CN104261386A - Method for preparing carbon dots with hydrothermal process on basis of plant leaves - Google Patents
Method for preparing carbon dots with hydrothermal process on basis of plant leaves Download PDFInfo
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- CN104261386A CN104261386A CN201410542310.6A CN201410542310A CN104261386A CN 104261386 A CN104261386 A CN 104261386A CN 201410542310 A CN201410542310 A CN 201410542310A CN 104261386 A CN104261386 A CN 104261386A
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Abstract
The invention discloses a method for preparing carbon dots with a hydrothermal process on the basis of plant leaves. The plant leaves are transferred into a reaction kettle, ultrapure water is added, and the mixture is uniformly mixed and subjected to hydrothermal treatment at the temperature of 130 DEG C-250 DEG C for 2-15 hours; the mixture is cooled and filtered to obtain a brown yellow liquid, the brown yellow liquid is subjected to dialysis for 15-48 hours by a dialysis bag with interception of 3,500, and dialysate is collected; or high-speed centrifugation is performed, and fluorescent carbon dots are obtained. The method is simple and safe to operate, environment-friendly raw materials are used, chemical reagents and surface passivation are not required for assisting synthesis, and the method can be applied to the fields of fluorescence labeling, analysis, sensing, catalyzing and the like.
Description
Technical field
The invention belongs to technical field of nano material, relate to a kind of method preparing carbon point based on plant leaf hydrothermal method, is especially that carbon source one step hydro thermal method prepares carbon point with plant leaf.
Background technology
Carbon point (also referred to as carbon quantum dot) i.e. particle diameter is less than the carbon particles of 10nm, it is a kind of novel carbon material, namely study hotspot is become once discovery, because carbon point has good optical property, fluorescence intensity is high, good light stability, the advantages such as resistance to photobleaching, and good biocompatibility, toxicity are low, are excellent electron acceptor(EA) and electron donor, have broad application prospects in fields such as bio-imaging, analyzing and testing, sensing, photoelectricity.
The method for the preparation of carbon point of current report is a lot.Two large classes can be divided into substantially: top-to-bottom method and bottom-to-top method.Top-to-bottom method, normally etches carbon point from larger carbon structure material, comprises arc discharge method, laser ablation and electrochemical oxidation process etc., and this type of methods experiment conditional request is high and need specific apparatus; Bottom-to-top method, carbon point is synthesized by molecular precursor, comprise wet oxidation method, high temperature pyrolytic cracking (HTP), hydrothermal method, Microwave-assisted synthesis method, ultrasonic and supported synthesis etc., but mostly these class methods are to use chemical reagent to environment, or the subsequent disposal such as finishing, operation more complicated, limits its scale operation and application, therefore finds the carbon source of cheap and easy to get, Nantural non-toxic, simple directly preparation method is problem demanding prompt solution.
Hydrothermal method is simple, high-level efficiency, is most widely used.Huang etc. are that carbon source has synthesized carbon point and the Hg set up based on strawberry juice
2+detection method; After orange peel is dried desolventing technology by Adhimoorthy etc., hydrothermal method obtains fluorescent carbon point, although employ green carbon source, to there is cost high, or process complexity, is not suitable for widespread use.
Summary of the invention
The object of the present invention is to provide a kind of environmental protection, easy and simple to handle, one step hydro thermal method with low cost prepares the method for carbon point, does not need to use any chemical reagent, assists synthesis, prepare simple without the need to pre-treatment, passivation.
For achieving the above object, the invention provides following technical scheme:
A kind of method preparing carbon point based on plant leaf hydrothermal method of the present invention, is characterized in that, comprise the following steps:
1) dry clean for plant leaf;
2) take plant leaf and be transferred in reactor, adding ultrapure water and mix;
3) reactor is positioned in baking oven, under temperature 130-250 DEG C of condition, hydro-thermal reaction 2-15 hour;
4) after being cooled to room temperature, filtering, obtain brown color liquid, be 3500 dialysis tubing dialysis 15-48 hour by brown color liquid molecular weight cut-off, collect dialyzate; Or under more than 10krpm rotating speed, high speed centrifugation 20-40min, obtains fluorescent carbon point.
Step 1) described in plant leaf carbon source be peppermint blade, broad-leaved epiphyllum branch, aloe leaf, Japanese Honeysuckle blade, Japan's blade etc.
Step 1) described in plant leaf carbon source be cured leaf sheet or fresh blade.
Step 3) described in temperature of reaction preferably more than 150 DEG C, reaction times preferred more than 4h.
Step 4) described in dialysis time, preferably collect the later dialyzate of 24h.
The invention has the advantages that:
The present invention uses plant leaf for carbon source, and materials safety is easy to get, and cost is low, is prepared by one step hydro thermal method carbonization, simple to operate, mild condition, and process control is reproducible, is easy to promote the use of.
Carbon point photoluminescent property prepared by the present invention is stablized, and fast light whitening capacity is strong, and good dispersity, has good water-soluble and higher quantum yield, go for the fields such as fluorescent mark, analysis, sensing, catalysis.
Accompanying drawing explanation
Fig. 1: high-resolution-ration transmission electric-lens (HRTEM) figure (corresponding embodiment 1 product) of carbon point.
Fig. 2: the uv absorption spectra of carbon point, embedded figure are the photo of carbon point solution under natural light and ultra violet lamp (corresponding embodiment 1 product).
Fig. 3: the best excitation-emission spectrogram (corresponding embodiment 1 product) of carbon point.
Fig. 4: the fluorescence spectrum figure of carbon point under different excitation wavelength (corresponding embodiment 1 product).
Fig. 5: carbon point in different ionic strength solution change in fluorescence figure (corresponding embodiment 1 product).
Fig. 6: the fluorescence times scintigram (corresponding embodiment 1 product) of carbon point.
Embodiment
With reference to the accompanying drawings and the present invention is described in further detail in conjunction with the embodiments.But the invention is not restricted to given example.
Embodiment 1
Take the fresh broad-leaved epiphyllum branch 2.58g cleaning and dry, shred, be transferred in 25mL reactor, the 10mL that adds water mixes, hydro-thermal reaction 8.5 hours at 180 DEG C.After being cooled to room temperature, filtering, obtain brown color liquid and under 10krpm rotating speed after centrifugal 25min, get supernatant liquor and get final product.
Embodiment 2
Take the dried peppermint blade 0.38g cleaning and dry, grind, be transferred in 25mL reactor, the 15mL that adds water mixes, and hydro-thermal reaction 9 hours at 180 DEG C, after being cooled to room temperature, filter and under 4000 turns after centrifugal 15min, obtain brown color liquid, get the dialysis tubing dialysis 24h that supernatant liquor molecular weight cut-off is 3500, collect dialyzate and get final product.
In addition to the implementation, the present invention can have other embodiments in addition.All employings are equal to the technical scheme of replacement or equivalent transformation formation, all drop on the protection domain of application claims.
Claims (6)
1. prepare a method for carbon point based on plant leaf hydrothermal method, it is characterized in that, concrete steps are:
1) dry clean for plant leaf;
2) take plant leaf and be transferred in reactor, adding ultrapure water and mix;
2) reactor is positioned in baking oven, under temperature 130-250 DEG C of condition, hydro-thermal reaction 2-15 hour;
4) after being cooled to room temperature, filtering, obtain brown color liquid, be 3500 dialysis tubing dialysis 15-48 hour by brown color liquid molecular weight cut-off, collect dialyzate; Or under more than 10krpm rotating speed, high speed centrifugation 20-30min, obtains fluorescent carbon point.
2. a kind of method preparing carbon point based on plant leaf hydrothermal method according to claim 1, is characterized in that: in described preparation method, plant leaf is carbon source, adopts hydrothermal method preparation.
3. a kind of method preparing carbon point based on plant leaf hydrothermal method according to claim 1, is characterized in that: step 1) described in plant leaf be peppermint blade, broad-leaved epiphyllum branch, aloe leaf, Japanese Honeysuckle blade, Japan's blade etc.
4. a kind of method preparing carbon point based on plant leaf hydrothermal method according to claim 3, is characterized in that: described plant leaf is cured leaf sheet or fresh blade.
5. a kind of method preparing carbon point based on plant leaf hydrothermal method according to claim 1, is characterized in that: step 3) described in temperature of reaction preferably more than 150 DEG C, reaction times preferred more than 4h.
6. a kind of method preparing carbon point based on plant leaf hydrothermal method according to claim 1, is characterized in that: step 4) described in dialysis time, preferably collect the later dialyzate of 24h.
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| CN104927847A (en) * | 2015-05-25 | 2015-09-23 | 浙江师范大学 | Preparation method for carbon quantum dot material for detecting Cu<2+> |
| CN105001862A (en) * | 2015-07-30 | 2015-10-28 | 西华师范大学 | Preparation of carbon quantum dots by use of aloe as carbon source and detection method of lemon yellow |
| CN105060273A (en) * | 2015-08-09 | 2015-11-18 | 安徽大学 | Super hydrophilic carbon quantum dot for promoting catalytic polymerization, preparation method therefor and application thereof |
| CN105295910A (en) * | 2015-11-27 | 2016-02-03 | 中国科学院山西煤炭化学研究所 | Method for preparing red light carbon dots by taking biomass as precursor |
| CN105542759A (en) * | 2015-12-28 | 2016-05-04 | 江南大学 | Method for preparing fluorescence carbon dots based on sweet potato extract |
| CN105542761A (en) * | 2015-12-28 | 2016-05-04 | 江南大学 | Method for preparing fluorescence carbon dots taking rice bran as carbon source |
| CN105905884A (en) * | 2016-04-23 | 2016-08-31 | 哈尔滨师范大学 | Preparation method and application of fluorescence carbon quantum dots |
| CN106629659A (en) * | 2016-12-09 | 2017-05-10 | 中国石油大学(华东) | Preparation method of fluorescent carbon quantum dots employing algae as carbon sources and application |
| CN106753354A (en) * | 2016-12-05 | 2017-05-31 | 广西师范学院 | The preparation method of the Water-soluble carbon quantum dot with sisal hemp as raw material |
| CN106829920A (en) * | 2017-01-18 | 2017-06-13 | 上海应用技术大学 | A kind of green fluorescence carbon quantum dot material and preparation method thereof |
| CN106967425A (en) * | 2016-11-23 | 2017-07-21 | 云南省烟草公司文山州公司 | Using cigarette stalk as the preparation method and application of the fluorescent carbon quantum dot of raw material |
| CN107311145A (en) * | 2017-08-29 | 2017-11-03 | 湖南农业大学 | A kind of fluorescent carbon point for the method and its preparation that fluorescent carbon point is prepared by raw material of silkworm excrement |
| CN107651665A (en) * | 2017-10-27 | 2018-02-02 | 西安理工大学 | A kind of method that water-solubility fluorescent carbon quantum dot is prepared with dried peppermint leaf |
| CN108084998A (en) * | 2018-01-29 | 2018-05-29 | 兴义民族师范学院 | It is a kind of using white orchid blade as fluorescent carbon quantum dot of carbon source and preparation method thereof |
| CN108083257A (en) * | 2017-12-28 | 2018-05-29 | 湖南科技大学 | A kind of method that fluorescent carbon point is prepared using chloroplaset as carbon source |
| CN108584916A (en) * | 2018-06-05 | 2018-09-28 | 桂林理工大学 | The method for preparing the luminous water-solubility fluorescent carbon quantum dot of visible region with sisal fiber |
| CN108872171A (en) * | 2018-06-19 | 2018-11-23 | 江苏大学 | A kind of application of fluorescent carbon point and preparation method thereof and detection tetracycline |
| CN109588375A (en) * | 2018-11-02 | 2019-04-09 | 大连工业大学 | Fluorescent natural silk preparation method based on Spanish mackerel internal organ and the compound carbon dots of mulberry leaf |
| CN109734073A (en) * | 2018-12-13 | 2019-05-10 | 南京师范大学 | It is a kind of using wormwood leaf as carbon quantum dot of carbon source and the preparation method and application thereof |
| CN109880620A (en) * | 2019-03-02 | 2019-06-14 | 福建医科大学 | It is a kind of using biomass as the preparation and application of the green fluorescence carbon quantum dot of presoma |
| CN109941988A (en) * | 2019-04-24 | 2019-06-28 | 铜仁学院 | A kind of preparation method and application of graphene quantum dot and device or device comprising it |
| CN110104629A (en) * | 2019-05-20 | 2019-08-09 | 河南师范大学 | The method for synthesizing fluorescent carbon point as raw material one step hydro thermal method using wild gleditsia sinensis |
| CN110308126A (en) * | 2019-08-02 | 2019-10-08 | 河南师范大学 | A method of using chinaberry hinge at fluorescence nano carbon dots cell imaging |
| CN110358536A (en) * | 2019-08-02 | 2019-10-22 | 河南师范大学 | Fluorescent carbon point, which is synthesized, as carbon source using southern magnolia detects Cr2O72-Method |
| CN110373185A (en) * | 2019-08-02 | 2019-10-25 | 河南师范大学 | Fluorescent carbon point selective enumeration method Bi is synthesized by carbon source of feed with paper-mulberry leaf3+Method |
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| CN113148978A (en) * | 2020-12-30 | 2021-07-23 | 宁德师范学院 | Method for synthesizing carbon dots by hydrothermal method by taking tea powder as raw material |
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| CN114854402A (en) * | 2022-03-22 | 2022-08-05 | 桂林师范高等专科学校 | Preparation method of fluorescent nano material capable of promoting growth of cherokee rose group culture seedling |
| CN114956049A (en) * | 2022-06-17 | 2022-08-30 | 山西大学 | Long wavelength ratio fluorescent carbon dot and preparation method and application thereof |
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