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Preparation method for monodisperse composite nanoparticle

A composite nanoparticle and composite particle technology are applied in the field of preparation of monodisperse composite nanoparticles, which can solve the problems of increased process, increased production cost, long time consumption, etc., and achieves the effect of reducing process, saving cost and having good monodispersity.

Inactive Publication Date: 2009-09-16
QINGDAO HEADLEY NANOTECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The current method for preparing composite particles with core-shell structure has the following defects: the price of silicon coupling agent is many times that of the shell monomer; there will be some SiO in the modification process. 2 Coagulation will waste a certain amount of silicon nuclei; use silicon coupling agent to SiO 2 It takes at least 24 hours to react for surface modification to have a good effect, and the best effect is 48 hours
to SiO 2 Surface - OH modification process is complex and time-consuming
In this way, in industrial production, due to the increase of processes, the use of more expensive materials, SiO 2 Increased production costs due to coagulation losses and increased production time

Method used

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  • Preparation method for monodisperse composite nanoparticle
  • Preparation method for monodisperse composite nanoparticle
  • Preparation method for monodisperse composite nanoparticle

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] as attached figure 1 As shown, set the constant temperature water bath 5, keep the water temperature constant at 75°C, and put 20ml of SiO 2 (solid content 0.3g*ml -1 ), added to 350mL of deionized water, dispersed by ultrasonic vibration for 30min, and then poured into the reactor. Turn on stirrer 1, stir with 120rpm, feed N from nitrogen inlet 3 2 In 30 minutes, potassium persulfate was added from the feed port 4 as an initiator, and the molar concentration of the initiator system was 1.6*10 -3 mol*L -1 . Use advection pump to drop the monomer, and control the feeding time according to the required shell thickness, you can get SiO 2 Composite nanoparticles with organic core as the shell. 35nmSiO 2 Using methyl methacrylate (MMA) as the core to prepare silica / polymethyl methacrylate core-shell composite particles. The feed rate is 0.02, 0.04, 0.06ml*min respectively -1 , take a sample every hour, and measure its average particle size and polydispersity (PDI) v...

Embodiment 2

[0031] as attached figure 1 As shown, set the temperature of the constant temperature water bath at 75°C, and put 20ml of SiO 2 Sol (solid content 0.3g*ml -1 ), added to 350mL deionized water, dispersed by ultrasonic vibration for 20min, and then poured into the reactor. Turn on stirring at 120rpm, feed N 2 After 30 minutes, add potassium persulfate as an initiator, and the molar concentration of the initiator system is 1.6*10 -3 mol*L -1 . Use advection pump to drop the monomer, and control the feeding time according to the required shell thickness, you can get SiO 2 Composite nanoparticles with organic core as the shell. 35nm SiO 2 As the core, use vinyl acetate (VAC) as the monomer to prepare SiO 2 / PVAC (polyvinyl acetate) core-shell structure composite particles. The feed rate is 0.02, 0.04, 0.06ml*min respectively -1 , take a sample every hour, and measure its average particle size and polydispersity PDI value with a laser particle size analyzer. The experiment...

Embodiment 3

[0038] as attached figure 1 shown, with 230nmSiO 2 As the core, SiO was prepared using methyl methacrylate (MMA) as the monomer 2 / PMMA composite particles. Set the temperature of the constant temperature water bath at 75°C, and put 100ml of SiO 2 Sol (solid content 0.05g*ml -1 , particle size 230nm), was added to 200mL deionized water, ultrasonically vibrated and dispersed for 20min, then poured into the reactor. Turn on stirring at 120rpm, feed N from nitrogen inlet 3 2 In 30 minutes, potassium persulfate was added from the feed port 4 as an initiator, and the molar concentration of the initiator system was 1.6*10 -3 mol*L -1 . , use the parallel flow pump to drop the monomer MMA, the feed rate is 0.06ml*min -1 , take a sample every hour, and use a laser particle size analyzer to measure its average particle size and PDI value. The experimental results are shown in Table 3. Control the feed time according to the desired shell thickness, and get SiO 2 Composite na...

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Abstract

The invention relates to a preparation method for a composite nanoparticle with a monodisperse core-shell structure. Nanometer SiO2 is taken as a core, and a SiO2 / high polymer composite nanoparticle is prepared by semi-continuous soap-free emulsion polymerization. The result shows that hydrophilic silicon dioxide which is not modified by a silane coupling agent is taken as the core, and a SiO2 / high polymer composite nanoparticle with the core-shell structure can be prepared by the semi-continuous soap-free emulsion polymerization, and particles have good particle monodispersity. The method has the advantages of few preparation processes, good particle monodispersity, flexible monomer switching, and the like.

Description

technical field [0001] The invention relates to a method for preparing monodisperse composite nanoparticles, which uses a semi-continuous feeding method to prepare monodisperse composite nanoparticles with a core-shell structure through soap-free emulsion polymerization. Background technique [0002] At present, scholars at home and abroad have studied SiO 2 The preparation of polymer / polymer composite nanoparticles has been extensively studied. The current research mainly focuses on two aspects: 1. Using silicon coupling agent to SiO 2 Hydrophobic modification of the surface to improve the SiO 2 Affinity with polymers, and then use styrene, methyl methacrylate or vinyl acetate as the monomer polymerization shell. Experiments show that the feed rate of the monomer, the hydrophilicity of the monomer, the amount of emulsifier, the amount of initiator, the SiO 2 The amount of nanoparticles and the reaction medium have a significant impact on the particle size and particle s...

Claims

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Application Information

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IPC IPC(8): C08F120/14C08F118/08C08F2/22C08K3/36
Inventor 李青松王志强赵辉刘晨光王云芳杨朝合刘相孙兰义
Owner QINGDAO HEADLEY NANOTECH
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