Preparation method of PMMA (Polymethyl Methacrylate) nano vacant shells with different thicknesses

A nanometer and empty shell technology is applied in the field of preparation of PMMA nanometer empty shell materials to achieve the effects of low production cost, cheap raw materials and simple process

Active Publication Date: 2014-04-02
泰安泰山科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

So far, few people have used the AGET ATRP method to prepare SiO with tunable shell thickness 2 / polymer, and SiO with tunable shell thickness prepared by the AGET ATRP met...

Method used

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  • Preparation method of PMMA (Polymethyl Methacrylate) nano vacant shells with different thicknesses
  • Preparation method of PMMA (Polymethyl Methacrylate) nano vacant shells with different thicknesses
  • Preparation method of PMMA (Polymethyl Methacrylate) nano vacant shells with different thicknesses

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] (1) Put a 100mL three-neck flask in an oil bath, add 8mL distilled water, 5mL ammonia water and 100mL absolute ethanol; add 5mL TEOS dropwise to the mixed solution under stirring, and stir at 40°C for 12h. After cooling, the obtained solution with white precipitate was centrifuged, and the obtained precipitate was repeatedly washed with distilled water, and dried at 40°C for 12 hours to obtain SiO with a suitable particle size. 2 nanospheres.

[0029] (2) Put a 100mL three-neck flask in an oil bath, add 1.0g SiO 2 , 20mL toluene, magnetically stirred and mixed evenly, 1.7g APTES was added dropwise into the flask, then the temperature was raised to 115°C and the reaction was stirred at this temperature for 18h. After cooling, the obtained solution with white precipitate was centrifuged, and the precipitate obtained after centrifugation was repeatedly washed with toluene by centrifugation. The obtained precipitate was vacuum-dried at 40°C for 12 h to obtain amino-modifi...

Embodiment 2

[0034] The difference from Example 1 is that in step (4), a 100mL three-neck flask was placed in an oil bath, and 6mL N,N-dimethylformamide (DMF), 0.25g SiO 2 -Br, 0.4g FeCl 3 ·6H 2 O, 0.74g PPh 3 After stirring evenly, pass N 2 , add 22.5mL MMA and 35μL ethyl 2-bromoisobutyrate (EBiB) to the mixed solution, after stirring evenly, slowly add the solution of 0.38g vitamin C (VC) dissolved in 3mL DMF to the above homogeneous solution, Then seal the three-neck bottle. The temperature was raised to 95°C for 12h. After cooling, the obtained solution with a light green precipitate was centrifuged, and the precipitate obtained after centrifugation was washed with DMF centrifugation. The obtained precipitate was dried under vacuum at 40 °C for 12 h to obtain SiO 2 - PMMA (ie SM2).

Embodiment 3

[0036] The difference from Example 1 is that in step (4), a 100mL three-neck flask was placed in an oil bath, and 6mL N,N-dimethylformamide (DMF), 0.25g SiO 2 -Br, 0.4g FeCl 3 ·6H 2 O, 0.74g PPh 3 After stirring evenly, pass N 2 , add 30mL MMA and 35μL ethyl 2-bromoisobutyrate (EBiB) to the mixed solution, after stirring evenly, slowly add the solution of 0.38g vitamin C (VC) dissolved in 3mL DMF to the above homogeneous solution, then Seal the three-neck bottle. The temperature was raised to 95°C for 12h. After cooling, the obtained solution with a light green precipitate was centrifuged, and the precipitate obtained after centrifugation was washed with DMF centrifugation.

[0037] The obtained precipitate was dried under vacuum at 40 °C for 12 h to obtain SiO 2 - PMMA (ie SM3).

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Abstract

The invention discloses a preparation method of PMMA (Polymethyl Methacrylate) nano vacant shells with different thicknesses, and relates to SiO2-PMMA nano composite materials with different shell thicknesses, a synthesizing method and regulation of shell thicknesses of vacant PMMA. The preparation method comprises the following steps: preparing spherical nano SiO2 with proper grain size; then, carrying out backflow at 95 DEG C for 12 hours by 3-aminopropyltriethoxysilane (APTES) to modify SiO2 to obtain SiO2-NH2; then carrying out bromine modification on SiO2-NH2 at 0 DEG C by 2-bromoisobutyryl bromine (BiB); successfully adjusting the shell thickness of PMMA by adjusting the amounts of monomer methyl methacrylate (MMA) and ligand triphenylphosphine (PPh3) in a reaction system by an AGET ATRP (Activator Generated by Electron Transfer Atom Transfer Radical Polymerization) method; and then, etching nanosilicon dioxide balls by hydrofluoric acid to obtain the PMMA polymer vacant shells with different thicknesses.

Description

technical field [0001] The invention relates to a preparation method of a PMMA nano hollow shell material with different shell thicknesses, belonging to the technical field of material synthesis. Background technique [0002] In recent years, with core-shell structure, functionalized SiO 2 It has attracted widespread attention due to its many potential uses in industry, such as reinforcement for coatings and plastic fillers, antibacterial agents, fluorescent materials, photocatalysts, and biotechnology. And because methyl methacrylate (MMA) is the most commonly used monomer for synthesizing polymers, atom transfer radical polymerization (ATRP) is the most widely used method for preparing functionalized silica and various polymers with a core-shell structure. , which is mainly because this method is suitable for a wide variety of monomers, and can obtain intact polymers with controllable molecular weight, low polydispersity index and various functionalizations. [0003] The...

Claims

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Application Information

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IPC IPC(8): B01J13/02C08F120/14
Inventor 周国伟张磊赵敏南张金玉
Owner 泰安泰山科技有限公司
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