A kind of hydrophilic ultra-macroporous polymer microsphere and preparation method thereof

A polymerization method and linear polymer technology, applied in the field of hydrophilic ultra-macroporous polymer microspheres and their preparation, can solve the problems of poor strength of microspheres

Active Publication Date: 2017-02-08
ZIBO KANGBEI MEDICAL DEVICES
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, although this method of preparing microspheres is convenient, it has certain limitations when used as a chromatographic separation medium due to the absence of crosslinking and poor microsphere strength.

Method used

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  • A kind of hydrophilic ultra-macroporous polymer microsphere and preparation method thereof
  • A kind of hydrophilic ultra-macroporous polymer microsphere and preparation method thereof
  • A kind of hydrophilic ultra-macroporous polymer microsphere and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0058] 1) Synthesis of poly 3-O-methacryloyl-diacetone-D-galactose (PMDAGal) by ATRP reaction

[0059] Add a stirring bar to the Schlenk bottle at room temperature, then add cuprous bromide (6.45mg), N,N,N,N',N'-pentamethyldiethylenetriamine (PMDETA) (9.0mg ), 3-O-methacryloyl-diacetone-D-galactose (MDAGal) (1.52g) and 4ml toluene, after three cycles of liquid nitrogen freezing-pumping-gassing-thawing to remove oxygen. Finally, the initiator 1-bromoethylbenzene (18.3mg) was added, reacted at 60°C for 4h, dissolved the reaction product with chloroform, diluted the reaction product, and removed the catalyst through an aluminum oxide column. The resulting colorless solution was precipitated twice with methanol, filtered with suction at room temperature, and dried in vacuo to obtain 0.79 g of PMDAGal, whose molecular weight Mn=6835 was detected by gel permeation chromatography (GPC).

[0060] 2) Synthesis of poly 3-O-methacryl-diacetone-D-galactose-polystyrene block copolymer (PM...

Embodiment 2

[0068] 1) Synthesis of PMDAGlu by ATRP reaction

[0069] Add a stirring bar to the Schlenk bottle at room temperature, then add cuprous chloride (3.2mg), PMDETA (7.1mg), MDAGlu (0.98g) and 3ml chlorobenzene in sequence, and go through three liquid nitrogen freezing-pumping-gassing -Thaw cycle process, remove oxygen. Finally, the initiator 2-bromoisobutyrate ethyl ester (30.4 mg) was added, reacted at 50°C for 4 hours, dissolved the reaction product with tetrahydrofuran, diluted the reaction product, and removed the catalyst through an aluminum oxide column. The resulting colorless solution was precipitated twice with methanol, filtered with suction at room temperature, and dried in vacuo to obtain 0.59 g of PMDAGlu, whose molecular weight Mn=4631 was detected by gel permeation chromatography (GPC).

[0070] 2) Synthesis of PMDAGlu-PS by ATRP reaction

[0071] Add a stirring bar to the Schlenk bottle at room temperature, then add cuprous bromide (14.6mg), PMDETA (22.8mg), sty...

Embodiment 3

[0078] 1) Synthesis of poly 3-O-methallyl-diacetone-D-glucose (PMAlDAGlu) by AGET-ATRP reaction

[0079] At room temperature, in a 100ml three-neck flask with a stopper, add 4ml of profloxacin, MAlDAGlu (1.42g), FeCl3 (8.4mg), triphenylphosphine (35.4mg), methyl 2-bromopropionate (75.3mg), and stir Make it evenly mixed, pass nitrogen gas to remove oxygen for 10 minutes, add reducing agent ascorbic acid (7.9mg), under nitrogen protection, react at 55°C for 2h, dissolve the reaction product with tetrahydrofuran, precipitate with methanol twice, suction filter at room temperature, and vacuum dry , to obtain 0.49gPMDAGal, the molecular weight Mn=1356 detected by gel permeation chromatography (GPC).

[0080] 2) Synthesis of poly 3-O-methallyl-diacetone-D-glucose-polystyrene block copolymer (PMAlDAGlu-PS) by AGET-ATRP reaction

[0081] Add styrene (2.36g), FeCl 3 (10.8mg), triphenylphosphine (44.96mg), PMAlDAGlu (0.26g), stir to mix evenly, deoxygenate with nitrogen gas for 10 min...

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Abstract

The invention relates to the field of polymer microsphere preparation, in particular to a hydrophilic super-macroporous polymer microsphere and a preparation method thereof. Using self-made amphiphilic diblock macromonomers as surfactants, microspheres were prepared by suspension polymerization. Since the hydrophilic segments will spontaneously arrange on the outer surface of the microspheres facing the water channel during the process of water absorption and swelling, The hydrophobic segment is combined into the microsphere skeleton through the double bond participating in the polymerization reaction, thus realizing the preparation and surface hydrophilic modification of the ultra-macroporous polymer microsphere in one step. The hydrophilic ultra-macroporous polymer microsphere prepared by the present invention has a microsphere skeleton of cross-linked polystyrene, high mechanical strength and good chemical stability, and the outer surface is a sugar-containing polymer or polyvinyl alcohol gel, which is hydrophilic Good and with extra large holes. The hydrophilic ultra-macroporous polymer microsphere has wide application space in the fields of enzyme immobilization and protein rapid separation and purification.

Description

technical field [0001] The invention relates to the field of polymer microsphere preparation, in particular to a hydrophilic super-macroporous polymer microsphere and a preparation method thereof. Background technique [0002] So far, chromatography technology is still an effective means for the efficient separation of biological macromolecules such as proteins and plasmids. Choosing a suitable separation medium is a key factor to ensure separation efficiency. Due to the complex three- and four-level structure of biological macromolecules, large size (protein molecular diameter is usually 1-100nm, and plasmid molecular diameter is between 150-250nm), poor stability and so on. In order to maintain the biological activity of biomacromolecules, it is required to shorten the separation time as much as possible under the premise of ensuring the separation purity, so as to reduce the degree of biomacromolecules being cut by fluid (Perfusive Chromatography, US Patent 5,833,861,199...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08F212/08C08F212/36C08F2/20C08F293/00B01J20/285B01J20/30B01D15/08C12N11/08C07K1/22
CPCY02P20/55
Inventor 曲剑波宦关生邵荟荟刘建国朱虎
Owner ZIBO KANGBEI MEDICAL DEVICES
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