Preparation method of water soluble fluorescent nano-particles

A fluorescent nanometer, water-soluble technology, applied in chemical instruments and methods, luminescent materials, etc., can solve the problems of poor particle size uniformity, not easy to disperse, low fluorescence sensitivity, etc., and achieve uniform particle size, low cost, and sensitive fluorescence intensity. Effect

Inactive Publication Date: 2013-04-03
NANJING UNIV OF TECH
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  • Abstract
  • Description
  • Claims
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Problems solved by technology

[0004] The purpose of the present invention is to provide a method for preparing water-soluble nanospheres with uniform size and dispersible in water for the problems of poor uniformity of particle size, low fluorescence sensitivity and difficulty in dispersing in water environment in traditional fluorescent particles.

Method used

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  • Preparation method of water soluble fluorescent nano-particles
  • Preparation method of water soluble fluorescent nano-particles
  • Preparation method of water soluble fluorescent nano-particles

Examples

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Embodiment 1

[0020] 1) Put 0.02 g of polystyrene-b-poly(2-vinylpyridine) (molecular weight 17.5K-b-9.5K) and 0.005 g of fluorescent substance perylene in a 50 ml glass flask with a reflux device, and then Add 20 grams of acetic acid into the bottle; heat the liquid in the glass flask to 110°C and keep it for 10 hours to obtain solution 1, which is directly used in the next reaction;

[0021] 2) Mix the above solution 1 and ethyl bromide at a volume ratio of 5:1, heat it to 110°C in a 50ml glass flask, and keep it for 3 hours, then redisperse the colloidal intermediate obtained by centrifugation in 20g of water Obtain solution 2;

[0022] 3) Put the solution 2 of the previous step in a 25 ml reaction kettle and heat it to 80°C and keep it for 2 hours to obtain polymer nanofluorescent microspheres dispersed in water.

[0023] The scanning electron microscope (SEM) image of the obtained nanofluorescent microspheres is shown in figure 1 As shown, the average particle diameter of the fluoresc...

Embodiment 2

[0025] Example 2 Compared with Example 1 step 1), the amount of block copolymer and fluorescent substance was increased to increase the yield, and the dissolution temperature was increased to reduce the time required for dissolution.

[0026] 1) Put 0.2 g of polystyrene-b-poly(2-vinylpyridine) (molecular weight 17.5K-b-9.5K) and 0.05 g of fluorescent substance perylene in a 50 ml glass flask with a reflux device, and then Add 20 grams of acetic acid into the bottle; heat the liquid in the glass flask to 130°C and keep it for 5 hours to obtain solution 1, which is directly used in the next reaction;

[0027] 2) Mix the solution 1 of the previous step and ethyl bromide at a volume ratio of 6:1, heat it to 110°C in a 50ml glass flask, and keep it for 3 hours, then redisperse the colloidal intermediate obtained by centrifugation in 10g of water Obtain solution 2;

[0028] 3) Put the solution 2 of the previous step in a 25 ml reaction kettle and heat it to 130° C. and keep it for ...

Embodiment 3

[0031] Compared with Example 1, Example 3 changed the molecular weight of the block copolymer used and the weight ratio of the segments, and increased the temperature of the quaternization reaction to obtain fluorescent microspheres with different particle sizes and reduce the quaternization reaction. the time required.

[0032] 1) Put 0.04 g of polystyrene-b-poly(2-vinylpyridine) (molecular weight 50K-b-16.5K) and 0.01 g of fluorescent substance perylene in a 50 ml glass flask with a reflux device, and then Add 20 grams of acetic acid to the bottle; heat the liquid in the glass flask to 110°C and keep it for 10 hours to obtain solution 1, which is directly used in the next reaction;

[0033] 2) Mix the above solution 1 and ethyl bromide at a volume ratio of 5:1, heat it to 130°C in a 50ml glass flask, and keep it for 1 hour, then redisperse the colloidal intermediate obtained by centrifugation in 15g of water Obtain solution 2;

[0034] 3) Put the solution 2 of the previous...

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Abstract

The invention relates to a preparation method of water soluble fluorescent nano-particles which are even and adjustable in size and have fluorescent marks; the preparation method comprises the following detailed steps of: mixing a segmented copolymer, a fluorescent material and an organic solvent in a certain ratio, heating the mixed solution and then holding for a certain time, adding a quanternization reagent in the obtained solution, heating and holding for a certain time; centrifuging, re-dispersing precipitate in water, and heating at a certain temperature, thereby obtaining the water soluble fluorescent nano-particles which are even and adjustable in size and have fluorescent marks, wherein the copolymer consists of a hydrophobic chain and a hydrophilic chain, preferably, the hydrophobic chain consists of the hydrophobic chain and polymethyl methacrylate, and the hydrophilic chain consists of poly(2-vinyl pyridine), poly(4-vinyl pyridine) and polymethyl methacrylate dimethylamino ethyl ester; the fluorescent nano-particles obtained by the method are even in size and have the hygrometric state particle size effectively adjustable within the range of 50nm to 400nm; and the method is simple, short in technological process, excellent in fluorescence effect and low in cost, and is suitable for large-scale production.

Description

technical field [0001] The invention relates to a preparation method of water-soluble nano microspheres with uniform and adjustable size and fluorescent labels, belonging to the field of polymer materials. Background technique [0002] Polymer nanofluorescent microspheres have received extensive attention from scholars at home and abroad in the fields of optical materials and other fields. Not only in the fields of biosensing, chemical medicine, clinical testing, environmental science, material science, etc., but also in high-precision and high value-added applications such as fluorescent probes and chemical separations, fluorescent labeling technology has made great progress and has become one of its main technical means. The size and distribution of fluorescent nanospheres, as well as fluorescence sensitivity determine the performance and use effect in the application process. [0003] The traditional methods for preparing polymer nanofluorescent microspheres mainly incl...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08J3/12C08J3/14C08L53/00C08F8/44C09K11/06
Inventor 汪勇杨智明邢卫红范益群
Owner NANJING UNIV OF TECH
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