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Method for preparing dissipated metal rhenium ionic liquid

A technology of ionic liquids and scattered metals, applied in chemical instruments and methods, organic compound/hydride/coordination complex catalysts, organic chemistry, etc. simple effect

Inactive Publication Date: 2010-06-16
LIAONING UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The ionic liquids of scattered metal gallium and indium that have been synthesized are unstable to air and moisture, which greatly limits their application in various fields of chemical industry.

Method used

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  • Method for preparing dissipated metal rhenium ionic liquid
  • Method for preparing dissipated metal rhenium ionic liquid
  • Method for preparing dissipated metal rhenium ionic liquid

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] Embodiment 1N-butylpyridine perrhenate ([BPy][ReO 4 ]) ionic liquid

[0018] The preparation method is as follows:

[0019] Take a certain amount of purified N-butylpyridine, add 2 to 4 times of deionized water to dissolve it, add it to OH type anion exchange resin for ion exchange, collect the outflowing solution until bromide ion is detected. Perform an accurate titration with hydrochloric acid of known concentration to calculate the concentration of the collected solution. Add it to the ammonium perrhenate aqueous solution, the molar ratio is 1:1, heat and stir at 70°C for 4 hours, remove the water by rotary evaporation, add excess anhydrous methanol and acetonitrile solution with a volume ratio of 1:9 after cooling , sealed and vigorously stirred, placed at -34°C for 12 hours, distilled under reduced pressure to remove methanol and acetonitrile, and dried the obtained product in a vacuum oven at 80°C for 48 hours. The resulting product is N-butylpyridine perrhena...

Embodiment 2

[0020] Embodiment 2N-Propylpyridine perrhenate ([TPy][ReO 4 ]) ionic liquid

[0021] The preparation method is as follows:

[0022] Take a certain amount of purified N-propylpyridine, add 2 to 4 times of deionized water to dissolve it, add it to OH type anion exchange resin for ion exchange, and collect the outflowing solution until bromide ion is detected. Perform an accurate titration with hydrochloric acid of known concentration to calculate the concentration of the collected solution. Add it to the ammonium perrhenate aqueous solution with a molar ratio of 1:2, heat and stir at 65°C for 4 hours, remove the water by rotary evaporation, and add excess anhydrous methanol and acetonitrile solution with a volume ratio of 1:9 after cooling , sealed and vigorously stirred, placed at -34°C for 12 hours, distilled under reduced pressure to remove methanol and acetonitrile, and dried the obtained product in a vacuum oven at 80°C for 48 hours. The resulting product is N-butylpyrid...

Embodiment 3

[0023] Embodiment 3N-ethylpyridine perrhenate ([EPy][ReO 4 ]) ionic liquid

[0024] The preparation method is as follows:

[0025] Take a certain amount of purified N-ethylpyridine, add 2 to 4 times of deionized water to dissolve it, add it to an OH-type anion exchange resin for ion exchange, and collect the outflowing solution until bromide ions are detected. Perform an accurate titration with hydrochloric acid of known concentration to calculate the concentration of the collected solution. Add it to the ammonium perrhenate aqueous solution, the molar ratio is 1:1.5, heat and stir at 60°C for 4 hours, remove the water by rotary evaporation, add excess anhydrous methanol and acetonitrile solution with a volume ratio of 1:9 after cooling , sealed and vigorously stirred, placed at -30°C for 12 hours, distilled under reduced pressure to remove methanol and acetonitrile, and dried the obtained product in a vacuum oven at 80°C for 48 hours. The resulting product is N-butylpyridi...

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Abstract

The invention relates to a method for preparing dissipated metal rhenium ionic liquid. The adopted technical scheme is as follows: the preparation method comprises the following steps: taking a certain amount of alkyl bromide pyridine compound, adding 2-4 times of deionized water for dissolution, adding into OH type anion exchange resin for carrying out ion exchange, and collecting effluent solution which is hydroxyalkyl pyridine; adding the hydroxyalkyl pyridine into ammonium perrhenate water solution, leading the molar ratio of the hydroxyalkyl pyridine to the ammonium perrhenate to be 1:1-1:2, stirring for 3-5 hours at the temperature of 70-90 DEG C, carrying out vacuum distillation for removing water, cooling, then adding mixed solution of anhydrous methanol and acetonitrile, sealing, churning, placing at the temperature of minus 30-minus 40 DEG C for 10-15 hours, carrying out the vacuum distillation, removing the methanol and the acetonitrile and carrying out vacuum drying. The ionic liquid has high yield and is stable to air and water.

Description

technical field [0001] The invention belongs to the field of chemical synthesis, and in particular relates to a preparation method of a dispersed metal rhenium ionic liquid. Background technique [0002] In recent years, the research on ionic liquids has become increasingly active, and governments and related companies in western countries have invested a lot of money to support the research on ionic liquids. At the same time, ionic liquids have also rapidly expanded from the fields of green chemistry and catalysis to functional materials, electro-optic and optoelectronic materials, solar energy storage, life sciences and other fields. In 2000, Professor Sedden of the United Kingdom and Professor Rogers of the United States held an expert meeting on ionic liquids in Crete, Greece. Since then, the Gordon Conference, the Annual Meeting of the American Chemical Society, the North Atlantic Treaty Organization, and the International Green Chemistry Conference have all held semin...

Claims

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Application Information

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IPC IPC(8): C07D213/20B01J31/02
Inventor 臧树良房大维谷学军李建新
Owner LIAONING UNIVERSITY
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