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 b

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
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Example Embodiment

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

[0032] Proceed as follows:

[0033] (1) Take 10g of silica gel and 100mL of 37% hydrochloric acid, mix the two evenly, stand to acidify for 12h, then separate the silica gel, wash with distilled water to neutrality, and finally vacuum dry at 120℃ for 12h to obtain the surface 10g of silica gel containing silanol groups;

[0034] (2) Add 10g of the silica gel with silanol on the surface obtained above to 100ml of anhydrous toluene, after the dispersion is uniform, add 8g of 3-aminopropyltriethoxysilane, mix the mixture uniformly by ultrasonic, and heat at 120°C Reflux, react for 12h; after the reaction, wash the packing with toluene, ethanol, and methanol successively, and dry the washed packing at 120℃ in a vacuum of 0.06Mpa for 24h to obtain NH 2 / SiO 2 ;

[0035] (3) Disperse 0.1 g of graphene oxide powder in 100 ml of deionized water and perform ultrasonic dispers...

Example Embodiment

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

[0039] Proceed as follows:

[0040] (1) Take 10g of silica gel and 100mL of 37% hydrochloric acid, mix the two evenly, stand for 24 hours to acidify, then separate the silica gel, wash with distilled water to neutrality, and finally vacuum dry at 120°C for 24 hours to obtain the surface 10g of silica gel containing silanol groups;

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

[0042] (3) Disperse 0.1 g of graphene oxide powder in 100 ml of deionized water, and perform ul...

Example Embodiment

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

[0046] Proceed as follows:

[0047] (1) Take 10g of silica gel and 100mL of 37% hydrochloric acid, mix the two evenly, stand for 24 hours to acidify, then separate the silica gel, wash with distilled water to neutrality, and finally vacuum dry at 120°C for 24 hours to obtain the surface 10g of silica gel containing silanol groups;

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

[0049] (3) Disperse 0.02 g of graphene oxide powder in 100 ml of deionized water, and perform u...

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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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