CN108483423A - A kind of fast preparation method of right-handed chirality carbon dots - Google Patents
A kind of fast preparation method of right-handed chirality carbon dots Download PDFInfo
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- CN108483423A CN108483423A CN201810304354.3A CN201810304354A CN108483423A CN 108483423 A CN108483423 A CN 108483423A CN 201810304354 A CN201810304354 A CN 201810304354A CN 108483423 A CN108483423 A CN 108483423A
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Abstract
The present invention relates to a kind of fast preparation methods of right-handed chirality carbon dots, and using dextrorotation tryptophan as carbon source and chiral source, sodium hydroxide is modifying agent, and deionized water is solvent, and through hydrothermal synthesis method synthesis, dialysis purification, freeze-drying, right-handed chirality carbon dots are made；This preparation method technique is advanced, and technical parameter data are accurately full and accurate, and aggregate velocity is fast, is the advanced method for quickly preparing right-handed chirality carbon dots.
Description
Technical field
The present invention relates to a kind of fast preparation methods of right-handed chirality carbon dots, belong to the preparation of nano-carbon material carbon dots and answer
Technical field.
Background technology
Carbon material carbon dots have good photoluminescent property, have low cost, hypotoxicity and good biocompatibility, in life
There are potential biological applications in terms of object imaging, bio-sensing and drug conveying；Currently, the synthesis of carbon dots, structural behaviour and
Application aspect has been had large improvement.Its chiral carbon dots has become focus of attention.
Chirality refers to the phenomenon that in kind and its mirror image cannot be overlapped, it is widely present in nature, is present in work
In large biological molecule for vital movement important foundation, such as protein, polysaccharide, nucleic acid and enzyme, be entirely almost it is chiral, these
Molecule has important physiological function in vivo, and is present in supermolecule and nanostructure；The research of chiral nano particle, pushes away
It has moved chirality identifying, sense, imaging, the application of be catalyzed etc..
Carbon dots Chiral properties are assigned, the left or right rotation chirality carbon dots of fluorescence and chiral performance can be prepared while have,
Carbon dots are made to have wider application in terms of chiral Recognition, chiral detection, chiral sensing；The synthetic method point of chirality carbon dots at present
For one-step method and two-step method, one-step method is that carbon source and chiral ligand are placed in same system, or directly using chiral ligand as carbon source,
Chirality carbon dots are made；Two-step method is first to prepare carbon dots, then modified with chiral ligand, obtains chiral carbon dots；This skill at present
Art is also in scientific research.
Invention content
Goal of the invention
The purpose of the present invention is being directed to background technology situation, using biological micromolecule dextrorotation tryptophan as carbon source and chiral source,
Deionized water is solvent, and through hydro-thermal method synthesis, dialysis purification, freeze-drying, right-handed chirality carbon dots are made；It is with L-tryptophan
Carbon source and chiral source, deionized water are solvent, left-handed chiral carbon dots are made through hydro-thermal method synthesis, to expand the use of chiral carbon dots
Range.
Technical solution
The chemical substance material that the present invention uses is：Dextrorotation tryptophan, L-tryptophan, sodium hydroxide, deionized water,
It is as follows that combination prepares dosage：It is measurement unit with gram, milliliter
Preparation method is as follows：
(1) selected chemical substance material
The chemical substance material that uses of preparation to be carried out selected, and carry out quality purity control：
(2) carbon dots aqueous solution is prepared
The preparation of carbon dots aqueous solution carries out in reaction kettle, completes in a heated state；
1. preparing solution
Weigh dextrorotation tryptophan 0.5g ± 0.0001g, sodium hydroxide 0.09g ± 0.0001g, measure deionized water 15mL ±
0.0001mL is added in polytetrafluoroethylcontainer container, then carries out ultrasonic disperse 5min, and ultrasonic frequency 60KHz makes it dissolve,
At mixed solution；
2. the polytetrafluoroethylcontainer container for filling mixed solution is placed in reaction kettle, and closed；
3. reaction kettle is placed in heating furnace, airtight heating, 120 DEG C ± 1 DEG C of heating temperature, heating time 16h；
Mixed solution during heating, will chemically react, reaction equation is as follows：
In formula：CDs-COONa：Contain the carbon quantum dot of carboxylic acid sodium in surface
4. after reaction, stopping heating, reaction kettle and its interior solution cool to 25 DEG C with the furnace；
(3) it filters
1. opening heating furnace, reaction kettle is opened, takes out polytetrafluoroethylcontainer container and its interior mixed solution；
2. mixed solution is filtered with three layers of middling speed qualitative filter paper, retains filtrate, discard sediment；
(4) dialysis purification
It dialyses 1. filtrate is added in bag filter, dialysis time 96h retains the solution in bag filter, i.e. dextrorotation after dialysis
Chiral carbon dots solution；
2. being freeze-dried
Right-handed chirality carbon dots solution after dialysis is purified moves into drying bottle, is subsequently placed in vacuum freezing drying oven,
Vacuum degree 2Pa is freeze-dried -80 DEG C of temperature, sublimation drying 8h；Right-handed chirality carbon dots solid powder is obtained after freeze-drying,
That is final product；
(5) test, analysis and characterization
Pattern, structure, the ingredient of the right-handed chirality carbon dots of preparation are detected, analyze, characterized；
The morphology analysis of right-handed chirality carbon dots is carried out with transmission electron microscope；
The functional group analysis of right-handed chirality carbon dots is carried out with infrared spectrometer；
The optical property of right-handed chirality carbon dots is carried out with ultraviolet-uisible spectrophotometer, Fluorescence Spectrometer and circular dichroism spectrometer
Analysis；
Conclusion：The particle diameter distribution of right-handed chirality carbon dots is relatively narrow, and aqueous solution issues green-yellow light in 365nm ultra violet lamps,
There is strong emission peak under the exciting light irradiation of 320-400nm, has and excite independent property；Product purity is up to 99.8%；
(6) product storage
The right-handed chirality carbon dots of preparation are stored in the glass container of amber transparent, it is closed to be kept in dark place, be placed in it is dry,
Clean environment wants waterproof, sun-proof, moisture-proof, anti-acid-alkali salt to corrode, 20 DEG C of storage temperature, relative humidity 10%.
Advantageous effect
There is apparent advance compared with the background technology, the present invention, be the hydrogen using dextrorotation tryptophan as carbon source and chiral source
Sodium oxide molybdena is modifying agent, and deionized water is solvent, and through hydrothermal synthesis method synthesis, dialysis purification, vacuum freeze drying, dextrorotation is made
Chiral carbon dots；This preparation method technique is advanced, and data are accurately full and accurate, and product purity is up to 99.8%, is advanced right-handed chirality
The preparation method of carbon dots.
Description of the drawings：
Fig. 1, right-handed chirality carbon dots aqueous solution hydrothermal synthesis state diagram
Fig. 2, right-handed chirality carbon dots shape appearance figure
Fig. 3, dextrorotation tryptophan and right-handed chirality carbon dots infrared spectrum compare figure
Fig. 4, right-handed chirality carbon dots UV-visible absorption spectrum
Fluorescence spectra under Fig. 5, right-handed chirality carbon dots difference excitation wavelength
Fig. 6, right-handed chirality carbon dots and left-handed two chromatogram of chiral carbon null circle
As shown in the figure, list of numerals is as follows：
1, heating furnace, 2, bell, 3, stove seat, 4, workbench, 5, reaction kettle, 6, polytetrafluoroethylcontainer container, 7, mixed solution,
8, display screen, 9, indicator light, 10, power switch, 11, heating temperature control, 12, heating time controller, 13, furnace chamber, 14,
React kettle cover.
Specific implementation mode：
Below in conjunction with attached drawing, the present invention will be further described：
Shown in Fig. 1, right-handed chirality carbon dots aqueous solution preparing processes figure, each portion position will correctly match, sequentially grasps according to quantity
Make.
The magnitude for preparing the chemical substance used is determined by pre-set range, is measurement unit with gram, milliliter.
The preparation of right-handed chirality carbon dots aqueous solution carries out in reaction kettle, is completed under heating furnace heated condition
's；
Heating furnace 1 is vertical, and the top of heating furnace 1 is bell 2, lower part is stove seat 3, is furnace chamber 13 in heating furnace 1；In stove
The interior bottom of chamber 13 is equipped with workbench 4, and reaction kettle 5 is put on workbench 4, polytetrafluoroethylcontainer container 6 is put in reaction kettle 5,
It is mixed solution 7 in polytetrafluoroethylcontainer container 6, reaction kettle 5 is closed by reaction kettle cover 14；It is equipped with display screen 8 on stove seat 3, refers to
Show lamp 9, power switch 10, heating temperature control 11, heating time controller 12.
It is the shape appearance figure of right-handed chirality carbon dots shown in Fig. 2, as shown in the figure, right-handed chirality carbon dots are in spherical, particle diameter distribution
Relatively narrow, favorable dispersibility is not reunited significantly.
Shown in Fig. 3, compare figure for dextrorotation tryptophan and right-handed chirality carbon dots infrared spectrum, as shown in the figure, it can be seen that right
The chiral carbon dots spectrum of rotation is different from the spectrum of dextrorotation tryptophan, but left-handed chiral carbon dots and right-handed chirality carbon dots have similar spy
Peak is levied, in 3402cm-1The absorption band at place belongs to the stretching vibration of O-H, 3254cm-1The absorption band at place is corresponding to the flexible of N-H
Vibration, these functional groups improve the hydrophily of chiral carbon dots in aqueous solution；3061cm-1The absorption band at place is attributed to-NH,
1662cm-1The absorption band at place belongs to the vibration of C=O, 1600cm-1And 1400cm-1Neighbouring absorption band respectively represents COO- not
Symmetrical and symmetrical stretching vibration, in 1244cm-1Place's absorption band is attributed to NHC=O, 1110cm-1The absorption band at place corresponds to C-
The stretching vibration of O；The above results confirm that carboxyl, amino and amido bond are contained in chiral carbon dots surface；These hydrophilic functional groups
So that chiral carbon dots have good dispersibility in water.
It is the UV-visible absorption spectrum of right-handed chirality carbon dots aqueous solution, as shown in the figure, right-handed chirality carbon shown in Fig. 4
Point aqueous solution has absorption near 220nm and 280nm.
It is right-handed chirality carbon dots aqueous solution fluorescence spectra under different excitation wavelengths, as shown in the figure, dextrorotation shown in Fig. 5
Chiral carbon dots have strong emission peak under the exciting light of 320-400nm near 475nm, belong to green-yellow light, and only with excitation
Vertical property.
It is as shown in the figure, left-handed for the circular dichroism spectrogram of left-handed chiral carbon dots and right-handed chirality carbon dots aqueous solution shown in Fig. 6
The circular dichroism signal of chiral carbon dots and right-handed chirality carbon dots is opposite and symmetrical, illustrates left-handed chiral carbon dots and right-handed chirality carbon
Point is enantiomer.
Embodiment 1
The preparation method of left-handed chirality carbon dots is as follows：
(1) L-tryptophan 0.5g ± 0.0001g, sodium hydroxide 0.09g ± 0.0001g are weighed, deionized water is measured
15mL ± 0.0001mL, is added in another polytetrafluoroethylcontainer container, is then added in another heating furnace, and seal；
120 DEG C ± 1 DEG C of hydrothermal synthesis reaction temperature, heating time 16h；
Cool to 25 DEG C after reaction with the furnace；
(2) it filters, is filtered with three layers of middling speed qualitative filter paper；
(3) bag filter dialysis purification：Filtrate is added in bag filter and is dialysed, dialysis time 96h retains bag filter after dialysis
Interior solution, i.e., left-handed chiral carbon dots solution；
(4) vacuum freeze drying, vacuum degree 2Pa are freeze-dried -80 DEG C of temperature, sublimation drying 8h；
At final product after freeze-drying：Left-handed chirality carbon dots.
Claims (2)
1. a kind of fast preparation method of right-handed chirality carbon dots, it is characterised in that：The chemical substance material used is：Dextrorotation color ammonia
Acid, L-tryptophan, sodium hydroxide, deionized water, it is as follows that a combination thereof prepares dosage：It is measurement unit with gram, milliliter
Preparation method is as follows：
(1) selected chemical substance material
The chemical substance material that uses of preparation to be carried out selected, and carry out quality purity control：
(2) carbon dots aqueous solution is prepared
The preparation of carbon dots aqueous solution carries out in reaction kettle, completes in a heated state；
1. preparing solution
Weigh dextrorotation tryptophan 0.5g ± 0.0001g, sodium hydroxide 0.09g ± 0.0001g, measure deionized water 15mL ±
0.0001mL is added in polytetrafluoroethylcontainer container, then carries out ultrasonic disperse 5min, and ultrasonic frequency 60KHz makes it dissolve, at
Mixed solution；
2. the polytetrafluoroethylcontainer container for filling mixed solution is placed in reaction kettle, and closed；
3. reaction kettle is placed in heating furnace, airtight heating, 120 DEG C ± 1 DEG C of heating temperature, heating time 16h；
Mixed solution during heating, will chemically react, reaction equation is as follows：
In formula：CDs-COONa：Contain the carbon quantum dot of carboxylic acid sodium in surface
4. after reaction, stopping heating, reaction kettle and its interior solution cool to 25 DEG C with the furnace；
(3) it filters
1. opening heating furnace, reaction kettle is opened, takes out polytetrafluoroethylcontainer container and its interior mixed solution；
2. mixed solution after cooling is filtered with middling speed qualitative filter paper, retains filtrate, discard sediment；
(4) dialysis purification
It dialyses 1. filtrate is added in bag filter, dialysis time 96h retains the solution in bag filter, i.e. right-handed chirality after dialysis
Carbon dots solution；
2. being freeze-dried
Right-handed chirality carbon dots solution after dialysis is purified moves into freeze-drying bottle, is placed in -80 DEG C of reach in freezer freezing, then
Right-handed chirality carbon dots solid powder must be purified by being suspended on after being dried on freeze drier；
(5) test, analysis and characterization
To the pattern of the right-handed chirality carbon dots of preparation, structure, ingredient, it is detected, analyzes, characterizes；
The morphology analysis of right-handed chirality carbon dots is carried out with transmission electron microscope；
The functional group analysis of right-handed chirality carbon dots is carried out with infrared spectrometer；
The optical property point of right-handed chirality carbon dots is carried out with ultraviolet-uisible spectrophotometer, Fluorescence Spectrometer and circular dichroism spectrometer
Analysis；
Conclusion：The particle diameter distribution of right-handed chirality carbon dots is relatively narrow, and aqueous solution issues green-yellow light in 365nm ultra violet lamps,
There is strong emission peak under the exciting light irradiation of 320-400nm, has and excite independent property；Product purity is up to 99.8%；
(6) product storage
The right-handed chirality carbon dots of preparation are stored in the glass container of amber transparent, it is closed to be kept in dark place, it is placed in dry, clean
Environment wants waterproof, sun-proof, moisture-proof, anti-acid-alkali salt to corrode, 20 DEG C of storage temperature, relative humidity 10%.
2. a kind of fast preparation method of right-handed chirality carbon dots according to claim 1, it is characterised in that：Right-handed chirality carbon
The preparation of point aqueous solution carries out in reaction kettle, is completed under heating furnace heated condition；
Heating furnace (1) is vertical, and the top of heating furnace (1) is bell (2), lower part is stove seat (3), is furnace chamber in heating furnace (1)
(13)；It is equipped with workbench (4) in the interior bottom of furnace chamber (13), reaction kettle (5) is put on workbench (4), reaction kettle (5) is built-in
Polytetrafluoroethylcontainer container (6) is put, is mixed solution (7) in polytetrafluoroethylcontainer container (6), reaction kettle (5) is by reaction kettle cover (14)
It is closed；Display screen (8), indicator light (9), power switch (10), heating temperature control (11), heating are equipped on stove seat (3)
Time controller (12).
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| CN115124997A (en) * | 2022-08-09 | 2022-09-30 | 西北师范大学 | Preparation of carbon quantum dot fluorescent probe and application of carbon quantum dot fluorescent probe in detection of iron ions and cysteine |
| CN115386372A (en) * | 2022-09-21 | 2022-11-25 | 中国科学院兰州化学物理研究所 | Preparation of chiral fluorescent carbon dots and application of chiral fluorescent carbon dots in identification and detection of tyrosine enantiomers |
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| CN115124997A (en) * | 2022-08-09 | 2022-09-30 | 西北师范大学 | Preparation of carbon quantum dot fluorescent probe and application of carbon quantum dot fluorescent probe in detection of iron ions and cysteine |
| CN115386372A (en) * | 2022-09-21 | 2022-11-25 | 中国科学院兰州化学物理研究所 | Preparation of chiral fluorescent carbon dots and application of chiral fluorescent carbon dots in identification and detection of tyrosine enantiomers |
| CN115386372B (en) * | 2022-09-21 | 2023-05-26 | 中国科学院兰州化学物理研究所 | Preparation of chiral fluorescent carbon dots and application of chiral fluorescent carbon dots in identification and detection of tyrosine enantiomers |
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