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

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

Example Embodiment

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

[0025] 5ml GMA, 0.10g azobisisobutyronitrile, 1.25g PVP and 50ml absolute ethanol were added to a 100ml flask, and the solution was fully dissolved by ultrasonic 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 30 hours of reaction, the product is left to settle and the supernatant liquid is poured out. The sediment was washed with absolute ethanol and settled three times. Wash with secondary water and settle for three times to obtain the polyglycidyl methacrylate microspheres provided by the present invention, which are stored in a PVA aqueous solution and dispersed into a 0.1 g / ml homogenate state.

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

Example Embodiment

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

[0028] 5ml GMA, 0.15g azobisisobutyronitrile, 0.5g PVP and 50ml absolute ethanol were added to the 100ml flask, and the solution was fully dissolved by ultrasonic 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 75°C. After 12 hours of reaction, the product is left to settle and the supernatant liquid is poured off. The sediment was washed with absolute ethanol and settled three times. Wash with secondary water and settle for three times to obtain the polyglycidyl methacrylate seed microspheres provided by the present invention, which are stored in a PVA aqueous solution and dispersed into a 0.1 g / ml homogenate state.

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

Example Embodiment

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

[0031] 5ml GMA, 0.15g azobisisobutyronitrile, 0.5g PVP, 2.5ml toluene and 47.5ml absolute ethanol were added to a 100ml flask, and the solution was fully dissolved by ultrasonic 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 24 hours of reaction, centrifuge at 3000 rpm to settle the product microspheres, and pour off the supernatant. The sediment was washed with absolute ethanol and settled three times. The polyglycidyl methacrylate seed microspheres provided by the present invention are obtained by washing and settling three times with secondary water, which are stored in a PVA aqueous solution and dispersed into a 0.1 g / ml homogenate state.

[0032] The diameter of the polyglycidyl methacrylate seed microspheres observed by optical microscope was...

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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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