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, limited doping amount, and insufficient stability of carbon nanotubes , to achieve the effect of strong tolerance, large doping amount and low cost

Inactive Publication Date: 2012-11-21
ZHEJIANG UNIV
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Problems solved by technology

The Chinese patent application number is 200910096189.8, which discloses the preparation method of polymer carbon nanotube composite chromatographic filler. Although the experimental method is simple, the doped carbon nanotubes are not stable enough in the composite material, and the doping amount is also limited, affecting Bulk Properties of Chromatographic Packing

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  • Preparation method of styrene-divinylbenzene-carbon nanometer tube copolymerization chromatograph packing material
  • Preparation method of styrene-divinylbenzene-carbon nanometer tube copolymerization chromatograph packing material
  • Preparation method of styrene-divinylbenzene-carbon nanometer tube copolymerization chromatograph packing material

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Experimental program
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Effect test

Embodiment 1

[0026] The manufacturing process of the styrene-divinylbenzene-carbon nanotube copolymer chromatography filler is as follows, and the steps are:

[0027] 1. First, synthesize monodisperse polystyrene seeds with a particle size of 0.8-3 μm by dispersion polymerization method, the concentration of monomer styrene is 5-40% (m / m) of the total amount, and the amount of stabilizer polyvinylpyrrolidone is the amount of the reaction medium. 0.5~4% (g / 100mL), the dosage of initiator azobisisobutyronitrile is 0.5~5% (m / m) of the monomer dosage, the reaction medium is ethanol aqueous solution, 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 the double bonds by the method of esterification. The dosage of multi-walled carbon nanotubes is 50-500 mg, dispersed in 100-300 mL of concentrated sulfuric a...

Embodiment 2

[0034] With reference to the method and steps of Example 1

[0035] 1. Synthesize 1.7 μm monodisperse polystyrene seeds by dispersion polymerization method, 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 rev / min, 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 and reflux at 80°C for 4 hours, remove the solvent, dropwise add 100 mL of allyl alcohol, stir magnetically at 50°C for 6 hours, and wash with water until neutral to obtain esterified multi-walled carbon nanotubes.

[0037] 3. Then, monodispersed polystyrene-divinylbenzene-carbon nanotube composit...

Embodiment 3

[0042] (1) Synthesize 1.8 μm monodisperse polystyrene seeds by dispersion polymerization method, the monomer concentration is 20%, the amount of stabilizer is 1.5%, the amount of initiator is 2%, the reaction medium is 95% ethanol aqueous solution, and the reaction temperature is 70 °C, the stirring speed is 250 rpm, and the reaction time is 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, and wash with water until neutral to obtain esterified multi-walled carbon nanotubes.

[0044] (3) Then, monodispersed polystyrene-divinylbenzene-carbon nanotube composite microspheres with a cross-linking degree of 55% are prepared by a seed swelling method. The monomer concentration is 10%, the content...

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Abstract

The invention relates to a preparation method for a styrene-divinylbenzene-carbon nanometer tube copolymerization chromatograph packing material, comprising three steps of the preparation of seeds, the esterification of a carbon nanometer tube and the packing of the styrene-divinylbenzene-carbon nanometer tube copolymerization chromatograph. Styrene, divinylbenzene and the esterified multi-walledcarbon nanometer tube are taken as raw materials. Monodisperse linear polystyrene microsphere seeds are prepared by adopting a dispersion polymerization method. After the seeds are activated, styrene-divinylbenzene-carbon nanometer tube copolymerization microspheres are synthesized through a one-step seed swelling method. A pore forming agent is removed through extraction, and the obtained chromatograph packing material is packed through a homogenate method. The invention has the advantages of simple preparation process, uniform granularity and no need of screening of the obtained packing material, and strong mechanical performance, heatproof capability and stability, and is suitable for the super-high-pressure liquid chromatograph and the high-temperature liquid chromatograph.

Description

technical field [0001] The invention relates to a high performance liquid chromatography filler and a preparation method thereof, in particular to a preparation method of a polymer carbon nanotube copolymer high performance liquid chromatography filler. Background technique [0002] As an indispensable traditional chromatographic technique, high performance liquid chromatography is widely used in various analytical fields. In order to overcome the shortcomings of traditional chromatography media and combine their advantages, the development of new chromatography media is always a major challenge in the field of chromatography separation science. With the development of science and technology, various new methods and new materials emerge in an endless stream in the field of chromatography. For the former, embedding and coupling techniques are most commonly used in the preparation of novel chromatographic packings, such as polymer-embedded silica gel, polymer-derived silica g...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J20/285B01J20/30B01J13/02
Inventor 钟莺莺朱岩
Owner ZHEJIANG UNIV
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