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Preparation method for photoresponse hybrid nano-particle

A technology for hybridizing nanoparticles and nanoparticles, which is applied in the nano field to achieve the effects of mild reaction conditions, reversible cross-linking-de-cross-linking process, and simple and easy method.

Active Publication Date: 2012-07-25
CHANGZHOU INST OF ENERGY STORAGE MATERIALS &DEVICES
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] However, the prior art rarely involves polymer / inorganic nanoparticle hybrid systems containing coumarin groups, so the preparation method of polymer / inorganic nanoparticle hybrid systems containing coumarin groups remains to be further studied

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  • Preparation method for photoresponse hybrid nano-particle

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[0028] The invention discloses a preparation method of photoresponsive hybrid nanoparticles, which is characterized in that it comprises the following steps: N, N-dimethylaminoethyl methacrylate (DMAEMA), double bond modified coumarin ( CMA), CuX 2 , pentamethyldiethylenetriamine (PMDETA), initiator-modified SiO 2 The nanoparticles are mixed with the first solvent to obtain a first mixed solution; the first mixed solution is subjected to deoxidation treatment, and CuX is added to obtain a reaction raw material solution, and the CuX 2 and X in CuX are respectively Cl or Br; the reaction raw material solution is subjected to deoxidation treatment, and photoresponsive hybrid nanoparticles are obtained after the reaction.

[0029] The above-mentioned feeding sequence determines whether the final grafting reaction can proceed smoothly. In the present invention, N,N-dimethylaminoethyl methacrylate, double bond modified coumarin, CuX 2 , pentamethyldiethylenetriamine, initiator-mo...

Embodiment 1

[0044] Example 1: Preparation of initiator-modified SiO 2 Nanoparticles:

[0045] Using absolute ethanol as a solvent, ammonia as a catalyst, and TEOS as a silicon source, anhydrous ethanol, ammonia, and tetraethyl orthosilicate (TEOS) were mixed to obtain 551.5 mL of a mixed solution (NH 3 , H 2 O, TEOS concentration is respectively 0.6mol / L, 1.7mol / L, 0.1mol / L), stirred at room temperature for 24h, obtained white transparent sol, centrifuged, washed with absolute ethanol, finally dispersed in absolute ethanol, in Ammonia (25wt%, 100μL) was catalyzed to react with silane coupling agent APTMS (0.8mL, 3.4mmol) at 60°C for 12h; centrifuged and washed with toluene; the washed nanoparticles were dispersed in anhydrous toluene, three Ethylamine (0.6mL, 7.4mmol) was used as a catalyst, and 2-bromoisobutyryl bromide (0.5mL, 4.0mmol) was added dropwise while stirring in an ice-water bath, reacted for 0.5h, then stirred at room temperature for 12h; centrifuged and washed with toluene...

Embodiment 2

[0046] Embodiment 2: the preparation of double bond modified coumarin monomer:

[0047] Add 5.0g of 7-hydroxy-4-methylcoumarin, 5.0g of 2-bromoethanol, 3.0g of potassium carbonate, 50mL of absolute ethanol into the two-necked flask, and reflux at 85°C for 20h, then cool the reaction liquid and wash it with anhydrous Wash with ether and water, wash the organic layer three times with anhydrous ether, add anhydrous magnesium sulfate to dry for 12 hours, remove the solvent, recrystallize from absolute ethanol three times, filter with suction, and dry in vacuum to obtain coumarin modified by 2-bromoethanol;

[0048] Add 5.0 g of triethylamine, 5.0 g of the 2-bromoethanol-modified coumarin prepared above, and 80 mL of anhydrous chloroform into a three-necked flask, and add 5.0 g of methacryloyl chloride dropwise in an ice-water bath. React for 12 hours, then add dichloromethane to the reaction solution to dilute the reaction solution, wash the organic layer three times with saturate...

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Abstract

The invention discloses a preparation method for a photoresponse hybrid nano-particle, which includes the steps: copolymerizing and grafting N, N-dimethylaminoethyl methacrylate (DMAEMA) and double-bond modified CMA (coumarin) on the surface of a SiO2 (silicon dioxide) nano-particle by means of ATRP (atom transfer radical polymerization), so that the photoresponse SiO2-g-P (DMAEMA-co-CMA) hybrid nano-particle is prepared. Compared with the prior art, the method is the first to copolymerize and graft the DMAEMA) and the CMA on the surface of the SiO2 nano-particle, so that the prepared hybrid nano-particle has photoresponse, biocompatibility and 'amphibiousness'. The preparation method is mild in reaction conditions, simple, convenient, feasible, short in preparation cycle and easy in large-scale production. As experimental results show, by means of adjusting the wavelength of ultraviolet illumination, the crosslinking-decrosslinking process of a photoresponse hybrid nano-particle polymer shell is reversible, and the prepared photoresponse hybrid nano-particle has the advantages of narrow size distribution and adjustability in size.

Description

technical field [0001] The invention relates to the field of nanotechnology, more specifically, to a method for preparing photoresponsive hybrid nanoparticles. Background technique [0002] As a kind of smart materials, photoresponsive materials are widely used in liquid crystals, fluorescent labels, liquid chromatography, and drug sustained release. Among them, coumarin is an important light-responsive compound and has been extensively studied. When coumarin and its derivatives are irradiated by ultraviolet light greater than 310nm, a cycloaddition reaction will occur to form a dimer; after being irradiated by ultraviolet light less than 260nm, the formed dimer will be disentangled and return to the original state. Since coumarin and its derivatives do not need to add other compounds, they can be cross-linked only by ultraviolet light irradiation, and no by-products are produced during the cross-linking process. The degree of cross-linking can be adjusted by changing the l...

Claims

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Application Information

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IPC IPC(8): C08F292/00C08F220/34C08F220/32C08J3/28C08J3/24
Inventor 董志鑫姬相玲毛骏王大鹏杨木泉薛彦虎
Owner CHANGZHOU INST OF ENERGY STORAGE MATERIALS &DEVICES
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