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Preparation method for one-size nano-particle fluorescence microsphere

A nanoparticle and fluorescent microsphere technology, which is applied in the preparation of microspheres, microcapsule preparations, chemical instruments and methods, etc., can solve the problems of uneven size, difficulty in stability, and inability to achieve control, and achieve basically consistent coupling between particles, The method is simple and the effect of improving the degree of aggregation

Inactive Publication Date: 2009-01-14
SOUTHEAST UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] At present, the preparation and surface modification technology of water-soluble quantum dots are relatively mature, and microemulsions are used to dissolve in the oil phase to form nanoparticle aggregates (Chem. Mater. 2003, 15, 528) or protein molecule aggregates (Pharmaceutical Research, 2004, 21 , 1445) have been reported, but the size of these reported microspheres is greater than 1 micron, and the size is not uniform, and the control of the size of the microspheres in the nanometer size range cannot be realized, and the particles are agglomerated by physical adsorption, which is difficult to store for a long time. , ultrasonic vibration, heating and other conditions stable

Method used

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  • Preparation method for one-size nano-particle fluorescence microsphere
  • Preparation method for one-size nano-particle fluorescence microsphere
  • Preparation method for one-size nano-particle fluorescence microsphere

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Effect test

Embodiment 1

[0034] 2.35mmol Cd(ClO 4 ) 2 2H 2 O was dissolved in 125ml of water, 5.7mmol of amino mercaptan was added under constant stirring, and the pH value of the system was adjusted to 5-7 by adding 1M NaOH solution. Nitrogen was passed through the system for about 30 minutes to ensure that the air was exhausted. With constant stirring, H 2 Te gas (by 0.46mmol Al 2 Te 3 with 15-20ml of 0.5M H 2 SO 4 (formed by reaction in a nitrogen environment) was slowly driven by nitrogen into the reaction system for 20 minutes, and the system was refluxed and heated to 100° C. in an air environment to obtain aminothiol-coated CdTe nanoparticles.

[0035] Add more than 30% propanol by volume to the nanoparticle aqueous solution, centrifuge, remove the supernatant solution, repeat washing with propanol for more than 6 times, add ultrapure water, and obtain a monodisperse nanoparticle aqueous solution from which impurities are removed.

Embodiment 2

[0037] In a glove box filled with high-purity nitrogen, dissolve 0.158g of selenium powder into 2ml of trioctyl phosphate, dissolve 0.12g of cadmium acetate in 3ml of trioctyl phosphate, and heat 8 grams of tri-n-octylphosphine oxide in a vacuum environment Keep at 180°C for 1 hour, cool down to 100°C, add 5g of hexadecylamine and 0.15g of n-tetradecyl phosphoric acid, keep at 120°C for 20 minutes in a vacuum environment, fill the reactor with flowing nitrogen, and dissolve the selenium Powdered trioctyl phosphate is added to the mixture, heated to 300°C, injected with trioctyl phosphate dissolved in cadmium acetate, and kept at 260°C for different times (5 minutes to 1 hour), to obtain CdSe nanoparticles of different particle sizes, Cool down to 140°C, stop nitrogen, and pass H over the liquid surface at a rate of 2ml per 10 minutes. 2 S gas, stir the solution, keep it for 30 minutes, cool down to 100°C, stir for 1 hour, stop adding H 2 S gas, lower the temperature to 50°C, ...

Embodiment 3

[0039] according to Figure 1 The design and preparation device shown, the oil phase solvent is a mixed solution of analytical pure ethyl acetate and 1-2 propylene glycol carbonate with a volume ratio of 2:1, the total volume is 200ml, the container and the return pipe are all made of polytetrafluoroethylene, and the return pump A stainless steel gear pump is used with a flow range of 1.3-2.6ml / sec. Take the above-mentioned quantum dot aqueous solution, adjust the concentration to 1 micromol, and inject it into the capillary ( figure 1 ), adjust the flow rate to 0.5-2.5ml / min, inject for 15 seconds, and the interval is 5 minutes; the coaxial capillary nozzle is made of hydrophobic treated glass material, the inner diameter of the capillary is 0.1mm, the outer diameter is 0.2mm, the inner diameter d of the outer tube is 1mm, and the capillary The end is flat, the distance h between the end and the opening of the outer tube is 1mm, the end of the outer tube is tapered, the openi...

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Abstract

The present invention provides a preparation method of an uniform-size nanoparticle fluorescent microsphere. The density of fluorescent nanoparticle colloidal aqueous solution of the microsphere is adjusted to the micro-mol level so as to obtain the colloidal solution evenly scattered in the aqueous solution; the evenly scattered colloidal solution in the aqueous solution is injected into oil-phase solvent through capillary at the speed of 0.5 to 1.25 percent Vs / min so as to form droplets and Vs is the volume of the oil-phase solvent; the oil-phase solvent adopts bi- or multi-mixture with the solubility between 2 to 10 percent and the density equal to the density of water; containers and reflux pipes adopt the hydrophobic material; the water in droplets is absorbed by the oil phase and the nanoparticles form a dense sphere; an absorbent continuously absorbs the water dissolved in the oil phase, so that the water content in the oil phase is far lower than the saturation; the nanoparticle polymer with the size from dozens of nano to hundreds of nano, the spherical height higher than 5 percent and the size error less than 10 percent is obtained through regulating the density of the quantum pot colloidal solution and the velocity of the reflux pipe.

Description

technical field [0001] The invention relates to controlling the size of nanoparticle aggregates by controlling the formation of microemulsions to achieve the preparation of fluorescent microspheres with uniform size, and belongs to the technical field of preparation of nanoscale nanoparticle aggregates. Background technique [0002] The unique fluorescent properties of nanoparticles can be used as biomarkers. The existing method is to coat the surface of nanoparticles with conjugated molecules with biospecific groups through chemical modification to achieve the labeling of different biological substances. However, due to a single semiconductor The fluorescence intensity of quantum dots is weak, and it is difficult to realize the identification of individual particles, and the surface modification of individual particles cannot effectively eliminate the non-specific binding caused by physical adsorption on the surface of small particles (<10 nanometers). Pack multiple nano...

Claims

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Application Information

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IPC IPC(8): B01J13/02C09K11/00
Inventor 巴龙周成喜朱庆文
Owner SOUTHEAST UNIV
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