Preparation method of organic/inorganic nano hybridized magnetic material

A technology of inorganic nano and magnetic materials, applied in the field of organic/inorganic microsphere preparation, can solve the problem of poor controllability, difficult to control the molecular weight and molecular weight distribution of the grafted polymer on the surface of inorganic particles, no active/controllable free radical polymerization, etc. problem, to achieve the effect of smooth surface, good controllability and convenient design

Inactive Publication Date: 2011-01-05
SUZHOU UNIV
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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 distribut

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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Example Embodiment

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

[0031] Synthesize magnetic Fe by co-precipitation method 3 O 4 Nanoparticles and then use Hydrolysis of tetraethyl orthosilicate to magnetic Fe 3 O 4 Nano particles are encapsulated to form Fe 3 O 4 @SiO 2 The core-shell structure.

[0032] Take 1.0g Fe 3 O 4 @SiO 2 Nanoparticles were added to 20 mL of dewatered and dried toluene, 0.5 mL of 4-chloromethylphenyltrimethoxysilane was added at 95°C, argon was ventilated for 20 minutes, then refluxed for 24 hours, and collected by centrifugation. Use a large amount of toluene and acetone to disperse by ultrasonic for many times-centrifugal washing, the product of chloromethylation Fe 3 O 4 @SiO 2 -Cl was dried under vacuum at room temperature and set aside.

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

Example Embodiment

[0034] Example 2: Soap-free RAFT emulsion graft polymerization synthesis (Fe 3 O 4 @SiO 2 @PSt)

[0035] Add Fe into 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 stirring magnet. Under ultrasonic conditions, the nanoparticles are uniformly dispersed in water to form a stable white emulsion. Charge it 5 times with N under constant stirring 2 -Vacuum cycle, finally at N 2 Closed system under atmosphere. Place the reaction flask in an oil bath with a preset temperature (85°C) for reaction. After the specified time (12h or 24h), cool it to break the emulsion. 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 use.

[0036] The particle size and distribution of the nanoparticles obtained before and after polymerization are sh...

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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 invention avoids 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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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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