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Preparation method of poly (ethylene glycol dimethacrylate) microspheres

A technology of poly(ethylene glycol dimethacrylate) microspheres and ethylene glycol dimethacrylate is applied in the field of preparation of poly(ethylene glycol dimethacrylate) microspheres, which can solve the problems of increasing cost and the like, and achieves the The effect of low toxicity, high yield and good thermal stability

Active Publication Date: 2016-01-20
UNIV OF SCI & TECH OF CHINA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] However, the above-mentioned reactions usually use highly toxic organic solvents as the reaction medium, such as acetonitrile, and also need to add initiator or chain transfer agent in the reaction system, which not only increases the cost of synthesis, but also removes the residue of initiator or chain transfer agent. Impurities such as bases are introduced into the microspheres, which limits the application of these preparation methods in the biological field

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  • Preparation method of poly (ethylene glycol dimethacrylate) microspheres
  • Preparation method of poly (ethylene glycol dimethacrylate) microspheres
  • Preparation method of poly (ethylene glycol dimethacrylate) microspheres

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preparation example Construction

[0028] The invention provides a kind of preparation method of poly(ethylene glycol dimethacrylate) microsphere, comprises the following steps:

[0029] A) mixing ethylene glycol dimethacrylate, 4-vinylpyridine, alcohol and water to obtain a mixed solution, the alcohol being methanol and / or ethanol;

[0030] B) irradiating the mixed solution with gamma rays to obtain polyethylene glycol dimethacrylate microspheres.

[0031] The preparation method provided by the invention has low toxicity, environmental friendliness, low cost and few impurities.

[0032] The present invention mixes ethylene glycol dimethacrylate (EGDMA), 4-vinylpyridine (4-vp), alcohol and water to obtain a mixed solution, and the present invention preferably mixes the alcohol and water first to obtain an alcohol-water mixed solution, Then add the ethylene glycol dimethacrylate and comonomer 4-vinylpyridine into the alcohol-water mixed solution to obtain a mixed solution. In the present invention, the volume ...

Embodiment 1

[0046] Add 4 mL of methanol and 1 mL of distilled water into a single-necked round bottom flask with a capacity of 10 mL. Then 0.08 mL of EGDMA and 0.01 mL of 4-Vp were added thereto. At this time, the volume ratio of the monomer to the total reaction system was 1.8%. After passing nitrogen into the system for 10 minutes, the single-necked flask was sealed with a ground vacuum plug and placed in 60 In the Co radioactive source field, under the conditions of magnetic stirring and absorbed dose rate of 83.5Gy / min, after 2 hours of irradiation, the resulting reaction solution was centrifuged with a HC-2518 high-speed centrifuge (8000rpm, 5min), and collected The lower precipitate was dispersed in absolute ethanol, and the dispersion was centrifuged again. The above steps were repeated twice, and the finally collected solid was dried in a GZX-9070MBE electric blast drying oven at 50° C. to a constant weight, and the yield of the reaction was 92.4%.

[0047] The present inventio...

Embodiment 2

[0051] Add 3.5 mL of ethanol and 1.5 mL of distilled water into a single-necked round bottom flask with a capacity of 10 mL. Then 0.08 mL of EGDMA and 0.01 mL of 4-Vp were added thereto. At this time, the volume ratio of the monomer to the total reaction system was 1.8%. After passing nitrogen into the system for 10 minutes, the single-necked flask was sealed with a ground vacuum plug and placed in 60 In the Co radioactive source field, under the conditions of magnetic stirring and absorbed dose rate of 83.5Gy / min, after 2 hours of irradiation, the resulting reaction solution was centrifuged with a HC-2518 high-speed centrifuge (8000rpm, 5min), and collected The lower precipitate was dispersed in absolute ethanol, and the dispersion was centrifuged again. The above steps were repeated twice, and the finally collected solid was dried in a GZX-9070MBE electric blast drying oven at 50° C. to constant weight. The reaction yield was 84.3%.

[0052] The morphology of the resulti...

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Abstract

The invention provides a preparation method of poly (ethylene glycol dimethacrylate) microspheres. The method comprises steps as follows: A), ethylene glycol dimethacrylate, 4-vinyl pyridine, alcohol and water are mixed, a mixed solution is obtained, and the alcohol is methyl alcohol or ethyl alcohol; B), the mixed solution is irradiated by gamma rays, and the poly (ethylene glycol dimethacrylate) microspheres are obtained. According to the preparation method, polymerization of ethylene glycol dimethacrylate monomers is initiated through gamma ray irradiation, an initiator is not required to be added, and impurities brought with initiator residues can be avoided. An alcohol-water solution is taken as a reaction solvent, aftertreatment is not required, and the poly (ethylene glycol dimethacrylate) microspheres have low toxicity and are environment-friendly. The poly (ethylene glycol dimethacrylate) microspheres prepared with the method have excellent monodispersity, higher yield and better heat stability.

Description

technical field [0001] The invention belongs to the field of polymer material synthesis, and in particular relates to a preparation method of polyethylene glycol dimethacrylate microspheres. Background technique [0002] Monodisperse cross-linked polymer microspheres refer to cross-linked polymer particles with a particle size ranging from tens of nanometers to hundreds of microns, uniform particle size distribution, and spherical or other geometric shapes. Monodisperse cross-linked polymer microspheres are widely used in biosensors, drug and catalyst supports, and liquid chromatography column stationary phases due to their high specific surface area and mechanical strength, excellent thermal stability and solvent resistance, and easy recycling and reuse. It is widely used in many fields such as liquid crystal display and so on. For example, polyethylene glycol dimethacrylate (PEGDMA) microspheres with high cross-linking degree synthesized from bifunctional monomer ethylene...

Claims

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Application Information

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IPC IPC(8): C08F222/14C08F226/06C08F2/46C08F2/06C08F6/12
Inventor 汪谟贞陈金星葛学武
Owner UNIV OF SCI & TECH OF CHINA
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