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Vinyl monomer-polyvinyl crosslinking agent copolymer non-porous microspheres and its preparation method and application

A vinyl monomer and polyvinyl technology, applied in chemical instruments and methods, other chemical processes, instruments, etc., can solve the problems of limited application, poor ion exchange performance, and affecting the service life of chromatographic packing, and achieve the elimination of non-specificity Adsorption, good mechanical stability, remarkable separation effect

Active Publication Date: 2022-05-10
SHENZHEN LIFOTRONIC TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the microspheres of non-porous fillers have the defect of low specific surface area, resulting in low separation capacity, which limits their many applications in protein separation.
In addition, chromatographic packing materials based on natural polymers usually exhibit poor rigidity and insufficient pressure resistance, and are mainly used for purification and separation of biopharmaceuticals
[0004] Traditional vinyl monomer-vinyl crosslinker copolymer non-porous microspheres are used as chromatographic fillers, mainly methacrylate copolymers and styrene-divinylbenzene copolymers, these two non-porous microspheres It has good rigidity, but at present, the ion exchange performance of this kind of non-porous microspheres is poor, and it has a strong non-specific adsorption on biological components, such as protein molecular loads, which affects the use of chromatographic fillers life

Method used

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  • Vinyl monomer-polyvinyl crosslinking agent copolymer non-porous microspheres and its preparation method and application
  • Vinyl monomer-polyvinyl crosslinking agent copolymer non-porous microspheres and its preparation method and application
  • Vinyl monomer-polyvinyl crosslinking agent copolymer non-porous microspheres and its preparation method and application

Examples

Experimental program
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preparation example Construction

[0105] The present invention also provides a method for preparing non-porous microspheres of vinyl monomer-polyvinyl crosslinking agent copolymer, comprising the following steps:

[0106] Preparing vinyl monomer-polyvinyl crosslinking agent copolymer cue balls, the vinyl monomer-polyvinyl crosslinking agent copolymer cue balls are modified with hydroxyl groups;

[0107] The epoxy compound is grafted onto the vinyl monomer-polyvinyl crosslinking agent copolymer cue ball through hydroxyl reaction, and the epoxy compound contains at least two epoxy groups.

[0108] Further, the method for preparing vinyl monomer-multi-vinyl crosslinking agent copolymer cue ball comprises the steps:

[0109] Prepare vinyl monomer-polyvinyl crosslinking agent copolymer particles, the vinyl monomer-polyvinyl crosslinking agent copolymer particles are modified with epoxy groups, the preparation steps include: using polystyrene seed microspheres as seeds , together with vinyl monomers and polyvinyl c...

Embodiment 14

[0178] The synthesis of embodiment 1 4-vinylphenyl glycidyl ether

[0179] In a 250mL three-necked flask, add 4-hydroxystyrene (7.22g, 60.1mmol) and ethanol (about 10mL) and stir to dissolve for later use; further add absolute ethanol (50mL) to a 100mL beaker equipped with a magnetic stirring bar and Dissolve NaOH (3.12 g, 78.0 mmol, 1.3 times the molar ratio) and stir for 30 minutes, then add to the above-mentioned three-necked flask. Epichlorohydrin (14.1 mL, 180 mmol, 3 times 1.3 times molar ratio) was then quickly added to the three-necked flask using a dropping funnel. Stirring at 150 rpm at room temperature, the reaction solution gradually became turbid, and sodium chloride slowly precipitated out. After continuing the reaction for 16 hours, 100 mL of water was added and stirred to dissolve the precipitated sodium chloride, and the mixture was extracted with hexane (2×100 mL) using a separatory funnel. Combine the organic phases with anhydrous MgSO 4 The oil phase was...

Embodiment 24

[0181] The synthesis of embodiment 2 4-vinylbenzyl glycidyl ether

[0182] A 500mL three-necked flask was fed with argon, and under an argon atmosphere, sodium hydride (60% in mineral oil, 13.1g, 327.60mmol, 2.00 times molar ratio) was added in DMF (300mL), and added dropwise at 0°C Glycidol (27.15 mL, 459.1 mmol, 2.50 times molar ratio). After the reaction mixture was stirred for 30 minutes, the stirring speed was controlled at 150 rpm, and 1-(chloromethyl)-4-vinylbenzene (23.3 mL, 163.80 mmol, 1.00 times molar ratio) was added dropwise, and stirring was continued at room temperature after the addition was completed React for 4 hours. The mixture was extracted with ethyl acetate (400 mL). Add saturated NH 4 Aqueous Cl solution (200 mL) was used to quench the reaction, and the aqueous layer was further extracted with ethyl acetate (3×100 mL). The combined organic layers were washed with anhydrous Na 2 SO 4 Dry the oil phase and remove the solvent under vacuum by rotary e...

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Abstract

The invention relates to a non-porous microsphere of a vinyl monomer-polyvinyl crosslinking agent copolymer, a preparation method and application thereof. Vinyl monomer-polyvinyl crosslinker copolymer non-porous microspheres include: vinyl monomer-polyvinyl crosslinker copolymer cue ball, vinyl monomer-polyvinyl crosslinker copolymer cue ball Modified with a hydroxyl group; an epoxy-based compound grafted to the vinyl monomer-polyvinyl cross-linking agent copolymer mother ball through the hydroxyl group, and the epoxy-based compound contains at least two epoxy groups. The vinyl monomer-polyvinyl cross-linking agent copolymer non-porous microsphere has good chemical and mechanical stability, has excellent ion exchange performance, and has high specific separation ability for hemoglobin and its variants.

Description

technical field [0001] The invention relates to the technical field of polymer microspheres, in particular to a vinyl monomer-polyvinyl crosslinking agent copolymer non-porous microsphere and its preparation method and application. Background technique [0002] Polymer microspheres usually have the characteristics of good spherical shape, small size, large specific surface area, strong adsorption performance and functional modification, so they are widely used as functional materials in various industries. In recent years, the use of ion-exchange high-performance liquid chromatography (HPLC) for the determination of biological components has increasingly attracted people's attention, and the liquid chromatography column packed with ion-exchange It is one of the core hardware of separation detection. [0003] The ion-exchange packing for filling the liquid chromatography column is divided into porous packing and non-porous packing. Compared with the porous packing, the non-p...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08F257/02C08F212/14C08F212/36C08F8/08C08F8/00C08F8/30B01J20/281B01J20/30G01N30/02G01N30/06
CPCC08F257/02C08F8/08C08F8/00C08F8/30G01N30/02G01N30/06B01J20/281B01J2220/52B01J2220/54C08F212/22C08F212/36B01J20/267B01J20/321B01J20/3219B01J20/3248B01J20/286C08F8/32C08F8/14
Inventor 丁忠刘先成
Owner SHENZHEN LIFOTRONIC TECH
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