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Organic-inorganic hybrid nanoparticle based on POSS (polysilsesquioxane) and ferrocene as well as preparation method of organic-inorganic hybrid nanoparticle

A technology of polysilsesquioxane and hybrid nanoparticles, which is applied in the field of organic-inorganic hybrid nanoparticles, can solve the problems of single redox responsiveness of nanoparticles, and achieve the effect of mild conditions and simple methods

Inactive Publication Date: 2017-06-13
CENT SOUTH UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, again, the nanoparticles only have a relatively simple redox responsiveness
At present, there are no related reports on organic-inorganic hybrid nanoparticles based on POSS and ferrocene

Method used

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  • Organic-inorganic hybrid nanoparticle based on POSS (polysilsesquioxane) and ferrocene as well as preparation method of organic-inorganic hybrid nanoparticle
  • Organic-inorganic hybrid nanoparticle based on POSS (polysilsesquioxane) and ferrocene as well as preparation method of organic-inorganic hybrid nanoparticle
  • Organic-inorganic hybrid nanoparticle based on POSS (polysilsesquioxane) and ferrocene as well as preparation method of organic-inorganic hybrid nanoparticle

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0038] Synthesis of Ferrocenyl Hydroxyethyl Methacrylate (MAEFc):

[0039]10.0g (43.47mmol) of ferrocenecarboxylic acid (Fc-COOH), 8.49g (65.21mmol) of hydroxyethyl methacrylate (HEMA) and 0.64g (5.22mmol) of N,N-dimethylaminopyridine (DMAP) Add it into a round-bottomed flask containing 300 mL of ultra-dry dichloromethane solvent, stir it magnetically, and place the reaction system in a low-temperature reactor to cool to 0°C. Under the protection of nitrogen, slowly drop the mixed solution of 10.75g (52.16mmol) N,N'-dicyclohexylcarboimide (DCC) and 50mL ultra-dry dichloromethane solvent from the constant pressure dropping funnel. Afterwards, the reaction was continued at 0°C for 2 hours, and then at room temperature for 24 hours. Suction filter the reaction solution, add silica gel powder to the filtrate to mix the sample, pass through the column in a dry method, the eluent is petroleum ether: ethyl acetate = 19:1, elute and separate the first point, spin the solvent with a r...

Embodiment 2

[0041] Synthesis of bromoisobutyramided hexahedral oligomeric silsesquioxane (POSS-Br):

[0042] Add 8g (9.15mmol) POSS-NH to a 250mL single-necked round bottom flask 2 , 3.71g (36.59mmol) triethylamine (NEt 3 ), 150mL of ultra-dry dichloromethane solvent and dissolved under magnetic stirring, the reaction system was placed in a low-temperature reactor and cooled to 0°C, and 4.21g (18.30mmol) of α-bromoiso A mixed solution of butyryl bromide (BIBB) and 20 mL of ultra-dry dichloromethane solvent was reacted at 0° C. for 2 hours after the dropwise addition, and then reacted at room temperature for 24 hours. The reaction solution was suction filtered to remove the white precipitate, concentrated to 40 mL by a rotary evaporator, and washed repeatedly with 1 mol / L dilute HCl solution, 1 mol / L NaOH solution, and deionized water until the pH of the solution was 7-8, and anhydrous MgSO 4 Dry, filter, and remove most of the solvent by rotary evaporation. Re-wet through the silica ge...

Embodiment 3

[0044] POSS-PDMAEMA 108 -Synthesis of Br:

[0045] Add 0.326g (0.318mmol) POSS-Br, 5.0g (31.8mmol) DMAEMA, 0.1102g (0.636mmol) PMDETA, and 5mLTHF into a polymer reaction bottle with a branch, freeze and vacuumize with liquid nitrogen, thaw with ethanol and blow with nitrogen , repeated 3 times, and finally added 0.0472g (0.477mmol) CuCl, the same liquid nitrogen freezing vacuum, ethanol thawing nitrogen, repeated 3 times, to eliminate the oxygen in the reaction system. React at 60°C for 3 hours. After the reaction, quench, expose the system to the air, and add 20mLTHF to terminate the reaction. Use THE as the mobile phase, pass through a 200-300 mesh neutral alumina column to remove copper salts, and concentrate with a rotary evaporator to Add 5mL dropwise to 40mL frozen petroleum ether for precipitation to obtain a white viscous solid, pour off the upper liquid, and repeat the precipitation for 3 to 4 times in order to completely remove unreacted monomers, and place the obta...

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Abstract

The invention discloses an organic-inorganic hybrid nanoparticle based on POSS (polysilsesquioxane) and ferrocene as well as a preparation method of the organic-inorganic hybrid nanoparticle. The organic-inorganic hybrid nanoparticle is obtained by self-assembling POSS-terminated poly(dimethylaminoethyl methacrylate)-b-poly(ferrocenyl hydroxyethyl methylacrylate) in an aqueous solution. The preparation method is simple, the condition is mild, the prepared organic-inorganic hybrid nanoparticle has the characteristics of temperature, pH and oxidation-reduction property response, the particle size can be regulated through temperature, pH, oxidation-reduction property and the like in the environment easily, and the organic-inorganic hybrid nanoparticle has potential application value in the field of functional polymers.

Description

technical field [0001] The invention relates to an organic-inorganic hybrid nanoparticle, in particular to an organic-inorganic hybrid nanoparticle based on hexahedral oligomeric silsesquioxane and ferrocene and a preparation method thereof, belonging to the field of polymer materials. Background technique [0002] Polyhedral Oligomeric Silsesquioxanes (Polyhedral Oligomeric Silsesquioxanes, POSS) is the smallest cage-shaped nano-silica, which has a very stable structure, contains an inorganic silicon-oxygen core, and eight corners are connected to change group, so POSS is a kind of organic-inorganic hybrid molecule with good reactivity. POSS can be used as biomedical materials due to its nontoxicity, good biocompatibility, chemical inertness, mechanical stability, and nanoscale size. POSS can be evenly distributed in various hybrid materials, so that the thermal and mechanical properties of the hybrid materials can be improved. [0003] Ferrocene is an organic transition ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08J3/07C08F293/00C08F220/34C08F230/04C08G77/385C08L53/00
CPCC08F220/34C08F230/04C08F293/005C08F2438/01C08G77/385C08J3/07C08J2353/00
Inventor 孙晓毅刘秀梅李娟王平山
Owner CENT SOUTH UNIV
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