionic liquid in presence of high-efficient catalyst. The method is characterized by comprising the following steps: performing refluxing reaction on 1-methylimidazole and Y-chloropropyl trimethoxy silane in a mol ratio of 1:1 at a temperature of 70 DEG C for 70 hours; then performing reaction in a mol ratio of Lewis acid anhydrous ferric chloride to a prepared product of 2:1 at a temperature of 70 DEG C for 24 hours; dispersing the obtained ionic liquid containing ferricyanide and chitosan which is 2 times of the ionic liquid in mass in acetonitrile to reflux for 20 hours; performing rotary evaporation to remove a solvent; and performing soxhlet extraction on the obtained solid with methylene dichloride for 30 hours to obtain a chitosan immobilized acidic ionic liquid catalyst PmimCl-FeCl3-CS. Anhydrous aluminum chloride and indium chloride are used for replacing anhydrous ferric chloride and serve as a Lewis acid in turn to obtain PmimCl-AlCl3-CS and PmimCl-InCl3-CS respectively. The method has the advantages of low-price and readily available reaction raw materials, mild reaction and simple condition.

Description

Technical field [0001] The invention relates to a preparation method of a class of chitosan immobilized Lewis acid ionic liquid and high-efficiency catalytic synthesis of DCPP. Background technique [0002] As a green catalyst, ionic liquids have gradually replaced traditional catalysts in chemical reactions. In the alkylation reaction, the ionic liquid is both a catalyst and a solvent. The acidity of ionic liquids is based on Lewis acid (AlCl 3 Etc.) The ratio of organic cations can be adjusted in a wide range to make it have Lewis basicity, Lewis acidity or even super acidity, so as to achieve the ideal catalytic effect. The immobilized ionic liquid developed in recent years is to immobilize the ionic liquid on an inorganic porous material or organic polymer material to prepare a heterogeneous catalyst, thereby transferring the characteristics of the ionic liquid to a heterogeneous solid catalyst. Compared with free-state ionic liquids, immobilized ionic liquids are more stab...

Claims

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Application Information

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IPC IPC(8): B01J37/00B01J31/30B01J31/26C07F9/48
Inventor 谢宇胡金刚
Owner NANCHANG HANGKONG UNIVERSITY
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