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Preparation method for SiO2-based organic-inorganic hybridized fluorescent material
Inactive Publication Date: 2013-07-10
BEIJING UNIV OF TECH
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Qiu Shilun et al. (Chemical Journal of Chinese Universities. 2006; 27:397-400) found that the organic-inorganic hybrid material formed by loading coumarin 151 on the surface of MCM-41 by the traditional co-hydrolysis polycondensation method, although it can maintain the fluorescent material Luminescent properties, but the preparation cycle is as long as 5 to 7 days, which seriously affects the synthesis efficiency; Li Zenghe et al. filed an application number of 200810104323.X on April 17, 2008. The name of the invention is a rare earth organic-inorganic hybrid fluorescent material Synthetic method, synthesized a kind of fluorescent material by hydrothermal method, this method has relatively high requirement to equipment, and cost is also higher, and safety performance is poorer; The patent for the synthesis method of organic / inorganic nano-hybrid materials, the patent of application number 98116430.7 of Dong Dewen et al. The invention title is the patent of the synthesis method of rare earth-containing organic / inorganic nano-hybrid luminescent materials, the application number of Chen Yanming et al. is 00128253.0 The patent of the invention titled the synthesis method of organic / inorganic nano-cadmiumsulfide hybrid luminescent material adopts the sol-gel method, and the entire sol-gel process takes a long time, often taking days or weeks
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Embodiment 1
[0024] A SiO 2 The preparation method of based organic-inorganic hybrid fluorescent material, such as figure 1 shown, including the following steps:
[0025] 1): dense nano-SiO 2 Functionalization of microspheres
[0026] nano-SiO 2 Dissolve the microspheres in an organic solvent, add a silanecoupling agent at the same time, continuously magnetically stir for 3-8 hours, filter and wash, and dry at 40-80°C. The obtained solid powder is the surface-functionalized nano-SiO 2 Microspheres;
[0027] 2): Preparation of organic-inorganic hybrid fluorescent materials
[0028] The above surface functionalized nano-SiO 2 Add microspheres, organic fluorescent molecules and organic solvents into a three-necked flask, stir at 18-28°C for 5-30 minutes, then raise the temperature of the reaction system to 100-130°C, condense and reflux for 2-4 hours, then cool the solution through Filter and wash, dry at 60-100°C, the resulting solid powder is SiO 2 based organic-inorganic hybrid fl...
Embodiment 2
[0031] At 25 °C, 0.25 g nano-SiO 2 The microspheres were dissolved in 25 mL of tetrahydrofuran solution, while 0.293 mL of 3-aminopropyltriethoxysilane was added, and stirring was continued for 5 hours. The resulting solution was then filtered, washed, and dried at 80°C for 4 hours to obtain surface-functionalized nano-SiO 2 The microspheres are designated as sample S-1.
[0032] 0.25g of the above-mentioned sample S-1, and 0.025g of 4-amino-1,8-naphthalene dioic anhydride and 25mL of N,N-dimethylformamide were simultaneously added to a 100mL three-necked flask, and stirred at 25°C for 5 Minutes later, the temperature was raised to 130° C. and condensed and refluxed for 3 hours, then the reaction solution was cooled, filtered, washed, and dried at 100° C. for 4 hours to obtain SiO 2 based organic-inorganic hybrid materials.
[0035] First, SiO with a diameter of 10 nm 2 The microspheres were dried at 150 °C for 5 h and cooled to room temperature under airtight conditions. At 18 °C, 0.25 g nano-SiO 2 The microspheres were dissolved in 10 mL of tetrahydrofuran solution, while 0.1772 mL of thiopropylmethyldimethoxysilane was added, and stirring was continued for 3 hours. Subsequently, the resulting solution was filtered and washed, and dried at 40°C for 4 hours to obtain surface-functionalized nano-SiO 2 The microspheres are designated as sample S-2.
[0036] Add 0.25g of the above sample S-2, and 0.00025g of 4-amino-1,8-naphthalene dioic anhydride and 10mL of N,N-dimethylformamide into a 100mL three-necked flask at the same time, and stir at 18°C After 15 minutes, the temperature was raised to 100°C for condensing and reflux for 2 hours, then the reaction solution was cooled, filtered, washed, and dried at 60°C for 4 hours to obtain SiO 2 based organic-inorganic hybrid materials.
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Abstract
The invention relates to a preparation method of a fluorescent material, amd in particular relates to a preparation method for a SiO2-based organic-inorganic hybridized fluorescent material. The preparation method comprises the following steps of: adding nanometer SiO2 microspheres into a certain amount of organic solvent and silanecoupling agent mixing solution, performing magnetic stirring for 3-8 hours, then filtering, washing, and drying to obtain solidpowder, namely surface-functionalized nanometer SiO2 microspheres; and adding the surface-functionalized nanometer SiO2 microspheres, organic fluorescent molecules and organic solvent into a three-neck flask according to certain proportion, stirring for 5-30 minutes, then increasing the temperature of a reaction system to 100-300 DEG C, performing condensation and reflux, filtering the solution, washing and drying to obtain solidpowder, namely the SiO2-based organic-inorganic hybridized fluorescent material. Compared with the original preparation method, the method is simple in technology, short in preparation period, low in cost and easy to realize.
Description
technical field [0001] The invention relates to a preparation method of a fluorescent material, in particular to a preparation method of an organic-inorganic hybrid fluorescent material. Background technique [0002] Since the discovery of fluorescence by British scientist G.G. Stokes in 1852, fluorescent materials have received widespread attention, the most common of which are organic small moleculefluorescent materials and organic macromolecular fluorescent materials. These fluorescent materials are gradually being used in dyes, electronics In the fields of switches, sensors, and biomedicine, especially after fluorescent molecules are used as tracers, great progress has been made in the field of sustained and controlled release of drugs. However, organic small molecule fluorescent materials are prone to fluorescencequenching in solid state (Zhang X, J Am Chem Soc. 2004; 126:12200-12201); organic macromolecular fluorescent materials mainly use main chain conjugation to f...
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