A kind of ionic liquid composite material and its preparation method for separating ephedrine in pinellia

A technology for ionic liquids and composite materials, applied in the field of ionic liquid composite materials and their preparation, can solve the problems of inability to perform selective adsorption and adsorption efficiency, difficulty in removing ephedrine, etc., achieve high selective adsorption and separation of ephedrine, and process synthesis is simple and easy Improvement of operation and adsorption efficiency

Active Publication Date: 2020-08-04
YANGTZE UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The object of the present invention is to: provide a kind of can carry out selective adsorption to the ephedrine in pinellia, the adsorption efficiency is high, the ionic liquid does not run off and the stability is strong, to solve the technological operation difficulty of removing ephedrine in the prior art, cannot carry out Ionic liquid composite material and preparation method for separating ephedrine in pinellia with selective adsorption and low adsorption efficiency

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036] Add 5.0g of silica gel, 10.0g of (3-chloropropyl)trimethoxysilane and 80.0g of toluene to a 250.0mL round bottom flask, (3-chloropropyl)trimethoxysilane is >99.5% in purity, and toluene is in purity >99.0%. Stir well and heat to 110 o C was reacted for 10 hours to obtain a translucent suspension; after the translucent suspension was naturally cooled to room temperature, it was suction-filtered under reduced pressure, and the filter cake was cleaned with 100.0 g of dehydrated alcohol and acetone with a volume ratio of 2:1. The purity of ethanol is >99.5%, and the purity of acetone is >99.5%. After drying in an oven at 80°C, 9.8g of white silanized silica gel powder is obtained;

[0037] Add 9.8g of white silanized silica gel powder, 5.0g of imidazole, 5.0g of triethylamine and 80.0g of toluene obtained above into a 250.0mL round-bottomed flask. Triethylamine has a purity of >99.0%, and toluene has a purity of >99.0%. After heating to 110 o C was reacted for 10 hours t...

Embodiment 2

[0044] Add 5.0g of silica gel, 13.5g of (3-chloropropyl)trimethoxysilane and 100.0g of toluene to a 250.0mL round bottom flask, (3-chloropropyl)trimethoxysilane is >99.5% in purity, and toluene is in purity >99.0%. Stir well and heat to 110 o C was reacted for 10 hours to obtain a translucent suspension; after the translucent suspension was naturally cooled to room temperature, it was suction-filtered under reduced pressure, and the filter cake was cleaned with 100.0 g of dehydrated alcohol and acetone with a volume ratio of 2:1. The purity of ethanol is >99.5%, and the purity of acetone is >99.5%. After drying in an oven at 80°C, 12.1g of white silanized silica gel powder is obtained;

[0045] Add 12.1g of white silanized silica gel powder, 7.5g of imidazole, 7.0g of triethylamine and 100.0g of toluene obtained above into a 250.0mL round-bottomed flask. Triethylamine has a purity of >99.0%, and toluene has a purity of >99.0%. Stir well After heating to 110 o C was reacted ...

Embodiment 3

[0052] Add 5.0g of silica gel, 16.3g of (3-chloropropyl)trimethoxysilane and 80.0g of toluene in a 250.0mL round bottom flask, (3-chloropropyl)trimethoxysilane is >99.5% in purity, and toluene is in purity >99.0%. Stir well and heat to 110 o C was reacted for 10 hours to obtain a translucent suspension; after the translucent suspension was naturally cooled to room temperature, it was suction-filtered under reduced pressure, and the filter cake was cleaned with 100.0 g of dehydrated alcohol and acetone with a volume ratio of 2:1. The purity of ethanol is>>99.5%, and the purity of acetone is>99.5%. After drying in an oven at 80°C, 17.1g of white silanized silica gel powder is obtained;

[0053] Add 17.1g of white silanized silica gel, 9.5g of imidazole, 10.5g of triethylamine and 80.0g of toluene into a 250.0mL round bottom flask. The purity of triethylamine is >99.0%, and the purity of toluene is >99.0%. Stir evenly and heat to 110 o C was reacted for 10 hours to obtain a tu...

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Abstract

The invention relates to an ionic liquid composite material for separating ephedrine in pinellia ternata and a preparation method thereof and belongs to the technical field of separation of natural products. The ionic liquid composite material and the preparation method thereof provided by the invention have the beneficial effects that the ionic liquid composite material takes a silica gel material as a substrate and is prepared by firstly performing functional group modification on the surface of the silica gel material through ionic liquid and then compounding a molecularly-imprinted polymerlayer on a functional group of the silica gel material; the ionic liquid silica gel-imprinted polymer composite material takes the silica gel material as the substrate and has good acid resistance and mechanical strength; then the group modification is performed on the surface through the ionic liquid, and the adsorption efficiency can be improved by utilizing the excellent solubility, the hydrophobicity and various chemical forces of the ionic liquid; finally, not only is the surface area of the compounded imprinted polymer material increased, but also the adsorption selectivity is greatly improved. The composite material is applied to the separation of a pinellia ternata extract, and the ephedrine can be subjected to highly-selective adsorption separation.

Description

technical field [0001] The invention relates to an ionic liquid composite material used for separating ephedrine from pinellia pinellia and a preparation method thereof, belonging to the technical field of ephedrine adsorption and separation. Background technique [0002] Pinellia is a traditional Chinese medicine substance, which contains phenols, organic acids, sterols, glycosides and other medicinal ingredients. The alkaloid components in the cough suppress the cough center to produce antitussive effect. But the ephedrine contained in Pinellia Pinellia is not conducive to the direct use of Pinellia Pinellia because of its toxic and side effects, so it is necessary to remove the ephedrine in Pinellia Pinellia extract. In the prior art, methods such as liquid-liquid extraction and cooking precipitation can be used to remove ephedrine in the solution, but the above-mentioned methods have higher requirements on pH and are more complicated to operate. The adsorption separati...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J20/26B01J20/30C07C213/10C07C215/30
CPCB01J20/268C07C213/10C07C215/30
Inventor 田明磊颜学敏肖围谢锦峰
Owner YANGTZE UNIVERSITY
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