Preparation method and application of tentacle type amino acid supported ionic liquid

An ionic liquid, amino acid type technology, applied in chemical instruments and methods, ion exchange, ion exchange regeneration, etc., can solve the problems of increased solid loading, limited carrier surface area, etc., and achieve the effect of large adsorption capacity

Active Publication Date: 2017-02-22
SICHUAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, at present, ionic liquids are all immobilized in a single layer, the surface area

Method used

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  • Preparation method and application of tentacle type amino acid supported ionic liquid
  • Preparation method and application of tentacle type amino acid supported ionic liquid
  • Preparation method and application of tentacle type amino acid supported ionic liquid

Examples

Experimental program
Comparison scheme
Effect test

Example Embodiment

[0016] Implementation example 1: Preparation method of L-proline methyl imidazole ionic liquid

[0017] (1) Weigh 0.1 mol of γ-chloropropyltrimethoxysilane into a 100 mL round-bottom flask, add 0.12 mol of N-methylimidazole, and heat up to 80°C under nitrogen protection and reflux for 16 hours to generate a light yellow viscous liquid. The product was washed 4 times with ethyl acetate to remove the unreacted N-methylimidazole, and then washed 4 times with anhydrous ether, and the solvent was distilled off under reduced pressure. The product was placed at 60° C. and vacuum dried for 36 hours. (2) Weigh 0.05 mol of the product of step (1) in a beaker, add 50 mL of absolute ethanol to dissolve it, and transfer the dissolved solution to a pre-treated strong basic anion exchange resin (201×7 -717) packed in the column (resin volume is 7 times the molar exchange volume, packing height is 300mm), the flow rate of the effluent is controlled not to exceed 2 drops per second, and ethanol i...

Example Embodiment

[0018] Implementation Example 2: Preparation method of antennae type silica gel intermediate

[0019] Weigh 3.0 g of silica gel and place it in a 100 mL round bottom flask. Add an appropriate amount of water-dispersed silica gel, add 15 mL of hydrochloric acid and 6.0 g of a glutaraldehyde aqueous solution with a mass fraction of 50% in a flask using a constant pressure dropping funnel, and react for 3 hours at room temperature. After that, 20 mL of 15% polyvinyl alcohol (polymerization degree 1700, alcoholysis rate 99%) solution was added dropwise, and the reaction was stirred at 35°C for 6 h. The product was washed with deionized water to neutrality, dried and stored in a desiccator. The product is white tentacled silica gel powder.

Example Embodiment

[0020] Implementation example 3: Preparation method of antenna type L-proline methylimidazole immobilized ionic liquid

[0021] Disperse 3.0 g of tentacled silica gel powder in 30 mL of acetonitrile, and add 0.03 mol of the product of step (4). Reflux at 80°C for 12h. The product was washed with deionized water three times to remove the unreacted L-proline imidazole ionic liquid, and dried in vacuum at 60°C for 8 hours to obtain the antenna-type amino acid immobilized ionic liquid. The final product is a light yellow solid powder, and the solid load of the ionic liquid is 0.3g ionic liquid / g adsorbent.

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Abstract

The invention discloses a method for preparing a supported ionic liquid from silicone, polyvinyl alcohol, methylimidazole and L-proline in a chemical bonding manner. The method comprises steps as follows: (1) gamma-chloropropyltrimethoxysilane is taken as a coupling agent to react with methylimidazole, and negative ions, namely, chloride ions, of a product are replaced with hydroxide ions with the adoption of ion exchange resin; (2) the product and L-proline react, and hydroxide negative ions are replaced with amino acid negative ions; (3) a polyvinyl alcohol long chain is bonded to the silicone surface, and silicone with polyhydroxy tentacles is obtained; (4) an amino acid type methylimidazole ionic liquid with coupling agent side chains is bonded to the silicone tentacles. The method is a novel method for preparing the supported ionic liquid with the adsorption function.

Description

technical field [0001] The invention relates to a method for preparing an immobilized ionic liquid, in particular to a method for preparing an antenna-type immobilized ionic liquid by using silica gel, methylimidazole and L-proline, and belongs to the field of chemical synthesis and separation. Background technique [0002] Ionic liquid is a liquid substance that exists completely in an ionic state at room temperature or near room temperature. Compared with traditional chemical media, it has structural designability, low vapor pressure, high polarization potential, excellent solubility, and high temperature. It has been widely used in the fields of organic synthesis and separation science due to its advantages of stability and favorable kinetic control. It has been found that there is a strong interaction between it and natural active molecules in the existing separation research and application. [0003] Immobilized ionic liquid refers to a supported ionic liquid or a solid...

Claims

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Application Information

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IPC IPC(8): B01D15/08B01J20/10B01J20/22B01J20/26
CPCB01D15/08B01J20/103B01J20/22B01J20/261
Inventor 姚舜张薇宋航聂丽蓉
Owner SICHUAN UNIV
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