A kind of loaded perrhenate ionic liquid and preparation method thereof

A perrhenate, 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 liquids, large amount of catalysts, 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: 2015-09-02
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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  • A kind of loaded perrhenate ionic liquid and preparation method thereof
  • A kind of loaded perrhenate ionic liquid and preparation method thereof
  • A kind of loaded perrhenate ionic liquid and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] Embodiment 1 supported perrhenate ionic liquid

[0018] In a 100mL reactor, add 25mL toluene, add MCM-41 (2g), chloropropyltriethoxysilane (1g), stir at 60°C for 12h under nitrogen protection, filter with suction, and wash with ethanol (5mL) 3 times, vacuum drying at 50°C for 10 h to obtain Intermediate A.

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

[0020] Using toluene (25mL) as solvent, add intermediate B (2g) and ammonium perrhenate (0.5g), react at room temperature for 24h, filter with suction, wash with water (10mL) three times, dry in a constant temperature oven at 110°C for 12h , to obtain the target product-loaded perrhenate ionic liquid, the structural formula of which is shown in I. Calculate its load to be about 8%.

[0021] The product w...

Embodiment 2

[0025] Embodiment 2 supported perrhenate ionic liquid

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

[0027] Using dichloromethane (25mL) as solvent, add intermediate A (2g), nitrogen methyl imidazole (1g) to react under nitrogen atmosphere, stir at 95°C for 15h, filter with suction, wash with methanol (5mL) three times, at 50 °C and vacuum-dried for 10 h to obtain the product intermediate B.

[0028] Using dichloromethane (25mL) as solvent, add intermediate B (2g) and ammonium perrhenate (0.5g), react at room temperature for 24h, filter with suction, wash with water (10mL) three times, and dry at 110°C After 12 hours in the box, the target product-loaded perrhenate ionic liquid was obtained, and its structural formula was shown in I. Calcula...

Embodiment 3

[0030] Embodiment 3 supported perrhenate ionic liquid

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

[0032] Using ethanol (25mL) as solvent, add intermediate A (2g), nitrogen methyl imidazole (1g) to react under nitrogen atmosphere, stir at 180°C for 8h, filter with suction, wash with methanol (5mL) three times, vacuum at 50°C After drying for 10 h, Intermediate B was obtained.

[0033] Using ethanol (25mL) as solvent, add intermediate B (2g) and ammonium perrhenate (0.5g), react at room temperature for 24h, filter with suction, wash with water (10mL) three times, dry in a constant temperature oven at 110°C for 12h , to obtain the target product-loaded perrhenate ionic liquid, the structural formula of which is shown in I. Calculate its load to be abou...

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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 novel load-type ionic liquid, which uses chloropropyltriethoxysilane, MCM-41, N-methylimidazole and ammonium perrhenate as raw materials to synthesize the perrhenate load-type ionic liquid. Background technique [0002] Perrhenate ionic liquid is a new type of 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 compounds. For example, in the olefin epoxidation reaction, rhenium ionic liquid is used as the reaction solvent and catalyst, and 30% hydrogen peroxide is used as the oxidant to epoxidize cyclooctene, and the yield of epoxide can reach more than 95%. 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. Contents of the invention [0003] The object of the present invention is to pro...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D301/12C07D303/04B01J31/02
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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