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Surface carboxyl functionalized polystyrene / nano silicon dioxide hybridization material and preparation thereof

A nano-silica, carboxyl functionalization technology, applied in the field of polymer materials

Inactive Publication Date: 2010-12-22
NORTHWEST NORMAL UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, due to the shortcomings of the ATRP system itself, there are still certain limitations in the synthesis of functional monomers containing amide and carboxyl groups, and the application of click chemistry to introduce special functional groups has better results.

Method used

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  • Surface carboxyl functionalized polystyrene / nano silicon dioxide hybridization material and preparation thereof
  • Surface carboxyl functionalized polystyrene / nano silicon dioxide hybridization material and preparation thereof
  • Surface carboxyl functionalized polystyrene / nano silicon dioxide hybridization material and preparation thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0056] (1) Terminal azido-based polystyrene / nano-silica particles

[0057] Add 5g of nano-silica particles to a 50ml round-bottomed flask, dry 30ml of toluene, ultrasonically disperse for 30min, add 40mmol of aminopropyltriethoxysilane coupling agent, and heat to reflux for 10h. After the reaction was completed, it was centrifuged at a speed of 4800 rpm, washed several times with chloroform, and then washed several times with ethanol. Nanoparticles were vacuum-dried at 40°C for 24 h, and recorded as surface-ammoniated silica particles (SiO 2 -NH 2 ). The above 1g SiO 2 -NH 2 Disperse the particles in 30ml of anhydrous acetonitrile, stir in an ice bath for 2 hours, then add 2mmol of triethylamine dropwise, continue stirring in an ice bath for 40 minutes, then add 2mmol of α-bromoisobutyl bromide dropwise, stir and react in an ice bath for 6 hours, then room temperature Stir the reaction for 24 hours to end the reaction, filter, and wash the product with saturated NaCl solu...

Embodiment 2

[0063] (1) Terminal azido-based polystyrene / nano-silica particles

[0064] Add 5g of nano-silica particles and 30ml of absolute ethanol to a 50ml round-bottomed flask, ultrasonically disperse for 30min, add 40mmol of aminopropyltrimethoxysilane coupling agent, and heat to reflux for 12h. After the reaction was completed, it was centrifuged at a speed of 4800 rpm, washed several times with chloroform, and then washed several times with ethanol. Nanoparticles were vacuum-dried at 40°C for 24 h, and recorded as surface-ammoniated silica particles (SiO 2 -NH 2 ). The above 2g SiO 2 -NH 2 Disperse the particles in 30-50ml of chloroform, stir in ice bath for 4h, add 4mmol triethylamine dropwise, continue stirring in ice bath for 60min, then add dropwise 4mmolα-bromoisobutyl bromide, stir in ice bath for 8h, then normal temperature Stir the reaction for 30 hours to end the reaction, filter, and wash the product with saturated NaCl solution, ethanol, and distilled water, then dry...

Embodiment 3

[0070] (1) Terminal azido-based polystyrene / nano-silica particles

[0071] Add 5g of nano-silica particles to a 50ml round bottom flask, dry 30ml of toluene, ultrasonically disperse for 30min, add 40mmol of aminopropyltriethoxysilane coupling agent, and heat to reflux for 9h. After the reaction was completed, it was centrifuged at a speed of 4800 rpm, washed several times with chloroform, and then washed several times with ethanol. Nanoparticles were vacuum-dried at 40°C for 24 h, and recorded as surface-ammoniated silica particles (SiO 2 -NH 2 ). The above 1.5g SiO 2 -NH 2 Disperse the particles in 45ml of anhydrous acetonitrile, stir in an ice bath for 3 hours, then add 3mmol of triethylamine dropwise, continue stirring in an ice bath for 40 minutes, then add 3mmol of α-bromoisobutyl bromide dropwise, stir in an ice bath for 6 hours, and then add to room temperature Stir the reaction for 24 hours to end the reaction, filter, and wash the product with saturated NaCl solu...

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Abstract

The invention discloses a method for preparing surface carboxylic group functional polystyrene / nano-silicon dioxide hybrid material by effectively combining click chemistry and ATRP; in the method, a silane coupling agent is adopted for linking an ATRP evocating agent to a SiO2 particle surface, and polystyrene (PSt) is grafted on the SiO2 particle surface by adopting the ATRP; then, carboxyl is led into a nano-silicon dioxide particle surface modified by the polystyrene by means of the click reaction, thus obtaining the surface carboxylic group functional polystyrene / nano-silicon dioxide hybrid material. After the infrared, nuclear magnetism and thermogravimetry mapping analysis, the surface carboxylic group functional polystyrene / nano-silicon dioxide hybrid material prepared by the invention has good thermal stability and dispersivity; in addition, as the carboxyl has wide reaction range and the characteristic of easy ionization, nano-particles has high reactive behavior so as to bewidely applied to the fields such as high polymer material modifying agents, water treatment agents, catalysts, sensing agents and protein carriers.

Description

technical field [0001] The invention belongs to the technical field of polymer materials, and relates to a surface carboxyl-functionalized polystyrene / nano-silicon dioxide hybrid material and its preparation, in particular to an effective combination of click chemistry and atom transfer radical polymerization (ATRP). A method for surface carboxyl functionalization of polystyrene / nanosilica hybrid materials. Background technique [0002] The properties of the material surface are an important part of the material properties, such as wetting, adsorption, etc. are related to the properties of the material surface. With the development of science and technology and the deepening of research in related fields, new requirements are put forward for the design and preparation of new materials with special surface properties. Nanomaterials are an important research direction of materials science, and their applications involve many fields. In the process of its application, on the ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08F292/00C08F8/00
Inventor 王云普陈久存卢全颜小东李宏军魏铄蕴
Owner NORTHWEST NORMAL UNIVERSITY
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