Method for preparation of composite chromatographic stuffing of polymer carbon nanometer tube

A carbon nanotube composite and chromatographic filler technology is applied in the field of preparation of polymer carbon nanotube composite high-performance liquid chromatography columns, and can solve the problems of low rigidity of organic matrix fillers, non-specific irreversible adsorption, and easy expansion and contraction. , to achieve the effect of low cost, narrow particle size distribution and enhanced hardness

Inactive Publication Date: 2009-08-26
ZHEJIANG UNIV
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Problems solved by technology

[0003] In order to overcome the disadvantages of poor chemical stability, acid and alkali resistance, non-specific and irreversible adsorption of inorganic matrix fillers, low rigidity of organic matrix fillers, complex pore structure, and easy expansion and contraction, the invention provides a low-cost, manufacturing Preparation method of novel polymer carbon nanotube composite chromatographic filler with simple process, excellent performance and long service life

Method used

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  • Method for preparation of composite chromatographic stuffing of polymer carbon nanometer tube
  • Method for preparation of composite chromatographic stuffing of polymer carbon nanometer tube
  • Method for preparation of composite chromatographic stuffing of polymer carbon nanometer tube

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Embodiment 1

[0023] Embodiment 1: the making process of polymer carbon nanotube composite chromatographic filler is as follows, and its steps are:

[0024] 1. Synthesize monodisperse polystyrene seeds with a particle size of 1 to 3 μm by dispersion polymerization, the concentration of monomeric styrene is 5 to 30% (m / m) of the total amount, and the amount of stabilizer polyvinylpyrrolidone is the reaction medium 0.5-4% (m / v), the amount of initiator azobisisobutyronitrile is 1-5% (m / m) of the monomer amount, the reaction medium is ethanol aqueous solution, and the concentration is 75-100% (v / v ), the reaction temperature is 40-85° C., the stirring speed is 100-400 rpm, and the reaction time is 8-24 hours.

[0025] 2. Then prepare monodisperse polystyrene-divinylbenzene-carbon nanotube composite microspheres with a crosslinking degree of 10-75% by seed swelling method. The concentration of monomer styrene is 10-20% (m / m) of the total organic phase, and the range of cross-linking degree of ...

Embodiment 2

[0030] With reference to the method and steps of embodiment 1

[0031] 1. First synthesize 1.8 μm monodisperse polystyrene seeds by dispersion polymerization, the concentration of monomer styrene is 20%, the amount of stabilizer polyvinylpyrrolidone is 1.5%, and the amount of initiator azobisisobutyronitrile is 2%. The medium is 95% ethanol aqueous solution, the reaction temperature is 80° C., the stirring speed is 400 rpm, and the reaction time is 24 hours.

[0032] 2. At the same time, the carbon nanotubes were treated with hydrogen peroxide, and then monodisperse polystyrene-divinylbenzene-carbon nanotube composite microspheres with a crosslinking degree of 55% were prepared by the seed swelling method, and the monomer styrene concentration was 12%. The content of carbon nanotubes accounts for 0.5% of monomer styrene, the amount of emulsifier sodium lauryl sulfate is 2%, the amount of stabilizer polyvinyl alcohol is 1%, and the amount of initiator benzoyl peroxide is 0.5%. ...

Embodiment 3

[0038] (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 80 °C, the stirring speed was 400 rpm, and the reaction time was 24 hours.

[0039] (2) The carbon nanotubes were oxidized with nitric acid, and then the 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 accounts for 0.8% of the monomer, the amount of emulsifier is 2.8%, the amount of stabilizer is 1%, the amount of initiator is 0.5%, the amount of porogen is 60%, and the swelling ratio 50, the emulsification temperature is 20°C, the reaction temperature is 75°C, the stirring speed is 300 rpm, and the reaction time is 48 hours.

[0040] (3) The co...

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Abstract

The invention provides a method for the preparation of the composite chromatographic stuffing of the polymer carbon nanometer tube, comprising: taking polystyrene-divinylbenzene and carbon nanometer tube as the base material, adopting the dispersion polymerization method to prepare monodispersity linear polystyrene microsphere seed, activating the feed, taking uni-step seed swell method to prepare the polystyrene-divinylbenzene and carbon nanometer tube composite microsphere, extracting to remove the pore-foaming agent to obtain the chromatographic stuffing, packing column by the uniform method. The stuffing prepared by the method has uniform granularity without screening and enhanced hardness compared with the traditional polymer chromatographic stuffing, can bear bigger pressure and is suitable for the new UPLC. The obtained polystyrene-divinylbenzene and carbon nanometer tube liquid phase chromatographic column can be stably used for the ion-pair chromatograph for along time and better performs the simultaneous separation of over ten organic acids.

Description

technical field [0001] The invention relates to a high performance liquid chromatography column and a preparation method thereof, in particular to a preparation method of a polymer carbon nanotube composite high performance liquid chromatography column. Background technique [0002] High-performance liquid chromatography is currently one of the most widely used and fastest-growing branches in the field of chromatographic analysis. Because of its high pressure, high speed, high efficiency, and high sensitivity, it is widely used in the environment, medicine, food, energy, materials, and life sciences. It can realize the separation and analysis of various organic and inorganic compounds and biomolecules. As with all chromatographic methods, columns are at the heart of HPLC separations. Common HPLC packings are generally divided into two categories: organic matrix packing and inorganic matrix packing. The most widely used inorganic matrix fillers are silica gel and bonded pha...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J20/281B01J20/30B01J13/02
Inventor 钟莺莺朱岩
Owner ZHEJIANG UNIV
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