CN107720734A - It is a kind of to prepare the method with fluorescent characteristic graphene quantum dot using waste biomass resource - Google Patents
It is a kind of to prepare the method with fluorescent characteristic graphene quantum dot using waste biomass resource Download PDFInfo
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- CN107720734A CN107720734A CN201711153089.5A CN201711153089A CN107720734A CN 107720734 A CN107720734 A CN 107720734A CN 201711153089 A CN201711153089 A CN 201711153089A CN 107720734 A CN107720734 A CN 107720734A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- 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
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
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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 kind of the method with fluorescent characteristic graphene quantum dot is prepared using waste biomass resource, it is to obtain carbon source through high temperature cabonization after drying longan branch or longan pericarp, then the graphene quantum dot with fluorescent characteristic is made after simple nitrification, ultrasonication, hydro-thermal process.The present invention turns waste into wealth, take full advantage of the local discarded living resources in Fujian Province, the pressure of local environment pollution can not only be alleviated to a certain extent, and it can pass through the fluorescence intensity and wavelength of the controlling changing graphene quantum dot of parameter in preparation process, to adapt to different demands, this helps lend some impetus to the development of local graphene related industry, increases economic well-being of workers and staff.
Description
Technical field
The invention belongs to technical field of nanometer material preparation, and in particular to a kind of to utilize discarded longan branch or longan pericarp system
The standby method with fluorescent characteristic graphene quantum dot.
Background technology
Graphene quantum dot（GQDs）It is graphene of its surface with oxy radical when graphene becomes smaller than 10nm
Piece, it is commonly called as small size graphene.Graphene quantum dot is in addition to the performance excellent with graphene, due to the spy of its quasi-zero dimension
Property, motion of the internal electron in all directions are all limited to, and the significant quantum confinement effect showed makes it have perhaps
More unique properties, in solar cell, electronic equipment, optical dye, biomarker and multiple microparticles system and new half
The fields such as conductor device have important potential using value.The synthesis mode of graphene quantum dot is broadly divided into from top to bottom at present
From bottom to top both.Include hydro-thermal method, electrochemical process and chemical stripping carbon fiber method from top to bottom, from bottom to top including molten
Liquid chemical method, supercritical ultrasonics technology and microwave method, controllable pyrolysis polycyclic aromatic hydrocarbon method etc..
Longan branch refers to the small limb for tying longan, and longan pericarp refers to the pericarp of longan.In Fujian Province, when longan maturation
Section, longan branch and longan pericarp are seen everywhere.The present invention is by recycling discarded longan branch or longan pericarp, and after being dried
Carbonization is carried out at high temperature and is used as green inexpensive carbon source, then by simply nitrification, ultrasonication, at hydro-thermal
Reason, obtains the graphene quantum dot of different fluorescence intensities, it is expected to be well used in fields such as solar cells.
The content of the invention
Being prepared it is an object of the invention to provide one kind using waste biomass resource has fluorescent characteristic graphene quantum dot
Method, it can not only make full use of waste biomass resource, and can it is easy, obtain the graphene with different fluorescent characteristics at a low price
Quantum dot.
To achieve the above object, the present invention adopts the following technical scheme that：
A kind of to prepare the method with fluorescent characteristic graphene quantum dot using waste biomass resource, it is by longan branch or longan
Shell is carbonized and is used as carbon source at high temperature after drying, and then by simple nitrification, ultrasonication, hydro-thermal process, the stone is made
Black alkene quantum dot；It specifically includes following steps：
（1）Longan branch or longan pericarp are cleaned after drying, high temperature cabonization for a period of time, then takes out under protective atmosphere, cleaning
Dry, and grind into powder, obtain carbon dust；
（2）Filtered after gained carbon dust is added into nitric acid oxidation, then drying, obtain black powder；
（3）Gained black powder is added in DMF solvent, the gained suspension transfer after ultrasonication
Hydro-thermal process is carried out into high-temperature high-pressure reaction kettle；
（4）Room temperature is cooled to after having handled, is taken out, is filtered, gained filtrate is the graphene quantum with different fluorescence intensities
Point.
Step（1）Middle protective atmosphere uses argon gas.
Step（1）Middle carburizing temperature be 600-800 DEG C, preferably 800 DEG C, carbonization time 2-3h, preferably 3h.Carbonization
In heating rate be 5-10 DEG C/min, preferably 5 DEG C/min.
Step（2）The reaction temperature of middle nitric acid oxidation be 70-90 DEG C, preferably 80 DEG C, reaction time 12-24h, preferably
For 12h；The mass concentration of nitric acid used is 65%-68%.
Step（2）Middle drying temperature is 70-90 DEG C, preferably 80 DEG C.
Step（3）The power of middle ultrasonication is 100-400W, and the time is 1 ~ 2h, preferably 2h.
Step（3）The temperature of middle hydro-thermal process be 180 ~ 200 DEG C, preferably 200 DEG C, processing time 10-12h, preferably
For 10h.
Filtered in operation using sand core funnel and 0.22 μm of miillpore filter.
The remarkable advantage of the present invention is：The present invention recycles discarded longan branch, longan pericarp, in height after being dried
The lower carbonization of temperature obtains green inexpensive carbon source, and tool then is made after simple nitrification, ultrasonication, hydro-thermal process
There is the graphene quantum dot of different fluorescence intensities.The present invention turns waste into wealth, and takes full advantage of the local discarded biology money in Fujian Province
Source, it can not only alleviate the pressure of local environment pollution to a certain extent, and it can pass through the regulation and control of parameter in preparation process
Change the fluorescence intensity and wavelength of graphene quantum dot, to adapt to different demands, this helps lend some impetus to the related production of local graphene
The development of industry, increase economic well-being of workers and staff.
Brief description of the drawings
Fig. 1 is the X-ray diffractogram of the gained longan branch carbon dust after high temperature cabonization.
Fig. 2 is embodiment 1 and the fluorescence spectra of the graphene quantum dot prepared by embodiment 2.
Fig. 3 is embodiment 2 and the fluorescence spectra of the graphene quantum dot prepared by embodiment 3.
Embodiment
In order that content of the present invention easily facilitates understanding, with reference to embodiment to of the present invention
Technical scheme is described further, but the present invention is not limited only to this.
High temperature cabonization uses Bei Yike vacuum tube furnaces.
Ultrasonication uses the D ultrasonic cell disruptors of SCIENTZ II.
Suction filtration uses sand core funnel and 0.22 μm of miillpore filter.
Embodiment 1
（1）7g longans branch is cleaned after drying, in 800 DEG C of high temperature cabonization 3h under argon atmosphere, then take out, use respectively
Second alcohol and water is cleaned 3-5 times, and 5h, and grind into powder are dried at 60 DEG C, obtains longan branch carbon dust；
（2）Longan branch carbon dust obtained by 1g is added in 150mL DMF solvents, through 100W ultrasonications
Gained suspension is transferred in the high-temperature high-pressure reaction kettle that 100mL polytetrafluoroethylene (PTFE) is liner after 2h, at 200 DEG C at hydro-thermal
Manage 10h；
（3）Room temperature is cooled to after having handled, is taken out, is filtered, gained filtrate is graphene quantum dot.
Embodiment 2
（1）7g longans branch is cleaned after drying, in 800 DEG C of high temperature cabonization 3h under argon atmosphere, then take out, use respectively
Second alcohol and water is cleaned 3-5 times, and 5h, and grind into powder are dried at 60 DEG C, obtains longan branch carbon dust；
（2）The nitric acid that 70mL mass concentrations are 68% is added in longan branch carbon dust obtained by 1g, using magnetic stirring apparatus at 80 DEG C
Filtered after lower oxidation processes 12h, then through 80 DEG C of drying, obtain 0.753g black powders；
（3）Gained black powder is added in 150mL DMF solvents, will after 100W ultrasonications 2h
Gained suspension is transferred in the high-temperature high-pressure reaction kettle that 100mL polytetrafluoroethylene (PTFE) is liner, the hydro-thermal process 10h at 200 DEG C；
（4）Room temperature is cooled to after having handled, is taken out, is filtered, gained filtrate is graphene quantum dot.
Embodiment 3
（1）6g longan pericarps are cleaned after drying, in 800 DEG C of high temperature cabonization 3h under argon atmosphere, then take out, use respectively
Second alcohol and water is cleaned 3-5 times, and 5h, and grind into powder are dried at 60 DEG C, obtains longan pericarp carbon dust；
（2）The nitric acid that 70mL mass concentrations are 65% is added in gained longan pericarp carbon dust, using magnetic stirring apparatus at 80 DEG C
Filtered after oxidation processes 12h, then through 80 DEG C of drying, obtain 0.841g black powders；
（3）Gained black powder is added in 150mL DMF solvents, will after 100W ultrasonications 2h
Gained suspension is transferred in the high-temperature high-pressure reaction kettle that 100mL polytetrafluoroethylene (PTFE) is liner, the hydro-thermal process 10h at 200 DEG C；
（4）Room temperature is cooled to after having handled, is taken out, is filtered, gained filtrate is graphene quantum dot.
The foregoing is only presently preferred embodiments of the present invention, all equivalent changes done according to scope of the present invention patent with
Modification, it should all belong to the covering scope of the present invention.
Claims (8)
1. a kind of prepare the method with fluorescent characteristic graphene quantum dot using waste biomass resource, it is characterised in that：Including
Following steps：
（1）Longan branch or longan pericarp are cleaned after drying, high temperature cabonization for a period of time, then takes out under protective atmosphere, cleaning
Dry, and grind into powder, obtain carbon dust；
（2）Filtered after gained carbon dust is added into nitric acid oxidation, then drying, obtain black powder；
（3）Gained black powder is added in DMF solvent, the gained suspension transfer after ultrasonication
Hydro-thermal process is carried out into high-temperature high-pressure reaction kettle；
（4）Room temperature is cooled to after having handled, is taken out, is filtered, gained filtrate is the graphene quantum dot with fluorescent characteristic.
2. the preparation method described in claim 1, it is characterised in that：Step（1）Middle protective atmosphere uses argon gas.
3. the preparation method described in claim 1, it is characterised in that：Step（1）Middle carburizing temperature is 600-800 DEG C, during carbonization
Between be 2-3h.
4. the preparation method described in claim 1, it is characterised in that：Step（2）The reaction temperature of middle nitric acid oxidation is 70-90
DEG C, in reaction time 12-24h, the mass concentration of nitric acid used is 65%-68%.
5. the preparation method described in claim 1, it is characterised in that：Step（2）Middle drying temperature is 70-90 DEG C.
6. the preparation method described in claim 1, it is characterised in that：Step（3）The power of middle ultrasonication is 100-400W, when
Between be 1 ~ 2h.
7. the preparation method described in claim 1, it is characterised in that：Step（3）The temperature of middle hydro-thermal process is 180 ~ 200 DEG C,
Processing time is 10-12h.
8. the preparation method described in claim 1, it is characterised in that：Filter in operation and use sand core funnel and 0.22 μm of micropore
Filter membrane is filtered.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109592672A (en) * | 2019-01-28 | 2019-04-09 | 三峡大学 | A method of graphene quantum dot is prepared using barley |
| CN112624093A (en) * | 2020-11-03 | 2021-04-09 | 中国科学技术大学 | Method for preparing graphene on large scale and application |
| CN116285968A (en) * | 2022-12-06 | 2023-06-23 | 延安大学 | Cerium-nitrogen co-doped biomass carbon quantum dot and preparation method and application thereof |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103553026A (en) * | 2013-10-14 | 2014-02-05 | 南京大学 | Method for preparing purple fluorescence reduced oxidized graphene quantum dot |
| CN104401981A (en) * | 2014-11-10 | 2015-03-11 | 朱熹 | Preparation method of nitrogen-containing oxidative graphene quantum dot capable of giving off fluorescence in three primary colors |
| CN105567230A (en) * | 2016-02-22 | 2016-05-11 | 桂林理工大学 | Nitrogen and sulfur-codoped graphene quantum dot and preparation method thereof |
-
2017
- 2017-11-20 CN CN201711153089.5A patent/CN107720734A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103553026A (en) * | 2013-10-14 | 2014-02-05 | 南京大学 | Method for preparing purple fluorescence reduced oxidized graphene quantum dot |
| CN104401981A (en) * | 2014-11-10 | 2015-03-11 | 朱熹 | Preparation method of nitrogen-containing oxidative graphene quantum dot capable of giving off fluorescence in three primary colors |
| CN105567230A (en) * | 2016-02-22 | 2016-05-11 | 桂林理工大学 | Nitrogen and sulfur-codoped graphene quantum dot and preparation method thereof |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109592672A (en) * | 2019-01-28 | 2019-04-09 | 三峡大学 | A method of graphene quantum dot is prepared using barley |
| CN112624093A (en) * | 2020-11-03 | 2021-04-09 | 中国科学技术大学 | Method for preparing graphene on large scale and application |
| CN116285968A (en) * | 2022-12-06 | 2023-06-23 | 延安大学 | Cerium-nitrogen co-doped biomass carbon quantum dot and preparation method and application thereof |
| CN116285968B (en) * | 2022-12-06 | 2024-03-15 | 延安大学 | Cerium-nitrogen co-doped biomass carbon quantum dot and preparation method and application thereof |
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Application publication date: 20180223 |