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A kind of preparation method of carboxyl polystyrene copolymerized fluorescent microsphere

A fluorescent microsphere, polystyrene technology, applied in chemical instruments and methods, luminescent materials, etc., can solve the problems of difficult microspheres, damage polymerization conditions, etc., and achieve the effects of low cost, high luminous efficiency, and not easy to leak

Inactive Publication Date: 2016-08-17
ZHONGBEI UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, according to the literature [Journal of Materials Chemistry, 2009, 19, 2018-2025], the fluorescent dye molecules with double bonds are relatively large, and there is a certain degree of steric hindrance during the copolymerization process, which has self-inhibiting polymerization. The double-bond fluorescent dye will destroy the stable polymerization conditions of the original blank microspheres, and it is not easy to form microspheres with uniform particle size

Method used

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  • A kind of preparation method of carboxyl polystyrene copolymerized fluorescent microsphere
  • A kind of preparation method of carboxyl polystyrene copolymerized fluorescent microsphere
  • A kind of preparation method of carboxyl polystyrene copolymerized fluorescent microsphere

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Embodiment 1

[0018] 1. Synthesis of allyl rhodamine B: According to the literature (J. Mater. Chem., 2009, 19, 2018-2025) method, put 240g of rhodamine B, 0.73g of potassium carbonate, and 2.65g of 3-bromopropene into the reaction In the bottle, add solvent DMF 50ml, catalyst iodine trace, polymerization inhibitor hydroquinone trace, under anhydrous and oxygen-free conditions, react at 71°C for 25h to synthesize allyl rhodamine B, and the crude product is obtained by column chromatography Pure.

[0019]

[0020] 2. Preparation of carboxypolystyrene copolymerized fluorescent microspheres: take 0.06g of azobisisobutyronitrile, 0.18g of polyvinylpyrrolidone, 9.6ml of absolute ethanol and 0.4ml of water respectively, put them in a microreactor, and ultrasonically clarify Clear solution. Add 3.02 g of styrene, 0.15 g of acrylic acid, and 15 mg of allyl rhodamine B, pass nitrogen to remove oxygen, and seal. Place in a constant temperature oscillator and react at 70°C for 12h. The obtained ...

Embodiment 2

[0024] 1. Synthesis of allyl fluorescein: According to the literature (J. Mater. Chem., 2009, 19, 2018-2025), 2.00 g of fluorescein, 2.42 g of 3-bromopropene and 4.97 g of anhydrous potassium carbonate were added In the reaction bottle, add 50ml of DMF as a solvent, a trace of iodine as a catalyst, and a trace of hydroquinone as a polymerization inhibitor, and react at 71°C for 25 hours under anhydrous and oxygen-free conditions to obtain a yellow crude product of allyl fluorescein, which is recrystallized from chloroform , the pure product was obtained by column chromatography.

[0025]

[0026] 2. Preparation of carboxypolystyrene copolymerized fluorescent microspheres: Take 0.07g of azobisisobutyronitrile, 0.21g of polyvinylpyrrolidone, 9ml of absolute ethanol and 1.2ml of water respectively, put them in a microreactor, and ultrasonically obtain clarity solution. Add 3.0 g of styrene, 0.11 g of acrylic acid, and 9 mg of allyl fluorescein, pass nitrogen to remove oxygen,...

Embodiment 3

[0028] 1. Synthesis of Allyl Nile Red: According to the literature (J. Mater. Chem., 2009, 19, 2018-2025) method, m-N,N-diethylaminophenol 1.65g, concentrated hydrochloric acid 3.40ml and water 1.70 ml into the reaction flask, stirred in an ice bath until dissolved, controlled the temperature at 0°C, and slowly added an aqueous solution of sodium nitrite (NaNO 2 0.78g, H 2 O 5.9mL), the addition was completed in 30min, reacted at 0-5°C for 4h, filtered to obtain the crude hydrochloride product, and dried in vacuum at 50°C for 8h. Dissolve the crude product in 25ml of boiling ethanol, cool to 40°C, add diethyl ether slowly until crystals appear, place the mixture in the refrigerator for 24 hours, and filter to obtain khaki needle-like crystals of 5-(diethylamino)-2-nitrosophenol .

[0029]

[0030] Put 0.50g of 5-(diethylamino)-2-nitrosophenol, 0.33g of 1,6-dihydroxynaphthalene and 40ml of dry DMF into the reaction flask, stir and heat to reflux, react for 4h and evaporat...

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Abstract

The invention discloses a preparation method of carboxyl polystyrene copolymerized fluorescent microspheres, which is to put absolute ethanol, initiator azobisisobutyronitrile, and dispersant polyvinylpyrrolidone in water to obtain a clear and transparent solution, and inject the same into the solution at the same time Styrene, acrylic acid and allyl fluorescent dye are added, and the copolymerization reaction is carried out under the protection of nitrogen to obtain carboxyl polystyrene copolymerized fluorescent microspheres. The invention adopts a dispersion polymerization method, and the prepared carboxyl polystyrene copolymerized fluorescent microsphere has good monodispersity and stable fluorescent performance.

Description

technical field [0001] The invention relates to a preparation method of fluorescent microspheres, in particular to a preparation method of carboxyl polystyrene copolymerized fluorescent microspheres. Background technique [0002] Fluorescent microspheres have good application prospects. Studies have shown that it can be widely used in the calibration of fluorescent instruments, the detection and analysis of biomolecules and synthetic molecules, especially the surface functionalized fluorescent microspheres, which have potential application value in the field of biomedicine, such as gene sequencing and expression, Protein sequencing, disease diagnosis and drug screening, etc. At the same time, there is also a large demand for fluorescent microspheres in environmental monitoring and food inspection. [0003] CN 102115508A discloses a method for synthesizing micron-scale polymer fluorescent microspheres. It first prepares high-quality quantum dots, and then uses dispersion po...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08F212/08C08F220/06C08F218/12C09K11/06
Inventor 刘清浩郭金春刘红彦王俊美
Owner ZHONGBEI UNIV
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