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Hydrophilic super-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: 2015-04-29
ZIBO KANGBEI MEDICAL DEVICES
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

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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  • Hydrophilic super-macroporous polymer microsphere and preparation method thereof
  • Hydrophilic super-macroporous polymer microsphere and preparation method thereof
  • Hydrophilic super-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 stir bar to the Schlenk bottle at room temperature, then add cuprous bromide (6.45mg), N,N,N,N',N'-pentamethyldiethylenetriamine (PMDETA) (9.0mg) in sequence ), 3-O-methacryloyl-diacetone-D-galactose (MDAGal) (1.52g) and 4ml of toluene. After three cycles of liquid nitrogen freezing-pumping-charging-thawing, oxygen is removed. Finally, the initiator 1-bromoethylbenzene (18.3mg) was added and reacted at 60°C for 4 hours. The reaction product was dissolved with chloroform, and the reaction product was diluted and passed through an alumina column to remove the catalyst. The colorless solution obtained was precipitated twice with methanol, filtered under suction at room temperature, and dried in vacuum to obtain 0.79 g of PMDAGal. The molecular weight Mn=6835 was determined by gel permeation chromatography (GPC).

[0060] 2) Synthesis of poly3-O-methacryloyl-diacetone-D-galacto...

Embodiment 2

[0068] 1) Synthesis of PMDAGlu using ATRP reaction

[0069] Add a stir bar to the Schlenk bottle at room temperature, and then add cuprous chloride (3.2mg), PMDETA (7.1mg), MDAGlu (0.98g) and 3ml chlorobenzene in sequence. After three liquid nitrogen freezing-pumping-aeration -Defrost cycle process to remove oxygen. Finally, add the initiator ethyl 2-bromoisobutyrate (30.4mg), react at 50°C for 4h, dissolve the reaction product with tetrahydrofuran, dilute the reaction product and pass through an alumina column to remove the catalyst. The colorless solution obtained was precipitated twice with methanol, filtered under suction at room temperature, and dried in vacuum to obtain 0.59 g of PMDAGlu. The molecular weight Mn=4631 was detected by gel permeation chromatography (GPC).

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

[0071] Add a stir bar to the Schlenk bottle at room temperature, then add cuprous bromide (14.6mg), PMDETA (22.8mg), styrene (2.43g) in sequence, and go th...

Embodiment 3

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

[0079] In a 100ml three-necked flask with a stopper at room temperature, add 4ml of rysulfen, MAlDAGlu (1.42g), FeCl3 (8.4mg), triphenylphosphine (35.4mg) and methyl 2-bromopropionate (75.3mg) in sequence, and stir Make it evenly mixed, deoxidize with nitrogen for 10 minutes, add the reducing agent ascorbic acid (7.9mg), react at 55°C for 2h under nitrogen protection, dissolve the reaction product with tetrahydrofuran, precipitate twice with methanol, filter with suction at room temperature, and dry in vacuum , Obtain 0.49gPMDAGal, the molecular weight Mn=1356 is 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) and FeCl into a 100ml three-neck bottle with stopper at room temperature 3 (10.8mg), triphenylphosphine (44.96mg), PMAlDAG...

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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. The microsphere is prepared by using self-made amphiphilic block macromonomer as a surfactant through a suspension polymerization process; since hydrophilic chain segments are spontaneously arranged on the outer surface, facing a water channel, of the microsphere in a water-absorbing swelling process, hydrophobic chain segments participate in polymerization reaction through double bonds to be combined to the interior of a microsphere framework, so that the preparation and surface hydrophilic modification of the super-macroporous polymer microsphere are realized by one step. The hydrophilic super-macroporous polymer microsphere prepared by the preparation method disclosed by the invention adopts crosslinked polystyrene as the microsphere framework, is high in mechanical strength, good in chemical stability, good in hydrophilicity and super-macroporous, the outer surface of the hydrophilic super-macroporous polymer microsphere is sugar-containing polymer or polyvinyl alcohol gel. The hydrophilic super-macroporous polymer microsphere has a wide application space in the fields of enzyme immobilization and rapid separation and purification of protein.

Description

Technical field [0001] The invention relates to the field of preparation of polymer microspheres, in particular to a hydrophilic super-macroporous polymer microsphere and a preparation method thereof. Background technique [0002] Chromatography technology is still an effective method to efficiently separate proteins, plasmids and other biological macromolecules. Choosing a suitable separation medium is a key factor to ensure separation efficiency. Due to the complicated tertiary and tertiary structure of biological macromolecules, large size (the diameter of protein molecules is usually 1-100nm, the diameter of plasmid molecules is between 150-250nm), and the characteristics of poor stability. In order to maintain the biological activity of biological macromolecules, it is required to shorten the separation time as much as possible under the premise of ensuring the purity of separation, so as to reduce the degree to which the biological macromolecules are cut by the fluid (Perf...

Claims

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Application Information

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Patent Type & Authority Applications(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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