Preparing method for carboxylation porous crosslinked polystyrene copolymerized fluorescent microspheres

A technology of cross-linked polystyrene and fluorescent microspheres, applied in chemical instruments and methods, luminescent materials, etc., can solve the problems of lack of functional groups on the surface of fluorescent microspheres, inconvenient biological research, leakage of fluorescent dyes, etc., and achieve the goal of preparing Low cost, uniform fluorescence intensity distribution, and high luminous efficiency

Inactive Publication Date: 2018-05-29
ZHONGBEI UNIV
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  • Abstract
  • Description
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  • Application Information

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Problems solved by technology

[0003] CN 104212087 A discloses fluorescently labeled polystyrene microspheres and a preparation method thereof. First, polystyrene nanospheres are prepared by soap-free emulsion polymerization, and then hydrophobic fluorescent substances are loaded on polystyrene by a swelling adsorption method. However, the surface of the fluorescent microsphere lacks functional groups, which is inconvenient for subsequent biological research.
[0004] CN 104209071 A discloses a method for preparing fluorescently labeled polysaccharide-modified fluorescent microspheres. Although it has good biocompatibility, carboxypolystyrene microspheres and fluorescently labeled polysaccharides are combined through polyelectrolytes. Easy to fall off, resulting in leakage and quenching of fluorescent dyes, causing sample contamination during testing

Method used

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  • Preparing method for carboxylation porous crosslinked polystyrene copolymerized fluorescent microspheres
  • Preparing method for carboxylation porous crosslinked polystyrene copolymerized fluorescent microspheres
  • Preparing method for carboxylation porous crosslinked polystyrene copolymerized fluorescent microspheres

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Experimental program
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Effect test

Embodiment 1

[0052] (1) Preparation of polystyrene seed balls

[0053] It is prepared by dispersion polymerization method: respectively take 0.024 g of initiator azobisisobutyronitrile, 0.072 g of dispersant polyvinylpyrrolidone, and 9.0 g of absolute ethanol in a micro-reactor, and ultrasound to obtain a clear and transparent solution. Add 1.2 g of styrene to the solution, purge nitrogen to remove oxygen, and seal. Place it in a constant temperature shaker and react for 12 hours at 70°C and 130 rpm. The obtained microspheres are washed repeatedly with water and ethanol successively, and dried under vacuum at 50°C to obtain polystyrene seed balls.

[0054] (2) Synthesis of allylcarbazole

[0055] Add 0.69g (4.00mmol) of carbazole, 0.62g (6.00mmol) of 3-bromopropene, 1.57g (28.00mmol) of KOH, hydroquinone and KI (trace amount) into a 100mL four-neck flask equipped with electromagnetic stirring. And dried DMF 10mL. In N 2 Under protection and dark conditions, the reaction mixture was heated to ...

Embodiment 2

[0068] (1) Preparation of polystyrene seed balls

[0069] It is prepared by dispersion polymerization method: respectively take 0.024 g of initiator azobisisobutyronitrile, 0.072 g of dispersant polyvinylpyrrolidone, and 9.0 g of absolute ethanol in a micro-reactor, and ultrasound to obtain a clear and transparent solution. Add 1.2 g of styrene to the solution, purge nitrogen to remove oxygen, and seal. Place it in a constant temperature shaker and react for 12 hours at 70°C and 130 rpm. The obtained microspheres are washed repeatedly with water and ethanol successively, and dried under vacuum at 50°C to obtain polystyrene seed balls.

[0070] (2) Synthesis of allyl fluorescein

[0071] Synthesized according to the literature (J.Mater.Chem.,2009,19,2018-2025) method:

[0072]

[0073] (3) Activation of bulb

[0074] Weigh 0.1g of polystyrene seed balls and disperse them in a 0.25% sodium lauryl sulfate solution with ultrasound to obtain a uniformly dispersed seed ball solution. At th...

Embodiment 3

[0084] (1) Preparation of polystyrene seed balls

[0085] It is prepared by dispersion polymerization method: respectively take 0.024 g of initiator azobisisobutyronitrile, 0.072 g of dispersant polyvinylpyrrolidone, and 9.0 g of absolute ethanol in a micro-reactor, and ultrasound to obtain a clear and transparent solution. Add 1.2 g of styrene to the solution, purge nitrogen to remove oxygen, and seal. Place it in a constant temperature shaker and react for 12 hours at 70°C and 130 rpm. The obtained microspheres are washed repeatedly with water and ethanol successively, and dried under vacuum at 50°C to obtain polystyrene seed balls.

[0086] (2) Eu(AA) rare earth europium complex with double bond 3 Synthesis of Phen

[0087] Called Eu 2 O 3 (0.70g, 2mmol) add concentrated hydrochloric acid to dissolve and steam until nearly dry, add 40mL absolute ethanol to dissolve, make EuCl 3 Ethanol solution, the reaction formula is as follows:

[0088] Eu 2 O 3 +6HCl→2EuCl 3 +3H 2 O

[0089] W...

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Abstract

The invention discloses a preparing method for carboxylation porous crosslinked polystyrene copolymerized fluorescent microspheres. The preparing method is characterized by including the following steps of polystyrene seed sphere preparing, seed sphere activating, seed sphere swelling, polymerizing and pore-forming agent extracting. Compared with the prior art, the preparing method for the carboxylation porous crosslinked polystyrene copolymerized fluorescent microspheres has the advantages that the carboxylation porous crosslinked polystyrene copolymerized fluorescent microspheres with blue fluorescence, green fluorescence and red fluorescence are obtained; fluorochrome is evenly distributed in the microspheres, and therefore the high whole luminous efficiency of the microspheres is guaranteed; the fluorochrome stably exists in the microspheres, leakage and cancellation are not prone to occurrence, and pollution on test samples can be avoided; the grain size of the fluorescent microspheres prepared with the method is uniform, and is 7.5 microns, the specific area is large, and the good monodispersity is achieved; the light intensity is even in distribution; the preparing cost is low.

Description

Technical field [0001] The invention belongs to the technical field of preparation methods of fluorescent microspheres, and specifically relates to a preparation method of carboxylated porous crosslinked polystyrene copolymer fluorescent microspheres. Background technique [0002] Fluorescent microspheres have stable morphology and high luminous efficiency, and are less affected by external conditions such as solvents, heat, electricity, and magnetism than pure fluorescent compounds. They have extremely important applications in many fields, especially biomedicine. Compared with non-porous dense fluorescent microspheres, the internal fluorescence intensity distribution of porous fluorescent microspheres is more uniform, and can stably bind to antigen (human IgG), and can specifically recognize the corresponding antibody (ACS Appl.Mater.Interfaces 2015,7 , 9118-9127). Porous polymer microspheres have the advantages of porosity, large specific surface area, high mechanical strengt...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F212/08C08F212/36C08F226/06C08F220/06C08F218/12C08F230/04C08J9/28C09K11/02C09K11/06
CPCC08F212/08C08J9/28C08J2325/08C09K11/025C09K11/06C09K2211/1007C09K2211/1029C09K2211/1088C09K2211/182C08F212/36C08F226/06C08F220/06C08F218/12C08F230/04
Inventor 刘清浩郭金春刘红彦胡志勇
Owner ZHONGBEI UNIV
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