CN105366659A - Method for hydro-thermal synthesis of carbon quantum dots based on fruits - Google Patents
Method for hydro-thermal synthesis of carbon quantum dots based on fruits Download PDFInfo
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- CN105366659A CN105366659A CN201510929542.1A CN201510929542A CN105366659A CN 105366659 A CN105366659 A CN 105366659A CN 201510929542 A CN201510929542 A CN 201510929542A CN 105366659 A CN105366659 A CN 105366659A
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- 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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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer
Abstract
The invention discloses a method for hydro-thermal synthesis of carbon quantum dots based on fruits. The fruits are completely washed, cut into small pieces or squeezed into juice, treated for a period of time in a stirrer and then placed in a hydro-thermal reaction kettle, the hydro-thermal reaction is conducted for 4-72 h at the temperature of 100-250 DEG C, centrifugation and dialysis are conducted, and then the carbon quantum dots are obtained. The novel method for hydro-thermal synthesis of the carbon quantum dots based on the fruits is provided, the raw materials are wide in source and environmentally friendly, and the method is suitable for large-scale preparation.
Description
Technical field
The present invention relates to a kind of preparation method of inorganic nano material, be specifically related to a kind of method based on fruit Hydrothermal Synthesis carbon quantum dot.
Background technology
Carbon quantum dot have good water solubility, luminous along with excitation wavelength change, bio-toxicity is low, chemical stability is high, fluorescence along with advantages such as pH value change, fluorescence salt tolerances, make it have potential application prospect in a lot of fields.Green syt carbon quantum dot is carried out with biological raw material, meet the requirement of chemical developer and the theory of Atom economy, the document about biological raw material synthesis carbon quantum dot of report is had to have: ZhouJJ, ShengZH, HanHY, ZouMQ, LiCX.Mater.Lett.2012,66,222-224 (carbonization at low temperature of Watermelon rind); ; LuWB, QinXY, LiuS, ChangGH, ZhangYW, LuoYL, AsiriAM, Al-YoubiAO, SunXP.Anal.Chem.2012,84,5351-5357 (hydrothermal treatment consists of orange peel); MehtaV.N., JhaS., BasuH., SinghalR.K., KailasaS.K., SensorsandActuatorsB:Chemical2015,213,434-443 (preparation of Sucus Mali pumilae hydro-thermal).
Through retrieval, publication number is the Chinese invention patent of CN103911151A, disclose " nitrogen co-doped carbon point of the sulphur phosphorus that a kind of fluorescence property is adjustable and preparation method thereof ", comprise the following steps: the nitrogen co-doped carbon point of the sulphur phosphorus that a kind of fluorescence property is adjustable, be that precursor utilizes hydrothermal method one step to be prepared from Sucus Cucumidis sativi, its particle size range is 2 ~ 8nm, this sulphur phosphorus nitrogen co-doped carbon point is the unformed fluorescent carbon point that median size is respectively 5.6,3.5 and 2.7nm, and the wavelength of corresponding fluorescence spectrum is respectively 450,505 and 571nm.The invention also discloses the preparation method of the nitrogen co-doped carbon point of the adjustable sulphur phosphorus of this fluorescence property.Preparation method of the present invention, without the need to adding any chemical reagent, only using Sucus Cucumidis sativi as unique raw material, reacts and carries out in hydrothermal reaction kettle, environmental protection, has the convenient, fast and advantage of favorable reproducibility.
Through retrieval, publication number is the Chinese invention patent of CN104560035A, discloses " a kind of take peel of Citrus reticulata Blanco as carbon quantum dot fluorescence labeling material of carbon source and its preparation method and application " and it is characterized in that comprising the following steps: by peel of Citrus reticulata Blanco and water mix and blend; Again by mixed solution and vitriol oil mix and blend; PH is regulated again, the undissolved residue of centrifugal segregation with NaOH; Again methylene dichloride is added centrifugal after supernatant liquor, the non-blooming lipid-soluble substance of centrifugal segregation; Finally the supernatant liquor after centrifugal is crossed film, obtained fluorescence labeling material.Present method is in building-up process, high temperature, reaction under high pressure is carried out without the need to equipments such as plasma emitters, hydrothermal reaction kettle or retort furnaces, reaction conditions is gentle, easy and simple to handle, cost is very low, common laboratory all can be carried out, and the fluorescence labeling material of synthesis is applied to the work such as biomarker, Analysis of Heavy Metal, antibody labeling, cell dyeing and lays a good foundation for next step.
Through retrieval, publication number is the Chinese invention patent of CN104560035A, disclose " a kind of preparation method of environment-friendlyeconomic economic luminescent carbon quantum dot " to it is characterized in that comprising the following steps: take bagasse as carbon source material, join in the mineralizer aqueous solution, utilize hydrothermal synthesis reaction still, 180 DEG C of heating 4h in retort furnace; After brownish black reaction solution high speed centrifugation, collect supernatant liquor and dialyse; Collect reaction solution in dialysis tubing freezing after proceed to freeze-drying in freeze drier, finally obtain powder formed carbon quantum dot.Preparation method of the present invention has simple to operate, convenient and swift, the feature of preparation technology's device simple; And be raw material with general wastes, with low cost, environmental protection is easy to promote.Carbon quantum dot prepared by the present invention has good dispersiveness, water-soluble, the excellent specific property such as fluorescent stability and biocompatibility, and is successfully applied to viable cell imaging and mark.
Through retrieval, publication number is the Chinese invention patent of CN104495784A, disclose " extract residue with Rhizome of Peltate Yam and prepare the method for carbon quantum dot " to it is characterized in that comprising the following steps: (1) accurately takes 0.5g, Rhizome of Peltate Yam at 105 DEG C after dry 2h extracts residue, add 40mL intermediate water again, heated and stirred dispersion 20min in 100 DEG C of boiling water baths; (2) 0.007gAgNO is taken
3in the beaker of shading, use 1mL water dissolution; (3) get 100 μ L Thiovanic acids and TGA, 50 μ L ammoniacal liquor and 0.01g thioacetamide, stir and make it fully mix; (4) step (1), step (2) and step (3) gained solution are poured in the liner of stainless steel hydrothermal reaction kettle of 50mL, in 180 ~ 220 DEG C of temperature ranges, the near-infrared luminous carbon quantum dot of different wave length under the differential responses time, can be obtained.
Summary of the invention
Because the defect of prior art, technical problem to be solved by this invention avoids using valuable instrument, provides a kind of Hydrothermal Synthesis technology to obtain the method for carbon quantum dot.
For achieving the above object, invention provides a kind of method based on fruit Hydrothermal Synthesis carbon quantum dot, by fruit washes clean, to cut into pieces or squeeze out juice, first in agitator, process for some time, then be placed in hydrothermal reaction kettle, 100 ~ 250 DEG C of Water Under thermal response 4 ~ 72h, more centrifugal and dialysis treatment obtains carbon quantum dot.Detailed technology scheme is as follows:
Based on a method for fruit Hydrothermal Synthesis carbon quantum dot, comprise the following steps:
Step 1, by fruit washes clean, juice of cutting into pieces or squeeze out; Small pieces or juice is stir process in agitator first, is then placed in hydrothermal reaction kettle and carries out hydro-thermal reaction;
Step 2, after hydro-thermal reaction completes, carries out centrifugal and dialysis treatment to reaction product and obtains carbon quantum dot.
Further, fruit is strawberry, pineapple, mango, apricot, plum, watermelon, pawpaw, hami melon, mangosteen, cherry, banana, Hylocereus undatus, apple, bergamot pear, hawthorn, orange, longan, grape, lichee, ponkan, durian, navel orange, pomegranate, Chinese olive, gingko, rambutan, kumquat, honey peach, satsuma orange, betel nut, muskmelon, mulberries, persimmon, carambola, loquat, cherry tomato, kiwi fruit, Kiwifruit, shaddock, longan, sugarcane, dark plum, passion fruit, lemon, piscidia, orange, coconut, sweet angle, Fructus Citri Sarcodactylis, Pon mandarin orange, orange, olive, red date, Kiwifruit, Fructus Fici, cranderry, blackberry, blueberry, raspberry, the red vinegar certain kind of berries, Liu Ding, natsudaidai, lime, a kind of or mutual mixing in pomelo several arbitrarily.
Further, in step 1, in agitator, the time of stir process is 5 ~ 60min.
Further, the fruit quality after stir process is 50mg ~ 1kg.
Further, hydrothermal reaction kettle volume is 5mL ~ 5L.The temperature of hydro-thermal reaction is 100 ~ 250 DEG C.The time of hydro-thermal reaction is 4 ~ 72h, timing from temperature is raised to temperature of reaction.
Further, centrifugal speed is 3000 ~ 15000rpm.The centrifugal time is 10 ~ 200min.
Further, the dialysis tubing of dialysis employing 100 ~ 3500Da, is put in dialysis treatment in the beaker of 100mL ~ 25L.
The present invention has following beneficial effect: hydrothermal method synthesis carbon quantum dot, can synthesize the carbon quantum dot that size of particles is homogeneous, controllability is good.Raw material sources are extensive, green friendly.
Below will be described further specific embodiment of the invention details, to understand object of the present invention, characteristic sum effect fully.
Accompanying drawing explanation
The fluorescence spectrum figure of Fig. 1 cherry tomato;
The fluorescence spectrum figure of Fig. 2 strawberry;
The fluorescence spectrum figure of Fig. 3 Banana peel and pulp.
Embodiment
Elaborate to embodiments of the invention below, the present embodiment is implemented under premised on technical solution of the present invention, give detailed embodiment and concrete operating process, but protection scope of the present invention is not limited to following embodiment.
Embodiment 1
Step 1, by 50mg Hylocereus undatus washes clean, cuts into pieces, first in agitator, stirs 30min, is then placed in 50mL hydrothermal reaction kettle, 180 DEG C of hydro-thermal reaction 24h;
Step 2, more centrifugal 60min and the 1000Da dialysis treatment of 5000rpm obtains carbon quantum dot.
Embodiment 2
Step 1, by 50mg mango washes clean, cuts into pieces, first in agitator, stirs 30min, is then placed in 50mL hydrothermal reaction kettle, 180 DEG C of hydro-thermal reaction 24h;
Step 2, more centrifugal 60min and the 1000Da dialysis treatment of 5000rpm obtains carbon quantum dot.
Embodiment 3
Step 1, by 1g mango washes clean, cuts into pieces, first in agitator, stirs 30min, is then placed in 100mL hydrothermal reaction kettle, 200 DEG C of hydro-thermal reaction 48h;
Step 2, more centrifugal 100min and the 3500Da dialysis treatment of 10000rpm obtains carbon quantum dot.
Embodiment 4
Step 1, by 500g muskmelon washes clean, cuts into pieces, first in agitator, stirs 45min, is then placed in 5L hydrothermal reaction kettle, 250 DEG C of hydro-thermal reaction 72h;
Step 2, more centrifugal 120min and the 2000Da dialysis treatment of 12000rpm obtains carbon quantum dot.
Except above fruit, can also according to the method in above-described embodiment, use the various fruit such as cherry tomato, strawberry, banana to prepare carbon quantum dot as raw material, Fig. 1 to Fig. 3 is respective fluorescence spectrum figure.
More than describe preferred embodiment of the present invention in detail.Should be appreciated that those of ordinary skill in the art just design according to the present invention can make many modifications and variations without the need to creative work.Therefore, all technician in the art, all should by the determined protection domain of claims under this invention's idea on the basis of existing technology by the available technical scheme of logical analysis, reasoning, or a limited experiment.
Claims (10)
1. based on a method for fruit Hydrothermal Synthesis carbon quantum dot, it is characterized in that, comprise the following steps:
Step 1, by fruit washes clean, juice of cutting into pieces or squeeze out; Described small pieces or described juice is stir process in agitator first, is then placed in hydrothermal reaction kettle and carries out hydro-thermal reaction;
Step 2, after described hydro-thermal reaction completes, carries out centrifugal and dialysis treatment to reaction product and obtains carbon quantum dot.
2. according to the method based on fruit Hydrothermal Synthesis carbon quantum dot a kind of described in claim 1, it is characterized in that, described fruit is strawberry, pineapple, mango, apricot, plum, watermelon, pawpaw, hami melon, mangosteen, cherry, banana, Hylocereus undatus, apple, bergamot pear, hawthorn, orange, longan, grape, lichee, ponkan, durian, navel orange, pomegranate, Chinese olive, gingko, rambutan, kumquat, honey peach, satsuma orange, betel nut, muskmelon, mulberries, persimmon, carambola, loquat, cherry tomato, kiwi fruit, Kiwifruit, shaddock, longan, sugarcane, dark plum, passion fruit, lemon, piscidia, orange, coconut, sweet angle, Fructus Citri Sarcodactylis, Pon mandarin orange, orange, olive, red date, Kiwifruit, Fructus Fici, cranderry, blackberry, blueberry, raspberry, the red vinegar certain kind of berries, Liu Ding, natsudaidai, lime, a kind of or mutual mixing in pomelo several arbitrarily.
3. according to the method based on fruit Hydrothermal Synthesis carbon quantum dot a kind of described in claim 1, it is characterized in that, in step 1, in agitator, the time of stir process is 5 ~ 60min.
4. according to the method based on fruit Hydrothermal Synthesis carbon quantum dot a kind of described in claim 1, it is characterized in that, the fruit quality after described stir process is 50mg ~ 1kg.
5. according to the method based on fruit Hydrothermal Synthesis carbon quantum dot a kind of described in claim 1, it is characterized in that, described hydrothermal reaction kettle volume is 5mL ~ 5L.
6. according to the method based on fruit Hydrothermal Synthesis carbon quantum dot a kind of described in claim 1, it is characterized in that, the temperature of described hydro-thermal reaction is 100 ~ 250 DEG C.
7. according to the method based on fruit Hydrothermal Synthesis carbon quantum dot a kind of described in claim 1, it is characterized in that, the time of described hydro-thermal reaction is 4 ~ 72h, timing from temperature is raised to temperature of reaction.
8. according to the method based on fruit Hydrothermal Synthesis carbon quantum dot a kind of described in claim 1, it is characterized in that, described centrifugal speed is 3000 ~ 15000rpm.
9. according to the method based on fruit Hydrothermal Synthesis carbon quantum dot a kind of described in claim 1, it is characterized in that, the described centrifugal time is 10 ~ 200min.
10. according to the method based on fruit Hydrothermal Synthesis carbon quantum dot a kind of described in claim 1, it is characterized in that, the dialysis tubing of described dialysis employing 100 ~ 3500Da, is put in dialysis treatment in the beaker of 100mL ~ 25L.
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Cited By (27)
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|---|---|---|---|---|
| CN105602559A (en) * | 2016-03-09 | 2016-05-25 | 河南师范大学 | Method for one-step synthesis of fluorescent carbon quantum dots by taking pomegranate seeds as carbon source |
| CN105802622A (en) * | 2016-04-15 | 2016-07-27 | 哈尔滨工业大学 | Method for directionally converting carrot biomass into amphoteric fluorescence carbon spots |
| CN106596874A (en) * | 2017-01-20 | 2017-04-26 | 中国海洋大学 | Carbon quantum dots in starch-based food and detection method and application of carbon quantum dots |
| CN106629663A (en) * | 2016-12-26 | 2017-05-10 | 齐齐哈尔大学 | Preparation method of garcinia mangostana-based carbon nanodot and application of carbon nanodot to detecting ferric ions as fluorescent probe |
| CN106629664A (en) * | 2016-12-27 | 2017-05-10 | 江南大学 | Method for synthesizing carbon quantum dots from water chestnuts and application of carbon quantum dots |
| CN106744810A (en) * | 2016-12-05 | 2017-05-31 | 广西师范学院 | The preparation method of the Water-soluble carbon quantum dot with banana skin as raw material |
| CN107311143A (en) * | 2016-04-18 | 2017-11-03 | 青岛大学 | A kind of method that utilization Enteromorpha prepares carbon quantum dot |
| CN107555416A (en) * | 2017-08-07 | 2018-01-09 | 河南师范大学 | The method of hydro-thermal method synthetic nitrogen doping fluorescent carbon point |
| CN107555417A (en) * | 2017-08-29 | 2018-01-09 | 湖南农业大学 | Commercialization beverage prepares the method for fluorescent carbon point and its fluorescent carbon point of preparation |
| CN107986257A (en) * | 2017-12-19 | 2018-05-04 | 重庆文理学院 | A kind of method for preparing nitrogen and sulphur codope carbon quantum dot |
| CN108084999A (en) * | 2018-01-29 | 2018-05-29 | 兴义民族师范学院 | A kind of plant source environmental protection fluorescent carbon quantum dot, its preparation method and application |
| CN109111918A (en) * | 2018-09-19 | 2019-01-01 | 中国日用化学研究院有限公司 | An a kind of one step preparation method of nitrogen-doped carbon quantum dot |
| CN110376174A (en) * | 2019-08-02 | 2019-10-25 | 河南师范大学 | Fluorescent carbon point selective enumeration method CrO is synthesized by carbon source of hawthorn42-Method |
| CN110452693A (en) * | 2019-08-12 | 2019-11-15 | 长沙学院 | A kind of green fluorescent carbon dots and preparation method thereof, fluorescent detection probe and its construction method and application |
| CN110451483A (en) * | 2019-09-02 | 2019-11-15 | 中国农业科学院郑州果树研究所 | It is a kind of using Kiwi berry as the preparation method of Material synthesis fluorescent carbon quantum dot |
| CN110624011A (en) * | 2018-06-22 | 2019-12-31 | 北京中医药大学 | Preparation and application of coke hawthorn carbon quantum dots (nano particles/nano particles) |
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