CN106744808B - It is a kind of using fish scale as carbon quantum dot of raw material and its preparation method and application - Google Patents
It is a kind of using fish scale as carbon quantum dot of raw material and its preparation method and application Download PDFInfo
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Abstract
The present invention relates to a kind of using fish scale as carbon quantum dot of raw material and its preparation method and application.It after fish scale is mixed with ultrapure water, is transferred in reaction kettle, is put into rupture pressure disc, seal, be placed in microwave attenuation materials instrument, microwave heating obtains suspension；Suspension is stood, is cooled to room temperature, filtrate is filtered to take, obtains concentrate；Concentrate both ends are clipped in dialysis bag with dialysis clamp, under conditions of 4 DEG C of darknesses, for 24 hours, every 8h changes a ultrapure water, obtains carbon quantum dot for dialysis.The method of the present invention is simple and novel, recycles discarded fish scale, and natural non-impurity-doped, quantum yield is high, turns waste into wealth, develops a circular economy, effective refuse reclamation and recycling.And the present invention is conducive to the quick detection of mercury ion, can discover problems and solve them early, establishes perfect emergency preplan, prevents and treats further pollution.
Description
Technical field
It is specifically a kind of using the fish scale rich in natural cystein as carbon the invention belongs to technical field of nanometer material preparation
Source prepares Water-soluble carbon quantum dot, and application during rapid mercury detection ion using microwave attenuation materials method.
Background technique
Mercury be it is a kind of can long-term existence in environment, and have persistence, property easy to migrate, high bioconcentration and height biology
The substance of the characteristics such as toxicity.Mercury and its derivative organic mercury, can be in atmosphere as a kind of important poisonous and harmful environmental contaminants
With exist for a long time in food chain, and can migrate at a distance.China is with a long history using mercury, also once occurs because of industry in history
Accident of mercury pollution caused by with mercury, the current water body of certain mercury ores and non-ferrous metal metallurgy area in the neighbourhood, soil and rice
In still can be detected higher concentration mercury, mercury pollution and control have become Present Global concern hot spot, difficult point and focus ask
Topic, the Environmental risk management of mercury pollution has been trend of the times in the world.Mercury is inorganic in nature mainly with Elemental Mercury
3 kinds of forms of mercury and organic mercury exist, and by the enrichment of biology, enter in food chain, the excessive Hg of absorption of human body2+After can lead
The damage for causing central nervous system, liver, kidney and enteron aisle can even cause death when serious.Therefore, Hg in organism and environment2+
Detection it is particularly significant.In recent years, Hg is detected2+Method mainly have Atomic absorption-emission spectrometry, spectrophotometry, efficiently
Liquid chromatography, electrochemical process and fluorescence analysis etc..
Fluorescence analysis is convenient because having, single-minded, is concerned the advantages that sensitive and in due course in situ detection.It is several recently
Year, the research of quantum dot is very active, and quantum dot is usually to extract in the mixture of cadmium and silicon, but this tittle from lead
Son point is general toxic, also there is very big harm to environment.The scientist of Clemson University, the U.S. produces a kind of novel for the first time
Carbon nanomaterial-carbon quantum dot, similar with various metal quantum points, carbon quantum dot can issue bright in the case where illumination
Light.Carbon nano-particles have very big surface area, and this nanoparticle compares macroscopical carbon, has very peculiar physics and change
Property is learned, for opposing metallic quantum dot, carbon quantum dot nonhazardous effect, to the harm very little of environment, preparation cost is cheap, is
A kind of environmentally friendly fluorescent nano material compared to semiconductor-quantum-point with similar optical performance.Carbon quantum dot, which is removed, possesses light
Function admirable is learned, outside the advantages of conventional semiconductors quantum dot such as size is small is had, also has cytotoxicity low, bio-compatible
Property it is good, be easy to synthesize on a large scale and functional modification, the unrivaled advantages such as preparation cost is cheap and reaction condition is mild.It
It is including improving biosensor, before having application in the very wide field of medical imaging devices and small light emitting diode
Scape.
Currently, in detection Hg2+Carbon quantum dot preparation in, in order to improve the fluorescence intensity of carbon quantum dot and to Hg2+Spy
Different selectivity, often adulterates nitrogen, element sulphur and the metallic elements such as other Au, Cd, this mode can improve to a certain extent
Quantum yield enhances to Hg2+Single-minded recognition detection ability, but often artificial doping can all influence quantum dot self character, change
Ingredient, will affect absorbing ability, changes its electronic structure, can reduce quantum dot itself luminous power.
Summary of the invention
Mercury ion is detected on the spot in time in order to solve the problem of that mercury ion pollutes the environment, and the present invention designs one kind
Using the new method of carbon quantum dot and rapid mercury detection ion that fish scale is prepared as raw material.
The technical solution adopted by the present invention is that: it is a kind of using fish scale as the carbon quantum dot of raw material, the preparation method is as follows:
(1) fish scale is cleaned, is dried, shredded；The preferred grass carp scales of the fish scale；
(2) it after mixing fish scale with ultrapure water, is transferred in reaction kettle, is put into rupture pressure disc, seal, place into Microwave Water
In thermal synthesis instrument, microwave heating obtains suspension；
(3) suspension is stood, is cooled to room temperature, filter to take filtrate, obtain concentrate；
(4) concentrate both ends are clipped in dialysis bag with dialysis clamp, under conditions of 4 DEG C of darknesses, for 24 hours, every 8h is changed for dialysis
Ultrapure water, obtains carbon quantum dot.
Above-mentioned is a kind of using fish scale as the carbon quantum dot of raw material, and the solid-to-liquid ratio of fish scale and ultrapure water is 1g:70-90mL.
Above-mentioned is a kind of using fish scale as the carbon quantum dot of raw material, in microwave attenuation materials instrument, seven ranks of microwave heating point
Section: the first stage is warming up to 120 DEG C in 10min；Second stage is in 120 DEG C of constant temperature 5min；Phase III is warming up in 10min
150℃；Fourth stage is in 150 DEG C of constant temperature 5min；5th stage was warming up to 180 DEG C in 10min；6th stage is in 180 DEG C of constant temperature
5min；7th stage was the stage of reaction, and reaction temperature is 210 DEG C, heated 2h；Microwave attenuation materials instrument parameter setting, power are
1000W, upper pressure limit 1.500MPa.
Above-mentioned is a kind of using fish scale as the carbon quantum dot of raw material, and the molecular weight of dialysis bag is 3500Da.
The above-mentioned application using fish scale as the carbon quantum dot of raw material in specific detection mercury ion.Method is as follows: normal
Under the conditions of normal temperature and pressure, mercury solution to be measured is mixed with carbon quantum dot solution 1:1, with ultraviolet light irradiation, observes whether fluorescence quenches.
Water is prepared using the natural fish scale rich in cysteine as carbon source using microwave attenuation materials instrument in the present invention
Dissolubility carbon quantum dot.It is well known that generally can be divided into 2 classes there are many synthetic methods of carbon quantum dot: from top to bottom synthetic method and
Synthetic method from bottom to top, the former is based on itself biggish carbon skeleton (such as carbon target) from the synthesis side of nano carbon particle under upper peeling
Method, the latter are then directly to be modified with smaller carbon particle, passivation, thus the method for synthesizing fluorescent carbon quantum dot.From top to bottom
Synthetic method, it is difficult to carbon skeleton is thoroughly ground into nano particle, yield is extremely low；From bottom to top in synthetic method, if having with macromolecular
Machine object is raw material, and macromolecular is become small molecule generally by the mode of carbonization, a large amount of non-carbon are eliminated in carbonisation
Substance, therefore yield is also very low (highest only up to 1%).The general unstressed configuration of the carbon quantum dot just prepared or fluorescence quantum yield are lower
(most of be no greater than 10%), is not able to satisfy application, is such as used for fluorescent marker or bio-imaging condition.It then passes through at modification
Reason is to stablize its optical property and improve fluorescence quantum yield.Modify principle are as follows: introducing on carbon quantum dot surface includes that amino exists
Interior some special groups fill up the defect on carbon quantum dot surface or carbon quantum dot surface are made to generate energy potential well, send out fluorescence
Penetrate it is more stable, to improve fluorescence quantum yield.The present invention utilizes this synthetic method from bottom to top of microwave hydrothermal, to be rich in cysteine
Natural fish scale as preparation carbon quantum dot carbon source, under conditions of unmodified, quantum yield i.e. can reach 20%, not only
It effectively improves synthetic yield and the reaction time is greatly shortened.
The beneficial effects of the present invention are:
1. the invention discloses a kind of new sides for preparing carbon quantum dot and rapid mercury detection ion using grass carp scales as raw material
Method.Crude protein and ash content rich in grass carp scales, there are also a small amount of fat and sugar substances, are wherein rich in thick protein
A large amount of cysteine contains sulfydryl in cysteine.Using this characteristic of sulphur parent mercury, using grass carp scales as carbon source, utilize
The method of microwave attenuation materials prepares carbon quantum dot, to Hg2+Carry out specific detection.
2. the present invention is stablized using the carbon quantum dot property of microwave-hydrothermal method preparation, the reaction time is short, easy to operate, is easy to get
To Water-soluble carbon quantum dot, and fluorescence intensity is strong, and quantum yield is high, and thermal stability is good, and anti-light bleaching power is strong, to Hg2+'s
Detection has selection specificity, other ions coexisted in water body with mercury and same period, and same main group has phase with mercury ion
Like the metal ion of chemical property, the fluorescence intensity of the carbon quantum dot is not interfered significantly.
3. the present invention, obtains carbon quantum dot, no other elements doping and modification, without by-product using natural fish scale as raw material
Object neither changes the fluorescence activity of itself, and efficiently can quickly detect Hg2+, safety and environmental protection is pollution-free, can be applied to prepare glimmering
Light probe and biosensor etc. are a kind of sensitive materials that preferably can be applied to prepare high sensitivity thin-film type senser element
Material.
4. the method for the present invention is simple and novel, discarded grass carp scales are recycled, natural non-impurity-doped, quantum yield is high, turns waste into wealth,
It develops a circular economy, effective refuse reclamation and recycling.And the present invention is conducive to the quick detection of mercury ion, Neng Gouji
It early discovers problems and solve them, establishes perfect emergency preplan, prevent and treat further pollution
Detailed description of the invention
Fig. 1 is Water-soluble carbon quantum dot uv absorption spectra prepared by embodiment 1.
Fig. 2 a is Water-soluble carbon quantum dot fluorescence emission spectrogram of compound (320-355nm) prepared by embodiment 1.
Fig. 2 b is Water-soluble carbon quantum dot fluorescence emission spectrogram of compound (355-400nm) prepared by embodiment 1.
Fig. 3 is Fourier's infrared spectrum of Water-soluble carbon quantum dot prepared by embodiment 1.
Fig. 4 is the X-ray powder diffraction figure of Water-soluble carbon quantum dot prepared by embodiment 1.
Fig. 5 be embodiment 1 prepare Water-soluble carbon quantum dot in the presence of other metal ions to fluorescence intensity interference figure.
Fig. 6 is that Water-soluble carbon quantum dot prepared by embodiment 1 quenches intensity contrast figure to mercury ion under condition of different pH.
Fig. 7 be embodiment 1 prepare Water-soluble carbon quantum dot in the presence of various concentration mercury ion fluorescence intensity influence diagram.
Specific embodiment
Embodiment 1 is a kind of using grass carp scales as the carbon quantum dot of raw material
(1) preparation method is as follows
1) recycling grass carp scales remove extra blood and grease with warm water repeated flushing, are laid in stainless steel after cleaning
Ventilation is dried on disk, is shredded.
2) it is transferred in reaction kettle, puts after mixing 0.5g grass carp scales with 40mL ultrapure water by solid-to-liquid ratio 1g:80mL
Enter in rupture pressure disc, seal, be then placed in microwave attenuation materials instrument, the microwave heating 2.00h at 210 DEG C, it is outstanding to obtain brown color
Turbid.
In microwave attenuation materials instrument, microwave heating process is: in microwave attenuation materials instrument, seven ranks of microwave heating point
Section: the first stage is warming up to 120 DEG C in 10min；Second stage is in 120 DEG C of constant temperature 5min；Phase III is warming up in 10min
150℃；Fourth stage is in 150 DEG C of constant temperature 5min；5th stage was warming up to 180 DEG C in 10min；6th stage is in 180 DEG C of constant temperature
5min；7th stage was to be warming up to 210 DEG C, heated 2h；Microwave attenuation materials instrument parameter setting, power 1000W, upper pressure limit
For 1.500MPa.
3) brown color suspension is put into draught cupboard and is stood, is cooled to room temperature, first use 15-20 μm of filtered on buchner funnel
Remove unreacted bulk fish scale, takes filtrate.Centrifuge is used again, after elder generation is with 1500rpm low-speed centrifugal, then with 3500rpm high speed
Centrifugation is centrifuged 10min, obtains yellow transparent concentrate.
4) yellow transparent concentrate both ends are clipped in molecular weight with dialysis clamp is in the dialysis bag of 3500Da, in 4 DEG C of darknesses
Under conditions of, for 24 hours, every 8h changes a ultrapure water, and the carbon quantum dot using grass carp scales as raw material can be obtained for dialysis.
(2) it detects
1. obtained carbon quantum dot is diluted with ultrapure water, diluted multiple is 1:15, obtains diluted carbon quantum dot solution,
Detection UV absorption wavelength is carried out, as a result such as Fig. 1.
As seen from Figure 1, a faint peak is seen at 290nm wavelength, and a stronger purple is seen at 220nm wavelength
Outer absorption peak, it is available with ultraviolet spectrophotometry, using the maximum absorption band for the carbon quantum dot that grass carp scales are prepared as raw material,
Wavelength is 220nm.
2. from 320nm to 400nm, 10nm incremented by successively is obtained corresponding range by the excitation wavelength for changing luminoscope
Fluorescence emission spectrogram of compound, such as Fig. 2 a and Fig. 2 b.
The fluorescence intensity curves that comparison diagram 2a is obtained under the conditions of can be seen that different excitation wavelengths from Fig. 2 b are different, fluorescence
Intensity constantly enhances with the rising of wavelength 320nm to 355nm, and under the excitation of 355nm wavelength, fluorescence intensity reaches commanding elevation,
Then at wavelength 355nm to 400nm, fluorescence intensity declines with the increase of excitation wavelength.The excitation wavelength of portable ultraviolet lamp
Usually 350nm to 360nm, the quantum dot can issue higher fluorescence intensity, can be applied to room under the excitation of this section of wavelength
Outside, under field condition in water body mercury ion direct detection, it is convenient and efficient.
3. obtained carbon quantum dot is carried out Fourier's infrared detection, as a result such as Fig. 3.
Fourier's infrared spectrum of the present invention, the carbon quantum dot prepared using grass carp scales as raw material are shown, with grass carp scales
For raw material preparation carbon quantum dot in 1656cm-1There is characteristic absorption peak at place, prompts its surface with the presence of carboxyl, 3412cm-1Place has
Absorption peak is hydroxyl peak, i.e., can reach under natural conditions using the carbon quantum dot that grass carp scales are prepared as raw material in unmodified
It is preferable water-soluble；Especially in 627cm-1There is characteristic peak in place, prompts the presence for having C-S key, illustrates that sulfydryl takes part in fish scale
Reaction, and C-S key is generated, in next step to Hg2+The great advantage of specific detection offer is provided.
4. obtained carbon quantum dot is carried out X-ray powder diffraction detection, as a result such as Fig. 4.
From fig. 4, it can be seen that being illustrated by X powder diffraction figure with grass carp fish it can be found that there is characteristic diffraction peak at 23 °
Squama is that the carbon quantum dot of raw material preparation is unordered carbon structure inside it, i.e. the structure of the random arrangement of carbon atom.
Application of the embodiment 2 using fish scale as the carbon quantum dot of raw material in specific detection mercury ion
(1) influence of other metal ions
0.0150g Ni (NO is accurately weighed respectively3)2·6H2O, 0.0130g CuSO4·5H2O, 0.0145g Co
(NO3)2·6H2O, 0.0169g AgNO3, 0.0090g MnSO4, 0.0144g ZnSO4, 0.0140g FeCl3·6H2O,
0.0135g FeSO4·7H2O, 0.0830g Pb (NO3)2, 0.0200g Cr (NO3)3, 0.0154g Cd (NO3)2, 0.0158g
Ba(OH)2·8H2O, 0.0309g (NH4)6Mo7O24·4H2O, 0.0122g Bi (NO3)3·5H2Totally 14 kinds of different metal salt are solid by O
Body is dissolved in ultrapure water, is settled to 500mL, respectively obtain variant concentration of metal ions be 100 μM metal ion it is molten
Liquid, it is stand-by that placement is protected from light shady place.
Carbon quantum dot prepared by embodiment 1 is diluted with ultrapure water, diluted multiple is 1:3, obtains diluted carbon quantum dot
Solution.
Carbon quantum dot solution is uniformly mixed with 100 μM of different metal ions solution, volume ratio 1:1 respectively, is mixed
Uniformly, the carbon quantum dot prepared using grass carp scales as raw material is observed under other metal ion existence conditions to the shadow of fluorescence intensity
It rings.As a result such as Fig. 5.
As shown in Figure 5, under conditions of the different metal ions of 50 μM of same concentrations are respectively present, Hg2+Addition make with
Grass carp scales are the carbon quantum dot solution fluorescence intensity decline 1/2 of raw material preparation, other metal ions almost do not have fluorescence intensity
Have an impact, uniquely having obvious fluorescence intensity decline is Cu2+, but quenching rate only reaches 1/4, is not enough to influence pair
Hg2+Detection.It shows, the cation coexisted in water body and same period, same to main group, element chemistry property has similitude
Metal ion will not generate interference, it was confirmed that the carbon quantum dot solution prepared using grass carp scales as raw material has to Hg2+Specifically
The potential quality of property detection probe.
(2) influence under condition of different pH to detection mercury ion quenching intensity.
Carbon quantum dot prepared by embodiment 1 is diluted with ultrapure water, diluted multiple is 1:1, obtains diluted carbon quantum dot
Solution.
Preparation carbon quantum dot (CDs) solution by raw material of grass carp scales is picked with glass bar, is dripped on accurate pH test paper, half
After second compared with Standard colour board, carbon quantum dot solution pH value itself is about 6, and it is former for being adjusted respectively with NaOH solution with grass carp scales
The carbon quantum dot pH value of solution of material preparation is 6.0,6.5,7.0,7.5,8.0,8.5,9.0.Then 50 μM of Hg is added2+Carry out fluorescence
Detection, as a result such as Fig. 6.
As seen from Figure 6, although fluorescence intensity quenching rate is different under condition of different pH, have no effect on probe acid and
To Hg in neutral environment2+Identification, illustrate the carbon quantum dot solution prepared using grass carp scales as raw material in weak acid and weak base, neutral pH
Under the conditions of mercury ion can be detected, in the actual environment application create good condition.
(3) carbon quantum dot fluorescence intensity is influenced under the conditions of various concentration mercury ion solution is existing
Carbon quantum dot prepared by embodiment 1 is diluted with ultrapure water, diluted multiple is 1:1, obtains diluted carbon quantum dot
Solution.
It with the mercury ion solution of various concentration, mixes for 1:1 with carbon quantum dot solution, is existed respectively with fluorescent machine by volume
To Hg under 355nm wavelength2+It is detected, records the Hg of various concentration2+To the carbon quantum solution prepared using grass carp scales as raw material
The influence of fluorescence intensity, as a result such as Fig. 7.
As seen from Figure 7, the Hg of 0.5 μM of -300 μM of concentration is added2+When, fluorescence intensity is declined slightly；As the Hg of addition2+It is dense
When degree is 40 μM, fluorescence intensity is decreased obviously, i.e. quenching efficiency is obvious；It will be clear that with Hg2+The liter of concentration
Height, fluorescence intensity constantly decline, and Hg is worked as in quenching efficiency enhancing2+When concentration is 300 μM, fluorescence intensity drops to original 1/2.
Claims (5)
1. a kind of application using fish scale as the carbon quantum dot of raw material in specific detection mercury ion, which is characterized in that preparation side
Method is as follows:
(1) grass carp scales are cleaned, is dried, shredded；
(2) it after mixing grass carp scales with ultrapure water, is transferred in reaction kettle, is put into rupture pressure disc, seal, be then placed in Microwave Water
In thermal synthesis instrument, microwave heating obtains suspension；
(3) suspension is stood, is cooled to room temperature, filter to take filtrate, obtain concentrate；
(4) concentrate both ends are clipped in dialysis bag with dialysis clamp, under conditions of 4 DEG C of darknesses, for 24 hours, every 8h is changed once for dialysis
Ultrapure water obtains carbon quantum dot.
2. application described in accordance with the claim 1, which is characterized in that method is as follows: under normal temperature and pressure conditions, mercury to be measured is molten
1:1 is mixed liquid by volume with carbon quantum dot solution, with ultraviolet light irradiation, observes whether fluorescence quenches.
3. it is according to claim 1 or 2 it is a kind of using fish scale be the carbon quantum dot of raw material in specific detection mercury ion
Using, it is characterised in that: the solid-to-liquid ratio of fish scale and ultrapure water is 1g:70-90mL.
4. it is according to claim 1 or 2 it is a kind of using fish scale be the carbon quantum dot of raw material in specific detection mercury ion
Using, it is characterised in that: in microwave attenuation materials instrument, seven stages of microwave heating point: the first stage is warming up in 10min
120℃；Second stage is in 120 DEG C of constant temperature 5min；Phase III is warming up to 150 DEG C in 10min；Fourth stage is in 150 DEG C of constant temperature
5min；5th stage was warming up to 180 DEG C in 10min；6th stage is in 180 DEG C of constant temperature 5min；7th stage was the stage of reaction, instead
Answering temperature is 210 DEG C, heats 2h；Microwave attenuation materials instrument parameter setting, power 1000W, upper pressure limit 1.500MPa.
5. it is according to claim 1 or 2 it is a kind of using fish scale be the carbon quantum dot of raw material in specific detection mercury ion
Using, it is characterised in that: the molecular weight of dialysis bag is 3500Da.
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| CN107955603B (en) * | 2017-11-28 | 2020-01-07 | 广东工业大学 | Water-soluble fluorescent carbon quantum dot, preparation method thereof and method for detecting fructose |
| CN108562564B (en) * | 2018-03-29 | 2021-04-02 | 青岛大学 | Carbon quantum dot for detecting activity of inulase, and preparation method and application thereof |
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