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Capillary electrochromatographic monolithic column modified with single-walled carbon nanohorns and preparation method thereof

A technology of single-walled carbon nanohorns and capillary electrochromatography, which is applied in separation methods, chemical instruments and methods, and other chemical processes, to achieve simple preparation processes, controllable reaction conditions, and ideal preparation effects

Inactive Publication Date: 2018-08-24
HANGZHOU NORMAL UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

So far, the application of carbon nanohorns in analytical chemistry has mainly focused on electrochemical sensors and adsorbents, and the application of carbon nanohorns directly as separation functional groups has not been reported yet.

Method used

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  • Capillary electrochromatographic monolithic column modified with single-walled carbon nanohorns and preparation method thereof
  • Capillary electrochromatographic monolithic column modified with single-walled carbon nanohorns and preparation method thereof
  • Capillary electrochromatographic monolithic column modified with single-walled carbon nanohorns and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] Preparation of monolithic columns for capillary electrochromatography modified with single-walled carbon nanohorns

[0033] (1) Weigh 15 mg of single-walled carbon nanohorns to a test tube, add 30 mL of styrene, 25KHz ultrasonic treatment for 2.5 h to uniformly disperse the single-walled carbon nanohorns in styrene, and obtain a styrene dispersion of single-walled carbon nanohorns ( figure 1 is a TEM image of a styrene dispersion of single-walled carbon nanohorns).

[0034] (2) Weigh the styrene dispersion of single-walled carbon nanohorns (50 μL, 45.56 mg) obtained in step (1) and add it to 450 μL cyclohexanol (432 mg), and sonicate at 25 KHz for 2.5 h until the dispersion is uniform. Then DVB (50 μL, 45.95 mg), toluene (225 μL, 194.85 mg), AIBN (1.8 mg) and AMPS (0.9 mg) were added, and ultrasonic dispersion was continued at 25 KHz for 35 min, followed by nitrogen gas for 15 min to obtain a reaction mixture.

[0035] (3) Use a syringe to inject the reaction mixture o...

Embodiment 2

[0037] Preparation of monolithic columns for capillary electrochromatography modified with single-walled carbon nanohorns

[0038] (1) Weigh 15 mg of single-walled carbon nanohorns into a test tube, add 30 mL of styrene, and conduct ultrasonic treatment at 25 KHz for 2.5 hours to uniformly disperse the single-walled carbon nanohorns in styrene to obtain a styrene dispersion of single-walled carbon nanohorns.

[0039] (2) Weigh the styrene dispersion of single-walled carbon nanohorns obtained in step (1) (50 μL, 45.56 mg) and add it to 400 μL of cyclohexanol (384 mg), and sonicate at 25 KHz for 2.5 h until the dispersion is uniform. Then add DVB (100 μL, 91.9 mg), toluene (200 μL, 173.2 mg), AIBN (2 mg) and AMPS (1 mg), continue ultrasonic dispersion at 25 KHz for 35 min, and then blow nitrogen gas for 15 min to obtain a reaction mixture.

[0040] (3) Use a syringe to inject the reaction mixture obtained in step (2) into the pretreated 45cm capillary, and control the liquid inj...

Embodiment 3

[0042] Preparation of monolithic columns for capillary electrochromatography modified with single-walled carbon nanohorns

[0043] (1) Weigh 15 mg of single-walled carbon nanohorns into a test tube, add 30 mL of styrene, and conduct ultrasonic treatment at 25 KHz for 2.5 hours to uniformly disperse the single-walled carbon nanohorns in styrene to obtain a styrene dispersion of single-walled carbon nanohorns.

[0044] (2) Weigh the styrene dispersion of single-walled carbon nanohorns obtained in step (1) (50 μL, 45.56 mg) into 300 μL of cyclohexanol (288 mg), and sonicate at 25 KHz for 2.5 h until the dispersion is uniform. Then DVB (200 μL, 183.8 mg), toluene (150 μL, 129.9 mg), AIBN (2.2 mg) and AMPS (1.1 mg) were added, and ultrasonic dispersion was continued at 25 KHz for 35 min, followed by nitrogen gas for 15 min to obtain a reaction mixture.

[0045] (3) Use a syringe to inject the reaction mixture obtained in step (2) into the pretreated 45cm capillary, and control the ...

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Abstract

A capillary electrochromatography monolithic column modified with single wall carbon nanohorns is provided. A preparing method of the capillary electrochromatography monolithic column includes mixing the single wall carbon nanohorns with styrene, performing ultrasonic dispersing to obtain a styrene dispersion of the single wall carbon nanohorns, mixing the dispersion with cyclohexanol, adding divinylbenzene, toluene, a radical initiator and 2-acrylamido-2-methylpropane sulfonic acid after ultrasonic dispersing, continuously ultrasonic dispersing, feeding nitrogen to obtain a reaction mixture liquid, introducing the reaction mixture liquid into a preset stationary phase position in a pretreated capillary, sealing ports at two ends of the capillary with silica gel, solidifying at 40-100 DEG C for 2-8 h, and subjecting the capillary to after-treatment to obtain the capillary electrochromatography monolithic column. The single wall carbon nanohorns are applied into the capillary electrochromatography monolithic column for the first time, and a preparing process is simple, few in steps, controllable in reaction conditions and ideal in preparing effects.

Description

(1) Technical field [0001] The invention relates to a capillary electrochromatographic monolithic column and a preparation method thereof, in particular to a capillary electrochromatographic monolithic column modified by single-wall carbon nanohorns and a preparation method thereof. (2) Background technology [0002] Single-Walled Carbon Nanohorns (SWNHs) is lijima (lijima et al., Chemical Physics Letters, 309 (1999) 165) at room temperature with CO 2 Made and named by laser ablation method. SWNHs is a new type of nanomaterial with a closed cone at one end (cone angle about 20°), and the rest is similar to single-walled carbon nanotubes (SWNTs). Since its discovery in 1999, it has attracted the attention of researchers due to its unique structure. The diameter of a single SWNHs is 2-5nm, and the length is 20-50nm. In the normal state, about 2000 single SWNHs gather together to form spherical particles with a diameter of about 100nm. [0003] SWNHs have many unique propert...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J20/286B01D15/38B01D15/22
CPCB01D15/22B01D15/3885B01J20/286B01J2220/84B01J2220/86
Inventor 王园朝赵红岩程和勇
Owner HANGZHOU NORMAL UNIVERSITY
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