Method for preparing magnetic POSS

A magnetic and modified technology, applied in inductor/transformer/magnet manufacturing, nanotechnology for materials and surface science, nanotechnology, etc., can solve problems such as high cost and reduced polymer strength, and achieve improved battery performance, The effect of improving the use efficiency and life, excellent electrochemical performance

Inactive Publication Date: 2015-01-14
TIANJIN POLYTECHNIC UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Due to the hole structure, Leu Chyi-Ming et al. (Macromolecules2003, 36, 9122-9127) reported that POSS was introduced into polyimide to reduce the dielectric constant of the polymer and achieved a relatively ideal effect. Imine carries out fluorination and reduces dielectric constant, but this method makes the strength of polymer reduce and cost is too high, and introducing POSS can improve the mechanical property of polymer simultaneously; Chinnam Parameswara Rao etc. (Chemistry of Materials2011,23,5111-5...

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] (1) Fe 3 o 4 (I) Preparation

[0021] 1.17g Fe 3 o 4 Disperse in 30ml of distilled toluene, ultrasonic for 3 hours, add 1ml of triethylamine to the above solution as an acid-binding agent, under the protection of nitrogen, inject 1ml of methyldichlorosilane at a slow speed at room temperature, stir rapidly for 30min, then heat to 65°C The reaction was carried out for 15 hours. After the reaction was completed, the product was precipitated with a magnet, washed several times with absolute ethanol, and dried in vacuum.

[0022] (2) Preparation of POSS (I)

[0023] Dissolve 1.0g of cyclopentyl dihydroxy POSS in 40ml of distilled tetrahydrofuran, place in an ice-water bath, add 0.8ml of diethylamine as an acid-binding agent, add 0.16ml of methylvinyldichlorosilane under nitrogen protection, and react for 1h After rising to room temperature, the reaction was continued for 5-6 hours. After the reaction was completed, the by-products were filtered off, the solvent was dis...

Embodiment 2

[0027] (1) Fe 3 o 4 (I) Preparation

[0028] 0.5g Fe 3 o 4 Disperse in anhydrous toluene and sonicate for 1 h, add 1 ml of bis-(3-methoxy-silyl)-propyl methacrylate, and react for 8 h at 55°C under nitrogen protection.

[0029] (2) Preparation of POSS (I)

[0030]Dissolve 0.3g of cyclopentyl trihydroxy POSS in 30ml of distilled tetrahydrofuran, add 0.5ml of diethylamine, place in an ice-water bath, add 0.06ml of trichlorosilane under nitrogen protection, and react for 11 hours. After the reaction, the white by-product After filtration, the tetrahydrofuran was evaporated to dryness, and the product was precipitated with ethanol and dried in vacuo.

[0031] (3) Fe 3 o 4 - Preparation of POSS

[0032] POSS (I) 0.12g, dissolve in 20ml distilled toluene, add 0.05g Fe 3 o 4 (1) Ultrasound for 30 min, react in an oil bath at 75° C., add 10 ml of toluene solution containing 0.1 ml of platinum catalyst, react for 25 h under nitrogen protection, wash repeatedly with ethanol af...

Embodiment 3

[0034] (1) Fe 3 o 4 (I) Preparation

[0035] 1.10g Fe 3 o 4 Disperse in 30ml of dehydrated methyl sulfoxide, add 2.6ml of diethylamine to the solution, after ultrasonication for 1h, inject 1ml of methylchlorosilane, react at 60°C for 5h, precipitate the product with a magnet after the reaction is completed, and use anhydrous Washed repeatedly with ethanol and dried.

[0036] (2) Preparation of POSS (I)

[0037] Dissolve 0.3g of cyclopentyl trihydroxy POSS in 30ml of dehydrated tetrahydrofuran, place it in a water bath at 40°C, and add 0.084ml of tris-(3-methoxy-silyl)-methacrylic acid to the solution under nitrogen protection Propyl ester, the solvent was removed after 8 hours of reaction, the product was precipitated with acetone and washed repeatedly, and dried.

[0038] (3) Fe 3 o 4 - Preparation of POSS

[0039] POSS(I) and Fe 3 o 4 (1) Add reaction in equimolar ratio, disperse in 30ml of distilled toluene, sonicate for 1h, add 0.1ml of platinum catalyst, react ...

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PUM

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Abstract

The invention discloses a method for preparing a magnetic POSS compound. The method comprises the steps that first, magnetic spherical Fe3O4 particles are prepared with a coprecipitation method, the diameter of each magnetic spherical Fe3O4 particle is 20 nm, and then dichloromethylsilane or 3-(trimethoxysilyl)propyl methacrylate is used for modifying the magnetic spherical Fe3O4 particles, and magnetic Fe3O4 containing Si-H or C=C is obtained; second, cyclopentyltrichlorosilane carries out self-assembly in an aqueous solution to form cyclopentyl trihydroxy POSS, dichloromethylvinylsilane or trichlorosilane or 3-(trimethoxysilyl)propyl methacrylate is used for modifying the cyclopentyl trihydroxy POSS, and POSS containing Si-H or C=C is obtained; third, the modified Fe3O4 and the modified POSS are processed through hydrosilylation under the condition of a Pt catalyst so that the magnetic POSS can be obtained. The method has the advantages of being easy to operate, low in reaction temperature and easy to implement. The strength of the modified POSS reaches 18.7 emu/g.

Description

technical field [0001] The present invention belongs to Fe 3 o 4 / POSS nanocomposite material field, in particular to a preparation method of magnetic POSS (polyhedral oligomeric silsesquioxane). Background technique [0002] Fe 3 o 4 It is a kind of magnetic particle, which has superparamagnetism when the particle size is less than 50nm. Monodisperse Fe3O4 magnetic nanoparticles have been widely studied due to their potential value in biomedicine and their unique physicochemical properties. Its specific applications involve selective adsorption of heavy metal ions in wastewater, cell separation, drug delivery carriers, tumor treatment, compounding with polymers, catalysts, magnetic fluids, magnetic recording materials, magnetic resonance imaging, etc. Due to Fe 3 o 4 Belongs to the category of inorganic materials, poor compatibility with organic materials, and pure Fe 3 o 4 It is easily oxidized when exposed to the air, has extremely high surface energy, and has se...

Claims

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Application Information

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IPC IPC(8): H01F41/02C07F7/21C08L83/04C08K9/06C08K3/22B82Y30/00B82Y40/00
Inventor 宋晓艳周胜之程博闻
Owner TIANJIN POLYTECHNIC UNIV
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