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Amino group-containing ionic liquid-modified graphene oxide-wrapped silica gel-based chromatographic filling material

A graphene-wrapped, ionic liquid technology, used in ion exchange, ion exchange regeneration, ion exchange treatment devices, etc., to achieve the effect of excellent chromatographic performance

Inactive Publication Date: 2018-06-15
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, there is no report on the preparation of chromatographic packing materials by modifying ionic liquid and graphene oxide on the surface of silica gel in the prior art

Method used

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  • Amino group-containing ionic liquid-modified graphene oxide-wrapped silica gel-based chromatographic filling material
  • Amino group-containing ionic liquid-modified graphene oxide-wrapped silica gel-based chromatographic filling material
  • Amino group-containing ionic liquid-modified graphene oxide-wrapped silica gel-based chromatographic filling material

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] Example 1 Preparation of ionic liquid-modified graphene oxide-wrapped silica gel-based chromatographic material

[0032] Proceed as follows:

[0033] (1) Take 10g of silica gel and 100mL of hydrochloric acid with a mass fraction of 37%, mix the two evenly, let stand for acidification for 12h, then separate the silica gel, wash with distilled water until neutral, and finally vacuum dry at 120°C for 12h to obtain the surface 10g of silica gel containing silanol;

[0034] (2) Add 10g of silica gel containing silanol on the surface obtained above into 100ml of anhydrous toluene, after dispersing evenly, add 8g of 3-aminopropyltriethoxysilane, mix the mixture uniformly by ultrasonic, then heat at 120°C Reflux and react for 12 hours; after the reaction, wash the filler with toluene, ethanol, and methanol in sequence, and dry the washed filler at 120°C for 24 hours under vacuum at 0.06Mpa to obtain NH 2 / SiO 2 ;

[0035] (3) Get 0.1g of graphene oxide powder and disperse i...

Embodiment 2

[0038] Example 2 Preparation of ionic liquid-modified graphene oxide-wrapped silica gel-based chromatographic material

[0039] Proceed as follows:

[0040] (1) Take 10g of silica gel and 100mL of hydrochloric acid with a mass fraction of 37%, mix the two evenly, let it stand for acidification for 24 hours, then separate the silica gel, wash it with distilled water until it is neutral, and finally dry it in vacuum at 120°C for 24 hours to obtain the surface 10g of silica gel containing silanol;

[0041](2) Add 10g of silica gel containing silanol on the surface obtained above to 100ml of anhydrous toluene, after dispersing evenly, add 8g of 3-aminopropyltriethoxysilane, mix the mixture uniformly by ultrasonic, then heat and reflux at 150°C , reacted for 12h; after the reaction, wash the filler with toluene, ethanol and methanol in turn, and dry the washed filler at 120°C for 24h under vacuum at 0.06Mpa to obtain NH 2 / SiO 2 ;

[0042] (3) Take 0.1g of graphene oxide powder...

Embodiment 3

[0045] Example 3 Preparation of ionic liquid-modified graphene oxide-wrapped silica gel-based chromatographic material

[0046] Proceed as follows:

[0047] (1) Take 10g of silica gel and 100mL of hydrochloric acid with a mass fraction of 37%, mix the two evenly, let it stand for acidification for 24 hours, then separate the silica gel, wash it with distilled water until it is neutral, and finally dry it in vacuum at 120°C for 24 hours to obtain the surface 10g of silica gel containing silanol;

[0048] (2) Add 10g of silica gel containing silanol on the surface obtained above to 100ml of anhydrous toluene, after dispersing evenly, add 8g of 3-aminopropyltriethoxysilane, mix the mixture uniformly by ultrasonic, then heat and reflux at 150°C , reacted for 12h; after the reaction, wash the filler with toluene, ethanol and methanol in turn, and dry the washed filler at 120°C for 24h under vacuum at 0.06Mpa to obtain NH 2 / SiO 2 ;

[0049] (3) Take 0.02g of graphene oxide powd...

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Abstract

The invention discloses an amino group-containing ionic liquid-modified graphene oxide-wrapped silica gel. A preparation method for the silica gel comprises the following steps: (1) adding silica gelcontaining silicon hydroxyl groups on its surface into the solvent toluene, then adding aminopropyl triethoxysilane, and carrying out heating reflux for surface amination of the silica gel so as to obtain aminopropyl silica gel; (2) adding the aminopropyl silica gel into an aqueous solution of graphene oxide and carrying out a reaction so as to obtain graphene oxide-modified silica gel; (3) preparing amino group-containing ionic liquid by reacting 2-bromoethylamine hydrobromide and 1-methylimidazole in the solvent acetonitrile; and (4) reacting the graphene oxide-modified silica gel with the amino group-containing ionic liquid in the solvent methanol and successively carrying out centrifugation, washing with deionized water and drying. The graphene-oxide-wrapped silica gel modified by theamino-group-containing ionic liquid can be used as a chromatographic stationary-phase material for separation and analysis of substances and has excellent chromatographic performance.

Description

technical field [0001] The invention relates to a silica gel-based chromatographic packing modified with amino ionic liquid modified graphene oxide and a preparation method thereof, belonging to the field of silica gel chromatographic packing. Background technique [0002] Ionic liquid (ionic liquid, abbreviated as IL), as a new type of solvent, has attracted more and more interest of scientific researchers. At present, IL has been widely used in various fields, and also shows its own advantages. Like IL, graphene oxide (GO for short) is also a new type of material. Because GO contains a large number of oxygen-containing functional groups (such as: C-O-C, C-OH, –-COOH, etc.), it can be easily bonded to the surface of the substrate material through chemical reactions. At present, in the prior art, there is no report about modifying ionic liquid and graphene oxide onto the surface of silica gel to prepare chromatographic packing. Contents of the invention [0003] Aiming ...

Claims

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Application Information

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IPC IPC(8): B01J20/286B01J20/30B01D15/08
CPCB01D15/08B01J20/286B01J2220/52
Inventor 曹绪龙马宝东周敏郭兰磊祝仰文王红艳李向良王其伟张书栋汤战宏张文张林彦丁玉娟
Owner CHINA PETROLEUM & CHEM CORP
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