Preparation method of organic/inorganic nano hybridized magnetic material

A technology of inorganic nano and magnetic materials, applied in the field of preparation of organic/inorganic microspheres, can solve the problem of not using active/controllable free radical polymerization, poor controllability, difficulty in controlling the molecular weight and molecular weight distribution of grafted polymers on the surface of inorganic particles, etc. problems, to achieve good controllability, smooth surface and uniform particle size

Inactive Publication Date: 2012-10-31
SUZHOU UNIV
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  • Abstract
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  • Application Information

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Problems solved by technology

[0004] But above-mentioned technical scheme does not adopt active / controllable radical polymerization, therefore, the process controllability of grafting organic polymer on the surface of inorganic particles is poor, makes the molecular weight and the molecular weight distribution of the grafted polymer on the surface of inorganic particles difficult to control
[0005] In the prior art, there is no report on the method of preparing organic / inorganic hybrid particles by surface RAFT polymerization in the environment of soap-free emulsion polymerization.

Method used

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  • Preparation method of organic/inorganic nano hybridized magnetic material
  • Preparation method of organic/inorganic nano hybridized magnetic material
  • Preparation method of organic/inorganic nano hybridized magnetic material

Examples

Experimental program
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Effect test

Embodiment 1

[0030] Example 1: Immobilization of RAFT reagents on the surface of magnetic nanoparticles

[0031] Synthesis of Magnetic Fe by Co-precipitation3 o 4 nanoparticles, and then use Hydrolysis of Tetraethyl Orthosilicate to Magnetic Fe 3 o 4 Nanoparticles are encapsulated to form Fe 3 o 4 SiO 2 core-shell structure.

[0032] Take 1.0g Fe 3 o 4 SiO 2 Add 0.5 mL of 4-chloromethylphenyltrimethoxysilane to 20 mL of toluene that has been dehydrated and dried at 95 ° C, flow argon for 20 min, then reflux for 24 h, and collect by centrifugation. Using a large amount of toluene and acetone for multiple ultrasonic dispersion-centrifugal washing, the chloromethylated product Fe 3 o 4 SiO 2 -Cl was vacuum-dried at room temperature for use.

[0033] In DMSO (20mL) solution with 0.13g KOH dissolved, add 0.39g carbazole, after stirring for 1h, slowly add 0.2mL C 2 S, after the resulting red solution was stirred at room temperature for 12 hours, the chloromethylated product Fe of ...

Embodiment 2

[0034] Embodiment two: soap-free RAFT emulsion graft polymerization synthesis (Fe 3 o 4 SiO 2 PSt)

[0035] Add Fe to a 200mL reaction flask 3 o 4 SiO 2 - BCBD (50 mg), St (0.5 mL, 4.3 mmol), KPS (40 mg, 0.15 mmol), deionized water (50 mL) and a magnetic stirrer. Under ultrasonic conditions, the nanoparticles are uniformly dispersed in water to form a stable white emulsion. It was filled with N 5 times under the condition of constant stirring 2 - Vacuum cycle, finally at N 2 Close the system under atmosphere. The reaction bottle was placed in an oil bath with preset temperature (85°C) for reaction, and after the specified time (12h or 24h), it was cooled to break the emulsification. The product was collected by centrifugation, and the centrifuged product was washed and separated with a large amount of THF: the free PSt precipitate was collected, and the obtained hybrid particles were dried in a vacuum oven for future use.

[0036] The particle size and distribution o...

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Abstract

The invention belongs to the technical field of the preparation of organic / inorganic microspheres, and in particular relates to a method for grafting an organic polymer on the surface of an inorganic nano magnetic particle by adopting a soap-free emulsion polymerization method. The method comprises the following steps of: (1) preparing and obtaining a magnetic nano particle with a reversible addition fragmentation chain transfer agent decorated on the surface according to the prior art, wherein a Z radical is carbazole, and an R radical is a magnetic monox composite nano particle with benzyl;and (2) combining a polymerization system from the magnetic nano particle with the reversible addition fragmentation chain transfer agent decorated on the surface, which is obtained from the steps (1), an oil-soluble monomer, an initiator and water to form a polymerization system, carrying out reversible addition fragmentation chain transfer polymerization in a soap-free emulsion system in an inert atmosphere under a stirring condition and centrifugally separating to obtain the magnetic nano particle which has a polymer shell and uses the magnetic silica nano particle as a core. The inventionavoids using an organic solvent andor an emulsifier in one aspect and has acan controllable the polymerization process in the other aspect.

Description

technical field [0001] The invention belongs to the field of preparation of organic / inorganic microspheres, and in particular relates to a method for grafting organic polymers on the surface of inorganic nano magnetic particles by using a soap-free emulsion polymerization method. Background technique [0002] Emulsion polymerization has been proven to be a very good way to prepare polymer latex particles and organic / inorganic hybrid particles. In recent years, more and more literatures have reported the combined application of "living" controlled free radical polymerization and microemulsions, miniemulsions, etc. However, due to the addition of emulsifiers, it has brought great troubles to the purification of late-polymerization products, and the use of these surfactant-based emulsifiers has caused certain pollution to the environment. [0003] Matsumoto and Ochi first reported the preparation of polystyrene latex particles by soap-free emulsion polymerization (Matsumoto, T...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08F292/00C08F112/08C08F120/14C08F2/22
Inventor 程振平李强朱秀林张丽芬
Owner SUZHOU UNIV
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