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Magnetic nano polystyrene carboxyl microspheres and preparation method thereof

A polystyrene carboxyl and magnetic nano technology, which is applied in the field of magnetic nano polystyrene carboxyl microspheres and its preparation, can solve the problems of large particle size, inability to separate magnetic particles, and small magnetic content, so as to ensure magnetic response. good coating effect and ensure the effect of consistency

Active Publication Date: 2019-10-01
DONGGUAN DONGYANG SOLAR SCI RES & DEV CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The current common preparation method of nano magnetic beads is to 3 o 4 Surface modified polymer layer, on the one hand, Fe will appear during the preparation process 3 o 4 The agglomeration of nanoparticles causes the problem of uneven particle size. On the other hand, it also causes inconsistent magnetic content of the particles. The response is weak, and the magnetic particles cannot be separated from the solution well during use

Method used

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Examples

Experimental program
Comparison scheme
Effect test

preparation example Construction

[0026] The invention relates to a method for preparing magnetic nanometer PS carboxyl microspheres by using cross-linked PS carboxyl microspheres. Among them, the experimental synthesis parameters of the preparation method of crosslinked PS carboxyl microspheres include: the volume ratio of St monomer to pure water is 1:4 to 1:20; the mass of divinylbenzene (DVB) accounts for 1% to 10% of the mass of St monomer The quality of enoic acid accounts for 1%~10% of St monomer quality; Initiator is a kind of in potassium persulfate (KPS), azobisisobutyronitrile (AIBN), benzoyl peroxide (BPO), The mass of the initiator accounts for 0.3%~3% of the mass of the St monomer; the reaction temperature is 60~90°C; the stirring speed is 150~500r / min; the reaction time is 6~20h; the centrifugal speed is 5000r / min~10000r / min ; FeCl 3 The dosage is 0.5% to 3% of the mass of the emulsion.

[0027] In some embodiments, the volume ratio of St monomer to pure water is 1:4 to 1:10; for example: 1:4,...

Embodiment 1

[0063] Example 1: Preparation of cross-linked PS carboxyl microspheres X1

[0064] Measure 5mL of purified St monomer (4.55g), 0.15gDVB and 0.3gAA into a four-necked flask with mechanical stirring, then measure 50mL of pure water and 0.1g potassium persulfate into the four-necked flask, and put the four-necked The flask was placed in a water bath at room temperature, and condensed water and high-purity N 2 , adjust the stirring speed to 250r / min, start to heat up to 70°C after 15min, and end the reaction after 8h.

[0065] Pass the emulsion produced by the reaction through a 400-mesh standard sieve, and then centrifuge it at 7000r / min for 10 minutes. After the centrifugation, take the unprecipitated emulsion and add 0.1g FeCl to the emulsion. 3 ·6H 2 O to make it flocculate, remove the supernatant after centrifuging again, wash the precipitate with water and absolute ethanol three times respectively, and set aside for later use to obtain cross-linked PS carboxyl microspheres...

Embodiment 2

[0066] Embodiment 2: Preparation of cross-linked PS carboxyl microspheres X2

[0067] Measure 10mL of purified St monomer (9.09g), 0.3gDVB and 0.3gAA into a four-necked flask with mechanical stirring, then measure 50mL of pure water and 0.1g potassium persulfate into the four-necked flask, and add the four-necked The flask was placed in a water bath at room temperature, and condensed water and high-purity N 2 , adjust the stirring speed to 500r / min, start to heat up to 90°C after 15min, and end the reaction after 20h.

[0068] Pass the emulsion formed by the reaction through a 400-mesh standard sieve, and then centrifuge at 5000r / min for 10 minutes. After centrifugation, take the unprecipitated emulsion and add 0.3g FeCl dropwise to the emulsion. 3 ·6H 2 O to make it flocculate, remove the supernatant after centrifuging again, wash the precipitate with water and absolute ethanol three times, and then set aside to obtain cross-linked PS carboxyl microspheres X2.

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Abstract

The invention relates to magnetic nano polystyrene carboxyl microspheres and a preparation method thereof. The magnetic nano polystyrene carboxyl microspheres are obtained by firstly synthesizing crosslinked polystyrene carboxyl microspheres with stable carboxy groups on the surface by a polymerization reaction of a styrene monomer, a crosslinking agent and gadoleic acid, removing large particlesin the microspheres, maintaining a uniform particle size of 60 nm to 300 nm, then dispersing uniform crosslinked nano polystyrene carboxyl microspheres into an iron / cobalt / manganese / nickel salt solution containing a reductive organic solvent to form homogeneous liquid, performing a high-pressure thermal insulation reaction on the homogeneous liquid under high temperature and high pressure conditions to synthesize composite magnetic nanoparticles, and removing the magnetic particles on the surface of the composite magnetic nanoparticles with acid. The magnetic nano polystyrene carboxyl microspheres prepared by the method involved in the invention have the advantages of good magnetic responsiveness, uniform particle size, good monodispersity, uniform magnetic content of particles, good magnetic particle embedding effect, stable functional group modification, and the like.

Description

technical field [0001] The invention relates to the technical field of composite material preparation, in particular to a magnetic nano polystyrene carboxyl microsphere and a preparation method thereof. Background technique [0002] Magnetic beads are composite functional microspheres with superparamagnetism. Because of their surface modification with functional groups such as amino groups and carboxyl groups, they can be coupled to proteins, DNA, etc. Therefore, it has a wide range of applications in cell separation, immobilized enzymes, immunodiagnosis, tumor targeted therapy, and DNA extraction. In actual operation, well-applied nano magnetic beads must have uniform particle size, consistent magnetic content of each particle, good magnetic particle embedding effect, good monodispersity, stable functional group modification and good magnetic response. The current common preparation method of nano magnetic beads is to 3 o 4 Surface modified polymer layer, on the one hand...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F212/08C08F212/36C08F220/06C08K3/22C08L25/08
CPCC08F212/08C08K3/22C08K2003/2275C08K2201/01C08F212/36C08F220/06
Inventor 王鹏侯立威吴志能徐玲玲杨远博谌庆春周政
Owner DONGGUAN DONGYANG SOLAR SCI RES & DEV CO LTD
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