CN107033884A - A kind of preparation method of carbon quantum dot for Visual retrieval heavy metal ion - Google Patents
A kind of preparation method of carbon quantum dot for Visual retrieval heavy metal ion Download PDFInfo
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- CN107033884A CN107033884A CN201610975932.7A CN201610975932A CN107033884A CN 107033884 A CN107033884 A CN 107033884A CN 201610975932 A CN201610975932 A CN 201610975932A CN 107033884 A CN107033884 A CN 107033884A
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- quantum dot
- carbon quantum
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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
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- 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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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y20/00—Nanooptics, e.g. quantum optics or photonic crystals
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
- G01N21/63—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light optically excited
- G01N21/64—Fluorescence; Phosphorescence
- G01N21/6428—Measuring fluorescence of fluorescent products of reactions or of fluorochrome labelled reactive substances, e.g. measuring quenching effects, using measuring "optrodes"
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N23/00—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00
- G01N23/20—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by using diffraction of the radiation by the materials, e.g. for investigating crystal structure; by using scattering of the radiation by the materials, e.g. for investigating non-crystalline materials; by using reflection of the radiation by the materials
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
- G01N21/63—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light optically excited
- G01N21/64—Fluorescence; Phosphorescence
- G01N21/6428—Measuring fluorescence of fluorescent products of reactions or of fluorochrome labelled reactive substances, e.g. measuring quenching effects, using measuring "optrodes"
- G01N2021/6432—Quenching
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N2223/00—Investigating materials by wave or particle radiation
- G01N2223/05—Investigating materials by wave or particle radiation by diffraction, scatter or reflection
- G01N2223/056—Investigating materials by wave or particle radiation by diffraction, scatter or reflection diffraction
Abstract
The present invention discloses a kind of preparation method of the carbon quantum dot for Visual retrieval heavy metal.A kind of preparation method of carbon quantum dot for Visual retrieval heavy metal ion of the present invention is that L-cysteine is soluble in water in mass ratio for 0.017 ~ 0.117%, is then fully reacted at 160 ~ 200 DEG C, obtains the carbon nano-quantum point aqueous solution.Raw material used in preparation method of the present invention is single, synthesis technique simple, and synthesis temperature is relatively low, with low cost, green non-pollution, and resulting carbon quantum dot good water solubility, can be directly used for Cu2+Ion or Pb2+The Visual retrieval of ion in aqueous, reduces the complexity and cost of detection.
Description
Technical field
The present invention relates to a kind of preparation method of carbon quantum dot, exactly it is used for Visual retrieval weight the present invention relates to one kind
The preparation method of the carbon quantum dot of metal.
Background technology
Carbon quantum dot has unique luminosity, and the luminous of carbon quantum dot has size and wavelength dependency.It is glimmering at present
The preparation method of light carbon quantum dot has hydro-thermal method, nanolithographic method, electrochemical process, solvent-thermal method, chemical stripping carbon fiber method, micro-
Ripple auxiliary law, solution chemical method etc., referring to:Wang Jiaojiao, Feng Miao, Zhan Hong soldier " preparation of graphene quantum dot " [J] chemistry enters
Exhibition, the 2013, the 1st phase.Wherein, hydro-thermal method is a kind of effective method for preparing carbon quantum dot material.Hydrothermal reaction process refers to
Under certain temperature and pressure, the general name conducted in the fluids such as water, the aqueous solution or steam about chemically reacting.Hydro-thermal method
It is an important problem in science to select presoma.At present, hydro-thermal method prepares most of presomas used in quantum dot to have
Malicious harmful organic substance presoma, causes that production cost is higher and preparation method does not meet environmental protection, how Effective selection
Low cost, the persursor material of environmental protection are the current important research directions for preparing carbon quantum dot.
Further, since carbon quantum dot has special two-photon excitation characteristic and upper conversion function, carbon quantum dot is applied
The numerous areas such as cell imaging, photoelectricity dynamics, the detection of biochemical analysis and detection and heavy metal ions in sewage.Wherein, it is sharp
There is preferable potential using value with the fluorescence property detection heavy metal ion of carbon quantum dot.Due to contents of many kinds of heavy metal ion
The aqueous solution is all clear solution, adds not obvious color change, therefore common means are by carbon after carbon quantum dot
Photoluminescent property before and after quantum dot is added changes to judge the species and concentration of heavy metal ion, therefore, adds answering for detection
Polygamy, and cost is too high.
Based on above research background and real current situation, it is necessary to develop that a kind of raw material is cheap, environmental protection presoma to be to make
Standby carbon quantum dot material, the carbon quantum dot for the heavy metal ion that particularly a kind of material can be used for efficiently in quickly detection water.
The content of the invention
The present invention, which provides one kind, can overcome prior art not enough, and its preparation technology is simple, low cost, the energy of environmental protection are used
In the preparation method of Visual retrieval heavy metal lead or the fluorescent carbon quantum dot of copper.
A kind of preparation method of carbon quantum dot for Visual retrieval heavy metal ion of the present invention is by L-half Guang ammonia
Acid is soluble in water for 0.017 ~ 0.117% in mass ratio, is then fully reacted at 160 ~ 200 DEG C, obtains carbon nano-quantum point
The aqueous solution.
Preferably, the preparation method of the carbon quantum dot that can be used for detection heavy metal ion of the invention is in preparation process
In, the mass ratio of L-cysteine and water is 0.017~0.117%, and preferred mass ratio is 0.05%.
Further, in the preparation method of the carbon quantum dot that can be used for detection heavy metal ion of the invention, hydro-thermal reaction temperature
Spend for 190 DEG C.
Further, in the preparation method of the carbon quantum dot that can be used for detection heavy metal ion of the invention, the reaction time is 6
Hour.
Herein proportioning, temperature and luminous intensity highest carbon quantum dot material is resulted under the reaction time so that its
Possesses more preferable ion detection performance.
The carbon quantum dot that the method for the present invention is prepared can be used for the detection of heavy metal ion, particularly for Cu2+Ion
Or Pb2+The Visual retrieval of ion.
The present invention chooses L-cysteine as presoma, and its raw material is single, synthesis technique simple, and synthesis temperature is relatively low,
It is with low cost, green non-pollution, and resulting carbon quantum dot good water solubility, it is used directly for Cu2+Ion or Pb2+From
The Visual retrieval of son in aqueous, reduces the complexity and cost of detection.
Brief description of the drawings
The carbon quantum dot X-ray diffraction picture that Fig. 1 is prepared for the present invention
Fig. 2 is the luminescence generated by light figure for the carbon quantum dot that different instances are prepared.
Intensity of emission spectra after different metal ions solution is added in the carbon quantum dot aqueous solution that Fig. 3 is prepared for the present invention
Picture
Cu is added in the carbon quantum dot aqueous solution that Fig. 4 is prepared for the present invention2+Quantum dot solution face of the present invention before and after solion
Left bottle is that right bottle is in carbon in the pure carbon quantum dot solution that is prepared by above-described embodiment, figure in colour contrast photo, wherein figure
Cu is added dropwise in quantum dot solution2+Photo after solution.
Pb is added in the carbon quantum dot aqueous solution that Fig. 5 is prepared for the present invention2+Quantum dot solution of the present invention before and after solion
Color contrast photo.
Embodiment
Prepare embodiment 1
Weigh 0.0125g Cys and accurately measure 30mL deionized waters in beaker, be uniformly mixed at room temperature;
Above-mentioned solution is transferred in reactor, is reacted 6 hours under the conditions of 190 DEG C, reacted solution is collected and produced
To a kind of carbon nano-quantum point aqueous solution of the present invention.
Detect embodiment 1
Weigh 0.0150g Cys and accurately measure 30mL deionized waters in beaker, mix it even equal;
Above-mentioned solution is transferred in reactor, reacts and collects reacted solution as carbon in 6 hours under the conditions of 190 DEG C
The nano-quantum point aqueous solution.Gained carbon quantum dot X-ray diffraction photo of the invention is shown in Fig. 1, and the present invention is prepared using different ratio
Carbon quantum dot intensity of emission spectra picture see Fig. 2.
The carbon quantum dot X-ray diffraction photo obtained by above example is shown in Fig. 1.Fig. 2 is that embodiment 1 and embodiment 2 are made
It is standby go out carbon quantum dot luminescence generated by light figure, as shown in Figure 2 the luminous intensity of embodiment 2 be higher than embodiment 1;Some metals from
Son and the coupling of the functional group on carbon quantum dot surface can produce quenching effect to the luminescence generated by light of quantum dot, and Fig. 3 is different metal
Ion is separately added into the luminescence generated by light figure measured after carbon quantum dot solution, it can be seen that copper, the addition of two kinds of ions of lead are to carbon amounts
The luminous of son point has obvious quenching effect, and this effect is also a kind of method for detecting ion of copper and lead.Fig. 4 and Fig. 5 are respectively
Copper ion and lead ion add the forward and backward comparison diagram of carbon quantum solution, and solution colour has obvious change, and this is also this patent
The described method by color change, intuitively progress ion detection.
Prepare embodiment 2
Weigh 0.0150g Cys and accurately measure 30mL deionized waters in beaker, be uniformly mixed at room temperature;
Above-mentioned solution is transferred in reactor, is reacted 6 hours under the conditions of 190 DEG C, reacted solution is collected as this hair
The bright another carbon nano-quantum point aqueous solution.
Take resulting quantum dot aqueous solution 5ml that 1ml Na are added dropwise respectively in the present embodiment+、Ag+、Mg2+、K+、Ca2+、Fe2 +、Fe3+、Pb2+、Cu2+、Hg2+In solion, ion concentration is 20mmol/L, its intensity of emission spectra is surveyed, referring to Fig. 3.
Detect embodiment 2
Weigh 0.0150g Cys and accurately measure 30mL deionized waters in beaker, be uniformly mixed at room temperature;
Above-mentioned solution is transferred in reactor, under the conditions of 190 DEG C react 6 hours, by reacted solution collect as
The carbon nano-quantum point aqueous solution.It is 20mmol/L's to take gained quantum dot aqueous solution 3ml to instill 2ml concentration in the present embodiment
Cu2+Color change after solution is referring to accompanying drawing 4.Visually observe visible, the pure carbon quantum dot solution that the present embodiment is prepared is
Clear colorless liquid, is added dropwise to Cu wherein2+Brown color is rapidly gone to after solution.
Prepare embodiment 3
Weigh 0.0150g Cys and accurately measure 30mL deionized waters in beaker, be uniformly mixed at room temperature;
Above-mentioned solution is transferred in reactor, reacted 6 hours under the conditions of 190 DEG C, reacted solution is collected and obtains this
The third carbon nano-quantum point aqueous solution of invention.
Detect embodiment 3
Gained quantum dot aqueous solution 3ml is taken, the Pb that 2ml concentration is 20mmol/L is added2+Solution, naked eyes are that observable instills Pb2 +Quantum dot is the color change situation of the aqueous solution before and after solution, referring to accompanying drawing 5.As seen in Fig., when not instilling metal ion solution
The transparent colourless liquid of carbon quantum dot solution, is being added dropwise to Pb2+Grey is rapidly gone to after solution, and precipitation production is had when standing
It is raw.
Claims (8)
1. a kind of preparation method of carbon quantum dot for Visual retrieval heavy metal ion, by L-cysteine in mass ratio
0.017 ~ 0.117% is soluble in water, is then fully reacted at 160 ~ 200 DEG C, obtains the carbon nano-quantum point aqueous solution.
2. the preparation method according to claim 1 that can be used for detecting the carbon quantum dot of heavy metal ion, it is characterised in that
The mass ratio of L-cysteine and water is 0.05%.
3. the preparation method of the carbon quantum dot according to claim 1 or 2 for Visual retrieval heavy metal ion, it is special
Levy and be 190 DEG C of hydrothermal temperature.
4. the preparation method of the carbon quantum dot for Visual retrieval heavy metal ion according to claim 1 or 2 or 3,
It is characterized in that the reaction time is 6 hours.
5. carbon quantum dot prepared by the preparation method described in Claims 1-4.
6. carbon quantum dot prepared by the preparation method described in Claims 1-4 is used for the detection of heavy metal ion.
7. carbon quantum dot prepared by the preparation method described in Claims 1-4 is used for Cu2+The Visual retrieval of ion.
8. carbon quantum dot prepared by the preparation method described in Claims 1-4 is used for Pb2+Visualization ion detection.
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Cited By (8)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN107573933A (en) * | 2017-10-26 | 2018-01-12 | 辽宁大学 | A kind of carbon quantum dot copper ion fluorescence probe and its preparation method and application |
CN107652971A (en) * | 2017-09-11 | 2018-02-02 | 东华大学 | A kind of preparation method of low cytotoxicity taurine carbon point |
CN107727619A (en) * | 2017-09-11 | 2018-02-23 | 东华大学 | One kind using taurine carbon point be probe to Fe3+Carry out qualitative and quantitative detecting method |
CN109187470A (en) * | 2018-09-10 | 2019-01-11 | 广西师范大学 | A kind of mediated with aptamers mixes silver-colored carbon dots catalysis H2O2The method of fluorescence spectrometry lead is reacted with TMB |
CN110041924A (en) * | 2019-05-08 | 2019-07-23 | 山东师范大学 | A kind of two-photon fluorescence carbon dots material and synthetic method and application |
CN110361371A (en) * | 2019-08-06 | 2019-10-22 | 福州大学 | A kind of fluorescent optical sensor and its construction method and application based on N doping carbon dots and catalytic oxidation |
CN110499156A (en) * | 2019-09-10 | 2019-11-26 | 中南民族大学 | A kind of sulfur doping fluorescent carbon point and its application for detecting copper ion |
CN112852420A (en) * | 2021-02-04 | 2021-05-28 | 四川农业大学 | Carbon quantum dot fluorescent probe and method for detecting thiamphenicol content |
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Cited By (12)
Publication number | Priority date | Publication date | Assignee | Title |
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CN107652971A (en) * | 2017-09-11 | 2018-02-02 | 东华大学 | A kind of preparation method of low cytotoxicity taurine carbon point |
CN107727619A (en) * | 2017-09-11 | 2018-02-23 | 东华大学 | One kind using taurine carbon point be probe to Fe3+Carry out qualitative and quantitative detecting method |
CN107573933A (en) * | 2017-10-26 | 2018-01-12 | 辽宁大学 | A kind of carbon quantum dot copper ion fluorescence probe and its preparation method and application |
CN107573933B (en) * | 2017-10-26 | 2020-08-25 | 辽宁大学 | Carbon quantum dot-copper ion fluorescent probe and preparation method and application thereof |
CN109187470A (en) * | 2018-09-10 | 2019-01-11 | 广西师范大学 | A kind of mediated with aptamers mixes silver-colored carbon dots catalysis H2O2The method of fluorescence spectrometry lead is reacted with TMB |
CN110041924A (en) * | 2019-05-08 | 2019-07-23 | 山东师范大学 | A kind of two-photon fluorescence carbon dots material and synthetic method and application |
CN110041924B (en) * | 2019-05-08 | 2021-11-09 | 山东师范大学 | Two-photon fluorescent carbon dot material, and synthesis method and application thereof |
CN110361371A (en) * | 2019-08-06 | 2019-10-22 | 福州大学 | A kind of fluorescent optical sensor and its construction method and application based on N doping carbon dots and catalytic oxidation |
CN110361371B (en) * | 2019-08-06 | 2021-06-22 | 福州大学 | Fluorescence sensor based on nitrogen-doped carbon dots and catalytic oxidation reaction, and construction method and application thereof |
CN110499156A (en) * | 2019-09-10 | 2019-11-26 | 中南民族大学 | A kind of sulfur doping fluorescent carbon point and its application for detecting copper ion |
CN112852420A (en) * | 2021-02-04 | 2021-05-28 | 四川农业大学 | Carbon quantum dot fluorescent probe and method for detecting thiamphenicol content |
CN112852420B (en) * | 2021-02-04 | 2022-04-26 | 四川农业大学 | Carbon quantum dot fluorescent probe and method for detecting thiamphenicol content |
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Application publication date: 20170811 |