Preparation of rare earth doping fluorescent functional mesoporous material

A rare earth doped, mesoporous material technology, applied in the direction of color-changing fluorescent materials, chemical instruments and methods, silicon oxide, etc., can solve the problem of the decrease of the loading rate of the pore channels, and achieve the effect of good luminescence performance, simple method and high-efficiency loading.

Inactive Publication Date: 2009-07-08
DONGHUA UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Recently, Yang et al. reported (P.P.Yang, S.S.Huang, D.Y.Kong, J.Lin, and H.G.Fu, Inorg.Chem.2007, 46, 3203-3211) to introduce YVO4:Eu 3+ particle, successfully realized the fluorescent functionalization of the carrier, but the YVO4:Eu loaded in the hole 3+ Changed the connected structure of the channels and decreased the loading rate of the channels

Method used

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  • Preparation of rare earth doping fluorescent functional mesoporous material
  • Preparation of rare earth doping fluorescent functional mesoporous material
  • Preparation of rare earth doping fluorescent functional mesoporous material

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] Dissolve 1.0 g of polyoxyethylene-polyoxypropylene-polyoxyethylene triblock copolymer (P123) (molecular weight 5800) in a certain amount of deionized water and stir until clear, stir for 1 hour, then add 2.08 g of tetraethyl orthosilicate ( TEOS) and 4ml of RE 3+ (where RE contains Y 3+ and Eu 3+ The molar ratio is n Y / n E=4.0) the total amount is 0.5mol / L rare earth nitrate solution, then add a certain amount of HCl solution so that its concentration in the final reaction medium is respectively 0.15, 0.30, 0.45 and 0.60mol / L, the final mixed solution The quantity ratio is: TEOS:RE:P123:H 2 O=1:0.2:0.017:210; the mixed solution continued to be stirred at 40°C for 24h, then transferred to a reactor with a plastic substrate and crystallized at 100°C for 48h, the obtained product was filtered, washed with deionized water, and Dry at room temperature, and then bake in static air at a rate of 1°C per minute to 500°C for 4 hours to remove the tri-block copolymer to obta...

Embodiment 2

[0033] 1.0g polyoxyethylene-polyoxypropylene-polyoxyethylene triblock copolymer (P123) and 0.10g dodecyltrimethylammonium bromide (C 12 TAB) was dissolved in a certain amount of deionized water and stirred until clear, stirred for 1h, then added 1.52g of methyl orthosilicate and 8.0, 4.0, 2.0, 1.0 and 0.5ml of RE 3+ (where RE contains Y 3+ and Eu 3+ The molar ratio is n Y / n Eu =4.0) the total amount is 0.5mol / L rare earth nitrate solution, then add a certain amount of HBr solution so that its concentration in the final reaction medium is respectively 0.45mol / L, and the amount ratio of substances in the final mixed solution is: orthosilicon Acid methyl ester:RE:P123:C 12 TAB:H 2 O=1: (0.40, 0.20, 0.10, 0.05, 0.025): 0.017:0.032:180; the mixed solution was stirred at 40°C for 24h, then transferred to a reactor with a plastic substrate and crystallized at 100°C for 48h. The obtained product was filtered, washed with deionized water, dried at room temperature, and then cal...

Embodiment 3

[0035] 0.51g cetyltrimethylammonium bromide (C 16 TAB) was dissolved in a certain amount of deionized water and stirred until clear, stirred for 1h, then added 1.22g of sodium silicate (Na 2 SiO 3 ) and 4.0ml of RE 3+ , the total amount is 0.5mol / L rare earth nitrate solution, where RE contains Y 3+ and Eu 3+ The molar ratio is n Y / n Eu =2.3, 3.0, 4.0, 5.7, 9.0, then add a certain amount of HNO 3 The concentration of the solution in the final reaction medium is 0.45mol / L respectively, and the ratio of substances in the final mixed solution is: Na 2 SiO 3 :RE:CTAB:H 2 O=1:(0.40, 0.20, 0.10, 0.05, 0.025):0.14:150; the mixed solution was stirred at 40°C for 24h, then transferred to a reactor with a plastic substrate and crystallized at 100°C for 48h, and the obtained The product was filtered, washed with deionized water, dried at room temperature, and then calcined in static air at a rate of 1 °C per minute to 500 °C for 4 h to remove the triblock copolymer to obtain r...

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PUM

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Abstract

The invention relates to a method for preparing a rare-earth doped fluorescence functionalized mesoporous material. The method comprises that: (1) one or more surfactants as a pore forming agent is dissolved in deionized water and is stirred to clarification; (2) a silicon source and a salt solution of rare-earth ion RE are added to the solution; the acidity of a reaction medium is regulated by acid; the mixed solution is continuously stirred for 6 and 24 hours at a temperature of between 25 and 60 DEG C to generate white precipitate; (3) the white precipitate and the solution are transferred to a polytetrafluoroethylene reaction kettle, and are subjected to hydrothermal treatment for 24 to 48 hours under the condition of temperature of between 80 and 140 DEG C; and (4) the solution is cooled, filtered, washed and roasted to obtain a product. The method is simple; the obtained mesoporous material has good luminous performance; a pore canal has an ordered structure; and a pore wall is provided with a great amount of silicon oxhydryls which have interaction with a loaded substance to realize high-efficient loading of medicine, gene, and the like; and the method can be used in the fields such as fluorescence-tracked medical or biological carrier.

Description

technical field [0001] The invention belongs to the field of preparation of mesoporous functional materials, in particular to a preparation method of rare earth-doped fluorescent functionalized mesoporous materials. Background technique [0002] Mesoporous material is a new type of nanostructure material that emerged rapidly in the 1990s. It has been highly valued by the international physics, chemistry and materials science circles since its birth, and has rapidly developed into one of the interdisciplinary research hotspots. Using the supramolecular structure formed by the surfactant as a template, through the directional interaction between the organic-inorganic interface, it can be assembled into an inorganic porous material with a uniform pore size distribution and a regular pore structure with a pore size between 2-30 nm. After the scientists of Mobil Corporation prepared the M41S series of ordered mesoporous silica-alumina materials in 1992, mesoporous materials, espe...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B33/18C09K9/00
Inventor 光善仪张超徐洪耀
Owner DONGHUA UNIV
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