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Graphene oxide bonding capillary electrochromatography monolithic column and preparing method thereof

A technology of capillary electrochromatography and graphene, which is applied in the field of graphene oxide-bonded capillary electrochromatography monolithic columns and its preparation, can solve the problems of difficult control of conditions and many reaction steps, and achieve controllable reaction conditions, fewer steps, The effect of simple reaction process

Inactive Publication Date: 2016-06-29
HANGZHOU NORMAL UNIVERSITY
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Tong et al. (Tongetal., Analyst138(2013)1549) proposed an in-column in-situ 3-step reaction method to prepare a graphene / graphene oxide bonded enrichment monolithic column, which was not used for separation, although electroosmotic flow can be generated by adding Reactive monomer, extended to monolithic column for electrochromatographic separation, but there are many reaction steps, the acylation reaction occurs in situ in the column, and the conditions are not easy to control

Method used

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  • Graphene oxide bonding capillary electrochromatography monolithic column and preparing method thereof
  • Graphene oxide bonding capillary electrochromatography monolithic column and preparing method thereof
  • Graphene oxide bonding capillary electrochromatography monolithic column and preparing method thereof

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Experimental program
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Effect test

Embodiment 1

[0029] Preparation of Graphene Oxide Bonded Capillary Electrochromatographic Monolithic Column

[0030] (1) Weigh 20 mg of graphene oxide (GO) into a test tube, add 50 mL of N,N-dimethylformamide (DMF), and treat with 25KHz ultrasonic for 2.5 hours to uniformly disperse the graphene oxide in DMF. Then add 200mg of p-aminostyrene (pAS) and 20mg of N,N'-dicyclohexylcarbodiimide (DCC) to the dispersion, put it in a 50℃ oil bath, protected from light, protected by argon, and stirred magnetically Reaction for 24h (reaction formula such as figure 1 ), and filtered to obtain 22 mg of solid product, which was recorded as pAS-GO.

[0031] (2) Weigh 0.20 mg pAS-GO and add it to 450 μL cyclohexanol (432 mg), and sonicate at 25 KHz for 2.5 hours until the dispersion is uniform. Then add styrene (25μL, 22.73mg), DVB (50μL, 45.95mg), toluene (225μL, 194.85mg), AIBN (1.8mg) and AMPS (0.9mg), continue to disperse by 25KHz ultrasonic for 35min and then bubbling with nitrogen for 15min , Get the r...

Embodiment 2

[0033] Preparation of Graphene Oxide Bonded Capillary Electrochromatographic Monolithic Column

[0034] (1) Weigh 20 mg of graphene oxide (GO) into a test tube, add 50 mL of N,N-dimethylformamide (DMF), and treat with 25KHz ultrasonic for 2.5 hours to uniformly disperse the graphene oxide in DMF. Then add 200mg of p-aminostyrene (pAS) and 20mg of N,N'-dicyclohexylcarbodiimide (DCC) to the dispersion, put it in a 50℃ oil bath, protected from light, protected by argon, and stirred magnetically Reaction for 24h (reaction formula such as figure 1 ), and filtered to obtain 22 mg of solid product, which was recorded as pAS-GO.

[0035] (2) Weigh 0.2 mg of pAS-GO and add it to 400 μL of cyclohexanol (384 mg), and sonicate at 25KHz for 2.5 hours until the dispersion is uniform. Then add styrene (50μL, 45.45mg), DVB (100μL, 91.9mg), toluene (200μL, 173.2mg), AIBN (2mg) and AMPS (1mg), continue to disperse by 25KHz ultrasonic for 35min and then bubbling in nitrogen for 15min to obtain Reac...

Embodiment 3

[0037] Preparation of Graphene Oxide Bonded Capillary Electrochromatographic Monolithic Column

[0038] (1) Weigh 20 mg of graphene oxide (GO) into a test tube, add 50 mL of N,N-dimethylformamide (DMF), and treat with 25KHz ultrasonic for 2.5 hours to uniformly disperse the graphene oxide in DMF. Then add 200mg of p-aminostyrene (pAS) and 20mg of N,N'-dicyclohexylcarbodiimide (DCC) to the dispersion, put it in a 50℃ oil bath, protected from light, protected by argon, and stirred magnetically Reaction for 24h (reaction formula such as figure 1 ), and filtered to obtain 22 mg of solid product, which was recorded as pAS-GO.

[0039] (2) Weigh 0.20 mg pAS-GO and add it to 300 μL cyclohexanol (288 mg), sonicate at 25 KHz for 2.5 h until the dispersion is uniform. Then add styrene (100μL, 90.9mg), DVB (200μL, 183.8mg), toluene (150μL, 129.9mg), AIBN (2.2mg) and AMPS (1.1mg), continue to disperse by 25KHz ultrasonic for 35min and then bubbling with nitrogen for 15min , Get the reaction ...

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Abstract

The invention provides a graphene oxide bonding capillary electrochromatography monolithic column. A preparing method of the graphene oxide bonding capillary electrochromatography monolithic column comprises the steps that GO and DMF are mixed and subjected to ultrasonic dispersion, then, pAS and DCC are added, reaction is conducted at the temperature of 40-80 DEG C under the argon protection condition in dark in a stirring mode for 12-48 h, reaction liquid is filtered, and pAS-GO is obtained; the pAS-GO is mixed with cyclohexanol and subjected to ultrasonic dispersion, then, styrene, DVB, methylbenzene, a radical initiator and AMPS are added, ultrasonic dispersion continues to be conducted, nitrogen is injected into the mixture, and reaction mixed liquid is obtained; the obtained reaction mixed liquid is introduced into a position of a preset stationary phase in a preprocessed capillary tube, then, the two ends of the capillary tube are sealed through silica gel, the capillary tube is put at the temperature of 40-100 DEG C to be subjected to curing reaction for 6-24 h, post-processing is conducted on the capillary tube, and the graphene oxide bonding capillary electrochromatography monolithic column is prepared. The reaction process is simple, the number of steps is small, reaction conditions are controllable, and the preparation effect is more ideal.

Description

(1) Technical field [0001] The invention relates to a capillary electrochromatographic monolithic column, in particular to a graphene oxide bonded capillary electrochromatographic monolithic column and a preparation method thereof. (2) Background technology [0002] Graphene (G) is a carbon atom with sp 2 The hybrid orbitals form a two-dimensional hexagonal honeycomb crystal form, and graphene oxide (GO) is obtained by oxidation of graphene. Both have large specific surface area, strong thermal stability, and good electrical conductivity. Compared with G, the surface of GO contains a large number of active groups such as hydroxyl, carboxyl and alkoxy, and has better dispersibility, water solubility and modifiable properties. Because GO has a strong π-π electron accumulation effect, it can be used as an adsorbent for the extraction and enrichment of polycyclic aromatic hydrocarbons and benzene ring-containing substances in samples (Tangetal., J. Am. Chem. Soc. 132 (2010) 10976; ...

Claims

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Application Information

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IPC IPC(8): B01J20/286B01D15/22B01D15/38
CPCB01D15/22B01D15/3885B01J20/286
Inventor 王园朝赵红岩程和勇沈依俐
Owner HANGZHOU NORMAL UNIVERSITY
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