CN103254890A - Preparation method of hyperbranched poly-glycidyl ether grated rare earth up-conversion luminescence nanocrystal - Google Patents
Preparation method of hyperbranched poly-glycidyl ether grated rare earth up-conversion luminescence nanocrystal Download PDFInfo
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- CN103254890A CN103254890A CN2013101870680A CN201310187068A CN103254890A CN 103254890 A CN103254890 A CN 103254890A CN 2013101870680 A CN2013101870680 A CN 2013101870680A CN 201310187068 A CN201310187068 A CN 201310187068A CN 103254890 A CN103254890 A CN 103254890A
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Abstract
The invention discloses a preparation method of hyperbranched poly-glycidyl ether grated rare earth up-conversion luminescence nanocrystal. The preparation method comprises the following steps of: adding 1 part by weight of rare earth up-conversion luminescence nanocrystal into 10-100 parts by weight of tetrahydrofuran for ultrasonic dispersion, further adding potassium methoxide, stirring for 30 minutes at 30-50 DEG C, subsequently heating to be 70 DEG C so as to evaporate the solvent, further adding the components into 10-100 parts by weight of dioxane for ultrasonic dispersion, introducing argon for 5-30 minutes, raising the temperature to 90-120 DEG C, dropwise adding 1-50 parts by weight of glycidol, and reacting for 4-48 hours so as to obtain the hyperbranched poly-glycidyl ether grated rare earth up-conversion luminescence nanocrystal. The preparation method disclosed by the invention is simple to operate, the raw materials are easily available, the prepared nanocrystal has excellent up-conversion luminescence property and is high in luminescence intensity, good in photostability and good in solubility, and due to rich hydroxyl functional groups on the surface, the nanocrystal has good application prospects in aspects such as fluorescence labeling, biological detection and luminescent devices.
Description
Technical field
The invention belongs to the nano composite material technical field, particularly a kind of preparation method of rare earth up-conversion luminescence nanometer crystal of hyperbranched polyglycidyl ether grafting.
Background technology
The rare earth up-conversion luminescent material refers to can launch the fluorescent material of visible light under the exciting of infrared or near infrared light; Because it has high-fluorescence quantum yield, narrow emission peak, advantage such as high-light-fastness and hypotoxicity and being paid close attention to widely; Compare with traditional luminous marker (as quantum dot, organic dye), up-conversion luminescent material has the luminous intensity height, advantages such as stoke shift is big, it excites the employing infrared light, have high penetration depth and can effectively avoid the interference of biological sample autofluorescence and scattered light, reduced detection background, improved signal to noise ratio, so up-conversion luminescent material is a kind of up-and-coming bioprobe material.Hyperbranched glycidyl ether has excellent solvability and excellent biological compatibility, owing to have a large amount of hydroxyls, can give hyperbranched glycidyl ether more function by chemical modification easily, and polymer materials has good toughness and excellent workability, also is subjected to the extensive concern of material educational circles always; Although the synthetic report of existing more relevant rare earth up-conversion luminescence nanometer crystal, but transform the synthetic rarely seen report of luminescence nanocrystalline on the polymers function rare earth, therefore, with both combinations, synthetic fluorescence property excellence, the nano composite material of Application Areas broadness has far-reaching theory significance and application prospect.
Summary of the invention
The purpose of this invention is to provide a kind of preparation method of rare earth up-conversion luminescence nanometer crystal of hyperbranched polyglycidyl ether grafting, prepare the functional rare earth up-conversion luminescence nanometer crystal material, enlarge its range of application.
Concrete steps are:
(1) 1 weight part rare earth up-conversion luminescence nanometer crystal is joined ultra-sonic dispersion in 10 ~ 100 weight part tetrahydrofuran (THF)s, the potassium methylate that adds 0.005 ~ 0.1 weight part again, 30 ~ 50 ℃ were stirred 30 minutes, be heated to 70 ℃ then, make solvent evaporation, make the rare earth up-conversion luminescence nanometer crystal that contains potassium methylate.
(2) the rare earth up-conversion luminescence nanometer crystal that contains potassium methylate that 1 weight part step (1) is made mixes with 10 ~ 100 weight part dioxane, and ultra-sonic dispersion obtains rare earth up-conversion luminescence nanometer crystal dispersion liquid.
(3) feed argon gas in the rare earth up-conversion luminescence nanometer crystal dispersion liquid that makes to step (2) after 5 ~ 30 minutes, be warming up to 90 ~ 120 ℃, slowly be added dropwise to the R-GLYCIDOL of 1 ~ 50 weight part again by constant pressure funnel, reacted 4 ~ 48 hours, and namely made the rare earth up-conversion luminescence nanometer crystal of hyperbranched polyglycidyl ether grafting.
Described rare earth up-conversion luminescence nanometer crystal contains the NaYF of hydroxyl for the surface
4: the NaYF of hydroxyl is contained on Yb/Er up-conversion luminescence nanometer crystal or surface
4: the Yb/Tm up-conversion luminescence nanometer crystal.
Described chemical reagent and raw material are the above purity of chemical pure.
Preparation method of the present invention is simple to operate, raw material is easy to get, and the rare earth up-conversion luminescence nanometer crystal of prepared hyperbranched polyglycidyl ether grafting has excellent up-conversion luminescence performance, its luminous intensity height, good light stability, solvability is good, and abundant hydroxy functional group is contained on the surface, at aspects such as fluorescent mark, biological detection and luminescent devices good application prospects is arranged.
Description of drawings
Fig. 1 is the NaYF of the hyperbranched polyglycidyl ether grafting of the embodiment of the invention 1 preparation
4: the photo of the Yb/Er up-conversion luminescence nanometer crystal aqueous solution under white light and 980 nanometer excitation light sources.
Fig. 2 is the NaYF of the hyperbranched polyglycidyl ether grafting of the embodiment of the invention 1 preparation
4: the fluorescence spectrum figure of Yb/Er up-conversion luminescence nanometer crystal, excitation wavelength is 980 nanometers.
Fig. 3 is the NaYF of the hyperbranched polyglycidyl ether grafting of the embodiment of the invention 1 preparation
4: the thermogravimetric curve of Yb/Er up-conversion luminescence nanometer crystal.
Fig. 4 is the NaYF of the hyperbranched polyglycidyl ether grafting of the embodiment of the invention 1 preparation
4: the infrared spectrogram of Yb/Er up-conversion luminescence nanometer crystal.
Embodiment
Employed chemical reagent and raw material are analytical pure in following examples.
Embodiment 1:
(1) 100 milligrams of surfaces is contained the NaYF of hydroxyl
4: the Yb/Er up-conversion luminescence nanometer crystal joins ultra-sonic dispersion in the 5 gram tetrahydrofuran (THF)s, adds 10 milligrams of potassium methylates again, and 50 ℃ were stirred 30 minutes, were heated to 70 ℃ then, made solvent evaporation, made the NaYF that contains potassium methylate
4: the Yb/Er up-conversion luminescence nanometer crystal.
(2) NaYF that contains potassium methylate that step (1) is made
4: the Yb/Er up-conversion luminescence nanometer crystal mixes with 5 gram dioxane, and ultra-sonic dispersion obtains NaYF
4: Yb/Er up-conversion luminescence nanometer crystal dispersion liquid.
(3) NaYF that makes to step (2)
4: feed argon gas 5 minutes in the Yb/Er up-conversion luminescence nanometer crystal dispersion liquid, be warming up to 95 ℃, slowly be added dropwise to 2 gram R-GLYCIDOLs by constant pressure funnel again, reacted 48 hours, namely make the NaYF of hyperbranched polyglycidyl ether grafting
4: the Yb/Er up-conversion luminescence nanometer crystal.
Tested the NaYF of the hyperbranched polyglycidyl ether grafting of present embodiment preparation by fluorescence spectrophotometer
4: the optical property of Yb/Er up-conversion luminescence nanometer crystal shows that it has excellent up-conversion luminescence performance, its luminous intensity height, good light stability; Thermogravimetic analysis (TGA) as can be seen, at 400 ℃, weightlessness reaches 27%, has shown in the successful grafting in rare earth up-conversion luminescence nanometer crystal surface hyperbranched polyglycidyl ether; With the NaYF of infrared spectrometer to the hyperbranched polyglycidyl ether grafting of present embodiment preparation
4: the surface group of Yb/Er up-conversion luminescence nanometer crystal is tested, and confirms that its surface contains a large amount of hydroxy functional groups.
Embodiment 2:
(1) 120 milligrams of surfaces is contained the NaYF of hydroxyl
4: the Yb/Tm up-conversion luminescence nanometer crystal joins ultra-sonic dispersion in the 2 gram tetrahydrofuran (THF)s, adds 6 milligrams of potassium methylates again, and 30 ℃ were stirred 30 minutes, were heated to 70 ℃ then, made solvent evaporation, made the NaYF that contains potassium methylate
4: the Yb/Tm up-conversion luminescence nanometer crystal.
(2) NaYF that contains potassium methylate that step (1) is made
4: the Yb/Tm up-conversion luminescence nanometer crystal mixes with 2 gram dioxane, and ultra-sonic dispersion obtains NaYF
4: Yb/Tm up-conversion luminescence nanometer crystal dispersion liquid.
(3) NaYF that makes to step (2)
4: feed argon gas 30 minutes in the Yb/Tm up-conversion luminescence nanometer crystal dispersion liquid, be warming up to 90 ℃, slowly be added dropwise to 2 gram R-GLYCIDOLs by constant pressure funnel again, reacted 24 hours, namely make the NaYF of hyperbranched polyglycidyl ether grafting
4: the Yb/Tm up-conversion luminescence nanometer crystal.
Embodiment 3:
(1) 150 milligrams of surfaces is contained the NaYF of hydroxyl
4: the Yb/Er up-conversion luminescence nanometer crystal joins ultra-sonic dispersion in the 2 gram tetrahydrofuran (THF)s, adds 5 milligrams of potassium methylates again, and 45 ℃ were stirred 30 minutes, were heated to 70 ℃ then, made solvent evaporation, made the NaYF that contains potassium methylate
4: the Yb/Er up-conversion luminescence nanometer crystal.
(2) NaYF that contains potassium methylate that step (1) is made
4: the Yb/Er up-conversion luminescence nanometer crystal mixes with 2 gram dioxane, and ultra-sonic dispersion obtains NaYF
4: Yb/Er up-conversion luminescence nanometer crystal dispersion liquid.
(3) NaYF that makes to step (2)
4: feed argon gas 15 minutes in the Yb/Er up-conversion luminescence nanometer crystal dispersion liquid, be warming up to 120 ℃, slowly be added dropwise to 0.2 gram R-GLYCIDOL by constant pressure funnel again, reacted 4 hours, namely make the NaYF of hyperbranched polyglycidyl ether grafting
4: the Yb/Er up-conversion luminescence nanometer crystal.
Embodiment 4:
(1) 20 milligrams of surfaces is contained the NaYF of hydroxyl
4: the Yb/Er up-conversion luminescence nanometer crystal joins ultra-sonic dispersion in the 0.2 gram tetrahydrofuran (THF), adds 0.1 milligram of potassium methylate again, and 45 ℃ were stirred 30 minutes, were heated to 70 ℃ then, made solvent evaporation, made the NaYF that contains potassium methylate
4: the Yb/Er up-conversion luminescence nanometer crystal.
(2) NaYF that contains potassium methylate that step (1) is made
4: the Yb/Er up-conversion luminescence nanometer crystal mixes with 0.3 gram dioxane, and ultra-sonic dispersion obtains NaYF
4: Yb/Er up-conversion luminescence nanometer crystal dispersion liquid.
(3) NaYF that makes to step (2)
4: feed argon gas 20 minutes in the Yb/Er up-conversion luminescence nanometer crystal dispersion liquid, be warming up to 100 ℃, slowly be added dropwise to 0.5 gram R-GLYCIDOL by constant pressure funnel again, reacted 12 hours, namely make the NaYF of hyperbranched polyglycidyl ether grafting
4: the Yb/Er up-conversion luminescence nanometer crystal.
Embodiment 5:
(1) 100 milligrams of surfaces is contained the NaYF of hydroxyl
4: the Yb/Er up-conversion luminescence nanometer crystal joins ultra-sonic dispersion in the 10 gram tetrahydrofuran (THF)s, adds 6 milligrams of potassium methylates again, and 40 ℃ were stirred 30 minutes, were heated to 70 ℃ then, made solvent evaporation, made the NaYF that contains potassium methylate
4: the Yb/Er up-conversion luminescence nanometer crystal.
(2) NaYF that contains potassium methylate that step (1) is made
4: the Yb/Er up-conversion luminescence nanometer crystal mixes with 10 gram dioxane, and ultra-sonic dispersion obtains NaYF
4: Yb/Er up-conversion luminescence nanometer crystal dispersion liquid.
(3) NaYF that makes to step (2)
4: feed argon gas 25 minutes in the Yb/Er up-conversion luminescence nanometer crystal dispersion liquid, be warming up to 98 ℃, slowly be added dropwise to 5 gram R-GLYCIDOLs by constant pressure funnel again, reacted 24 hours, namely make the NaYF of hyperbranched polyglycidyl ether grafting
4: the Yb/Er up-conversion luminescence nanometer crystal.
Embodiment 6:
(1) 60 milligrams of surfaces is contained the NaYF of hydroxyl
4: the Yb/Tm up-conversion luminescence nanometer crystal joins ultra-sonic dispersion in the 2 gram tetrahydrofuran (THF)s, adds 4 milligrams of potassium methylates again, and 35 ℃ were stirred 30 minutes, were heated to 70 ℃ then, made solvent evaporation, made the NaYF that contains potassium methylate
4: the Yb/Tm up-conversion luminescence nanometer crystal.
(2) NaYF that contains potassium methylate that step (1) is made
4: the Yb/Tm up-conversion luminescence nanometer crystal mixes with 3 gram dioxane, and ultra-sonic dispersion obtains NaYF
4: Yb/Tm up-conversion luminescence nanometer crystal dispersion liquid.
(3) NaYF that makes to step (2)
4: feed argon gas 30 minutes in the Yb/Er up-conversion luminescence nanometer crystal dispersion liquid, be warming up to 96 ℃, slowly be added dropwise to 1.5 gram R-GLYCIDOLs by constant pressure funnel again, reacted 36 hours, namely make the NaYF of hyperbranched polyglycidyl ether grafting
4: the Yb/Tm up-conversion luminescence nanometer crystal.
Claims (1)
1. the preparation method of the rare earth up-conversion luminescence nanometer crystal of a hyperbranched polyglycidyl ether grafting is characterized in that concrete steps are:
(1) 1 weight part rare earth up-conversion luminescence nanometer crystal is joined ultra-sonic dispersion in 10 ~ 100 weight part tetrahydrofuran (THF)s, the potassium methylate that adds 0.005 ~ 0.1 weight part again, 30 ~ 50 ℃ were stirred 30 minutes, be heated to 70 ℃ then, make solvent evaporation, make the rare earth up-conversion luminescence nanometer crystal that contains potassium methylate;
(2) the rare earth up-conversion luminescence nanometer crystal that contains potassium methylate that 1 weight part step (1) is made mixes with 10 ~ 100 weight part dioxane, and ultra-sonic dispersion obtains rare earth up-conversion luminescence nanometer crystal dispersion liquid;
(3) feed argon gas in the rare earth up-conversion luminescence nanometer crystal dispersion liquid that makes to step (2) after 5 ~ 30 minutes, be warming up to 90 ~ 120 ℃, slowly be added dropwise to the R-GLYCIDOL of 1 ~ 50 weight part again by constant pressure funnel, reacted 4 ~ 48 hours, and namely made the rare earth up-conversion luminescence nanometer crystal of hyperbranched polyglycidyl ether grafting;
Described rare earth up-conversion luminescence nanometer crystal contains the NaYF of hydroxyl for the surface
4: the NaYF of hydroxyl is contained on Yb/Er up-conversion luminescence nanometer crystal or surface
4: the Yb/Tm up-conversion luminescence nanometer crystal;
Described chemical reagent and raw material are the above purity of chemical pure.
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| CN103446964A (en) * | 2013-08-29 | 2013-12-18 | 西北工业大学 | Preparation method of carboxyl functionalized hyperbranched magnetic mesoporous silica composite microspheres |
| CN104371714A (en) * | 2014-11-28 | 2015-02-25 | 赵兵 | Molybdenum trioxide-graphene oxide composite material and preparation method thereof |
| CN104371715A (en) * | 2014-11-28 | 2015-02-25 | 赵兵 | Water-soluble molybdenum trioxide up-conversion nanometer material and preparation method thereof |
| CN104371727A (en) * | 2014-11-28 | 2015-02-25 | 赵兵 | Water-soluble up-conversion nanoparticles and preparation method thereof |
| CN104449714A (en) * | 2014-11-28 | 2015-03-25 | 赵兵 | UCNP (up-conversion nanoparticle)-graphene oxide composite material and preparation method thereof |
| CN104498037A (en) * | 2014-11-28 | 2015-04-08 | 赵兵 | PAMAM (polyamide-amine)-modified water-soluble upconversion nanoparticles and preparation method thereof |
| CN106220840A (en) * | 2016-08-18 | 2016-12-14 | 浙江大学 | A kind of synthetic method of hyperbranched poly oxolane |
| CN107587345A (en) * | 2017-09-17 | 2018-01-16 | 赵兵 | A kind of nano silver wire functional fibre for strengthening up-conversion fluorescence |
| CN112108128A (en) * | 2020-08-31 | 2020-12-22 | 西安交通大学 | Hydrophilic hyperbranched polyglycidyl ether anion magnetic adsorbent and preparation method and application thereof |
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| CN103446964A (en) * | 2013-08-29 | 2013-12-18 | 西北工业大学 | Preparation method of carboxyl functionalized hyperbranched magnetic mesoporous silica composite microspheres |
| CN104371714A (en) * | 2014-11-28 | 2015-02-25 | 赵兵 | Molybdenum trioxide-graphene oxide composite material and preparation method thereof |
| CN104371715A (en) * | 2014-11-28 | 2015-02-25 | 赵兵 | Water-soluble molybdenum trioxide up-conversion nanometer material and preparation method thereof |
| CN104371727A (en) * | 2014-11-28 | 2015-02-25 | 赵兵 | Water-soluble up-conversion nanoparticles and preparation method thereof |
| CN104449714A (en) * | 2014-11-28 | 2015-03-25 | 赵兵 | UCNP (up-conversion nanoparticle)-graphene oxide composite material and preparation method thereof |
| CN104498037A (en) * | 2014-11-28 | 2015-04-08 | 赵兵 | PAMAM (polyamide-amine)-modified water-soluble upconversion nanoparticles and preparation method thereof |
| CN104371727B (en) * | 2014-11-28 | 2016-06-22 | 赵兵 | Conversion nano granule and preparation method thereof on a kind of water solublity |
| CN104371715B (en) * | 2014-11-28 | 2016-06-22 | 赵兵 | A kind of water solublity molybdenum trioxide up-conversion nano material and preparation method thereof |
| CN104498037B (en) * | 2014-11-28 | 2016-06-22 | 赵兵 | Conversion nano granule and preparation method thereof on the water solublity that a kind of PAMAM modifies |
| CN106220840A (en) * | 2016-08-18 | 2016-12-14 | 浙江大学 | A kind of synthetic method of hyperbranched poly oxolane |
| CN107587345A (en) * | 2017-09-17 | 2018-01-16 | 赵兵 | A kind of nano silver wire functional fibre for strengthening up-conversion fluorescence |
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Application publication date: 20130821 |