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Supported ionic liquid catalyst, as well as preparation and application thereof

An ionic liquid and catalyst technology, applied to the supported ionic liquid catalyst and its preparation and application fields, can solve the problems of difficult purification and separation of products and catalysts, harsh reaction conditions, inconvenient recycling, etc., and achieve thermal stability and chemical stability. Good, simple preparation, pore structure controllable effect

Inactive Publication Date: 2015-05-13
EAST CHINA NORMAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] At present, reports on catalysts for the cycloaddition reaction of carbon dioxide and epoxy compounds have made great progress (Chem. Rev. 2007, 107, 2365-2387). Disadvantages such as difficult purification and separation of product and catalyst, inconvenient catalyst recovery and recycling
Heterogeneous catalysts solve the problems of catalyst separation and recovery, but generally have low activity, poor stability, harsh reaction conditions, and many of them need to add organic solvents and additives

Method used

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  • Supported ionic liquid catalyst, as well as preparation and application thereof
  • Supported ionic liquid catalyst, as well as preparation and application thereof
  • Supported ionic liquid catalyst, as well as preparation and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] (1) Chloromethylation of organic mesoporous materials

[0024] Mix 5g of FDU-type mesoporous phenolic resin with 60ml of chloromethyl ether at -5°C under the protection of argon, then weigh 21g of anhydrous aluminum trichloride and add it to the above mixture three times. The time is 0.5 hours. Stir at room temperature for 12 hours to carry out chloromethylation reaction. After the reaction, add an appropriate amount of pure water to completely hydrolyze aluminum trichloride, then cool to 0°C and filter. The filtrate is mixed with 500ml pure water and 200ml acetone Alternately washing to obtain a brown solid, and after vacuum drying, a chloromethylated FDU organic mesoporous material was obtained.

[0025] (2) Imidazolization of organic mesoporous materials

[0026] After mixing 5g of chloromethylated FDU mesoporous phenolic resin with 60ml of acetonitrile solution, add 4g of imidazole to carry out imidazole reaction at 80°C for 12 hours. After the reaction, the filtra...

Embodiment 2

[0030] (1) Chloromethylation of organic mesoporous materials

[0031] Mix 5g of FDU-type mesoporous phenolic resin with 60ml of chloromethyl ether at -5°C under the protection of argon, then weigh 21g of anhydrous aluminum trichloride and add it to the above mixture three times. The time is 0.5 hours. Stir at room temperature for 12 hours to carry out chloromethylation reaction. After the reaction, add an appropriate amount of pure water to completely hydrolyze aluminum trichloride, then cool to 0°C and filter. The filtrate is mixed with 500ml pure water and 200ml acetone Alternately washing to obtain a brown solid, and after vacuum drying, a chloromethylated FDU organic mesoporous material was obtained.

[0032] (2) Imidazolization of organic mesoporous materials

[0033] After mixing 5g of chloromethylated FDU mesoporous phenolic resin with 60ml of acetonitrile solution, add 4g of imidazole to carry out imidazole reaction at 80°C for 12 hours. After the reaction, the filtra...

Embodiment 3

[0037] 1.75g ​​(30mmol) propylene oxide (1a) and 0.28g mesoporous phenolic resin supported 3-hydroxyethylimidazolium bromide salt ionic liquid catalyst (R 1 =(CH 2 ) 2 , R 2 =OH) Fill the autoclave with CO 2 , and then heated to 120°C to carry out the cycloaddition reaction of the following structural formula,

[0038]

[0039] The reaction pressure is 1MPa, during the reaction CO 2 The pressure was kept constant, and the reaction time was 4 hours. After the reaction, the reactor was cooled to 0°C, and excess carbon dioxide gas was slowly released, and then the reaction liquid was filtered. The filtrate was analyzed qualitatively by GC-MS, and 0.2 g of biphenyl was added as The standard substance was quantitatively analyzed by gas chromatography, and the product obtained was propylene carbonate (2a), with a yield of 99.0% and a selectivity of 99.8%. The filtered catalyst can be recycled after being washed with acetone and dried.

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Abstract

The invention discloses a supported ionic liquid catalyst. The supported ionic liquid catalyst is characterized in that imidazole is immobilized onto chloromethylated FDU mesoporous phenolic resin by nucleophilic reaction and reacts with halides containing different functional groups to prepare a mesoporous material supported functional imidazole type ionic liquid catalyst. The preparation of the catalyst comprises the following steps: chloromethylation of a mesoporous material, imidazolation and supporting of ionic liquid. The catalyst is used for synthesizing a cyclic carbonate by cyclic addition reaction of carbon dioxide and an epoxy compound, and the using quantity of the catalyst is 0.1-2mol% of the liquid content of the epoxy compound. Compared with the prior art, a large number of hydroxyl groups exist in the mesoporous material, and the supported ionic liquid catalyst has the double advantages of an inorganic mesoporous material and an organic polymer, as well as large specific surface area, adjustable pore structure, good hydrophobicity and chemical stability, high catalytic activity, good chemical selectivity, easiness in separation and recovery, mild reaction conditions, environmental friendliness and easiness in industrial implementation.

Description

technical field [0001] The invention relates to the field of chemical catalytic materials and synthesis technology, in particular to a supported ionic liquid catalyst and its preparation and application. Background technique [0002] As the main greenhouse gas, carbon dioxide is also the most abundant C on earth. 1 Resources. Due to the dual needs of environmental protection and energy utilization, the fixed conversion of carbon dioxide has become the focus of global attention. CO 2 The cycloaddition reaction with epoxy compounds is one of the most effective ways to fix carbon dioxide. This reaction is environmentally friendly and has 100% atom economy. The obtained cyclic carbonate is an important industrial raw material and has wide applications in the synthesis of organic carbonates, pharmaceutical intermediates, battery electrolytes and organic solvents. [0003] At present, reports on catalysts for the cycloaddition reaction of carbon dioxide and epoxy compounds have...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J31/06C07D317/36C07D317/38C07D317/46
CPCY02P20/141
Inventor 吴海虹张伟吴鹏
Owner EAST CHINA NORMAL UNIV
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