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Diplopore nanoscale poly(glycidyl methacrylate)-ethylene glycol dimethacrylate (PGMA-EDMA) cross-linked microballoons and preparation method thereof

A technology of polyglycidyl methacrylate and ethylene glycol diester of methacrylate is applied to double-porous micron-scale polyglycidyl methacrylate-ethylene glycol diester cross-linked microspheres and In the field of preparation, it can solve the problems of residual hydrophobicity, high cost, unfavorable separation of biological macromolecules, etc., and achieve the effects of avoiding non-specific adsorption, improving separation load, and good chemical stability.

Inactive Publication Date: 2012-08-01
INST OF CHEM CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

From the above preparation process, it can be seen that the preparation process is complex, the yield is low, the cost is high, and it is difficult to prepare high-efficiency media with fine particle size and uniform particle size.
Sun Yan et al. (Chinese invention patents 200410019065.7, 200510013278.3) used an inorganic particle-organic solvent combined porogen method to prepare ultra-large porous microspheres, but the microspheres were obtained by suspension polymerization, and the particle size was large and unevenly distributed. Not conducive to efficient separation
Ma Guanghui and others have prepared PS-DVB and PGMA-EDMA microspheres with super large pores by the suspension polymerization method by adding a high content of surfactant in the oil phase (Chinese invention patent 200510087138.0), which also has a large particle size. and the problem of uneven distribution
Gong Bolin used linear polystyrene microspheres as seeds and prepared micron-sized non-porous monodisperse PGMA microspheres by swelling polymerization method (Chinese invention patent 200510119523.9). However, it will have residual hydrophobicity, which is not conducive to the separation of biomacromolecules
To sum up, the preparation of all-PGMA microspheres with micron-scale fine particle size, uniform particle size and ultra-large pores has not yet formed a proprietary technology.

Method used

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  • Diplopore nanoscale poly(glycidyl methacrylate)-ethylene glycol dimethacrylate (PGMA-EDMA) cross-linked microballoons and preparation method thereof
  • Diplopore nanoscale poly(glycidyl methacrylate)-ethylene glycol dimethacrylate (PGMA-EDMA) cross-linked microballoons and preparation method thereof
  • Diplopore nanoscale poly(glycidyl methacrylate)-ethylene glycol dimethacrylate (PGMA-EDMA) cross-linked microballoons and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] Example 1, Preparation of linear 1 μm polyglycidyl methacrylate seed microspheres

[0025] Add 5ml of GMA, 0.10g of azobisisobutyronitrile, 1.25g of PVP and 50ml of absolute ethanol into a 100ml flask, and ultrasonically dissolve it for 10min to form a homogeneous solution. Nitrogen was introduced to remove the oxygen in the system. Rotate and heat in a constant temperature oil bath at 70°C. After 30 hours of reaction, the product settles and the supernatant is discarded. The precipitate was washed with absolute ethanol and settled three times. Then washed with secondary water and settled three times to obtain polyglycidyl methacrylate microspheres provided by the present invention, stored in PVA aqueous solution, and dispersed into a 0.1 g / ml homogeneous state.

[0026] The diameter of polyglycidyl methacrylate seed microspheres observed by scanning electron microscope was 1 μm, and the diameter was uniform.

Embodiment 2

[0027] Example 2, Preparation of linear 2.5 μm polyglycidyl methacrylate seed microspheres

[0028] Add 5ml of GMA, 0.15g of azobisisobutyronitrile, 0.5g of PVP and 50ml of absolute ethanol into a 100ml flask, and ultrasonically dissolve it for 10min to form a homogeneous solution. Nitrogen was introduced to remove the oxygen in the system. Rotate and heat in a constant temperature oil bath at 75°C. After 12 hours of reaction, the product settles and the supernatant is discarded. The precipitate was washed with absolute ethanol and settled three times. Then washed with secondary water and settled three times to obtain polyglycidyl methacrylate seed microspheres provided by the present invention, stored in PVA aqueous solution, and dispersed into a 0.1 g / ml homogeneous state.

[0029] The diameter of polyglycidyl methacrylate seed microspheres observed by optical microscope was 2.5 μm, and the pore size was uniform.

Embodiment 3

[0030] Example 3, Preparation of linear low molecular weight 3.5 μm polyglycidyl methacrylate seed microspheres

[0031] Add 5ml of GMA, 0.15g of azobisisobutyronitrile, 0.5g of PVP, 2.5ml of toluene and 47.5ml of absolute ethanol into a 100ml flask, and ultrasonically dissolve it for 10min to form a homogeneous solution. Nitrogen was introduced to remove oxygen in the system. Rotate and heat in a constant temperature oil bath at 70°C. After reacting for 24 hours, centrifuge at 3000rpm to settle the product microspheres, and pour off the supernatant. The precipitate was washed with absolute ethanol and settled three times. Then washed and settled three times with secondary water to obtain polyglycidyl methacrylate seed microspheres provided by the present invention, stored in PVA aqueous solution, and dispersed into a 0.1 g / ml homogeneous state.

[0032] The diameter of polyglycidyl methacrylate seed microspheres was 3.5 μm and the pore size was uniform according to optical ...

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Abstract

The invention discloses diplopore nanoscale poly(glycidyl methacrylate)-ethylene glycol dimethacrylate (PGMA-EDMA) cross-linked microballoons and a preparation method thereof. The diplopore nanoscale PGMA-EDMA cross-linked microballoons have ultra-macroporous and mesoporous double structures uniformly arranged in the interiors and the exteriors of the diplopore nanoscale PGMA-EDMA cross-linked microballoons, diameters of 3 to 20 micrometers, dispersion coefficients of 2.5 to 5%, ultra-macroporous diameters of 200 to 600 nanometers and mesoporous diameters of 30 to 60 nanometers. The preparation method has the advantages that linear PGMA seeds obtained by dispersion polymerization and having uniform aperture sizes are utilized as templates and undergo a one-step swelling polymerization reaction, wherein formation and distribution of diameters are adjusted by a binary pore-foaming system and a phase-separation technology, and thus the diplopore nanoscale PGMA-EDMA cross-linked microballoons which are all-poly(glycidyl methacrylate) (PGMA-EDMA) microballoons having ultra-macroporous and mesoporous double structures, uniform aperture sizes and good biocompatibility are obtained. Therefore, the preparation method realizes high-efficiency, rapid and high-flux biochemical separation analysis.

Description

technical field [0001] The invention relates to a double-hole micron polyglycidyl methacrylate-ethylene glycol diester methacrylate crosslinked microsphere and a preparation method thereof. Background technique [0002] Since the 1980s, research on microspherical biomacromolecular separation media with high efficiency, high throughput, rapidity, and high biocompatibility has mainly focused on two directions. One is the preparation of uniform particle size or even monodisperse fillers; the other is the construction of dual-porous media with penetrating ultra-large pore structure and mesopore structure. [0003] Flow chromatography medium is a new type of high-performance liquid chromatography stationary phase developed in the 1990s. It has a unique dual-pore structure, which has not only the usual micropores or macropores, but also a diameter of about 600- 800nm ​​ultra-large pores. The mass transfer process has changed from diffusion control to convection control, and the ...

Claims

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Application Information

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IPC IPC(8): C08F265/04C08F220/32C08F222/14C08J9/28
Inventor 赵睿刘吉众黄嫣嫣刘国诠
Owner INST OF CHEM CHINESE ACAD OF SCI
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