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Preparation method of monodisperse porous polymer microspheres

A porous polymer, monodisperse technology, applied in the field of polymer materials, can solve the problems of low adsorption capacity, unfavorable chromatographic packing application, small surface area of ​​microspheres, etc.

Active Publication Date: 2021-03-19
UNIV OF JINAN
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, this method uses a single solvent system, and the obtained microspheres have a small surface area and low adsorption capacity, which is not conducive to the application in chromatographic packing.

Method used

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  • Preparation method of monodisperse porous polymer microspheres
  • Preparation method of monodisperse porous polymer microspheres

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] A method for preparing micron-scale monodisperse porous polymer microspheres, comprising the following steps:

[0030] Add 4.08 ml of divinylbenzene monomer, 0.96 ml of glycidyl methacrylate and 0.38 g of azobisisobutyronitrile to 27.24 ml of acetonitrile and 2.72 ml of toluene. After mixing, add to the polytetrafluoroethylene in the stainless steel reactor In the inner liner, nitrogen gas was introduced for 15 minutes, after removing oxygen, and then sealed; then placed in an oil bath, the temperature of the oil bath was set at 85°C, and the reaction time was 4 hours; the heating was stopped, washed with 50 ml of ethanol, and dried at 50°C to The polymer microspheres were obtained after constant weight. The average particle size was measured to be 5.26 µm, the polydispersity coefficient was 1.07, the yield was 66.9%, and the surface area (determined by nitrogen adsorption method) was 357.8 m 2 / g.

Embodiment 2

[0032] A method for preparing micron-scale monodisperse porous polymer microspheres, comprising the following steps:

[0033] 3.70 ml of divinylbenzene monomer and 0.87 ml of glycidyl methacrylate and 0.35 g of azobisisobutyronitrile were added to 28.92 ml of acetonitrile and 1.52 ml of tetrahydrofuran. After mixing, they were added to the polytetrafluoroethylene in the stainless steel reactor In the inner liner, nitrogen gas was introduced for 15 minutes, after removing oxygen, and then sealed; then placed in an oil bath, the temperature of the oil bath was set at 85°C, and the reaction time was 4 hours; the heating was stopped, washed with 50 ml of ethanol, and dried at 50°C to The polymer microspheres were obtained after constant weight. The average particle size was measured to be 5.13 µm, the polydispersity coefficient was 1.05, and the yield was 64.4%; the surface area (determined by nitrogen adsorption method) was 434.4 m 2 / g.

Embodiment 3

[0035] A method for preparing micron-scale monodisperse porous polymer microspheres, comprising the following steps:

[0036] 4.06 ml of divinylbenzene monomer and 0.95 ml of glycidyl methacrylate and 0.38 g of azobisisobutyronitrile were added to 27.27 ml of acetonitrile and 2.73 ml of propanol. In the ethylene liner, flow nitrogen for 15 minutes, remove oxygen, and seal; then place in an oil bath, the temperature of the oil bath is set at 85°C, and the reaction time is 4 hours; stop heating, wash with 50 ml of ethanol, and dry at 50°C Polymer microspheres were obtained after reaching constant weight. The average particle size was measured to be 6.13 µm, the polydispersity coefficient was 1.05, the yield was 50.6%, and the surface area (determined by nitrogen adsorption method) was 262.5 m 2 / g.

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Abstract

The invention relates to a preparation method of micron-sized monodisperse porous polymer microspheres. According to the method, the micron-sized monodisperse porous polymer microspheres are obtainedby conducting polymerization on glycidyl methacrylate serving as a monomer and divinyl benzene serving as a crosslinking agent, wherein the particle size of the microsphere is 2-10 [mu]m, the polydispersity index is 1.01-1.05, and the surface area of the microsphere is controllable between 2-500 m<2> / g. The preparation method comprises the following steps: adding an olefin monomer, divinyl benzeneand an initiator into a binary solvent system consisting of acetonitrile and tetrahydrofuran, conducting uniform mixing, putting the mixture into a stainless steel reaction kettle, introducing nitrogen, conducting sealing, conducting heating for polymerizing in an oil bath under the conditions that the reaction temperature is controlled to be 82-90 DEG C and the reaction time is controlled to be3-5 hours, and washing and drying the obtained reaction product to obtain the product. The obtained micron-sized microspheres are monodisperse in particle size, high in surface area and high in mechanical strength; and the method has the advantages of simple preparation process, safe and reliable reaction conditions, quick reaction, short consumed time, high solid content, environment-friendly preparation process and easiness in industrial production.

Description

technical field [0001] The invention relates to a preparation method of micron-scale monodisperse porous polymer microspheres, belonging to the technical field of polymer materials. Background technique [0002] Monodisperse polymer microspheres refer to spherical polymer materials with highly uniform particle size. Monodisperse polymer microspheres can be used as the core component of high performance liquid chromatography-the packing of liquid chromatography columns, which can realize rapid analysis and industrial-scale purification and separation of target molecules such as organic compounds, natural products, proteins, and peptides. Compared with silica-based fillers, the polymer microsphere matrix has the advantages of a wide range of pH tolerance, low non-specific adsorption and easy surface modification. [0003] Precipitation polymerization is currently the only method that does not require any additives to prepare micron-sized monodisperse polymer microspheres. It...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F212/36C08F220/32C08F220/14C08F220/06C08F220/20C08J9/28
CPCC08F212/36C08J9/286C08J2325/02C08F220/325
Inventor 王艳艳郭峰豪丁园园陈志勇
Owner UNIV OF JINAN