CN106479493A - A kind of method for carbon source, carbon quantum dot being prepared by hydrogen peroxide low-temperature oxidation with brown coal - Google Patents
A kind of method for carbon source, carbon quantum dot being prepared by hydrogen peroxide low-temperature oxidation with brown coal Download PDFInfo
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- CN106479493A CN106479493A CN201610838901.7A CN201610838901A CN106479493A CN 106479493 A CN106479493 A CN 106479493A CN 201610838901 A CN201610838901 A CN 201610838901A CN 106479493 A CN106479493 A CN 106479493A
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Abstract
The invention belongs to field of nano material preparation, a kind of method for carbon source, carbon quantum dot being prepared by hydrogen peroxide low-temperature oxidation with brown coal.Brown coal are mixed and stirred for deionized water, hydrogen peroxide, hydro-thermal reaction 6 18h under 60 DEG C of 110 DEG C of temperature conditionss, hydro-thermal reaction, with continuous magnetic agitation, wherein, adds the deionized water of 10 200ml and the hydrogen peroxide of 3 50ml in every 1g brown coal；After reaction terminates, cooling, centrifugation removes not oxidized bulky grain；By the liquid obtaining revolving eliminating water, obtain final product carbon quantum dot.The present invention is carbon source using the cheap brown coal being easy to get, and obtains the Water-soluble carbon quantum dot in 1 10nm for the substantial amounts of particle diameter through the low-temperature oxidation of hydrogen peroxide and filtration, high speed centrifugation, this carbon quantum dot shows good photoluminescent property.This method is green, cheap, simple to operate, efficiency high, is conducive to breaking through the bottleneck of large-scale commercial production, has significantly economic and social benefit.
Description
Technical field
The invention belongs to field of nano material preparation is and in particular to one kind passes through hydrogen peroxide low-temperature oxidation with brown coal for carbon source
The method of preparation carbon quantum dot.
Background technology
Carbon quantum dot (carbon dots, CQDs), also known as carbon point or carbon nano dot, be a class size 10 nanometers with
Under new zero dimension carbon nano luminescent material, be a kind of spherical carbon granule.For metal quantum point, carbon quantum
Point is nontoxic, and the harm to environment is little, and carbon quantum dot has traditional quantum dot and do not have the advantage that, the little chi of its existing nanoparticle
Very little feature, has the photoluminescent property of quantum dot again, also extraordinary biocompatibility.Because quantum dot size is little, its current-carrying
The energy of son is in quantization so that quantum dot has excellent optics, electric property.Carbon quantum dot is with its good chemically stable
Property and the advantage such as biocompatibility obtain increasing attention.This Illuminant nanometer material is in photoelectricity equipment, nanosensor
Device, medical imaging devices, biomarker, ion detection and photocatalysis field have important application prospect.
As a kind of novel nano material, many preparation methoies with regard to carbon quantum dot of having reported for work.The system of CQDs
Preparation Method mainly include nitration mixture oxidizing process, electrochemical oxidation process, hydro-thermal method, arc discharge, template synthesis method, laser ablation and
Small molecule synthetic method etc. from bottom to top.Although said method has prepared the preferable CQDs of fluorescence, these methods
Experimentation complex operation, higher to ingredient requirement, experimental provision is had high demands, unfriendly to environment etc. determine, thus limit
The industrialized preparation of CQDs.And coal is not only cheap and easy to get, and texture of coal is by nano junction chip and middle acyclic carbochain
Composition, but it is using nitration mixture (H that most of document is recorded2SO4/HNO3) or strong acid coal dust is carried out oxidation backflow 16-24 hour system
Standby go out water solublity and fluorescence characteristic all preferably CQDs, and the later stage also to carry out place to acid and go out, this when carrying out long with acid
Between oxidation backflow preparation carbon quantum dot when, CQDs can oxidized fall, reduction yield；And end processing sequences are number
Tired, and a large amount of waste liquids and toxic gas can be produced, also environment can be caused with a certain degree of pollution it is difficult to carry out industrialized
Generate.
Content of the invention
In order to overcome the above-mentioned deficiencies of the prior art, the invention provides one kind passes through hydrogen peroxide low temperature with brown coal for carbon source
The method of oxidation preparation carbon quantum dot, Chinese brown coal are possessed 130,000,000,000 tons of storage capacity, are accounted for national coal saving amount 13%, brown coal are former
Material is abundant, and cheap and easy to get, therefore the present invention selects brown coal is raw material.And select Green Oxidant H2O2As oxidant, after oxidation
The H producing2O and O2, environment will not be produced with pollution, method green.Prepare the high carbon quantum dot of good water solubility, fluorescence efficiency.
Technical scheme：
A kind of method preparing carbon quantum dot for carbon source by hydrogen peroxide low-temperature oxidation with brown coal, step is as follows：
100-1000 mesh brown coal and deionized water, hydrogen peroxide are mixed and stirred for, water under 60 DEG C of -110 DEG C of temperature conditionss
Thermal response 6-18h, hydro-thermal reaction with continuous magnetic agitation, wherein, add in every 1g brown coal the deionized water of 10-200ml with
The hydrogen peroxide of 3-50ml；After reaction terminates, cooling, centrifugation removes not oxidized bulky grain；By the liquid obtaining revolving
Eliminating water, obtains final product carbon quantum dot.
The mass concentration of described hydrogen peroxide is 30%.
The rotating speed of described centrifugation is 10000-18000rpm, and the time is 5-30min.
The temperature of described revolving is 40 DEG C -75 DEG C.
Beneficial effects of the present invention：The present invention with brown coal cheap and easy to get as raw material, by control brown coal coal dust, deionization
The parameters such as water, the ratio of hydrogen peroxide, hydrothermal temperature, time can achieve the macroscopic view preparation of Graphene.The present invention adopts green
Preparing carbon quantum dot, the water of the generation after oxidation and oxygen will not produce the oxidant hydrogen peroxide direct oxidation brown coal of color to environment
Raw pollution, the carbon quantum dot of preparation not only has the advantages that good water solubility, fluorescence efficiency are high, and preparation cost is cheap, operation
Simply, convenient post-treatment, yield is high, is easy to industrialized production.
Brief description
Fig. 1 is the particle diameter distribution by laser light scattering carbon quantum dot, and particle diameter distribution is between 1-10nm.
Fig. 2 is the UV-vis absorption spectrum of carbon quantum dot.
Specific embodiment
Below in conjunction with accompanying drawing and technical scheme, further illustrate the specific embodiment of the present invention.
Embodiment 1
The mass fraction of deionized water and 10ml that the lignite powder of 0.5 gram of drying is added to 100ml is 30% H2O2
In, flow back under conditions of 100 DEG C 8h.After room temperature, it is centrifuged under 18000rpm with High speed refrigerated centrifuge,
With Rotary Evaporators, gained liquid is evaporated after centrifugation, is vacuum dried at 65 DEG C, obtains the CQDs powder of rufous.
Embodiment 2
The mass fraction of deionized water and 15ml that the lignite powder of 2.00 grams of dryings is added to 50ml is 30% H2O2
In, flow back under conditions of 70 DEG C 15h.After room temperature, it is centrifuged 2 under 15000rpm with High speed refrigerated centrifuge
Secondary, every time for 20min, and with Rotary Evaporators, gained liquid is evaporated, is vacuum dried at 65 DEG C, obtains the CQDs powder of rufous
End.
Embodiment 3
The mass fraction of deionized water and 20ml that the lignite powder of 1 gram of drying is added to 30ml is 30% H2O2In,
Flow back under conditions of 80 DEG C 10h.After room temperature, it is centrifuged 2 times under 10000rpm with High speed refrigerated centrifuge,
It is 20min every time, and with Rotary Evaporators, gained liquid is evaporated, be vacuum dried at 65 DEG C, obtain the CQDs powder of rufous.
Embodiment 4
The mass fraction of deionized water and 10ml that the lignite powder of 0.5 gram of drying is added to 50ml is 30% H2O2
In, flow back under conditions of 60 DEG C 8h.After room temperature, it is centrifuged 2 under 10000rpm with High speed refrigerated centrifuge
Secondary, every time for 20min, and with Rotary Evaporators, gained liquid is evaporated, is vacuum dried at 65 DEG C, obtains the CQDs powder of rufous
End.
Claims (5)
1. a kind of with brown coal for carbon source by hydrogen peroxide low-temperature oxidation prepare carbon quantum dot method it is characterised in that step such as
Under：
100-1000 mesh brown coal and deionized water, hydrogen peroxide are mixed and stirred for, under 60 DEG C of -110 DEG C of temperature conditionss, hydro-thermal is anti-
Answer 6-18h, hydro-thermal reaction, with continuous magnetic agitation, wherein, adds deionized water and the 3- of 10-200ml in every 1g brown coal
The hydrogen peroxide of 50ml；After reaction terminates, cooling, centrifugation removes not oxidized bulky grain；The liquid obtaining revolving is removed
Water, obtains final product carbon quantum dot.
2. method according to claim 1 is it is characterised in that the mass concentration of described hydrogen peroxide is 30%.
3. method according to claim 1 and 2 is it is characterised in that the rotating speed of described centrifugation is 10000-
18000rpm, the time is 5-30min.
4. method according to claim 1 and 2 is it is characterised in that the temperature of described revolving is 40 DEG C -75 DEG C.
5. method according to claim 3 is it is characterised in that the temperature of described revolving is 40 DEG C -75 DEG C.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106978170A (en) * | 2017-05-25 | 2017-07-25 | 西安理工大学 | A kind of preparation method of water-solubility fluorescent carbon quantum dot |
| CN109097035A (en) * | 2018-08-31 | 2018-12-28 | 中国石油大学(北京) | Carbon quantum dot and its preparation and application with high fluorescent characteristic |
| CN109437154A (en) * | 2018-10-25 | 2019-03-08 | 河南理工大学 | A method of the controllable carbon quantum dot of energy band is prepared by raw material of coal |
| CN112608743A (en) * | 2020-12-24 | 2021-04-06 | 中国矿业大学(北京) | Preparation method of coal-based fluorescent carbon quantum dots |
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| CN104071769A (en) * | 2014-06-12 | 2014-10-01 | 大连理工大学 | Method for preparing fluorescent carbon point by virtue of chemical oxidation method, fluorescent carbon point and application of fluorescent carbon point |
| WO2014179708A1 (en) * | 2013-05-02 | 2014-11-06 | William Marsh Rice University | Methods of producing graphene quantum dots from coal and coke |
| CN104946252A (en) * | 2015-07-15 | 2015-09-30 | 中北大学 | Method for preparing fluorescent carbon dots by using coal |
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2016
- 2016-09-21 CN CN201610838901.7A patent/CN106479493A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2014179708A1 (en) * | 2013-05-02 | 2014-11-06 | William Marsh Rice University | Methods of producing graphene quantum dots from coal and coke |
| CN104071769A (en) * | 2014-06-12 | 2014-10-01 | 大连理工大学 | Method for preparing fluorescent carbon point by virtue of chemical oxidation method, fluorescent carbon point and application of fluorescent carbon point |
| CN104946252A (en) * | 2015-07-15 | 2015-09-30 | 中北大学 | Method for preparing fluorescent carbon dots by using coal |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106978170A (en) * | 2017-05-25 | 2017-07-25 | 西安理工大学 | A kind of preparation method of water-solubility fluorescent carbon quantum dot |
| CN106978170B (en) * | 2017-05-25 | 2019-09-27 | 西安理工大学 | A kind of preparation method of water-solubility fluorescent carbon quantum dot |
| CN109097035A (en) * | 2018-08-31 | 2018-12-28 | 中国石油大学(北京) | Carbon quantum dot and its preparation and application with high fluorescent characteristic |
| CN109097035B (en) * | 2018-08-31 | 2020-11-10 | 中国石油大学(北京) | Carbon quantum dot with high fluorescence characteristic and preparation and application thereof |
| CN109437154A (en) * | 2018-10-25 | 2019-03-08 | 河南理工大学 | A method of the controllable carbon quantum dot of energy band is prepared by raw material of coal |
| CN112608743A (en) * | 2020-12-24 | 2021-04-06 | 中国矿业大学(北京) | Preparation method of coal-based fluorescent carbon quantum dots |
| CN112608743B (en) * | 2020-12-24 | 2022-06-14 | 中国矿业大学(北京) | Preparation method of coal-based fluorescent carbon quantum dots |
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Application publication date: 20170308 |