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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  • Abstract
  • Description
  • Claims
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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 ho

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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
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Example Embodiment

[0023] Example 1:

[0024] As attached figure 1 As shown, set a constant temperature water bath 5, keep the water temperature constant at 75 ℃, add 20ml SiO 2 (Solid content 0.3g*ml -1 ), added to 350 mL of deionized water, dispersed by ultrasonic vibration for 30 minutes, and poured into the reactor. Turn on the stirrer 1, stir at 120 rpm, and pass N through the nitrogen inlet 3. 2 In 30 minutes, add potassium persulfate as initiator from feed port 4, the molar concentration of the initiator system is 1.6*10 -3 mol*L -1 . Use the advection pump to drop the monomer and control the feeding time according to the required thickness of the shell layer to obtain SiO 2 It is a composite nanoparticle with an organic shell as the core. Now 35nmSiO 2 As the core, methyl methacrylate (MMA) was used as the monomer to prepare silica / polymethyl methacrylate core-shell structure composite particles. The feed rate is 0.02, 0.04, 0.06ml*min -1 , Take a sample every hour, and measure its average ...

Example Embodiment

[0030] Example 2:

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

Example Embodiment

[0037] Example 3:

[0038] As attached figure 1 As shown, with 230nmSiO 2 As the core, SiO is prepared with methyl methacrylate (MMA) as the monomer 2 / PMMA composite particles. Set the constant temperature of the constant temperature water bath at 75 ℃, add 100ml SiO 2 Sol (solid content 0.05g*ml -1 , Particle size 230nm), added to 200mL deionized water, ultrasonic vibration dispersion for 20min, then poured into the reactor. Turn on the stirring at 120 rpm, and pass in N from the nitrogen inlet 3 2 In 30 minutes, add potassium persulfate as initiator from feed port 4, the molar concentration of the initiator system is 1.6*10 -3 mol*L -1 . , Use advection pump to add monomer MMA dropwise, feed rate is 0.06ml*min -1 , Take a sample every hour, and measure its average particle size and PDI value with a laser particle size analyzer. The experimental results are shown in Table 3. Control the feeding time according to the required thickness of the shell layer to obtain SiO 2 It is a ...

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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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