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Alkyl imidazoles perrhenate ion liquid and preparation method thereof

A perrhenate, ionic liquid technology, applied in chemical instruments and methods, organic compound/hydride/coordination complex catalysts, physical/chemical process catalysts, etc., can solve the instability of air and moisture, limit applications and other problems, to achieve the effect of protecting the environment, shortening the reaction time, and simplifying the process

Active Publication Date: 2009-03-18
辽宁中科航远科技有限公司
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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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  • Alkyl imidazoles perrhenate ion liquid and preparation method thereof
  • Alkyl imidazoles perrhenate ion liquid and preparation method thereof
  • Alkyl imidazoles perrhenate ion liquid and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0016] Embodiment 1 1-butyl-3-methyl-imidazole perrhenate ([Bmim][ReO 4 ]) ionic liquid

[0017] One) the structural formula is as follows:

[0018]

[0019] Two) preparation method is as follows:

[0020] (1) Synthesis of chloro-1-butyl-3-methyl-imidazole (BMIC):

[0021] Collect n-chlorobutane and N-methylimidazole in a distillation apparatus at 78°C and 188.5°C respectively to obtain pure products.

[0022] Take n-chlorobutane and N-methylimidazole with a molar ratio of 1.2:1, heat and reflux at 80°C for 72 hours, place it at 0-10°C for 7-9 hours, and obtain a white product after filtration , which is 1-butyl-3-methylimidazole chloride (BMIC).

[0023] (2) Purification of chlorination-1-butyl-3-methyl-imidazole (BMIC)

[0024] Add ethyl acetate and acetonitrile solution with a volume ratio of 2:1 to the above white product, and heat to reflux in an oil bath at 75°C to completely dissolve the white product. Cool at 0~-10°C, place for 7~9 hours, and obtain white crys...

Embodiment 2

[0033] Embodiment 2 1-ethyl-3-methyl-imidazole perrhenate ([Emim][ReO 4 ]) ionic liquid

[0034] One) the structural formula is as follows:

[0035]

[0036] Two) preparation method is as follows:

[0037] (1) Conversion of Hydroxide-1-Ethyl-3-Methyl-Imidazole (EMIOH)

[0038] Take a certain amount of chlorinated-1-ethyl-3-methylimidazole, add 2 to 4 times of deionized water to dissolve, add it to OH type anion exchange resin for ion exchange, collect the outflowing solution until chlorine is detected ions, the collected solution is the EMIOH solution;

[0039] (2) Take the hydroxide-1-ethyl-3-methyl-imidazole solution, carry out accurate titration with hydrochloric acid of known concentration, and calculate the concentration of the collected EMIOH solution. Add hydroxide-1-ethyl-3-methyl-imidazole to ammonium perrhenate aqueous solution, and the molar ratio of hydroxide-1-ethyl-3-methyl-imidazole to ammonium perrhenate is 1:1 After heating and stirring at 70°C for 3 h...

Embodiment 3

[0041] Example 3 1-propyl-3-methyl-imidazole perrhenate ([Tmim][ReO 4 ]) ionic liquid

[0042] One) the structural formula is as follows:

[0043]

[0044] Two) preparation method is as follows:

[0045] (1) Conversion of Hydroxide-1-Propyl-3-Methyl-Imidazole (TMIOH)

[0046] Take a certain amount of bromide-1-propyl-3 methylimidazole, add 2 to 4 times of deionized water to dissolve, add it to OH type anion exchange resin for ion exchange, collect the outflowing solution until bromide ion is detected So far, the collected solution is the TMIOH solution;

[0047] (2) Take the hydroxide-1-propyl-3-methyl-imidazole solution, carry out accurate titration with hydrochloric acid of known concentration, and calculate the concentration of the collected TMIOH solution. Add hydroxide-1-propyl-3-methyl-imidazole to ammonium perrhenate aqueous solution, the molar ratio of hydroxide-1-propyl-3-methyl-imidazole to ammonium perrhenate is 1:2, After heating and stirring at 70°C for 5 ...

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Abstract

The invention relates to alkyl imidazole perrhenate ionic liquid and a method for preparing the same. The adopted technical proposal is follows: the preparation method comprises the following steps: taking certain volume of alkyl imidazole chloride compounds or alky imidazole bromide compounds, adding deionized water the volume of which is 2 to 4 times of that of the alkyl imidazole chloride compounds or the alky imidazole bromide compounds to dissolve the alkyl imidazole chloride compounds or the alky imidazole bromide compounds, adding the mixture to OH-type anion exchange resin to perform ion exchange, and collecting outflow solution which is alkyl imidazole hydroxide; then adding the alkyl imidazole hydroxide to ammonium perrhenate aqueous solution, wherein the molar ratio of the alkyl imidazole hydroxide to the high ammonium perrhenate is between 1 to 1 and 1 to 2, then stirring the mixture for 3 to 5 hours at a temperature of between 70 and 90 DEG C, reducing the pressure and distilling the mixture to remove water, adding the mixed solution of anhydrous methanol and acetonitrile to the mixture after cooling the mixture, sealing and stirring the mixture intensely, keeping stand the mixture for 10 to 15 hours at a temperature of between 30 DEG C below zero and 40 DEG C below zero, reducing the pressure and distilling the mixture to remove the methanol and the acetonitrile, and performing vacuum drying on the treated mixture. The ionic liquid prepared by the method has the advantages of high yield and high stabilities of air and water.

Description

technical field [0001] The invention belongs to the field of chemical synthesis, and in particular relates to a novel rhenium-based ionic liquid and a preparation method thereof. Background technique [0002] Scattered metals (gallium, indium, thallium, germanium, selenium, tellurium, rhenium) and their compounds have attracted more and more researchers' attention because of their special physical and chemical properties, such as electrical conductivity and catalytic activity. my country is a big country producing rare metals. Scattered metals and their compounds are the supporting materials of many high-tech related to national defense, and are indispensable for many cutting-edge science and technology (such as electronic communications, energy, aerospace, catalysis and life sciences, etc.) The high-tech supporting materials are obviously of strong military color, so the development of the scattered metal industry is of great significance to the strengthening of national def...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D233/58B01J31/02
Inventor 臧树良房大维赵飞
Owner 辽宁中科航远科技有限公司
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