CN109095453A - A kind of preparation method of the fluorescent carbon point based on tealeaves and its manufactured fluorescent carbon point - Google Patents
A kind of preparation method of the fluorescent carbon point based on tealeaves and its manufactured fluorescent carbon point Download PDFInfo
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Abstract
The present invention relates to a kind of preparation method of fluorescent carbon point based on tealeaves and its manufactured fluorescent carbon points, and the method comprising the steps of are as follows: by tealeaves grinds, tea grounds is filtered to remove after extracting using dehydrated alcohol as Extraction solvent, collects gained extracting solution；It is transferred in reaction kettle after addition water in gained extracting solution and carries out hydrothermal carbonization, naturally cool to room temperature；Under the irradiation of ultraviolet lamp, column chromatography for separation is carried out to products therefrom, collects the fluorescent carbon point solution of different fluorescence colors, obtain fluorescent carbon point after revolving removes solvent.High temperature direct carbonization will be carried out after the tea grounds drying and crushing obtained after extraction, and naturally cool to room temperature, it is ultrasonically treated after obtained product is added deionized water, obtains fluorescent carbon point solution after filtering with microporous membrane, centrifugal treating and dialysis, obtain fluorescent carbon point after freeze-dried.All fluorescent carbon point yields of the present invention are high, stability is good, and method is simple, environmentally protective, at low cost, it is easy to accomplish scale and industrialized production.
Description
Technical field
The present invention relates to carbon nanomaterial, in particular to the preparation method of a kind of fluorescent carbon point based on tealeaves and its it is made
Fluorescent carbon point.
Background technique
Fluorescent carbon quantum dot, abbreviation carbon dots are a kind of carbon nanomaterials emerging in recent years, due to its superior low biology
Toxicity, good luminescent properties, in terms of cell imaging, biological detection, photocatalysis degradation organic contaminant, photoelectricity all
It is of great significance.Compared to semiconductor-quantum-point, carbon dots are more suitable for the fields such as cell imaging, and it is selected in raw material
It is even more varied to select aspect, is conducive to push its development.
The carbon source that can be used for preparing fluorescent carbon point has very much, inorganic (various carbon materials) and organic (small organic molecule, high score
Son, biomass) material is used equally for preparing fluorescent carbon point.Currently, using biological material as the report of carbon source preparation carbon dots
Very much, but mostly equal blue light-emitting, the carbon source of use have orange peel (Chinese Patent Application No. 201410841970.4)；Corncob
(Chinese Patent Application No. 201510147558.7)；Shaddock (Chinese Patent Application No. 201511004717.4) etc., in addition, using
Biomass is less for the report that various fluorescence color carbon dots are prepared in carbon source.
Contain the Multiple components such as tea polyphenols, protein, theanine, alkaloid, Tea Pigment, tea polysaccharide, cellulose in tealeaves,
The tea grounds even obtained after extracted effective component has been also enriched in the ingredients such as cellulose, protein, polyphenol, organic acid, tealeaves
It is all the ideal carbon source for preparing fluorescent carbon point with tea grounds.Using tealeaves or tea grounds as carbon source, fluorescent carbon point is prepared, is had
Report, such as Chang have obtained fluorescent carbon point in direct carbonization 2 hours at 300 DEG C for after dry green tea grinds
[Journal of Materials Chemistry B,2013,1,1774-1781]；Xi etc. is reaction with black tea leaf and water
Object is prepared for fluorescent carbon point [RSC Advances, 2017,7,28637-28646] for hydro-thermal reaction 5 hours at 200 DEG C；Ye Nan
Etc. directly adopt Iron Guanyin green tea tea grounds be carbon source, through microwave hydrothermal reaction be prepared for fluorescent carbon point [Ningde college of education journal,
2017,29,356-360], but carbon dots made above are single blue-fluorescence carbon dots, solvent used when using hydro-thermal method
For single water, it is unfavorable for other effective components in tealeaves and participates in reaction, and is still lacked using tealeaves and tea grounds preparation carbon dots and be
System Journal of Sex Research.
Summary of the invention
The purpose of the present invention is to provide a kind of preparation method of fluorescent carbon point based on tealeaves and its manufactured fluorescent carbons
The fluorescent carbon point solution of different fluorescence colors can be prepared in point from the extract of tealeaves, and preparation method is simple, green ring
It protects, is at low cost, it is easy to accomplish scale and industrialized production.
To achieve the above object, the present invention provides a kind of preparation method of fluorescent carbon point based on tealeaves comprising following
Step:
(1) by tealeaves grinds, using dehydrated alcohol as Extraction solvent, it is filtered to remove tea grounds after extracting, collects institute
Obtain extracting solution；
(2) extracting solution obtained by step (1) is taken, is transferred in reaction kettle after water is added, hydrothermal carbonization is carried out, naturally cools to room
Temperature；
(3) under the irradiation of ultraviolet lamp, column chromatography for separation is carried out to step (2) products therefrom, collects different fluorescence colors
Fluorescent carbon point solution, through revolving remove solvent after obtain fluorescent carbon point.
In step (1), the Extracting temperature that the tealeaves extracts is 20~80 DEG C, and extraction time is not less than 1h, and solid-to-liquid ratio is
1g:20~50mL.
In step (2), the volume ratio of the extracting solution and water is 1: 0~1, the temperature of the hydrothermal carbonization is 120 DEG C~
180 DEG C, the time is 2~8h.
In step (3), the stationary phase of the column chromatography is 200~300 mesh silica gel, and mobile phase is determined by thin-layered chromatography,
The fluorescent carbon point solution of the difference fluorescence color includes at least red, yellow, blue.
A kind of preparation method of the fluorescent carbon point based on tealeaves further include:
(4) tea grounds obtained by step (1) be successively dried, crushed, after the processing of high temperature direct carbonization, naturally cooling to room
Temperature；
(5) into step (4) products therefrom be added deionized water after be successively ultrasonically treated, filtering with microporous membrane, from
Fluorescent carbon point solution is obtained after heart processing and dialysis, obtains fluorescent carbon point after freeze-dried.
High temperature direct carbonization in the step (4) carries out in high temperature furnace, and treatment temperature is 150-300 DEG C, when reaction
Between be 2-15h.
Ultrasonic power is 500W, ultrasonic time 10-120min in the step (5)；Miillpore filter aperture is 0.22 μm；
Centrifugal speed is 1000-10000rpm, centrifugation time 5-60min；Dialysis uses the bag filter of 1000-3500Da, when dialysis
Between be 6-36h；Being freeze-dried temperature is -50 DEG C.
The tealeaves used in a kind of preparation method of fluorescent carbon point based on tealeaves is green tea, black tea or dark green tea etc..
To achieve the above object, the present invention also provides a kind of preparation methods of above-mentioned fluorescent carbon point based on tealeaves to be made
Fluorescent carbon point.
The method of the present invention is based on tealeaves, using dehydrated alcohol as extractant, passes through simple hydrothermal carbonization from the extracting solution of tealeaves
The fluorescent carbon point solution of the various fluorescence colors such as red, yellow, blue is prepared, the tea grounds obtained after extraction passes through direct pyrocarbon
Blue light carbon dots have also been prepared in change, and preparation method is simple, environmentally protective, at low cost, it is easy to accomplish the scale and work of carbon dots
Industry metaplasia produces, and obtained all fluorescent carbon point yields are high, stability is good.The partial size of obtained feux rouges carbon dots is small, is 2.6nm left
It is right.
Detailed description of the invention
Fig. 1 is the transmission electron microscope picture (scale 20nm) of feux rouges carbon dots of the present invention through tea extract preparation.
Fig. 2 be the UV-visible spectrum of feux rouges carbon quantum dot of the present invention through tea extract preparation, best excitation with
Best transmitting fluorescence spectra.
Fig. 3 is fluorescence spectra of the carbon dots of different fluorescence colors of the present invention through tea extract preparation at 360nm
(1 is blue light, and 2 be green light, and 3 be orange light, and 4 be feux rouges).
Fig. 4 be the UV-visible spectrum of the blue light carbon dots of gained tea grounds preparation after the present invention is extracted, best excitation with
Best transmitting fluorescence spectra.
Specific embodiment
The present invention will be further explained with reference to the examples below.
Embodiment 1
The green tea 2g of grinds is weighed, 50mL dehydrated alcohol is added, sealed soak extracts 12h at room temperature, crosses and filters out
Tea grounds is removed, takes 8mL extracting solution and 2mL deionized water in 25mL reaction kettle, 160 DEG C of heating 3h are cooled to room temperature, and solution is turned
Enter in the silicagel column having had been filled with, carry out column chromatography under ultraviolet light irradiation using petroleum ether and ethyl acetate as eluant, eluent,
The fluorescent carbon point solution for collecting different fluorescence colors respectively obtains fluorescent carbon point after revolving removes solvent.It is obtained after taking extraction
Drying tea grounds 1g, be put into porcelain boat, heat 5h at 180 DEG C, the black powder of generation is taken out in merging beaker, is added
10mL ultrapure water is ultrasonically treated 30min, and 0.22 μm of film filtering obtains red tan solution, and 8000rpm is centrifuged 5min, takes supernatant
It dialyses for 24 hours in merging 3500Da bag filter to get blue light carbon dots solution, fluorescent carbon point solution is obtained after freeze-dried.
Embodiment 2
Embodiment 2 difference from example 1 is that, weigh the black tea leaf 2g of grinds, the anhydrous second of 50mL be added
Alcohol, refluxing extraction 105min at 80 DEG C, is filtered to remove filter residue while hot, and takes 9mL extracting solution and 1mL deionized water in 25mL immediately
In reaction kettle, 160 DEG C of heating 3h are cooled to room temperature, solution are transferred in the silicagel column having had been filled with, with petroleum ether and acetic acid
Ethyl ester carries out column chromatography as eluant, eluent under ultraviolet light irradiation, collects the fluorescent carbon point solution of different fluorescence colors respectively, warp
Revolving obtains fluorescent carbon point after removing solvent.The drying tea grounds 1g obtained after extracting is taken, is put into porcelain boat, is heated at 160 DEG C
6h takes out the black powder of generation in merging beaker, and 10mL ultrapure water is added and is ultrasonically treated 20min, 0.22 μm of film filtering obtains
To red tan solution, 9000rpm is centrifuged 5min, take dialyse in supernatant merging 3500Da bag filter it is molten to get blue light carbon dots for 24 hours
Liquid obtains fluorescent carbon point solution after freeze-dried.
Embodiment 3
Embodiment 3 difference from example 1 is that, weigh the dark green tea tealeaves 2g of grinds, the anhydrous second of 50mL be added
Alcohol, refluxing extraction 120min at 80 DEG C, is filtered to remove filter residue, and take 10mL extracting solution in 25mL reaction kettle immediately while hot, and 180
DEG C heating 6h, is cooled to room temperature, solution is transferred in the silicagel column having had been filled with, using petroleum ether and ethyl acetate as eluting
Agent carries out column chromatography under ultraviolet light irradiation, collects the fluorescent carbon point solution of different fluorescence colors respectively, removes solvent through revolving
After obtain fluorescent carbon point.The drying tea grounds 1g obtained after extracting is taken, is put into porcelain boat, heats 8h at 180 DEG C, by the black of generation
Color powder takes out in merging beaker, and 20mL ultrapure water is added and is ultrasonically treated 30min, and 0.22 μm of film filtering obtains red tan solution,
6000rpm is centrifuged 5min, takes in supernatant merging 3500Da bag filter and dialyses for 24 hours to get blue light carbon dots solution, freeze-dried
After obtain fluorescent carbon point solution.
Each technical characteristic of embodiment described above can be combined arbitrarily, for simplicity of description, not to above-mentioned reality
It applies all possible combination of each technical characteristic in example to be all described, as long as however, the combination of these technical characteristics is not deposited
In contradiction, all should be considered as described in this specification.
The embodiments described above only express several embodiments of the present invention, and the description thereof is more specific and detailed, but simultaneously
It cannot therefore be construed as limiting the scope of the patent.It should be pointed out that coming for those of ordinary skill in the art
It says, without departing from the inventive concept of the premise, various modifications and improvements can be made, these belong to protection of the invention
Range.Therefore, the scope of protection of the patent of the invention shall be subject to the appended claims.
Claims (9)
1. a kind of preparation method of the fluorescent carbon point based on tealeaves, characterized in that it comprises the following steps:
(1) by tealeaves grinds, using dehydrated alcohol as Extraction solvent, it is filtered to remove tea grounds after extracting, collects gained and mentions
Take liquid；
(2) extracting solution obtained by step (1) is taken, is transferred in reaction kettle after water is added, hydrothermal carbonization is carried out, naturally cools to room temperature；
(3) under the irradiation of ultraviolet lamp, column chromatography for separation is carried out to step (2) products therefrom, collects the glimmering of different fluorescence colors
Light carbon dots solution obtains fluorescent carbon point after revolving removes solvent.
2. a kind of preparation method of fluorescent carbon point based on tealeaves according to claim 1, which is characterized in that step (1)
The Extracting temperature that the tealeaves extracts is 20~80 DEG C, and extraction time is not less than 1h, and solid-to-liquid ratio is 1g:20~50mL.
3. a kind of preparation method of fluorescent carbon point based on tealeaves according to claim 1, which is characterized in that step (2)
The volume ratio of the extracting solution and water is 1: 0~1, and the temperature of the hydrothermal carbonization is 120 DEG C~180 DEG C, and the time is 2~8h.
4. a kind of preparation method of fluorescent carbon point based on tealeaves according to claim 1, which is characterized in that step (3)
The stationary phase of the column chromatography is 200~300 mesh silica gel, and mobile phase is determined by thin-layered chromatography, the difference fluorescence color
Fluorescent carbon point solution includes at least red, yellow, blue.
5. a kind of preparation method of fluorescent carbon point based on tealeaves according to claim 1, it is characterised in that further include:
(4) tea grounds obtained by step (1) be successively dried, crushed, after the processing of high temperature direct carbonization, naturally cooling to room temperature；
(5) be added into step (4) products therefrom after deionized water be successively ultrasonically treated, filtering with microporous membrane, at centrifugation
Fluorescent carbon point solution is obtained after reason and dialysis, obtains fluorescent carbon point after freeze-dried.
6. a kind of preparation method of fluorescent carbon point based on tealeaves according to claim 5, which is characterized in that the step
Suddenly the high temperature direct carbonization in (4) carries out in high temperature furnace, and treatment temperature is 150-300 DEG C, reaction time 2-15h.
7. a kind of preparation method of fluorescent carbon point based on tealeaves according to claim 5, which is characterized in that the step
Suddenly ultrasonic power is 500W, ultrasonic time 10-120min in (5)；Miillpore filter aperture is 0.22 μm；Centrifugal speed is
1000-10000rpm, centrifugation time 5-60min；Dialysis uses the bag filter of 1000-3500Da, dialysis time 6-36h；
Being freeze-dried temperature is -50 DEG C.
8. a kind of preparation method of fluorescent carbon point based on tealeaves according to claim 1, which is characterized in that the tealeaves
For green tea, black tea or dark green tea.
9. fluorescent carbon point made of the preparation method of the fluorescent carbon point described in any one of -8 based on tealeaves according to claim 1.
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Cited By (13)
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| CN109593525A (en) * | 2019-01-04 | 2019-04-09 | 浙江工业大学 | It is a kind of using Longjing tea as carbon quantum dot of carbon source and its preparation method and application |
| CN109705858A (en) * | 2019-01-04 | 2019-05-03 | 河南大学 | A kind of preparation method and applications of cupric carbon dots |
| CN109722243A (en) * | 2019-01-04 | 2019-05-07 | 浙江工业大学 | A kind of incremental endogenous carbon quantum dot and the preparation method and application thereof |
| CN109777405A (en) * | 2019-02-03 | 2019-05-21 | 山西大同大学 | A kind of red blue pair emits fluorescent carbon points and for detecting Al simultaneously3+And Cu2+The fluorescence analysis method of ion |
| CN109913211A (en) * | 2019-04-08 | 2019-06-21 | 东北林业大学 | Carbon quantum dot and preparation method thereof, membrane material of carbon containing quantum dot and its preparation method and application |
| CN111773287A (en) * | 2020-06-30 | 2020-10-16 | 湖北大学 | Preparation method and application of tea nanoclusters |
| CN111892036A (en) * | 2020-07-10 | 2020-11-06 | 山西大学 | Method for preparing carbon quantum dots by using waste green tea residues and application thereof |
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| CN113390840A (en) * | 2021-06-12 | 2021-09-14 | 宁德师范学院 | Method for synthesizing carbon dots and detecting copper ions in water body |
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| CN109722243B (en) * | 2019-01-04 | 2021-12-21 | 浙江工业大学 | Gain endogenous carbon quantum dot and preparation method and application thereof |
| CN109705858A (en) * | 2019-01-04 | 2019-05-03 | 河南大学 | A kind of preparation method and applications of cupric carbon dots |
| CN109722243A (en) * | 2019-01-04 | 2019-05-07 | 浙江工业大学 | A kind of incremental endogenous carbon quantum dot and the preparation method and application thereof |
| CN109593525A (en) * | 2019-01-04 | 2019-04-09 | 浙江工业大学 | It is a kind of using Longjing tea as carbon quantum dot of carbon source and its preparation method and application |
| CN109705858B (en) * | 2019-01-04 | 2020-05-01 | 河南大学 | Preparation method and application of copper-containing carbon dots |
| CN109777405A (en) * | 2019-02-03 | 2019-05-21 | 山西大同大学 | A kind of red blue pair emits fluorescent carbon points and for detecting Al simultaneously3+And Cu2+The fluorescence analysis method of ion |
| CN109777405B (en) * | 2019-02-03 | 2022-02-08 | 山西大同大学 | Red-blue dual-emission fluorescent carbon dot and method for simultaneously detecting Al3+And Cu2+Method for fluorescence analysis of ions |
| CN109913211A (en) * | 2019-04-08 | 2019-06-21 | 东北林业大学 | Carbon quantum dot and preparation method thereof, membrane material of carbon containing quantum dot and its preparation method and application |
| US11220631B2 (en) | 2019-06-12 | 2022-01-11 | Zhejiang University Of Science & Technology | Method of making biomass fluorescent carbon quantum dots from soybean dregs by hydrothermal synthesis and uses thereof |
| CN111773287A (en) * | 2020-06-30 | 2020-10-16 | 湖北大学 | Preparation method and application of tea nanoclusters |
| CN111892036A (en) * | 2020-07-10 | 2020-11-06 | 山西大学 | Method for preparing carbon quantum dots by using waste green tea residues and application thereof |
| CN112376124A (en) * | 2020-11-20 | 2021-02-19 | 上海市第六人民医院 | Antibacterial dressing |
| CN113390840A (en) * | 2021-06-12 | 2021-09-14 | 宁德师范学院 | Method for synthesizing carbon dots and detecting copper ions in water body |
| CN116144355A (en) * | 2023-03-09 | 2023-05-23 | 郑州大学 | Ultra-long-time near-infrared water-soluble afterglow luminous carbon dot and preparation method and application thereof |
| CN116590009A (en) * | 2023-05-30 | 2023-08-15 | 聊城大学 | Composite film capable of being excited by blue light to generate white fluorescence and preparation method and application thereof |
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