CN110229662A - A kind of preparation method of carbon quantum dot and metal organic framework composite material - Google Patents
A kind of preparation method of carbon quantum dot and metal organic framework composite material Download PDFInfo
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- CN110229662A CN110229662A CN201910612873.0A CN201910612873A CN110229662A CN 110229662 A CN110229662 A CN 110229662A CN 201910612873 A CN201910612873 A CN 201910612873A CN 110229662 A CN110229662 A CN 110229662A
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- C—CHEMISTRY; METALLURGY
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- C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
- C09K11/06—Luminescent, e.g. electroluminescent, chemiluminescent materials containing organic luminescent materials
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
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- C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
- C09K11/08—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials
- C09K11/65—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing carbon
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- C09K2211/00—Chemical nature of organic luminescent or tenebrescent compounds
- C09K2211/18—Metal complexes
- C09K2211/183—Metal complexes of the refractory metals, i.e. Ti, V, Cr, Zr, Nb, Mo, Hf, Ta or W
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Abstract
The present invention relates to a kind of carbon quantum dot-metal organic framework composite material preparation methods, belong to new energy materials field.Its preparation characteristic is to sequentially add hafnium chloride with n,N-Dimethylformamide (DMF) for solvent, 4,4 '-biphenyl dicarboxylic acids, glacial acetic acid and carbon dots ultrasound make it completely dissolved, finally pass through filtration drying, a kind of carbon quantum dot-metal organic framework composite material is made.Of the invention we are based on carbon quantum dot and metal organic framework building fluorescence probe, have been successfully set up a kind of novel, simple, quick organic object detecting method.There is higher sensitivity and selectivity compared with traditional single-shot penetrates fluorescence probe, there is huge application potential.
Description
Technical field
The invention belongs to novel energy resource material technology fields, and in particular to a kind of carbon quantum dot and metal organic framework composite wood
The preparation and application of material.
Background technique
Metal-organic framework materials (MOFs) are a kind of by the either secondary construction unit of metal node and organic ligand
The material being self-assembly of by coordinate bond is ground extensively because of its topological structure abundant and in multi-field potential application
Study carefully.MOFs has feature that is controllable, can modifying, can cut, and microcellular structure provides specific surface area and the hole of super large for material
Volume, and strong coordinate bond effect can guarantee that MOFs material still maintains forever after losing guest molecule between metal and ligand
Long porosity.
With the continuous improvement of fluorescence probe synthesis and detection technique level, application has been deep into chemical analysis, environment
The fields such as detection, Food Science, medical diagnosis.Wherein, the selection of fluorescent material for the specificity of analysis detection, stability and
The influence of sensitivity is significant, includes that QDs, MOFs and CDs construct new fluorescence probe one using novel fluorescent material
Determine the detection sensitivity that fluorescence probe can be significantly improved in degree and identification specificity, this has not only opened up researcher
Open one's minds, more promote rapid advances of the fluorescent probe technique in human development history.
Summary of the invention
It is an object of the invention to propose the preparation method of a kind of carbon quantum dot and metal organic framework composite material.
The technical solution adopted by the present invention is that using following steps:
1) preparation of carbon quantum dot: being dissolved in 10 ml deionized waters with 1 g citric acid, adds the ethylenediamine stirring of 0.55 ml
It makes it completely dissolved, places into micro-wave oven to heat and obtain within 5 minutes solid product, standing allows to cool to room temperature and 30 ml are added
Water is sufficiently stirred to obtain required carbon quantum dot；
2) hafnium chloride of 1-1.5 mol, the 4 of 1-1.5 mol, 4 '-biphenyl dicarboxylic acids, the glacial acetic acid of 2-4ml, certain volume
The carbon quantum dot of n,N-Dimethylformamide (DMF), the step 1) preparation of certain volume is added in reaction kettle, 30 points of ultrasound
Clock makes it completely dissolved；
3) in reaction kettle being put into drying box, 120 DEG C of temperature controls is heated to and carry out synthetic reaction overnight, to after reaction,
Reaction kettle is removed, stands to room temperature, carbon quantum dot-metal organic framework white solid product is obtained by filtration；
4) DMF of certain volume is added into products therefrom, after next being washed twice with DMF, is steeped with methanol for the purifying of product
Two days, vacuum drying after the filtration of material finished is obtained carbon quantum dot-metal organic framework composite material；
5) by a certain amount of carbon quantum dot-metal organic framework composite material respectively with the hydroquinone of various concentration in centrifuge tube
In be sufficiently mixed uniformly, be separately added into the buffer solution of certain pH later, these mixed solutions placed into half an hour at room temperature
Or so, its emission spectrum is measured under 460 nm exciting lights.
Compared with prior art, the invention has the following advantages: the present invention we be based on carbon quantum dot and metal and have
Machine framework construction fluorescence probe has been successfully set up a kind of novel, simple, quick organic object detecting method.With traditional list
Emit fluorescence probe to compare with higher sensitivity and selectivity, there is huge application potential.
Detailed description of the invention
Fig. 1 is carbon quantum dot prepared by the present invention-metal organic framework composite material scanning electron mirror figure.
Fig. 2 is that the UV-Vis of present invention preparation carbon quantum dot diffuses spectrogram.
Specific embodiment
Embodiment 1:
The hafnium chloride of 1.05 mol, the 4 of 1.05 mol, 4 '-biphenyl dicarboxylic acids, the glacial acetic acid of 2 ml, the N of 40 ml, N- diformazan
Base formamide (DMF), the carbon quantum dot of 2 ml are added in reaction kettle, and ultrasound makes it completely dissolved for 30 minutes.Reaction kettle is put
It in entering into drying box, is heated to 120 DEG C of temperature controls and carries out synthetic reaction overnight, to after reaction, remove reaction kettle, stand
To room temperature, carbon quantum dot-metal organic framework white solid product is obtained by filtration.Certain volume is added into products therefrom
DMF after next being washed twice with DMF, is steeped two days with methanol.Vacuum drying after the filtration of material finished is finally obtained carbon amounts
Sub- point-metal organic framework composite material.
Embodiment 2:
The volume of carbon quantum dot in embodiment 1 is changed to 3 ml, other conditions are constant.
Embodiment 3:
The volume of carbon quantum dot in embodiment 1 is changed to 4 ml, other conditions are constant.
Embodiment 4:
The volume of carbon quantum dot in embodiment 1 is changed to 5 ml, other conditions are constant.
Embodiment 5:
The volume of carbon quantum dot in embodiment 1 is changed to 6 ml, other conditions are constant.
Claims (3)
1. the preparation method of a kind of carbon quantum dot and metal organic framework composite material, specific method include:
1) preparation of carbon quantum dot: being dissolved in 10 ml deionized waters with 1 g citric acid, adds the ethylenediamine stirring of 0.55 ml
It makes it completely dissolved, places into micro-wave oven to heat and obtain within 5 minutes solid product, standing allows to cool to room temperature and 30 ml are added
Water is sufficiently stirred to obtain required carbon quantum dot；
2) hafnium chloride of 1-1.5 mol, the 4 of 1-1.5 mol, 4 '-biphenyl dicarboxylic acids, the glacial acetic acid of 2-4ml, certain volume
The carbon quantum dot of n,N-Dimethylformamide (DMF), the step 1) preparation of certain volume is added in reaction kettle, 30 points of ultrasound
Clock makes it completely dissolved；
3) in reaction kettle being put into drying box, 120 DEG C of temperature controls is heated to and carry out synthetic reaction overnight, to after reaction,
Reaction kettle is removed, stands to room temperature, carbon quantum dot-metal organic framework white solid product is obtained by filtration；
4) DMF of certain volume is added into products therefrom for the purifying of product, after next being washed twice with DMF, with methanol bubble two
Vacuum drying after the filtration of material finished, is obtained carbon quantum dot-metal organic framework composite material by it；
5) by a certain amount of carbon quantum dot-metal organic framework composite material respectively with the hydroquinone of various concentration in centrifuge tube
In be sufficiently mixed uniformly, be separately added into the buffer solution of certain pH later, these mixed solutions placed into half an hour at room temperature
Or so, its emission spectrum is measured under 460 nm exciting lights.
2. carbon quantum dot-metal organic framework composite material preparation method according to claim 1, it is characterised in that change
The dosage of carbon quantum dot.
3. prepared composite material according to claim 1, it is characterised in that utilize fluorescence detection organic matter hydroquinone.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111154274A (en) * | 2019-12-05 | 2020-05-15 | 山西大学 | Preparation method and application of chemical sensor material |
| CN113413921A (en) * | 2021-07-30 | 2021-09-21 | 陕西科技大学 | ZIF-8 type composite photocatalyst and preparation method thereof |
| CN113731383A (en) * | 2021-08-10 | 2021-12-03 | 广西大学 | Method for preparing multifunctional fluorescent probe by thermal polymerization confinement growth and application thereof |
| CN116948639A (en) * | 2023-07-14 | 2023-10-27 | 安徽工程大学 | Carbon dot/dye@metal organic framework composite material and preparation method and application thereof |
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| CN106252676A (en) * | 2016-07-28 | 2016-12-21 | 青岛大学 | A kind of quantum dot modified metal organic backbone embeds the preparation of carbon nano-tube material |
| CN108201878A (en) * | 2018-02-08 | 2018-06-26 | 华南理工大学 | The preparation method and water pollutant of a kind of carbon dots modified metal organic backbone sorbing material administer application |
| CN108548801A (en) * | 2018-03-19 | 2018-09-18 | 西北师范大学 | Application of the metalloporphyrin framework encapsulation carbon quantum dot in detecting copper ion |
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- 2019-07-09 CN CN201910612873.0A patent/CN110229662A/en active Pending
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| CN106252676A (en) * | 2016-07-28 | 2016-12-21 | 青岛大学 | A kind of quantum dot modified metal organic backbone embeds the preparation of carbon nano-tube material |
| CN108201878A (en) * | 2018-02-08 | 2018-06-26 | 华南理工大学 | The preparation method and water pollutant of a kind of carbon dots modified metal organic backbone sorbing material administer application |
| CN108548801A (en) * | 2018-03-19 | 2018-09-18 | 西北师范大学 | Application of the metalloporphyrin framework encapsulation carbon quantum dot in detecting copper ion |
Non-Patent Citations (2)
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| MATTHEW J. CLIFFE等: "Metal−Organic Nanosheets Formed via Defect-Mediated Transformation of a Hafnium Metal−Organic Framework", 《JOURNAL OF THE AMERICAN CHEMICAL SOCIETY》 * |
| RUIHAN DAI等: "Electron Crystallography Reveals Atomic Structures of Metal−Organic Nanoplates with M12(μ3‑O)8(μ3‑OH)8(μ2‑OH)6 (M = Zr, Hf) Secondary Building Units", 《INORGANIC CHEMISTRY》 * |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111154274A (en) * | 2019-12-05 | 2020-05-15 | 山西大学 | Preparation method and application of chemical sensor material |
| CN113413921A (en) * | 2021-07-30 | 2021-09-21 | 陕西科技大学 | ZIF-8 type composite photocatalyst and preparation method thereof |
| CN113731383A (en) * | 2021-08-10 | 2021-12-03 | 广西大学 | Method for preparing multifunctional fluorescent probe by thermal polymerization confinement growth and application thereof |
| CN113731383B (en) * | 2021-08-10 | 2023-07-25 | 广西大学 | Method for preparing multifunctional fluorescent probe by thermal polymerization limited domain growth and application thereof |
| CN116948639A (en) * | 2023-07-14 | 2023-10-27 | 安徽工程大学 | Carbon dot/dye@metal organic framework composite material and preparation method and application thereof |
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Application publication date: 20190913 |