Preparation method of porous magnetic polystyrene microspheres

A technology of polystyrene microspheres and polyvinylpyrrolidone, applied in the direction of magnetism of organic materials/organic magnetic materials, to achieve good shape, improved stability, and uniform distribution of micropores

Active Publication Date: 2016-05-25
NANJING FORESTRY UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] At present, there are few reports on the preparation of porous magnetic polymer microspheres. In order to obtain porous magnetic polymer microspheres with smaller particle sizes, so that they can fully demonstrate the advantages of small-sized microspheres and expand their application range, The invention provides a preparation method of porous magnetic polymer microspheres

Method used

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  • Preparation method of porous magnetic polystyrene microspheres
  • Preparation method of porous magnetic polystyrene microspheres
  • Preparation method of porous magnetic polystyrene microspheres

Examples

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Embodiment 1

[0030] Example 1: Preparation of materials.

[0031] Refinement of styrene: repeatedly wash with 200ml 5wt% NaOH aqueous solution until colorless to remove the polymerization inhibitor, wash three times with distilled water, and then add anhydrous CaCl 2 Dry and store in a brown bottle for later use.

[0032] Refining of benzoyl peroxide (BPO): Dissolve 10g BPO in 50ml chloroform, stir and dissolve, filter, drop the filtrate into 100ml methanol, put it in the refrigerator to stand to obtain white needle-like crystals, wash three times with a small amount of cold methanol, and vacuum at room temperature Dry for 10h, put into a brown jar, and refrigerate for later use.

[0033] Fe 3 O 4 Preparation of magnetic nanoparticles: 4.28g FeCl 2 ·4H 2 O, 11.70g FeCl 3 ·6H 2 O was dissolved in 180ml of water, stirred to dissolve, purged with nitrogen for 0.5h, then heated to 60°C, and 20.0ml of NH was added rapidly under rapid stirring. 3 ·H 2 O, the system changes from transpar...

Embodiment 2

[0034] Example 2: Preparation of porous magnetic polystyrene microspheres.

[0035] Specifically include the following steps:

[0036] (1) Take 0.8g of dry Fe prepared in Example 1 3 O 4 Magnetic nanoparticles were added to 100ml of 50(v / v)% ethanol aqueous solution, then the mixture was ultrasonically treated for 30min, and 1ml of vinyltriethoxysilane was gradually added dropwise to dissolve Fe 3 O 4 in the suspension. After that, it was transferred into a 250m1 three-necked flask, under N2 Under the protection, rapid stirring at 40 ° C for 12 h constant temperature aging. The obtained product was washed three times with absolute ethanol and twice with deionized water, then vacuum-dried at 40° C. and ground into powder.

[0037] (2) Take 0.5 g of the powder obtained in step (1) and 0.2 g of purified BPO, add them to a test tube containing 6 ml of styrene, 2 ml of toluene, 1 ml of n-heptane and 0.5 ml of DVB cross-linking agent, and place them in a test tube. Ultrasonic ...

Embodiment 3

[0041] Specifically include the following steps:

[0042] (1) Take 1 g of dry Fe prepared in Example 1 3 O 4 Magnetic nanoparticles were added to 100ml of 40(v / v)% ethanol aqueous solution, then the mixture was ultrasonically treated for 20min, and 2ml of vinyltriethoxysilane was gradually added dropwise to dissolve Fe 3 O 4 in the suspension. After that, it was transferred into a 250m1 three-necked flask, under N 2 Under the protection, rapid stirring at 50 ℃ for 24h constant temperature aging. The obtained product was washed three times with absolute ethanol and three times with deionized water, then was vacuum dried at 60° C. and ground into powder.

[0043] (2) Take 0.34 g of the powder obtained in step (1) and 0.17 g of purified BPO, add them to a test tube containing 8 ml of styrene, 2 ml of toluene, 1 ml of n-heptane and 0.5 ml of DVB cross-linking agent, and place them in a test tube. Ultrasonic mixing in ultrasonic for 0.5h.

[0044] (3) Measure 100ml of deioni...

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Abstract

The invention discloses a preparation method of porous magnetic polystyrene microspheres. The method comprises steps of: (1) adding dry Fe3O4 magnetic nanoparticles into an aqueous ethanol solution, treating with ultrasonic, adding vinyltriethoxysilane, transferring into a reactor together, stirring under a constant temperature and a nitrogen atmosphere for aging, and then washing, drying under vacuum and grinding the obtained product into powder; (2) mixing the powder obtained in the step (1) and benzoyl peroxide, and then adding into styrene containing a pore forming agent and a cross-linking agent for the ultrasonic treating; (3) dissolving polyvinylpyrrolidone and sodium dodecyl sulfate into water by using the ultrasonic; and (4) adding the liquid obtained in the step (2) into the liquid obtained in the step (3), treating with the ultrasonic, pouring the obtained mixture into a reactor, heating for condensation reflux to obtain a suspension liquid, separating with magnet, washing with ethanol, re-separating with the magnet, re-washing with pure water, drying under vacuum and grinding to obtain claybank powdery product, extracting with a soxhlet way, and drying under vacuum to obtain the finish product.

Description

technical field [0001] The invention relates to a preparation method of porous magnetic polymer microspheres, in particular to a preparation method of porous magnetic polystyrene microspheres. Background technique [0002] With the development of life science, the rapid and efficient separation and analysis of biological macromolecules has attracted more and more attention. As a separation method developed in recent years, biomagnetic separation technology has the advantages of high efficiency, rapidity, low solvent consumption, and easy automation. It is popular in the fields of biology, biotechnology and biomedicine. Biomagnetic separation requires magnetic spheres with regular spherical shape, uniform particle size, good dispersion, strong magnetic responsiveness and superparamagnetic properties. In order to make biomagnetic separation technology more widely used, magnetic spheres with carboxyl, hydroxyl, epoxy, amine and other functional groups on the surface should be ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08F292/00C08F212/08C08F212/36C08F2/20C08J9/28H01F1/42
Inventor 徐鹏张蕤苏天翔
Owner NANJING FORESTRY UNIV
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