CN106430173A - Preparation method of highly dispersed graphene oxide quantum dots - Google Patents
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- CN106430173A CN106430173A CN201610427254.0A CN201610427254A CN106430173A CN 106430173 A CN106430173 A CN 106430173A CN 201610427254 A CN201610427254 A CN 201610427254A CN 106430173 A CN106430173 A CN 106430173A
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- C01B2204/00—Structure or properties of graphene
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Abstract
The invention provides a preparation method of highly dispersed graphene oxide quantum dots. According to the technical scheme of the invention, one or more components, selected from coking coal, bituminous coal, brown coal, peat and anthracite, is/are adopted as raw materials. The raw materials are subjected to oxidation, separation and lyophilization to obtain light-yellow graphene oxide quantum dots. The preparation method is low in production cost, simple in process, green and environment-friendly. Obtained graphene oxide quantum dots are controllable in size, good in fluorescence effect, excellent in monodispersity and good in water solubility. The prepared highly dispersed graphene oxide quantum dots have a very large application prospect in the fields of photoelectric materials, device preparation, biological images, display screens, drug carriers, solar cells, anti-counterfeiting coatings, novel semiconductor devices and the like.
Description
Technical field
The invention belongs to technical field of nano material is and in particular to arrive a kind of system of the graphene oxide quantum dot of high dispersive
Preparation Method.
Background technology
2004, Univ Manchester UK's physicist successfully isolated Graphene from graphite, due to Graphene tool
There are excellent electricity, calorifics, mechanics, optical characteristics to have a wide range of applications in field of nanometer technology, cause the wide of academia
General concern.However, Graphene is the quasiconductor of zero band gap, the Graphene of band gap is not had not observe fluorescence property, this is just
Limit its application in electronics and optoelectronic areas, but the size limitation of Graphene in below 10nm, using quantum local
Effect and side effect open band gap, and this undersized Graphene (i.e. graphene quantum dot) can be made to be endowed new physics
Property.Graphene quantum dot is the nano material of quasi-zero dimension, and the hardness not only with Graphene is strong, heat conductivity is high, electronics moves
Shifting rate is fast, outside the low advantage of resistivity, when it is smaller in size than 10nm, also as quantum confined effect and boundary effect and have
New physical property.So graphene quantum dot will bring revolutionary change for electronics, photoelectricity and electromagnetism field.Should
For photoelectric material and the aspects such as device preparation, biological fluorescent labelling, catalyst carrier and multiple microparticles system.
The preparation method of graphene quantum dot generally includes at present：The side such as microwave assisting method, hydro-thermal method, electrochemistry, etching
Method.But, it is more than 20nm and expensive not utilization using the graphene quantum dot general size that lithographic method prepares gained
Produce, although it is easy to prepare graphene quantum dot method using hydro-thermal method or electrochemical process, raw materials used for graphite, carbon nanometer
Pipe, carbon fiber, fullerene etc., the prices of raw materials are relatively expensive.
Content of the invention
It is an object of the invention to solving the deficiencies in the prior art and shortcoming, provide a kind of by coal dust (coking coal, brown coal,
One or more of anthracite, mud coal, bituminous coal) use oxidant direct oxidation to prepare the graphene oxide quantum dot of high dispersive
Method.It is raw material that the present invention adopts one or more of coking coal, brown coal, anthracite, mud coal, bituminous coal, by simply controlled
Wet chemical oxidation method prepare graphene oxide quantum dot, and will be obtained using activated carbon alkaline waste liquor in preparation process
Acid solution is neutralized to neutrality, prepares graphene oxide quantum dot low cost, process is simple, environmental protection, institute by the method
Graphene quantum dot size controlled, uniform particle diameter, the graphene oxide quantum dot of gained have excellent fluorescent effect,
The characteristics such as the strong and good water solublity of monodispersity, the preparation of photoelectric material and device, biological image, display screen, pharmaceutical carrier,
The aspects such as solaode, security coating, novel semi-conductor body have very big application prospect.
A kind of preparation method of the graphene oxide quantum dot of high dispersive is it is characterised in that comprise the steps：
1. according to certain mass volume ratio, coal dust is added in oxidizing acid solution, is stirred disperseing, is mixed
Close solution A；
2., by the mixed solution A rotary evaporation under vacuum of preparation in step 1, obtain residual solid；
3. the residual solid of preparation in step 2 is added in deionized water according to certain mass volume ratio, and mixes
Uniformly, obtain mixed solution B；
4. add proper amount of active carbon alkaline waste liquor to be neutralized toward in mixed solution B, until pH value of solution reaches 7, obtain mixing
Solution C；
5. the hollow fiber filter the use of molecular cut off being first 1 kilodalton by the mixed solution C of preparation in step 4
Filter, obtain filtrate 1, then filtrate 1 being used molecular cut off is that 3 kilodalton hollow fiber filters filter, and obtains
To filtrate 2；
6. the filtrate 2 of preparation in step 5 is carried out the graphene oxide quantum dot that lyophilization obtains high dispersive.
Coal dust described in step 1 is one or more of coking coal, brown coal, anthracite, mud coal, bituminous coal, wherein coal
The Average Particle Diameters of powder are 1～1000 μm；
Oxidizing acid described in step 1 is one kind or several of permanganic acid, potassium permanganate, concentrated sulphuric acid, nitric acid, perchloric acid etc.
Kind；
Coal dust described in step 1 is 5～15g: 90～250ml with the mass volume ratio of oxidizing acid；
The temperature of the stirring described in step 1 is 100～250 DEG C, and mixing time is 12～24h；
Described vacuum condition in step 2 is -0.1MPa, and the temperature of rotary evaporation is 60～100 DEG C；
Residual solid described in step 3 is 5～15g: 500～1000ml with the mass volume ratio of deionized water；
Activated carbon alkaline waste liquor described in step 4, its pH value is between 10～14；
The film of the hollow fiber filter described in step 5 is poly (ether sulfone) film, three cellulose acetate membrane, mixed cellulose ester
One of film, membrane area is 200～400cm2, film length 30～70cm, fibre inner diameter 0.05～1mm；
Lyophilization temperature described in step 6 is -50～80 DEG C, vacuum is 1～20Pa；
The graphene oxide quantum dot number of plies of the high dispersive obtaining in step 6 is 1～5 layer, and size is 1～30nm.
After the present invention adopts technique scheme, mainly have the following effects：
1. coal dust aboundresources of the present invention, cheap, reduces the production cost of graphene quantum dot.
2. the present invention adopts the operation such as chemical oxidation and hollow fibre filtering, process is simple, easy to operate, production efficiency
Height, is advantageously implemented large-scale production, easy to utilize；
3. the inventive method adopts in activated carbon alkaline waste liquor and acid solution in process of production, realizes the recovery profit of waste liquid
With reducing production cost, production technology environmental protection.
The preparation method of the graphene oxide quantum dot of high dispersive that the present invention provides, its synthesis technique is simple, low cost,
Raw material is cheap and easy to get, and the monodispersity of the graphene oxide quantum dot of preparation is strong, particle diameter is little, good water solubility and have strong glimmering
Optical property.In photoelectric material and device preparation, biological image, display screen, pharmaceutical carrier, solaode, security coating, new
The aspects such as plate for semiconductor equipment have very big application prospect.
Specific embodiment
With reference to specific embodiment, further illustrate the present invention.
Embodiment 1
A kind of graphene oxide quantum dot preparation method of high dispersive, wherein：
(1) coal dust is taken to add in oxidizing acid solution, according to coal dust: the ratio for 5g: 90ml for the ratio of oxidizing acid is joined
Put continuously stirred 24h at 100 DEG C, obtain mixed solution A；
(2) by middle for step (1) mixed solution prepared rotary evaporation under 60 DEG C, -0.1MPa vacuum condition, remnants are obtained
Solid；
(3) add deionized water, according to residual solid: deionized water ratio in the residual solid of preparation toward in step (2)
Configure for 5g: 500ml, mix homogeneously obtains mixed solution B；
(4) the activated carbon alkaline waste liquor that appropriate pH is 10 is added to be neutralized in the mixed solution of preparation toward in step (3),
Until pH value of solution reaches 7, obtain mixed solution C；
(5) hollow fibre filtering the use of molecular cut off being first 1 kilodalton by the mixed solution of preparation in step (4)
Device is filtrated to get filtrate 1, the hollow fiber filter the use of molecular cut off being then 3 kilodaltons by gained filtrate 1
It is filtrated to get filtrate 2, the film of hollow fiber filter is poly (ether sulfone) film, and membrane area is 400cm2, the long 70cm of film, fibre inner diameter
1mm；
(6) by the filtrate 2 in step (5), under conditions of -80 DEG C, 10Pa, lyophilization obtains the oxidation stone of high dispersive
Black alkene quantum dot.
Embodiment 2
A kind of graphene oxide quantum dot preparation method of high dispersive, with case study on implementation 1, wherein：
Coal dust described in step (1) is bituminous coal, and described oxidizing acid is nitric acid, and described solution A is according to coal dust: oxidation
Property acid ratio be 10g: 150ml configuration, described whipping temp is 100 DEG C, and mixing time is 12h；
The temperature of the rotary evaporation described in step (2) is 60 DEG C；
Described in step (3), solution B is according to residual solid: the ratio of deionized water is 10g: 750ml configuration.
Activated carbon alkaline waste liquor pH value described in step (4) is 11；
The film of the hollow fiber filter described in step (5) is poly (ether sulfone) film, and membrane area is 200cm2, the long 30cm of film,
Fibre inner diameter 0.05mm；
Lyophilization temperature described in step (6) is -80 DEG C, and vacuum is 10Pa.
Embodiment 3
A kind of graphene oxide quantum dot preparation method of high dispersive, with case study on implementation 1, wherein：
Coal dust described in step (1) is coking coal, and described oxidizing acid is concentrated sulphuric acid, and described solution A is according to coal dust:
The ratio of oxidizing acid is 15g: 250ml configuration, and described whipping temp is 150 DEG C, and mixing time is 18h；
The temperature of the rotary evaporation described in step (2) is 80 DEG C；
Described in step (3), solution B is according to residual solid: the ratio of deionized water is 15g: 1000ml configuration.
Activated carbon alkaline waste liquor pH value described in step (4) is 12；
The film of the hollow fiber filter described in step (5) is poly (ether sulfone) film, and membrane area is 300cm2, the long 50cm of film,
Fibre inner diameter 0.5mm；
Lyophilization temperature described in step (6) is -50 DEG C, and vacuum is 1Pa.
Embodiment 4
A kind of graphene oxide quantum dot preparation method of high dispersive, with case study on implementation 1, wherein：
Coal dust described in step (1) is anthracite, and described oxidizing acid is perchloric acid, described solution A is according to coal dust
: the ratio of oxidizing acid is 10g: 150ml configuration, and described whipping temp is 200 DEG C, and mixing time is 12h；
The temperature of the rotary evaporation described in step (2) is 100 DEG C；
Described in step (3), solution B is according to residual solid: the ratio of deionized water is 10g: 750ml configuration.
Activated carbon alkaline waste liquor pH value described in step (4) is 13；
The film of the hollow fiber filter described in step (5) is poly (ether sulfone) film, and membrane area is 400cm2, the long 70cm of film,
Fibre inner diameter 1mm；
Lyophilization temperature described in step (6) is -65 DEG C, and vacuum is 15Pa.
Embodiment 5
A kind of graphene oxide quantum dot preparation method of high dispersive, with case study on implementation 1, wherein：
Coal dust described in step (1) is mud coal, and described oxidizing acid is permanganic acid, and described solution A is according to coal dust: oxygen
The ratio of the property changed acid is 5g: 90ml configuration, and described whipping temp is 100 DEG C, and mixing time is 12h；
The temperature of the rotary evaporation described in step (2) is 80 DEG C；
Described in step (3), solution B is according to residual solid: the ratio of deionized water is 5g: 500ml configuration.
Activated carbon alkaline waste liquor pH value described in step (4) is 14；
The film of the hollow fiber filter described in step (5) is three cellulose acetate membrane, and membrane area is 300cm2, film is long
50cm, fibre inner diameter 0.5mm；
Lyophilization temperature described in step (6) is -75 DEG C, and vacuum is 20Pa.
Embodiment 6
A kind of graphene oxide quantum dot preparation method of high dispersive, with case study on implementation 1, wherein：
Coal dust described in step (1) is brown coal, and described oxidizing acid is potassium permanganate, and described solution A is according to coal dust:
The ratio of oxidizing acid is 10g: 150ml configuration, and described whipping temp is 150 DEG C, and mixing time is 24h；
The temperature of the rotary evaporation described in step (2) is 100 DEG C；
Described in step (3), solution B is according to residual solid: the ratio of deionized water is 10g: 750ml configuration；
Activated carbon alkaline waste liquor pH value described in step (4) is 12；
The film of the hollow fiber filter described in step (5) is three cellulose acetate membrane, and membrane area is 400cm2, film is long
70cm, fibre inner diameter 1mm；
Lyophilization temperature described in step (6) is -50 DEG C, and vacuum is 10Pa.
Embodiment 7
A kind of graphene oxide quantum dot preparation method of high dispersive, with case study on implementation 1, wherein：
Coal dust described in step (1) is the mixture of coking coal and bituminous coal, and described oxidizing acid is nitric acid and dense sulfur
Sour mixed liquor；Described solution A is according to coal dust: the ratio of oxidizing acid is 10g: 150ml configuration, and described whipping temp is 150
DEG C, mixing time is 12h；
The temperature of the rotary evaporation described in step (2) is 60 DEG C；
Described in step (3), solution B is according to residual solid: the ratio of deionized water is 10g: 750ml configuration；
Activated carbon alkaline waste liquor pH value described in step (4) is 13；
The film of the hollow fiber filter described in step (5) is mixed cellulose ester membrane, and membrane area is 300cm2, film is long
50cm, fibre inner diameter 0.5mm；
Lyophilization temperature described in step (6) is -50 DEG C, and vacuum is 20Pa.
Embodiment 8
A kind of graphene oxide quantum dot preparation method of high dispersive, with case study on implementation 1, wherein：
Coal dust described in step (1) is coking coal, brown coal and anthracitic mixture, and described oxidizing acid is Gao Meng
Sour potassium and the mixed solution of concentrated sulphuric acid, described solution A is according to coal dust: the ratio of oxidizing acid is 15g: 250ml configuration, described
Whipping temp is 150 DEG C, and mixing time is 18h；
The temperature of the rotary evaporation described in step (2) is 100 DEG C；
Described in step (3), solution B is according to residual solid: the ratio of deionized water is 15g: 1000ml configuration；
Activated carbon alkaline waste liquor pH value described in step (4) is 12；
The film of the hollow fiber filter described in step (5) is mixed cellulose ester membrane, and membrane area is 400cm2, film is long
70cm, fibre inner diameter 1mm；
Lyophilization temperature described in step (6) is -50 DEG C, and vacuum is 1Pa.
Embodiment 9
A kind of graphene oxide quantum dot preparation method of high dispersive, with case study on implementation 1, wherein：
Coal dust described in step (1) is the mixture of mud coal and bituminous coal, and described oxidizing acid is nitric acid and concentrated sulphuric acid,
Described solution A is according to coal dust: the ratio of oxidizing acid is 10g: 150ml configuration, and described whipping temp is 150 DEG C, during stirring
Between be 18h；
The temperature of the rotary evaporation described in step (2) is 80 DEG C；
Described in step (3), solution B is according to residual solid: the ratio of deionized water is 10g: 750ml configuration；
Activated carbon alkaline waste liquor pH value described in step (4) is 10；
The film of the hollow fiber filter described in step (5) is mixed cellulose ester membrane, and membrane area is 200cm2, film is long
30cm, fibre inner diameter 0.05mm；
Lyophilization temperature described in step (6) is -80 DEG C, and vacuum is 1Pa.
Claims (12)
1. a kind of preparation method of the graphene oxide quantum dot of high dispersive is it is characterised in that comprise the steps：
1) according to certain mass volume ratio, coal dust is added in oxidizing acid solution, continuously stirred carry out oxidation reaction, obtain
To mixed solution A；
2) by the mixed solution A rotary evaporation under vacuum of preparation in step 1, obtain residual solid；
3) residual solid of preparation in step 2 is added in deionized water according to certain mass volume ratio, and mix homogeneously,
Obtain mixed solution B；
4) add proper amount of active carbon alkaline waste liquor to be neutralized toward in mixed solution B, until pH value of solution reaches 7, obtain mixed solution
C；
5) the hollow fiber filter mistake the use of molecular cut off being first 1 kilodalton by the mixed solution C of preparation in step 4
Filter, obtains filtrate 1, then filters filtrate 1 using the hollow fiber filter that molecular cut off is 3 kilodaltons, obtains
To filtrate 2；
6) filtrate 2 of preparation in step 5 is carried out the graphene oxide quantum dot that lyophilization obtains high dispersive.
2. coal dust is one or more of coking coal, brown coal, anthracite, mud coal, bituminous coal as described in the appended claim 1, wherein
The Average Particle Diameters of coal dust are at 1～1000 μm.
3. oxidizing acid as described in claim 1 is one kind of permanganic acid, potassium permanganate, concentrated sulphuric acid, nitric acid, perchloric acid etc.
Or it is several.
4. the mass volume ratio of coal dust as described in claim 1 and oxidizing acid is 5～15g: 90～250ml.
5. stirring oxidizing reaction temperature as described in claim 1 is 100～250 DEG C, and the continuously stirred time is 12～24h.
6. vacuum condition as described in claim 1 is -0.1MPa.
7. rotating evaporation temperature as described in claim 1 is 60～100 DEG C.
8. residual solid as described in claim 1 and the mass volume ratio of deionized water are 5～15g: 500～1000ml.
9. activated carbon alkaline waste liquor as described in claim 1, its pH value is between 10～14.
10. the film of hollow fiber filter as described in claim 1 be poly (ether sulfone) film, three cellulose acetate membrane, mixing fine
One of dimension cellulose ester film, membrane area is 200～400cm2, film length 30～70cm, fibre inner diameter 0.05～1mm.
11. lyophilization temperature as described in claim 1 are -50～-80 DEG C, vacuum 1～20Pa.
The graphene oxide quantum dot number of plies of the high dispersive of 12. preparations as described in claim 1 is 1～5 layer, size
For 1～30mm.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN107632002A (en) * | 2017-09-13 | 2018-01-26 | 北京理工大学 | A kind of composite fluorescence biology sensor and its production and use |
| CN109437181A (en) * | 2018-12-07 | 2019-03-08 | 四川聚创石墨烯科技有限公司 | A kind of total system of graphene oxide slurry |
| CN109775729A (en) * | 2018-12-07 | 2019-05-21 | 四川聚创石墨烯科技有限公司 | A kind of processing system of graphene oxide waste liquid |
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| KR20160003231A (en) * | 2013-05-02 | 2016-01-08 | 윌리엄 마쉬 라이스 유니버시티 | Methods of producing graphene quantum dots from coal and coke |
| CN105271194A (en) * | 2015-10-29 | 2016-01-27 | 东华大学 | Preparation method of graphene quantum dots containing methoxyl |
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| KR20160003231A (en) * | 2013-05-02 | 2016-01-08 | 윌리엄 마쉬 라이스 유니버시티 | Methods of producing graphene quantum dots from coal and coke |
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| US20160060122A1 (en) * | 2013-05-02 | 2016-03-03 | William Marsh Rice University | Methods of producing graphene quantum dots from coal and coke |
| CN103922329A (en) * | 2014-04-22 | 2014-07-16 | 福州大学 | Method for extracting graphene quantum dots from coal |
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| CN107632002A (en) * | 2017-09-13 | 2018-01-26 | 北京理工大学 | A kind of composite fluorescence biology sensor and its production and use |
| CN107632002B (en) * | 2017-09-13 | 2020-03-17 | 北京理工大学 | Composite fluorescent biosensor and preparation method and application thereof |
| CN109437181A (en) * | 2018-12-07 | 2019-03-08 | 四川聚创石墨烯科技有限公司 | A kind of total system of graphene oxide slurry |
| CN109775729A (en) * | 2018-12-07 | 2019-05-21 | 四川聚创石墨烯科技有限公司 | A kind of processing system of graphene oxide waste liquid |
| CN109775729B (en) * | 2018-12-07 | 2021-02-02 | 四川聚创石墨烯科技有限公司 | Processing system of oxidation graphite alkene waste liquid |
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