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Supported perrhenate ionic liquid as well as preparation method thereof

A perrhenate and ionic liquid technology, applied in chemical instruments and methods, organic compound/hydride/coordination complex catalysts, organic chemistry, etc., can solve the problem of high cost of ionic liquid, large amount of catalyst, and difficult separation of products and other problems, to achieve the effect of promoting the reaction process, reducing the dosage, reducing the dosage of catalyst and the cost of catalytic reaction

Active Publication Date: 2013-12-25
LIAONING UNIVERSITY OF PETROLEUM AND CHEMICAL TECHNOLOGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, due to the high cost and high viscosity of ionic liquids, resulting in a large amount of catalyst and difficult separation of products, their application is limited.

Method used

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  • Supported perrhenate ionic liquid as well as preparation method thereof
  • Supported perrhenate ionic liquid as well as preparation method thereof
  • Supported perrhenate ionic liquid as well as preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] Example 1 Loaded perrhenate ionic liquid

[0018] In a 100mL reactor, add 25mL toluene, add MCM-41 (2g), chloropropyltriethoxysilane (1g), under nitrogen protection, stir at 60℃ for 12h, filter with suction, and wash with ethanol (5mL) Three times, vacuum drying at 50°C for 10 hours to obtain Intermediate A.

[0019] Using toluene (25mL) as solvent, add intermediate A (2g), N-methylimidazole (1g), stir for 12h at 60℃ under nitrogen atmosphere, filter with suction, wash with methanol (5mL) three times, and dry at 50℃ in vacuum Intermediate B was obtained in 10h.

[0020] Take toluene (25mL) as solvent, add intermediate B (2g), ammonium perrhenate (0.5g), react at room temperature for 24h, filter with suction, wash with water (10mL) three times, and hold in a constant temperature drying oven at 110℃ for 12h , The target product supported perrhenate ionic liquid is obtained, and its structural formula is shown in I. Calculate its load is about 8%.

[0021] The product undergoes...

Embodiment 2

[0025] Example 2 Loaded perrhenate ionic liquid

[0026] In a 100mL reactor, add 25mL of dichloromethane, add MCM-41 (2g), chloropropyltriethoxysilane (1g), under a nitrogen atmosphere, stir at 95℃ for 10h, filter with suction, and ethanol (5mL ) Wash three times and vacuum-dry at 50°C for 10h to obtain Intermediate A.

[0027] Using dichloromethane (25mL) as solvent, add intermediate A (2g), nitromethylimidazole (1g) was reacted under nitrogen atmosphere, stirred at 95℃ for 15h, filtered with suction, washed with methanol (5mL) three times, Vacuum drying at ℃ for 10h to obtain the product intermediate B.

[0028] Using dichloromethane (25mL) as solvent, add intermediate B (2g), ammonium perrhenate (0.5g), react at room temperature for 24h, filter with suction, wash with water (10mL) three times, and dry at 110℃ constant temperature In the tank for 12 hours, the target product-supported perrhenate ionic liquid is obtained, the structural formula of which is shown in I. Calculate i...

Embodiment 3

[0030] Example 3 Loaded perrhenate ionic liquid

[0031] In a 100mL reactor, add 25mL ethanol, add MCM-41 (2g), chloropropyltriethoxysilane (1g), under a nitrogen atmosphere, stir at 180℃ for 9h, filter with suction, and wash with ethanol (5mL) Three times, vacuum drying at 50°C for 10 hours to obtain Intermediate A.

[0032] Using ethanol (25mL) as solvent, add intermediate A (2g), nitromethylimidazole (1g) was reacted under nitrogen, stirred at 180℃ for 8h, filtered with suction, washed with methanol (5mL) three times, vacuum at 50℃ After drying for 10 hours, intermediate B was obtained.

[0033] Using ethanol (25mL) as solvent, add intermediate B (2g), ammonium perrhenate (0.5g), react at room temperature for 24h, filter with suction, wash with water (10mL) three times, and place in a constant temperature drying oven at 110°C for 12h , The target product supported perrhenate ionic liquid is obtained, and its structural formula is shown in I. Calculate its load is about 12%.

[0...

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Abstract

The invention relates to a supported perrhenate ionic liquid as well as a preparation method thereof. The technical scheme adopted is as follows: the preparation method comprises the following steps: selecting MCM-41 (Mobil Composition of Matters) as a carrier material; firstly, carrying out a reaction on chloropropyl triethoxysilane and the MCM-41; grafting a chloropropyl silicon structure to the surface of the MCM-41, and removing the byproduct ethanol; then, adding N-methyl imidazole so as to quaternize to obtain MCM-41 supported alkyl imidazole chlorine salt; and further adding ammonium perrhenate, and converting the chlorine salt into perrhenate through double-decompose reaction to obtain the MCM-41 supported alkyl imidazole perrhenate ionic liquid. The molar ratio of the reaction materials chloropropyl triethoxysilane, N-methyl imidazole, the MCM-41 and perrhenate is 1:(4-1):(3-1):(10-0.1). The method is applicable to support of various different types of alkyl imidazole perrhenate ionic liquids.

Description

Technical field [0001] The invention relates to a new type of supported ionic liquid, which uses chloropropyltriethoxysilane, MCM-41, N-methylimidazole and ammonium perrhenate as raw materials to synthesize perrhenate supported ionic liquid. Background technique [0002] Perrhenate ionic liquid is a new green rare metal ionic liquid catalyst, which can efficiently catalyze the epoxidation of olefins, the oxidation of alcohols and aldehydes, and the oxidation of sulfur-containing compounds. For example, in the olefin epoxidation reaction, the rhenium ionic liquid is used as the reaction solvent and catalyst, and 30% hydrogen peroxide is used as the oxidant to epoxidize cyclooctene. The yield of epoxide can reach more than 95%. However, due to the high cost and high viscosity of ionic liquids, problems such as large amount of catalyst and difficult separation of products have been caused, which limits its application. Summary of the invention [0003] The purpose of the present inv...

Claims

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Application Information

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IPC IPC(8): B01J31/02C07D301/12C07D303/04
Inventor 臧树良周明东颜文超李蕊东红
Owner LIAONING UNIVERSITY OF PETROLEUM AND CHEMICAL TECHNOLOGY
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