Preparation method of styrene-divinylbenzene-carbon nanometer tube copolymerization chromatograph packing material
A technology of divinylbenzene and carbon nanotubes, which is applied in the direction of microsphere preparation, chemical instruments and methods, microcapsule preparations, etc., can solve the problems affecting the overall properties of chromatographic packing, carbon nanotubes are not stable enough, and the amount of doping is limited. , to achieve the effect of strong tolerance, low cost and large amount of doping
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Embodiment 1
[0026] The production process of styrene-divinylbenzene-carbon nanotube copolymer chromatographic filler is as follows, and its steps are:
[0027] 1. Synthesize monodisperse polystyrene seeds with a particle size of 0.8 to 3 μm by dispersion polymerization, the concentration of monomeric styrene is 5 to 40% (m / m) of the total amount, and the amount of stabilizer polyvinylpyrrolidone is the reaction medium 0.5-4% (g / 100mL), the amount of initiator azobisisobutyronitrile is 0.5-5% (m / m) of the monomer amount, the reaction medium is ethanol aqueous solution, and the concentration is 70-95% (v / v ), the reaction temperature is 50-75°C, the stirring speed is 150-400 rpm, and the reaction time is 8-24 hours.
[0028] 2. Secondly, the multi-walled carbon nanotubes are reacted with allyl alcohol to couple double bonds through esterification. The amount of multi-walled carbon nanotubes is 50-500 mg, dispersed in 100-300 mL of concentrated sulfuric acid and concentrated nitric acid mix...
Embodiment 2
[0034] With reference to the method and steps of embodiment 1
[0035] 1. First synthesize 1.7 μm monodisperse polystyrene seeds by dispersion polymerization, the concentration of monomer styrene is 20%, the amount of stabilizer polyvinylpyrrolidone is 2%, the amount of initiator azobisisobutyronitrile is 3%, and the reaction The medium is 90% ethanol aqueous solution, the reaction temperature is 80° C., the stirring speed is 400 rpm, and the reaction time is 24 hours.
[0036] 2. At the same time, 50 mg of multi-walled carbon nanotubes were treated with 200 mL of mixed acid, ultrasonicated at 35° C. for 8 hours, washed until neutral and then dried. Add 200 mL of thionyl chloride to reflux at 80°C for 4 hours, remove the solvent, add 100 mL of allyl alcohol dropwise, stir magnetically at 50°C for 6 hours, wash with water until neutral to obtain esterified multi-walled carbon nanotubes.
[0037] 3. Then prepare monodisperse polystyrene-divinylbenzene-carbon nanotube composite ...
Embodiment 3
[0042] (1) Synthesize 1.8 μm monodisperse polystyrene seed by dispersion polymerization method earlier, monomer concentration is 20%, stabilizer consumption is 1.5%, initiator consumption is 2%, reaction medium is 95% ethanol aqueous solution, reaction temperature 70 °C, the stirring speed was 250 rpm, and the reaction time was 24 hours.
[0043] (2) 50 mg of multi-walled carbon nanotubes were oxidized with 200 mL of mixed acid, ultrasonicated at 35° C. for 10 hours, washed until neutral and then dried. Add 100 mL of thionyl chloride to reflux at 80°C for 6 hours, remove the solvent, add 150 mL of allyl alcohol dropwise, stir magnetically at 55°C for 6 hours, wash with water until neutral to obtain esterified multi-walled carbon nanotubes.
[0044] (3) Then, monodisperse polystyrene-divinylbenzene-carbon nanotube composite microspheres with a crosslinking degree of 55% were prepared by the seed swelling method. The monomer concentration is 10%, the content of carbon nanotubes...
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