Three-layer core-shell-structure inorganic nanoparticle/silicon dioxide/high polymer composite microspheres and preparation method thereof

A technology of inorganic nanoparticles and silicon dioxide, applied in the field of composite materials, to achieve the effects of shortened experiment time, uniform particle size, and simple operation

Inactive Publication Date: 2012-02-08
TIANJIN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0007] The purpose of the present invention is to provide a simple and efficient method for preparing three-layer core-shell structure inorganic nanoparticles/silicon dioxide/polymer composite micro

Method used

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  • Three-layer core-shell-structure inorganic nanoparticle/silicon dioxide/high polymer composite microspheres and preparation method thereof
  • Three-layer core-shell-structure inorganic nanoparticle/silicon dioxide/high polymer composite microspheres and preparation method thereof
  • Three-layer core-shell-structure inorganic nanoparticle/silicon dioxide/high polymer composite microspheres and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] Step 1: Weigh 2mg of CdSeTe quantum dots with an emission wavelength of 517nm, dissolve the quantum dots in 0.5ml of chloroform, add 10mg of PVP as a stabilizer, and disperse uniformly by ultrasonic;

[0033] Step 2, adding the reactant of step 1 into 10ml of ethanol, stirring until the system is uniform;

[0034] Step 3: Add 30 μl tetraethyl orthosilicate (TEOS) and 15 μl ammonia water to the reaction system in step 2, and react for 12 hours at a stirring speed of 3000 r / min.

[0035] Step 4: Add 30 μl of silane coupling agent (MPS) to the reaction system in Step 3, and react for 6 hours.

[0036] Step 5: Add 15 μl EGDMA, 45 μL MAA and 200 μL AIBN (1 g / mL) to the reaction system in step 4, heat the system to 90 ° C, and stop the reaction when half of the solvent is distilled off; centrifuge and wash to obtain a three-layer core-shell Structural inorganic nanoparticles / silica / polymer composite microspheres.

[0037] figure 1 The low-magnification photo of the prepared ...

Embodiment 2

[0039] Step 1: Weigh 1 mg of CdSe / ZnS quantum dots with an emission wavelength of 564 nm, dissolve the quantum dots in 1 ml of chloroform, add 200 mg of PEI as a stabilizer, and disperse uniformly by ultrasonic;

[0040] In step 2, the reactant in step 1 is added to 10ml of acetonitrile, and stirred until the system is uniform;

[0041] Step 3: Add 10 μl tetraethyl orthosilicate (TEOS) and 10 μl ammonia water to the reaction system in step 2, and react for 36 hours at a stirring speed of 3000 r / min.

[0042] Step 4: Add 30 μl of silane coupling agent (MPS) to the reaction system in Step 3, and react for 10 h.

[0043] Step 5: Add 15 μL DVB, 60 μL styrene and 60 μL BPO (1 g / mL) to the reaction system in step 4, heat the system to 95° C., and stop the reaction when half of the solvent is distilled off; after centrifugation and washing, three Inorganic nanoparticles / silica / polymer composite microspheres with layered core-shell structure.

[0044] The prepared composite microsph...

Embodiment 3

[0046] Step 1: Weigh 4mg of CdSe quantum dots with an emission wavelength of 650nm, dissolve the quantum dots in 2ml of cyclohexane, add 200mg of PEO as a stabilizer, and disperse uniformly by ultrasonic;

[0047] Step 2, adding the reactant in step 1 to 5ml of acetonitrile and 5ml of ethanol, stirring until the system is uniform;

[0048] Step 3: Add 60 μl of tetraethyl orthosilicate (TEOS) and 10 μl of ammonia water to the reaction system in Step 2, and react for 48 hours at a stirring speed of 3000 r / min.

[0049] Step 4: Add 20 μl of silane coupling agent (MPS) to the reaction system in Step 3, and react for 12 hours.

[0050] Step 5: Add 20 μl EGDMA, 20 μL MAA, 20 μL styrene, and 200 μL AIBN (1 g / mL) to the reaction system in step 4, heat the system to 90° C., and stop the reaction when half of the solvent is distilled off; after centrifugation and washing, prepare The average particle size is 80nm and the three-layer core-shell structure inorganic nanoparticle / silicon d...

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Abstract

The invention relates to three-layer core-shell-structure inorganic nanoparticle/silicon dioxide/high polymer composite microspheres and a preparation method thereof. The average particle size of the composite microspheres is 15-800nm, the particle size is uniform, the three-layer core-shell structure is obvious, and the inorganic nanoparticle is completely coated to enter the silicon dioxide and high polymer shell. By using the hydrophilic high polymer as the stabilizer, the inorganic nanoparticles can be uniformly dispersed in ethanol, acetonitrile or any other polar solvent, and can not generate the phenomenon of aggregation or precipitation; and thus, the invention can implement preparation of the silicon core and polymerization reaction of the high polymer shell in one reaction solvent, thereby saving the process of purifying and washing the silicon core and replacing the reaction system, simplifying the experimental process and greatly shortening the experimental time. Besides, a distillation precipitation polymerization method, which has the advantages of simple reaction and high polymerization efficiency, is adopted to prepare the high polymer shell.

Description

technical field [0001] The invention relates to a composite material applicable to the field of biomedicine, in particular to a method for preparing inorganic nanoparticle / silicon dioxide / polymer composite microspheres with a three-layer core-shell structure. Background technique [0002] Polymer microspheres with multifunctional and novel structures have become the focus of materials researchers. Polymer microspheres refer to polymer particles with a spherical shape and a particle size ranging from tens of nanometers to hundreds of microns. They have attracted the attention of researchers due to the following characteristics: (1) Small particle size and volume make When the whole particle is used as a microreactor, it has fast response and high reaction rate to external stimuli; (2) The large specific surface area can be used as a position for adsorption, desorption, chemical reaction and light scattering. Usually, 1g of polymer particles with a size of 100nm has a surface...

Claims

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Application Information

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IPC IPC(8): C08L33/02C08L25/06C08L25/08C08K3/36C08K3/30C08K3/22C08K3/08C08F120/06C08F112/08C08F220/06C08F212/08C08F2/44B01J13/14
Inventor 常津刘俊庆宋涛李云红张琼文
Owner TIANJIN UNIV
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