Method for preparing SiO2-poly(dimethylaminoethyl methacrylate) (PDMAEMA) nanoparticles having core-shell structure

A nanoparticle and shell structure technology, applied in the field of nanometers, can solve the problem of uncontrollable molecular weight of shell polymers, and achieve the effects of short preparation cycle, mild reaction conditions and controllable molecular weight

Active Publication Date: 2010-11-24
CHANGZHOU INST OF ENERGY STORAGE MATERIALS &DEVICES
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  • Summary
  • Abstract
  • Description
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  • Application Information

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Problems solved by technology

) This preparation method does not use a deactivator in the polymerization process, therefore, the molecular weight of the shell polymer in the prepared core-shell structure is uncontrollable

Method used

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  • Method for preparing SiO2-poly(dimethylaminoethyl methacrylate) (PDMAEMA) nanoparticles having core-shell structure
  • Method for preparing SiO2-poly(dimethylaminoethyl methacrylate) (PDMAEMA) nanoparticles having core-shell structure
  • Method for preparing SiO2-poly(dimethylaminoethyl methacrylate) (PDMAEMA) nanoparticles having core-shell structure

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preparation example Construction

[0032] The embodiment of the present invention provides a core-shell structure of SiO 2 The preparation method of @PDMAEMA nanoparticles is characterized in that it includes:

[0033] CuX 2 , ligand, initiator modified SiO 2The nanoparticles, the solvent and N,N-dimethylaminoethyl methacrylate are mixed to obtain the first mixed liquid, and the ligands are pentamethyldiethylenetriamine, 2,2-bipyridine, 4, 4-Dinonyl-2,2-bipyridine, tetramethylethylenediamine, hexamethyltriethylenetetramine, tris[2-(dimethylamino)ethyl]amine or tris[(2-pyridine base) methyl] amine, the SiO modified by the initiator 2 The initiator in the nanoparticles is 2-bromoisobutyryl bromide or a compound shown in (I),

[0034]

[0035] Wherein, n≥3, R is an ethoxy group or a chlorine atom;

[0036] 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 is Cl or Br;

[0037] Deoxidize the reaction raw ...

Embodiment 1

[0060] When the initiator modified SiO 2 Preparation of initiator-modified SiO2 when the initiator in the nanoparticles is 2-bromoisobutyryl bromide 2 Nanoparticles:

[0061] Mix 100ml of absolute ethanol, ammonia water and tetraethyl orthosilicate (TEOS) (NH 3 , H 2 (0, 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, obtained the first product;

[0062] Disperse the first product in absolute ethanol, mix it with the silane coupling agent 3-aminopropyltrimethoxysilane under the catalysis of ammonia water, stir at 60°C for 12 hours, centrifuge and wash with toluene to obtain the first product Second product;

[0063] Disperse the second product in anhydrous toluene, add triethylamine, add 2-bromoisobutyryl bromide dropwise while stirring in an ice-water bath, stir at room temperature for 12 hours after 0.5h, centrifuge and wash with toluene, and ...

Embodiment 2

[0065] When the initiator modified SiO 2 Preparation of initiator-modified SiO2 when the initiator in the nanoparticles is 2-bromodimethylhexylpropionate triethoxysilane2 Nanoparticles:

[0066] At 0°C, 2-bromoisobutyryl bromide (63mL, 510mmol) was added dropwise to 5-hexenyl-1-ol (43g, 430mmol), triethylamine (71mL, 510mmol) and anhydrous tetrahydrofuran (1L) In the mixed solution, after stirring for 3 hours, stir at room temperature for 10 hours, filter the reaction solution with suction, distill the filtrate under reduced pressure, dilute the residue with chloroform (500 mL), and wash twice with 1 mol / L hydrochloric acid, saturated sodium bicarbonate, and deionized water , dry and suction filter over anhydrous sodium sulfate, and finally pass through a silica gel column (n-hexane / ethyl acetate with a volume ratio of 15 / 1 as eluent) to obtain transparent liquid 2-bromodimethylpropionate 5-hexenyl ;

[0067] Add 5-hexenyl 2-bromodimethylpropionate (40g, 160mmol) into a two-...

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Abstract

The invention relates to the field of nano technology and discloses a method for preparing SiO2-PDMAEMA nanoparticles having a core-shell structure. The method comprises the following steps of: selecting 2-bromideisobutyryl bromide with a higher initiation activity or a compound represented by a formula (I) as an initiator by using an atom-transfer radical-polymerization method; and during reaction, mixing CuX2 serving as a passivator, a ligand, SiO2 nanoparticles modified by the initiator, a solvent and diethylaminoethyl methacrylate at first and then adding CuX to perform a grafting reaction to obtain the SiO2-PDMAEMA nanoparticles with the core-shell structure. Experiments show that: the prepared SiO2-PDMAEMA nanoparticles have the advantages of controllable particle size, narrow particle size distribution and controllable molecular weight of the polymer PDMAEMA grafted on the surface of SiO2. Moreover, the preparation method provided by the invention has the characteristics of mild reaction conditions, convenience, feasibility and short preparation period and is easy for mass production.

Description

technical field [0001] The present invention relates to a kind of nanotechnology field, more specifically, relate to a kind of core-shell structure SiO 2 Preparation method of @PDMAEMA nanoparticles. Background technique [0002] In recent years, core-shell nanocomposites are gradually becoming a research hotspot in the field of nanotechnology. Since the structure and composition of composite nanoparticles with core-shell structure can be tailored and designed at the nanoscale, they have many unique physical and chemical properties, such as optical, electrical, and magnetic, which are different from single-component particles. At present, there are many types of core-shell structure composite particles involved in research at home and abroad, mainly including semiconductor core-semiconductor shell, metal core-metal shell and inorganic core-polymer shell composite particles, among which inorganic core-polymer shell Nanocomposite materials composed of nanoparticles are devel...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F292/00
Inventor 董志鑫姬相玲魏华毛骏
Owner CHANGZHOU INST OF ENERGY STORAGE MATERIALS &DEVICES
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