CN109486485A - A method of fluorescent carbon quantum dot is prepared using short chain volatile fatty acid as carbon-based material - Google Patents

A method of fluorescent carbon quantum dot is prepared using short chain volatile fatty acid as carbon-based material Download PDF

Info

Publication number
CN109486485A
CN109486485A CN201811431532.5A CN201811431532A CN109486485A CN 109486485 A CN109486485 A CN 109486485A CN 201811431532 A CN201811431532 A CN 201811431532A CN 109486485 A CN109486485 A CN 109486485A
Authority
CN
China
Prior art keywords
quantum dot
carbon
fatty acid
short chain
volatile fatty
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
CN201811431532.5A
Other languages
Chinese (zh)
Inventor
王进
岳正波
彭书传
周岳陵
胡馥鹏
段立明
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Hefei University of Technology
Original Assignee
Hefei University of Technology
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Hefei University of Technology filed Critical Hefei University of Technology
Priority to CN201811431532.5A priority Critical patent/CN109486485A/en
Publication of CN109486485A publication Critical patent/CN109486485A/en
Pending legal-status Critical Current

Links

Classifications

    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09KMATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
    • C09K11/00Luminescent, e.g. electroluminescent, chemiluminescent materials
    • C09K11/08Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials
    • C09K11/65Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing carbon
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B82NANOTECHNOLOGY
    • B82YSPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y20/00Nanooptics, e.g. quantum optics or photonic crystals
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B82NANOTECHNOLOGY
    • B82YSPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y40/00Manufacture or treatment of nanostructures

Landscapes

  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Nanotechnology (AREA)
  • Physics & Mathematics (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Optics & Photonics (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Biophysics (AREA)
  • Organic Chemistry (AREA)
  • Materials Engineering (AREA)
  • Inorganic Chemistry (AREA)
  • Condensed Matter Physics & Semiconductors (AREA)
  • General Physics & Mathematics (AREA)
  • Manufacturing & Machinery (AREA)
  • Luminescent Compositions (AREA)
  • Carbon And Carbon Compounds (AREA)

Abstract

The invention discloses a kind of methods for preparing fluorescent carbon quantum dot as carbon-based material using short chain volatile fatty acid, it is using short chain volatile fatty acid as carbon-based material, liquid nitrogen source and ultrapure water and after mixing evenly is added, carries out hydro-thermal reaction, that is, obtains target product fluorescent carbon quantum dot.Method of the invention, raw material sources are extensive and cheap, easy to operate, and preparation condition requirement is low and relatively mild, solve the problems, such as that existing fluorescent carbon quantum dot preparation method can not large-scale production because of raw material and technique limitation.

Description

It is a kind of to prepare fluorescent carbon quantum dot using short chain volatile fatty acid as carbon-based material Method
Technical field
The present invention relates to a kind of method for preparing fluorescent carbon quantum dot as carbon-based material using short chain fatty acids, belonging to Learn technical field of nano material.
Background technique
Fluorescent carbon quantum dot has as a kind of novel carbon nanomaterial and prepares simple, good light stability, bio-compatible The advantages that property good, excitation-emission wavelength dependence, environmental monitoring, the removal of heavy metal, bio-imaging, in terms of It has a wide range of applications.
Mainly there are several types of (1) arc discharge methods at present for the preparation method of fluorescent carbon quantum dot.Pass through arc discharge method The carbon light quantum amount of preparation has larger oxygen content, is not necessarily to surface modification.Its purification process is complicated, and yield is lower, collects and produces Object is relatively difficult.Such as Xu[1]Carbon nano-particle is prepared for carbon ash using arc discharge method, wherein the yield of fluorescent quantum Have 1.6%.(2) laser ablation method.The carbon quantum dot of fluorescence is prepared with using laser ablation method, instrument is expensive, and Need to add organic solvent to modify the surface state of carbon quantum dot.(3) electrochemical process.Electrochemical process is prepare carbon quantum dot normal With method, researcher makes the anodic oxidation of electrolyte, then from using carbon as the work of material by the value of change potential or electric current Make to obtain small carbon nano-particle on electrode, suspension is then obtained by centrifugation.The fluorescence nano obtained by this method Grain has more tiny partial size, but during the preparation process, due to oxidation, increases the defect of carbon nano tube surface.(4) Ultrasonic treatment.Using Ultrasonic treatment, the requirement to equipment is relatively low, carbon easy to operate and cheap, but obtaining The performance of quanta point material is not sufficiently stable.(5) organic carbon method.Organic carbon method uses the side of organic matter precursor carbonization Method prepares carbon quantum dot, can not only launch fluorescence, oil-soluble or water-soluble carbon quantum dot can also be made surface-functionalized. Organic carbon method has the shortcomings that very much, not only has unstable fluorescence quantum yield, there are also very in the carbon quantum dot of generation More oxygen usually will also be passivated operation.(6) template.General template all selects mesoporous silicon oxide (MS) ball, it has The advantage that specific surface area is high, gap is uniform, plot ratio is high.But template preparation is difficult to separate carbon quantum dot with support, Narrow distribution simultaneously, it is necessary to could be dispersed in water with ultrasonic treatment.(7) microwave method.Microwave (frequency be 300MHz~ 300GHz) technology is that a kind of energy is concentrated, reacts fast, high-efficient and uniform technology of preparing, in the field of chemical synthesis using non- Chang Duo.Wang etc.[2]Using eggshell membrane (ESM) ashes as carbon source, by microwave technology, it is prepared for partial size about 5nm and can emits The carbon quantum dot of blue-fluorescence.(8) hydro-thermal method.Hydro-thermal method is to use water as solvent in high temperature and pressure, is with reaction kettle Vessel, the method for synthesizing carbon nano-particle.The advantages of hydro-thermal method is that control is simple, process is easy, and simultaneous reactions kettle can be effective Reduce the volatilization of organic matter.In addition to this, carbon quantum dot made from different solvents has different property.(9) combustion method.Combustion The advantages of burning method is that equipment is simple, operating process is easy, and repeats operation, the disadvantage is that being difficult to control particle diameter distribution.Yuan Deng[3]Carbon nano-particle is prepared for ethanol combustion device.
The carbon-based material for preparing raw material currently as fluorescent carbon quantum dot is varied.Patent publication No. is The patent of invention of CN101973541A provides a kind of method that fluorescent carbon quantum dot is extracted in active carbon, is made using active powdered carbon For carbon source, by chemical oxidation of gold and subsequent evaporation, neutralizes, centrifugation, hyperfiltration treatment, a large amount of fluorescence carbon amounts can be obtained Sub- point.Patent publication No. is related to a kind of compound micro- based on magnetic carbon quantum dot/chitosan for the patent of invention of CN102973948B The preparation method of the pharmaceutical carrier of ball is to pass through the microwave radiation system of reacting using glucose with polyethylene glycol mixed liquor as carbon-based material Standby fluorescent carbon quantum dot, then magnetic carbon quantum dot composite particles are formed by electrostatic adsorption.Patent publication No. is The patent of invention of CN103771390B discloses one kind using citric acid, citrate, glucose, fructose or amylose as carbon Precursor passes through the method for bioactive enzyme assisted microwave synthesis method synthesizing super-strong fluorescent carbon quantum dot.Patent publication No. is The patent of invention of CN104031642B provides a kind of fluorescent carbon quantum dot and preparation method thereof of high quantum production rate, is with shell Glycan is carbon source, and glacial acetic acid and ethylenediamine is added as passivator.The patent of invention that patent publication No. is CN104087296B is public A kind of method that laser irradiation prepares fluorescent carbon quantum dot has been opened, has been with one of benzene, substituted benzene or more benzene ring compounds For carbon source.Patent publication No. is that the patent of invention of CN104629760B and CN104927847B is utilized respectively Jinhua Fingered Citron and black wood Ear prepares fluorescent carbon quantum dot as carbon source, by hydrothermal synthesis method.Patent publication No. is the patent of invention of CN104759283A It discloses a kind of based on copper complex formazan fluorescent carbon quantum dot and preparation method thereof.Patent publication No. is the hair of CN105067576A Bright patent provides a kind of method for preparing fluorescent carbon quantum dot based on electrochemical techniques.Patent publication No. is CN105694879B Patent of invention provide a kind of organic wastewater and prepare fluorescent carbon quantum dot and its coagulation recovery method, be to be with organic wastewater Carbon source prepares fluorescent carbon quantum dot using micro-wave oven as reaction platform, recycles quanta point material using coagulation technology.Patent is public The number of opening provides a kind of fluorescent carbon quantum dot preparation method of sulfur doping for the patent of invention of CN106829921A, is with half Guang Propylhomoserin hydrochloride is carbon-based material.Patent publication No. provides a kind of fluorescence of N doping for the patent of invention of CN107446578A Carbon quantum dot material preparation method is using pericarp and polyethyleneimine as carbon source and nitrogen source.
In addition to the carbon-based material of foregoing invention patent disclosure, there are also apples for the carbon-based material of existing synthesis fluorescent carbon quantum dot Acid, chloroform, graphite powder, clay, ethyl alcohol, candle cigarette ash, octadecylamine, citric acid, starch, organic wastewater, chitosan, grape Sugar, natural gas ash, pollen, fructose, glutaraldehyde, glycerine, fragrant hydrocarbon compound etc..The part material of above-mentioned carbon-based material is can not The renewable sources of energy or part material is with high costs is unfavorable for continuing and large-scale production fluorescent carbon quantum dot;And organic wastewater etc. by Aftertreatment technology unstable in the fluorescent carbon quantum dot material property of its complexity, synthesis and that needs are stringent.Therefore, one is found The carbon-based material cheap and easy to get, that property is stable of kind helps to reduce the production cost of fluorescent carbon quantum dot material, pushes the green wood Expect the extensive use in multiple fields.
Short chain volatile fatty acid (VFAs) includes formic acid, acetic acid, propionic acid, butyric acid, valeric acid, caproic acid and their isomery Body.VFAs is the intermediate product of anaerobic fermentation of organisms process, and the precursor substance of many chemicals synthesis, cheap and easy to get, Stable components.Therefore, cost is advantageously reduced using VFAs the carbon-based material for preparing fluorescent carbon quantum dot, is realized sustainable Quantization production, improves the stability of fluorescent carbon quantum dot material property.It discloses in the fluorescent carbon quantum dot preparation process of report Glacial acetic acid is used as passivating material, and prepares the technology of fluorescent carbon quantum dot not yet using VFAs solution as carbon-based material See open report.
Bibliography in above-mentioned background technique is as follows:
[1]Xu X,Ray R,Gu Y,et al.Electrophoretic analysis and purification of fluorescent single-walled carbon nanotube fragments.[J].Journal of the American Chemical Society,2004,126(40):12736-7.
[2]Wang Q,Liu X,Zhang L,et al.Microwave-assisted synthesis of carbon nanodots through an eggshell membrane and their fluorescent application[J] .The Analyst,2012,137(22):5392-5397.
[3]Yuan L,Dai J,Fan X,et al.Self-cleaning flexible infrared nanosensor based on carbon nanoparticles[J].Acs Nano,2011,5(5):4007.
Summary of the invention
The present invention in order to avoid in place of above-mentioned the deficiencies in the prior art, provide it is a kind of be simple and efficient prepare fluorescence carbon quantum The method of point material.
The present invention solves technical problem, adopts the following technical scheme that
The invention discloses a kind of sides that fluorescent carbon quantum dot is prepared using short chain volatile fatty acid as carbon-based material Method, it is characterized in that: it is that liquid nitrogen source and ultrapure water is added and stirs evenly using short chain volatile fatty acid as carbon-based material Afterwards, the hydro-thermal reaction 4-10h at 160-220 DEG C, gained reaction solution obtain target after dialysing, then through vacuum freeze drying Product fluorescent carbon quantum dot.Specifically includes the following steps:
(1) short chain volatile fatty acid is placed in the stainless steel autoclave of polytetrafluoroethyllining lining, adds liquid State nitrogen source and ultrapure water, stir, and obtain mixed solution;
(2) reaction kettle equipped with mixed solution is placed in airtight heating device, hydro-thermal reaction 4-10h at 160-220 DEG C;
(3) after reaction, reaction kettle is taken out, natural cooling, it is the saturating of 3500Da that reaction solution, which is poured into molecular cut off, Bag is analysed, every 6h changes a water, dialyses 3 days in glass container, obtain the aqueous solution of fluorescent carbon quantum dot;
(4) vacuum freeze drying is carried out to the aqueous solution of the fluorescent carbon quantum dot to get fluorescent carbon quantum dot powder is arrived.
Further, the short chain volatile fatty acid is formic acid, acetic acid, propionic acid, butyric acid, valeric acid, caproic acid and its isomery At least one of body.
Further, the liquid nitrogen source is the urea liquid that ammonium hydroxide, ethylenediamine or mass concentration are 20%-30%.
Further, the volume ratio of the short chain volatile fatty acid, liquid nitrogen source and ultrapure water is 5-15:0.5-2:3- 14.5。
Further, the airtight heating device is Muffle furnace, tube furnace or electric drying oven with forced convection.
Further, the temperature of the vacuum freeze drying is -80 DEG C.
Compared with the prior art, the beneficial effects of the present invention are embodied in:
(1) method that the present invention prepares fluorescent carbon quantum dot, raw materials used short chain volatile fatty acid (VFAs) and nitrogen source It is general reagent, it is from a wealth of sources, cheap;
(2) method reaction condition of the invention is mild, energy conservation and environmental protection, purifying process are simple, and repeatability is high;
(3) present invention through a step hydro-thermal can volume production fluorescent carbon quantum dot, easy to operate, device therefor is easy to get;
(4) a kind of short chain volatile fatty acid (VFAs) provided by the invention prepares the recycling increment of fluorescent carbon quantum dot Method enriches the raw material store of fluorescent carbon quantum dot preparation;
To sum up, method of the invention, technological operation is simple, raw material sources are extensive and cheap, and preparation condition requires low And it is relatively mild, solve existing fluorescent carbon quantum dot preparation method because technique and raw material limit due to can not large-scale production ask Topic.
Detailed description of the invention
Fig. 1 be the uv-visible absorption spectra (ABS) of fluorescent carbon quantum dot, fluorescence prepared by embodiment 1 excite (EX) and Fluorescence emission spectrum (EM);
Fig. 2 is fluorescence emission spectrum of the fluorescent carbon quantum dot of the preparation of embodiment 1 under 300~400nm excitation wavelength;
Fig. 3 is the infrared spectrogram of fluorescent carbon quantum dot prepared by embodiment 1;
Fig. 4 is the transmission electron microscope (Fig. 4 (a)) and grain size distribution (Fig. 4 (b)) of fluorescent carbon quantum dot prepared by embodiment 1;
Fig. 5 is the XRD spectrum figure of fluorescent carbon quantum dot prepared by embodiment 1.
Specific embodiment
It elaborates below with reference to embodiment to the present invention, following embodiments give detailed embodiment and specific Operating process, but protection scope of the present invention is not limited to following embodiments.
Embodiment 1
The present embodiment prepares fluorescent carbon quantum dot as follows:
(1) 5mL glacial acetic acid is pipetted in ptfe autoclave, and 0.5mL ethylenediamine then is added and 14.5mL is ultrapure Water stirs, and obtains mixed solution;
(2) reaction kettle equipped with mixed solution is placed in electric drying oven with forced convection, 200 DEG C of reaction 5h are obtained faint yellow Solution;
(3) reaction kettle is taken out, yellow solution is transferred to the bag filter that molecular cut off is 3500Da by natural cooling In, every 6h changes a water, dialyses 3 days, obtains the aqueous solution of pure fluorescent carbon quantum dot;
(4) aqueous solution of fluorescent carbon quantum dot is placed in -20 DEG C of refrigerators and freezes 3h, transfer to vacuum freeze drying Machine, vacuum freeze drying 1 day is to get arriving fluorescent carbon quantum dot powder at -80 DEG C.
Fig. 1 is the uv-visible absorption spectra (ABS) of the present embodiment products therefrom, fluorescence excitation (EX) and fluorescent emission Spectrum (EM) shows that the fluorescent carbon quantum dot of synthesis respectively has a typical absorption peak in 270nm and 320nm or so in figure. Absorption peak at 270nm corresponds to n → π * transition of C=O, and apparent absorption peak is then due to surface defect state at 320nm N → π * transition caused by.The best excitation peak position of the fluorescent carbon quantum dot is 380nm, and corresponding best transmitting peak position is 460nm, and the half-peak breadth of emission peak is relatively narrow (75nm).
Fig. 2 is fluorescence emission spectrum of the present embodiment products therefrom under 300~400nm excitation wavelength, it can be seen that Under the excitation of 300~400nm, emission peak is from 450nm slight red shift to 470nm, and fluorescence intensity becomes because of exciting light Change, this illustrates that carbon quantum dot has exciting light dependence fluorescent emission phenomenon.This phenomenon is by surface additive group (C=O/ C-NH2) (surface state) π * → n transition caused by, this is corresponding with absorption peak (n → π * transition) of absorption spectrum.From Fig. 2, I.e. fluorescence emission spectrum is, it can be seen that fluorescent carbon quantum dot is emitted as blue region.
Fig. 3 is the infrared absorption spectrum of the present embodiment products therefrom.Characteristic absorption peak CON-H's is curved as we can see from the figure Qu Zhendong (1560cm-1And 3294cm-1) and amide groups CO-N (1365cm-1) stretching vibration, show in the fluorescent carbon quantum dot On there is amido functional groups.In addition, detecting C=O (1650cm-1)、O-H(1321cm-1)、C-H(2935cm-1)、C-O (1107cm-1) and C-O-C (1043cm-1) corresponding to absorption peak.These groups come volatile fatty acid and nitrogen source.Upper figure Show that amido bond has been formed, this dehydration and condensation reaction between carboxyl and amino is related, illustrates that nitrogen source is a kind of dopant And surface passivator, promote the formation of fluorescent carbon quantum dot.
Fig. 4 is the TEM (Fig. 4 (a)) and grain size distribution (Fig. 4 (b)) of the present embodiment products therefrom.From fluorescent carbon quantum dot TEM figure as can be seen that the fluorescent carbon quantum dot be the preferable black particle of monodispersity;The result table of high-resolution-ration transmission electric-lens Bright most of particles are no crystalline state carbon particle;From the point of view of particle diameter distribution, the partial size of the fluorescent carbon quantum dot is 1.8~4.2nm, is put down Equal partial size is 2.5nm or so.
Fig. 5 is that the XRD of the present embodiment products therefrom is composed, and map shows one 25 ° (0.34nm) Zuo You broad peak, this is As caused by highly disordered carbon atom, illustrate that the fluorescent carbon quantum dot of synthesis is in highly disordered state, this and TEM figure As a result corresponding.
Embodiment 2
(1) 10mL glacial acetic acid is pipetted in ptfe autoclave, and 1mL ethylenediamine and 9mL ultrapure water is then added, fills Divide and stir evenly, obtains mixed solution;
(2) reaction kettle equipped with mixed solution is placed in electric drying oven with forced convection, 200 DEG C of reaction 8h are obtained faint yellow Solution;
(3) reaction kettle is taken out, yellow solution is transferred to the bag filter that molecular cut off is 3500Da by natural cooling In, every 6h changes a water, dialyses 3 days, obtains the aqueous solution of pure fluorescent carbon quantum dot;
(4) aqueous solution of fluorescent carbon quantum dot is placed in -20 DEG C of refrigerators and freezes 3h, transfer to vacuum freeze drying Machine, vacuum freeze drying 1 day is to get arriving fluorescent carbon quantum dot powder at -80 DEG C.Through characterizing, fluorescence carbon amounts obtained by the present embodiment The photoluminescent property of son point is similar to Example 1.
Embodiment 3
(1) 5mL propionic acid is pipetted in ptfe autoclave, and 2mL ammonium hydroxide and 13mL ultrapure water is then added, sufficiently stirs It mixes uniformly, obtains mixed solution;
(2) reaction kettle equipped with mixed solution is placed in electric drying oven with forced convection, 220 DEG C of reaction 8h are obtained faint yellow Solution;
(3) reaction kettle is taken out, yellow solution is transferred to the bag filter that molecular cut off is 3500Da by natural cooling In, every 6h changes a water, dialyses 3 days, obtains the aqueous solution of pure fluorescent carbon quantum dot;
(4) aqueous solution of fluorescent carbon quantum dot is placed in -20 DEG C of refrigerators and freezes 3h, transfer to vacuum freeze drying Machine, vacuum freeze drying 1 day is to get arriving fluorescent carbon quantum dot powder at -80 DEG C.Through characterizing, fluorescence carbon amounts obtained by the present embodiment The photoluminescent property of son point is similar to Example 1.
Embodiment 4
(1) 2mL glacial acetic acid, 3mL propionic acid, 5mL butyric acid are pipetted in ptfe autoclave, 1mL second two is then added Amine and 9mL ultrapure water, stir, and obtain mixed solution;
(2) reaction kettle equipped with mixed solution is placed in electric drying oven with forced convection, 180 DEG C of reaction 6h are obtained faint yellow Solution;
(3) reaction kettle is taken out, yellow solution is transferred to the bag filter that molecular cut off is 3500Da by natural cooling In, every 6h changes a water, dialyses 3 days, obtains the aqueous solution of pure fluorescent carbon quantum dot;
(4) aqueous solution of fluorescent carbon quantum dot is placed in -20 DEG C of refrigerators and freezes 3h, transfer to vacuum freeze drying Machine, vacuum freeze drying 1 day is to get arriving fluorescent carbon quantum dot powder at -80 DEG C.Through characterizing, fluorescence carbon amounts obtained by the present embodiment The photoluminescent property of son point is similar to Example 1.
Embodiment 5
(1) 5mL propionic acid, 5mL butyric acid are pipetted in ptfe autoclave, 2mL ammonium hydroxide then is added and 8mL is ultrapure Water stirs, and obtains mixed solution;
(2) reaction kettle equipped with mixed solution is placed in electric drying oven with forced convection, 220 DEG C of reaction 8h are obtained faint yellow Solution;
(3) reaction kettle is taken out, yellow solution is transferred to the bag filter that molecular cut off is 3500Da by natural cooling In, every 6h changes a water, dialyses 3 days, obtains the aqueous solution of pure fluorescent carbon quantum dot;
(4) aqueous solution of fluorescent carbon quantum dot is placed in -20 DEG C of refrigerators and freezes 3h, transfer to vacuum freeze drying Machine, vacuum freeze drying 1 day is to get arriving fluorescent carbon quantum dot powder at -80 DEG C.Through characterizing, fluorescence carbon amounts obtained by the present embodiment The photoluminescent property of son point is similar to Example 1.

Claims (9)

1. a kind of method for preparing fluorescent carbon quantum dot as carbon-based material using short chain volatile fatty acid, it is characterised in that: It is liquid nitrogen source and ultrapure water and after mixing evenly to be added, progress hydro-thermal is anti-using short chain volatile fatty acid as carbon-based material It answers, gained reaction solution is post-treated, i.e. acquisition target product fluorescent carbon quantum dot.
2. according to claim 1 a kind of fluorescent carbon quantum dot is prepared using short chain volatile fatty acid as carbon-based material Method, it is characterised in that: the temperature of the hydro-thermal reaction is 160-220 DEG C, time 4-10h.
3. according to claim 1 a kind of fluorescent carbon quantum dot is prepared using short chain volatile fatty acid as carbon-based material Method, it is characterised in that: the post-processing is after dialysing to reaction solution, then carries out vacuum freeze drying.
4. according to claim 1,2 or 3 a kind of fluorescent carbon is prepared using short chain volatile fatty acid as carbon-based material The method of quantum dot, which comprises the following steps:
(1) short chain volatile fatty acid is placed in the stainless steel autoclave of polytetrafluoroethyllining lining, adds liquid nitrogen Source and ultrapure water, stir, and obtain mixed solution;
(2) reaction kettle equipped with mixed solution is placed in airtight heating device, hydro-thermal reaction 4-10h at 160-220 DEG C;
(3) after reaction, reaction kettle is taken out, reaction solution is poured into the bag filter that molecular cut off is 3500Da by natural cooling, Every 6h changes a water, dialyses 3 days in glass container, obtains the aqueous solution of fluorescent carbon quantum dot;
(4) vacuum freeze drying is carried out to the aqueous solution of the fluorescent carbon quantum dot to get fluorescent carbon quantum dot powder is arrived.
5. according to claim 1,2 or 3 a kind of fluorescent carbon is prepared using short chain volatile fatty acid as carbon-based material The method of quantum dot, it is characterised in that: the short chain volatile fatty acid be formic acid, acetic acid, propionic acid, butyric acid, valeric acid, caproic acid and At least one of its isomers.
6. according to claim 1,2 or 3 a kind of fluorescent carbon is prepared using short chain volatile fatty acid as carbon-based material The method of quantum dot, it is characterised in that: the liquid nitrogen source is the urea that ammonium hydroxide, ethylenediamine or mass concentration are 20%-30% Solution.
7. according to claim 1,2 or 3 a kind of fluorescent carbon is prepared using short chain volatile fatty acid as carbon-based material The method of quantum dot, it is characterised in that: the volume ratio of the short chain volatile fatty acid, liquid nitrogen source and ultrapure water is 5-15: 0.5-2:3-14.5.
8. according to claim 4 a kind of fluorescent carbon quantum dot is prepared using short chain volatile fatty acid as carbon-based material Method, it is characterised in that: the airtight heating device be Muffle furnace, tube furnace or electric drying oven with forced convection.
9. according to claim 4 a kind of fluorescent carbon quantum dot is prepared using short chain volatile fatty acid as carbon-based material Method, it is characterised in that: the vacuum freeze drying temperature be -80 DEG C.
CN201811431532.5A 2018-11-27 2018-11-27 A method of fluorescent carbon quantum dot is prepared using short chain volatile fatty acid as carbon-based material Pending CN109486485A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201811431532.5A CN109486485A (en) 2018-11-27 2018-11-27 A method of fluorescent carbon quantum dot is prepared using short chain volatile fatty acid as carbon-based material

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201811431532.5A CN109486485A (en) 2018-11-27 2018-11-27 A method of fluorescent carbon quantum dot is prepared using short chain volatile fatty acid as carbon-based material

Publications (1)

Publication Number Publication Date
CN109486485A true CN109486485A (en) 2019-03-19

Family

ID=65698009

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201811431532.5A Pending CN109486485A (en) 2018-11-27 2018-11-27 A method of fluorescent carbon quantum dot is prepared using short chain volatile fatty acid as carbon-based material

Country Status (1)

Country Link
CN (1) CN109486485A (en)

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103756675A (en) * 2014-01-17 2014-04-30 西安亚博生物技术有限公司 Nitrogen doped carbon quantum dot as well as preparation method and application thereof
CN105647526A (en) * 2015-12-30 2016-06-08 五邑大学 Near-full-spectrum fluorescent nanocarbon dots and preparation method thereof
CN108128767A (en) * 2018-01-03 2018-06-08 辽宁大学 A kind of method and its application that carbon quantum dot is quickly prepared in room temperature environment

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103756675A (en) * 2014-01-17 2014-04-30 西安亚博生物技术有限公司 Nitrogen doped carbon quantum dot as well as preparation method and application thereof
CN105647526A (en) * 2015-12-30 2016-06-08 五邑大学 Near-full-spectrum fluorescent nanocarbon dots and preparation method thereof
CN108128767A (en) * 2018-01-03 2018-06-08 辽宁大学 A kind of method and its application that carbon quantum dot is quickly prepared in room temperature environment

Similar Documents

Publication Publication Date Title
CN104449693B (en) The preparation method of the fluorescent carbon quantum dot of nitrogen sulfur doping
CN107418567B (en) Biomass-based carbon quantum dot and preparation method thereof
CN103342347A (en) Preparation method of carbon quantum dots with high fluorescence property
CN109385275B (en) Method for preparing fluorescent carbon quantum dots by using organic matter anaerobic fermentation intermediate product as carbon-based material
CN103172051A (en) Water-soluble carbon quantum dot and preparation method thereof
CN111606319B (en) Carbon nano coil, preparation method and application thereof, and carbon nano belt
CN106467744B (en) A kind of preparation method of the carbon quantum dot with adjustable photo-electro-luminescence and photoluminescence performance
CN107603611A (en) One kind has Catalyzed Synthesis By Peroxidase active fluoro carbon quantum dot and preparation method thereof
CN110252367B (en) Solvothermal method for preparing few-layer carbon nitride supported vanadium dioxide catalyst and desulfurization application thereof
CN111495402B (en) Molybdenum-based composite material prepared by microwave spark and preparation method and application thereof
CN112007632B (en) Flower-shaped SnO 2 /g-C 3 N 4 Preparation method of heterojunction photocatalyst
CN106883850B (en) Carbon quantum dot fluorescent marking material and preparation method thereof
CN108394885B (en) Method for synthesizing solid carbon quantum dots by gas-phase detonation
CN110548483A (en) preparation method and application of biochar/nano ferroferric oxide composite material
CN111154485B (en) Preparation of sulfur-nitrogen double-doped carbon quantum dot and application of sulfur-nitrogen double-doped carbon quantum dot in tetracycline detection
CN115920890A (en) Preparation method of iron monoatomic-doped fluorescent carbon dot nanoenzyme
CN103771391A (en) Preparation method of water-soluble carbon nanoparticles having fluorescent properties
CN109455692A (en) A kind of chirality carbon quantum dot and preparation method thereof
CN113278415A (en) Preparation method and application of sulfur-nitrogen co-doped yellow fluorescent carbon dots
CN113403068A (en) Fused carbon dot, preparation method and application thereof
CN110817843B (en) Eutectic solvent, application thereof, carbon quantum dot and preparation method thereof
CN109486485A (en) A method of fluorescent carbon quantum dot is prepared using short chain volatile fatty acid as carbon-based material
CN107555416A (en) The method of hydro-thermal method synthetic nitrogen doping fluorescent carbon point
CN107149939A (en) A kind of g C3N4/Al2O3/ZnO hetero-junctions of visible light catalysis activity and preparation method thereof
CN104910904A (en) Method for preparing fluorescent carbon quantum dot by using ozone oxidation photo-reduction technique by taking sulfonated coal as carbon source

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination
RJ01 Rejection of invention patent application after publication
RJ01 Rejection of invention patent application after publication

Application publication date: 20190319