A green synthesis method for carbon quantum dot bonded silica gel chromatography filler

A technology of carbon quantum dots and chromatographic packing, which is applied in the field of green synthesis of carbon quantum dot-bonded silica gel chromatographic packing. The effect of combining the amount and avoiding the use of organic reagents

Inactive Publication Date: 2017-01-04
LANZHOU INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0002] Due to their unique physical and chemical properties, carbon quantum dots are widely used in bioimaging, sensing, drug / gene carriers, catalysis, and optoelectronic devices. However, the preparation of carbon quantum dot-bonded chromatographic stationary phases has not been reported yet.

Method used

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  • A green synthesis method for carbon quantum dot bonded silica gel chromatography filler
  • A green synthesis method for carbon quantum dot bonded silica gel chromatography filler
  • A green synthesis method for carbon quantum dot bonded silica gel chromatography filler

Examples

Experimental program
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Effect test

Embodiment 1

[0039] Preparation of Carbon Quantum Dots Bonded Silica Gel Chromatographic Packing (Sil-NCDs (DES))

[0040] Steps:

[0041] ① First, weigh the solid powder of aconitic acid and tryptophan according to the molar ratio of 1:2, mix and grind them evenly, place them in a reaction kettle at 200 °C for 6 h, and dissolve the obtained solids in water, centrifuge, and freeze-dry to obtain Amino functionalized carbon quantum dots (NCDs);

[0042] ② Disperse 0.02 g NCDs in DES, add 0.47 g GPTMS, 2 Stir the reaction at 60°C for 24h under protection;

[0043] ③ Add 1 g of silica gel (SiO 2 ), at N 2 Under protection, the stirring reaction was continued at 60 °C for 24 h;

[0044] ④ After the reaction, the prepared chromatographic material was alternately washed with water and absolute ethanol several times, and then dried in a vacuum oven for 12 h.

Embodiment 2

[0046] Preparation of carbon quantum dot-bonded silica gel packing (Sil-NCDs (DMF))

[0047] Steps:

[0048] ① First, weigh the solid powder of aconitic acid and tryptophan according to the molar ratio of 1:2, mix and grind them evenly, place them in a reaction kettle at 200 °C for 6 h, and dissolve the obtained solids in water, centrifuge, and freeze-dry to obtain Amino functionalized carbon quantum dots (NCDs);

[0049] ② Disperse 0.02 g NCDs in DMF, add 0.47 g GPTMS, 2 Stir the reaction at 60°C for 24h under protection;

[0050] ③ Add 1 g of silica gel (SiO 2 ), at N 2 Under protection, the stirring reaction was continued at 60 °C for 24 h;

[0051] ④ After the reaction, the prepared chromatographic material was alternately washed with water and absolute ethanol several times, and then dried in a vacuum oven for 12 h.

Embodiment 3

[0053] Preparation of Carbon Quantum Dots Bonded Silica Gel Chromatographic Packing (Sil-NCDs (THF))

[0054] Steps:

[0055] ① First, weigh the solid powder of aconitic acid and tryptophan according to the molar ratio of 1:2, mix and grind them evenly, place them in a reaction kettle at 200 °C for 6 h, and dissolve the obtained solids in water, centrifuge, and freeze-dry to obtain Amino functionalized carbon quantum dots (NCDs);

[0056] ② Disperse 0.02 g NCDs in THF, add 0.47 g GPTMS, 2 Stir the reaction at 60°C for 24h under protection;

[0057]③ Add 1 g of silica gel (SiO 2 ), at N 2 Under protection, the stirring reaction was continued at 60 °C for 24 h;

[0058] ④ After the reaction, the prepared chromatographic material was alternately washed with water and absolute ethanol several times, and then dried in a vacuum oven for 12 h.

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Abstract

This invention has discloses a green synthesis method for carbon quantum dot bonded silica gel chromatography filler, which comprises the concrete steps of: mixing the solid powder of aconitic acid and tryptophan to be ground evenly, letting the mixture react under the temperature of 180oC- 200oC for 3 - 6 hours. Through dissolution, centrifugation and freeze drying of the generated solid, the amino-functionalized carbon quantum dots (NCDs) are obtained; After that, NCDs are dispersed in DES and added with gamma-glycidoxypropyl trimethoxy siloxane(GPTMS). Under the protection of N2 and the temperature of 55oC- 65oC, the mixture is stirred to react for 22 - 25 hours, then the silica gel (SiO2) is added to react for another 12 - 48 hours. Water and absolute ethyl alcohol are alternatively used to wash the raw product generated from the reaction. Silica gel chromatography filler modified by carbon quantum dots will be generated after drying. This green synthesis method realizes the surface bond of carbon quantum dots and silica gel through epoxy group and amino. DES used in the process of reaction is reaction solvent, which serves as an excellent dispersing agent for carbon quantum dots and silica gel, ensures higher bonded amount, and at the same time, meets the requirements of green chemistry.

Description

technical field [0001] The invention relates to a green synthesis method of carbon quantum dot-bonded silica gel chromatographic packing, specifically a kind of reaction medium of deep eutectic solvent (DES), which is prepared by reacting carbon quantum dots with silylating reagents and silica gel Green synthesis of carbon quantum dot-modified silica gel chromatography packing materials (Sil-NCDs). Background technique [0002] Due to their unique physical and chemical properties, carbon quantum dots are widely used in bioimaging, sensing, drug / gene carriers, catalysis, and optoelectronic devices. However, the preparation of carbon quantum dot-bonded chromatographic stationary phases has not been reported yet. Contents of the invention [0003] The object of the present invention is to provide a green synthesis method of carbon quantum dot-bonded silica gel chromatographic filler. [0004] A green synthesis method of carbon quantum dot bonded silica gel chromatographic fi...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J20/286B01J20/22B01J20/30B01D15/08G01N30/02
CPCB01J20/286B01D15/08B01J20/103B01J20/22G01N30/02
Inventor 张海娟邱洪灯
Owner LANZHOU INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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