CN107903894A - A kind of method using cypress shell synthesis nitrogen-doped carbon quantum dot - Google Patents
A kind of method using cypress shell synthesis nitrogen-doped carbon quantum dot Download PDFInfo
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Abstract
A kind of method using cypress shell synthesis nitrogen-doped carbon quantum dot is to comprise the following steps to be made：Cypress shell powder is added in hydrothermal reaction kettle together with ammonium hydroxide, ultra-pure water and carries out hydro-thermal reaction, after hydro-thermal reaction, water heating kettle is taken out, natural cooling, then pour out the reaction solution in hydrothermal reaction kettle, then by centrifugation, filtering, freeze-drying and etc. up to nitrogen-doped carbon quanta point material.Raw material of the present invention has the advantages that environmentally protective, cheap and easy to get.Gained carbon quantum dot has preferable water solubility, high-purity, dispersiveness, size uniformity, high stability, high nitrogen content（Nitrogen content is up to 6.6%）Etc. series of advantages.The present invention prepare nitrogen-doped carbon quantum dot method have the advantages that it is of low cost, environmentally protective, easy to operate, low for equipment requirements, be convenient on a large scale prepare and industrialized production.
Description
Technical field
The invention belongs to field of material synthesis technology, and in particular to one kind is using cypress shell as Material synthesis nitrogen-doped carbon quantum dot
Method.
Background technology
Quantum dot is a kind of nano material of quasi-zero dimension, refers to that radius is less than the semiconductor nano of Exciton Bohr Radius
Body, has significant quantum confined effect.Common quantum dot refers to traditional semiconductor-quantum-point, by rare earth element II-VI
Formed with III-group Ⅴ element, such as CdS, CdSe, CdTe, ZnSe, ZnS.The toxicity of semiconductor-quantum-point is big, manufacturing cost is high,
Environmental pollution is serious, limits its practical application in various fields.
Carbon quantum dot（Carbon quantum dots, CQDs）It is the scientist by U.S.'s Clemson University in 2004
A kind of new fluorescence carbon nanomaterial manufactured first, is usually the carbon nanometer micro ball that size is less than 10 nm.With traditional half
Conductor quantum dot is compared, and carbon quantum dot does not contain heavy metal element, has low bio-toxicity.In addition, carbon quantum dot also has
The advantages that prominent fluorescence property, good optical stability, it is considered to be the potential material of alternative semiconductors fluorescent material.
The preparation method of carbon quantum dot can be mainly divided into two major classes at present：From top to bottom and bottom-to-top method.Before
Person be by large-sized carbon structure such as graphene, carbon nanotubes, carbon fiber, carbon black etc. using arc discharge, laser ablation, with
And the methods of electrochemical oxidation carries out broken cutting, the carbon quantum dot of small size is formed.The latter be then by using citrate,
Carbohydrate equimolecular is as presoma, by synthesizing carbon quantum dot the methods of chemical oxidation and heat treatment.However, mesh
The preceding above method there is the raw material used and experiment equipment costliness, preparation flow take, operating process is complicated or product yield is low
The defects of so that the manufacturing cost of carbon quantum dot remains high and is difficult to a large amount of samples are made, and limits the big rule of carbon quantum dot
Mould produces and application.Therefore, cheap and easy to get, environment friendly material is found, is prepared using simple efficient method rapid batch
Carbon quantum dot has highly important theory significance and actual application value.
Using biomass resource as raw material, energy conservation and environmental protection, and do not contain the toxic components such as heavy metal ion, be more advantageous to its
The application of carbon material preparation field.Biomass resource is widespread in nature, is cheap and easy to get, is inexhaustible, is nexhaustible,
Prepared by the green that biomass resource is used for carbon nanomaterial, that is, expanded the application field of biomass resource, and protect ring
Border, therefore have broad application prospects.At present, there are some reports that carbon quantum dot is prepared on biomass resource, such as
RSC Advances, 2012, 2: 8599-8601; Chemical Communications, 2012, 48: 8835-
8837; Materials Letters, 2012, 66: 222-224; Catalysis Science and Technology,
2013, 3: 1027-1035; Analytical Methods, 2013, 5: 3023-3027; Journal of
Materials Chemistry B, 2013, 1: 2868-2873; Environmental Science and
Technology Letters, 2014, 1: 87-91; Chemical Communications, 2015, 51: 16625-
16628; Journal of Materials Science, 2016, 51:8108-8115 etc..However, do not adopt also at present
It is the relevant report that raw material prepares carbon material with cypress shell.
The content of the invention
It is an object of the invention to provide a kind of method using cypress shell as Material synthesis nitrogen-doped carbon quantum dot.
The purpose of the present invention is what is realized by following technical measures：
A kind of method using cypress shell synthesis nitrogen-doped carbon quantum dot, it is characterised in that it is to comprise the following steps to be made：By cypress
Shell powder is added in hydrothermal reaction kettle and seals together with ammonium hydroxide, ultra-pure water, is then placed in baking oven or Muffle furnace, sets temperature
Spend for 180-250 DEG C carry out hydro-thermal reaction 5-30 it is small when；After hydro-thermal reaction, water heating kettle is taken out, naturally cools to 20 ~ 25
DEG C, then pour out the reaction solution in hydrothermal reaction kettle, then by centrifugation, filtering, freeze-drying and etc. up to N doping carbon amounts
Son point material.
Further, above-mentioned cypress shell powder need to be by 80 mesh sieves, and the ammoniacal liquor mass concentration is 25% ~ 28%, the cypress shell powder
End, ammonium hydroxide, mass/volume/volume ratio of ultra-pure water（g/ml/ml）For 1:5~10:10 ~ 50, the centrifugation step is using ladder
Spend what centrifugal process carried out, place reaction liquid into low speed centrifuge 3000 ~ 5000r/min first and centrifuge 5 ~ 30 minutes, collect from
Supernatant liquor in heart pipe, is placed in supercentrifuge 10000 ~ 16000r/min and centrifuges 5 ~ 30 minutes, collect again from
Supernatant liquor in heart pipe, to obtain the final product.
Further, above-mentioned filtering is by the supernatant after centrifugation, first with 0.45 μm of cellulose mixture fat water system micropore
Membrane filtration, collects filtrate, then is filtered with 0.22 μm of cellulose mixture fat water system miillpore filter, filtrate is collected, finally with 0.1
μm cellulose mixture fat water system miillpore filter filtering, collect filtrate, to obtain the final product.
Further, above-mentioned freeze-drying is that precooling 8 ~ 15 is small in freezer compartment of refrigerator by the aqueous solution of carbon quantum dot
When, the freezing liquid for the carbon quantum dot freezed；Freeze drier is opened, when -60 DEG C of precoolings 3 ~ 6 are small, then add and waits to do
Dry carbon quantum dot freezing liquid, starts to vacuumize freeze-drying, and vacuum is below 20Pa, and freeze-drying temperature is -50 ~ -59
DEG C, sublimation drying for 28 ~ 53 it is small when, by the further 50-70 in vacuum drying oven of the product after vacuum freeze drying
DEG C drying 45-60 it is small when, up to nitrogen-doped carbon quantum dot.
The beneficial effects of the present invention are：
A kind of method using cypress shell synthesis nitrogen-doped carbon quantum dot of the present invention, used raw material has environmentally protective, inexpensive
The advantages of being easy to get.In preparation process of the present invention, it is necessary to by reasonably select raw material, appropriate design raw material proportioning, accurately
Control high temperature and pressure hydro-thermal reaction parameter, filtered using level, gradient centrifugation, multiprogramization drying the methods of and technology hand
Section, just can ensure that and carbon quantum dot material in high yield is prepared by raw material of cypress shell, if controlling bad carbon quantum dot preparation
Full-flow process, on the one hand will cause to cannot get carbon quantum dot material, on the other hand can cause carbon quantum dot yield occur
Too low phenomenon.Gained carbon quantum dot of the invention has preferable water solubility, high-purity, good dispersion, size uniformity, stability
High, nitrogen content height（Nitrogen content is up to 6.6%）, the series of advantages such as yield height.The present invention prepare carbon quantum dot method have into
The advantages that this is cheap, environmentally protective, easy to operate, low for equipment requirements, is convenient for preparation and industrialized production on a large scale.
Brief description of the drawings
Fig. 1 is the transmission electron microscope picture of 1 gained nitrogen-doped carbon quantum dot of embodiment.
Fig. 2 is the transmission electron microscope picture of 2 gained nitrogen-doped carbon quantum dot of embodiment.
Fig. 3 is the transmission electron microscope picture of 3 gained nitrogen-doped carbon quantum dot of embodiment.
Fig. 4 is the transmission electron microscope picture of the carbon-nitrogen doped quantum dot of the gained of embodiment 4.
A kind of process flow charts using cypress shell synthesis nitrogen-doped carbon quantum dot of Fig. 5.
Embodiment
The present invention is specifically described below by embodiment, it is necessary to which indicated herein is that following embodiments are only used
It is further described in the present invention, it is impossible to limiting the scope of the invention is interpreted as, without departing substantially from spirit of the invention
In the case of essence, the modifications or substitutions made to the method for the present invention, step or condition belong to the scope of the present invention.
Embodiment 1
By the cleaning of cypress shell, drying, 80 mesh sieves crushed using Universalpulverizer, collect cypress shell powder, weigh 3.0 grams of cypress shell powder
The ammonium hydroxide and 80 milliliters of ultra-pure waters that end, 15 milliliters of mass concentrations are 25%, are added in water heating kettle, in an oven 220 DEG C of hydro-thermals 12
Hour, after hydro-thermal reaction, water heating kettle is taken out, naturally cools to 25 DEG C, then pours out the reaction solution in hydrothermal reaction kettle；
Separated 30 minutes by the rotating speed low-speed centrifugal of 3000r/min, collect supernatant liquor, be further continued for the rotating speed using 16000r/min
It is centrifuged at a high speed 5 minutes, collects supernatant liquor again；0.45 micron, 0.22 micron, 0.1 micron of mixing fibre are used successively
The plain fat of dimension（Water system）Miillpore filter carries out Purification by filtration, obtains carbon quantum dot solution.Carbon quantum dot solution is sampled and is positioned over 4
Cord blood in DEG C refrigerator, setting-out are observed for 1 year, it is found that carbon quantum dot solution still never degenerates, and illustrates gained carbon quantum dot with excellent
Different water solubility, is capable of the scattered of stable and uniform in water.
Then when by carbon quantum dot solution, precooling 8 is small in refrigerator, the freezing liquid for the carbon quantum dot freezed；Open
Freeze drier, when -60 DEG C of precoolings 3 are small, then adds carbon quantum dot freezing liquid to be dried, starts to vacuumize to freeze and does
Dry, vacuum is below 20Pa, and freeze-drying temperature is -50 DEG C, when sublimation drying is 53 small.It will be done by vacuum refrigeration
Product after dry obtains nitrogen-doped carbon quanta point material when further 50 DEG C of drying 60 are small in vacuum drying oven.
The transmission electron microscope picture of gained carbon quantum dot is as shown in Figure 1.As can be seen that substantial amounts of carbon quantum dot material is with non-
Often good dispersiveness, does not have agglomeration；Also illustrate gained carbon quantum dot tool without the presence for finding impurity in the product
There is very high purity；The size of gained carbon quantum dot is also very homogeneous, and average grain diameter is 2.2 nanometers；Gained carbon quantum dot material
With high nitrogen content, nitrogen content 5.5%.It can be seen from the above that present invention gained carbon quantum dot is with preferable water-soluble, high-purity
The series of advantages such as degree, dispersiveness, size uniformity, high stability, high nitrogen content.
Embodiment 2
By the cleaning of cypress shell, drying, 80 mesh sieves crushed using Universalpulverizer, collect cypress shell powder, weigh 3.0 grams of cypress shell powder
The ammonium hydroxide and 85 milliliters of ultra-pure waters that end, 30 milliliters of mass concentrations are 28%, are added in water heating kettle, in an oven 160 DEG C of hydro-thermals 48
Hour, after hydro-thermal reaction, water heating kettle is taken out, naturally cools to 25 DEG C, then pours out the reaction solution in hydrothermal reaction kettle；
Separated 25 minutes by the rotating speed low-speed centrifugal of 3500r/min, collect supernatant liquor, be further continued for the rotating speed using 14000r/min
It is centrifuged at a high speed 8 minutes, collects supernatant liquor again；0.45 micron, 0.22 micron, 0.1 micron of mixing fibre are used successively
The plain fat of dimension（Water system）Miillpore filter carries out Purification by filtration, obtains carbon quantum dot solution.Carbon quantum dot solution is sampled and is positioned over 4
Cord blood in DEG C refrigerator, setting-out are observed for 1 year, it is found that carbon quantum dot solution still never degenerates, and illustrates gained carbon quantum dot with excellent
Different water solubility, is capable of the scattered of stable and uniform in water.
Then when by carbon quantum dot solution, precooling 15 is small in refrigerator, the freezing liquid for the carbon quantum dot freezed；Open
Freeze drier is opened, when -60 DEG C of precoolings 3 are small, make ability of the cold-trap with abundant adsorption moisture, then adds carbon to be dried
Quantum dot freezing liquid, starts to vacuumize freeze-drying, and vacuum is below 20Pa, and freeze-drying temperature is -53 DEG C, and freezing is dry
When the dry time is 48 small.When by the product after vacuum freeze drying, further 70 DEG C of drying 45 are small in vacuum drying oven, obtain
To nitrogen-doped carbon quanta point material.
The transmission electron microscope picture of gained carbon quantum dot is as shown in Figure 2.As can be seen that substantial amounts of carbon quantum dot material is with non-
Often good dispersiveness, does not have agglomeration；Also illustrate gained carbon quantum dot tool without the presence for finding impurity in the product
There is very high purity；The size of gained carbon quantum dot is also very homogeneous, and average grain diameter is 2.0 nanometers；Gained carbon quantum dot material
With high nitrogen content, nitrogen content 6.6%.It can be seen from the above that present invention gained carbon quantum dot is with preferable water-soluble, high-purity
The series of advantages such as degree, dispersiveness, size uniformity, high stability, high nitrogen content.
Embodiment 3
By the cleaning of cypress shell, drying, 80 mesh sieves crushed using Universalpulverizer, collect cypress shell powder, weigh 5.0 grams of cypress shell powder
The ammonium hydroxide and 70 milliliters of ultra-pure waters that end, 30 milliliters of mass concentrations are 27%, are added in water heating kettle, in an oven 200 DEG C of hydro-thermals 24
Hour, after hydro-thermal reaction, water heating kettle is taken out, naturally cools to 23 DEG C, then pours out the reaction solution in hydrothermal reaction kettle；
Separated 15 minutes by the rotating speed low-speed centrifugal of 4000r/min, collect supernatant liquor, be further continued for the rotating speed using 12000r/min
It is centrifuged at a high speed 15 minutes, collects supernatant liquor again；0.45 micron, 0.22 micron, 0.1 micron of mixing fibre are used successively
The plain fat of dimension（Water system）Miillpore filter filter membrane carries out Purification by filtration, obtains carbon quantum dot solution.Carbon quantum dot solution is sampled and is put
Cord blood in 4 DEG C of refrigerators is placed in, setting-out is observed for 1 year, it is found that carbon quantum dot solution still never degenerates, and illustrates gained carbon quantum dot
With excellent water solubility, it is capable of the scattered of stable and uniform in water.
Then when by carbon quantum dot solution, precooling 12 is small in refrigerator, the freezing liquid for the carbon quantum dot freezed；Open
Freeze drier is opened, when -60 DEG C of precoolings 5 are small, then adds carbon quantum dot freezing liquid to be dried, starts to vacuumize to freeze and does
Dry, vacuum is below 20Pa, and freeze-drying temperature is -56 DEG C, when sublimation drying is 36 small.It will be done by vacuum refrigeration
Product after dry obtains nitrogen-doped carbon quanta point material when further 60 DEG C of drying 50 are small in vacuum drying oven.
The transmission electron microscope picture of gained carbon quantum dot is as shown in Figure 3.As can be seen that substantial amounts of carbon quantum dot material is with non-
Often good dispersiveness, does not have agglomeration；Also illustrate gained carbon quantum dot tool without the presence for finding impurity in the product
There is very high purity；The size of gained carbon quantum dot is also very homogeneous, and average grain diameter is 2.1 nanometers；Gained carbon quantum dot material
With high nitrogen content, nitrogen content 6.1%.It can be seen from the above that present invention gained carbon quantum dot is with preferable water-soluble, high-purity
The series of advantages such as degree, dispersiveness, size uniformity, high stability, high nitrogen content.
Embodiment 4
By the cleaning of cypress shell, drying, 80 mesh sieves crushed using Universalpulverizer, collect cypress shell powder, weigh 6.0 grams of cypress shell powder
End, 35 milliliters of mass concentrations are 26% ammonium hydroxide and 80 milliliters of ultra-pure waters, are added in water heating kettle, 250 DEG C of hydro-thermals 5 in Muffle furnace
Hour, after hydro-thermal reaction, water heating kettle is taken out, naturally cools to 20-25 DEG C, then pours out the reaction in hydrothermal reaction kettle
Liquid；Separated 5 minutes by the rotating speed low-speed centrifugal of 5000r/min, collect supernatant liquor, be further continued for turning using 10000r/min
Speed is centrifuged at a high speed 30 minutes, collects supernatant liquor again；0.45 micron, 0.22 micron, 0.1 micron of mixing are used successively
Cellulose ester（Water system）Miillpore filter carries out Purification by filtration, obtains carbon quantum dot solution.Placement is sampled to carbon quantum dot solution
The Cord blood in 4 DEG C of refrigerators, setting-out are observed for 1 year, it is found that carbon quantum dot solution still never degenerates, and illustrate gained carbon quantum dot tool
There is excellent water solubility, be capable of the scattered of stable and uniform in water.
Then when by carbon quantum dot solution, precooling 10 is small in refrigerator, the freezing liquid for the carbon quantum dot freezed；Open
Freeze drier is opened, when -60 DEG C of precoolings 5 are small, then adds carbon quantum dot freezing liquid to be dried, starts to vacuumize to freeze and does
Dry, vacuum is below 20Pa, and freeze-drying temperature is -59 DEG C, when sublimation drying is 28 small.It will be done by vacuum refrigeration
Product after dry obtains nitrogen-doped carbon quanta point material when further 65 DEG C of drying 50 are small in vacuum drying oven.
The transmission electron microscope picture of gained carbon quantum dot is as shown in Figure 4.As can be seen that substantial amounts of carbon quantum dot material is with non-
Often good dispersiveness, does not have agglomeration；Also illustrate gained carbon quantum dot tool without the presence for finding impurity in the product
There is very high purity；The size of gained carbon quantum dot is also very homogeneous, and average grain diameter is 2.1 nanometers；Gained carbon quantum dot material
With high nitrogen content, nitrogen content 5.0%.It can be seen from the above that present invention gained carbon quantum dot is with preferable water-soluble, high-purity
The series of advantages such as degree, dispersiveness, size uniformity, high stability, high nitrogen content.
Claims (4)
- A kind of 1. method using cypress shell synthesis nitrogen-doped carbon quantum dot, it is characterised in that it is to comprise the following steps to be made：Will Cypress shell powder is added in hydrothermal reaction kettle and seals together with ammonium hydroxide, ultra-pure water, is then placed in baking oven or Muffle furnace, sets When temperature is 180-250 DEG C of progress hydro-thermal reaction 5-30 small；After hydro-thermal reaction, water heating kettle is taken out, naturally cool to 20 ~ 25 DEG C, then pour out the reaction solution in hydrothermal reaction kettle, then by centrifugation, filtering, freeze-drying and etc. up to nitrogen-doped carbon Quanta point material.
- A kind of 2. method using cypress shell synthesis nitrogen-doped carbon quantum dot as claimed in claim 1, it is characterised in that above-mentioned cypress Shell powder need to be by 80 mesh sieves, and the ammoniacal liquor mass concentration is 25% ~ 28%, the cypress shell powder, ammonium hydroxide, ultra-pure water quality/ Volume/volume ratio（g/ml/ml）For 1:5~10:10 ~ 50, the centrifugation step is carried out using gradient centrifugation, first will Reaction solution is placed in 3000 ~ 5000r/min in low speed centrifuge and centrifuges 5 ~ 30 minutes, the supernatant liquor in centrifuge tube is collected, by it Be placed in 10000 ~ 16000r/min in supercentrifuge to centrifuge 5 ~ 30 minutes, collect the supernatant liquor in centrifuge tube again, to obtain the final product.
- 3. a kind of method with cypress shell synthesis nitrogen-doped carbon quantum dot as claimed in claim 1, it is characterised in that above-mentioned filtering is By the supernatant after centrifugation, first filtered with 0.45 μm of cellulose mixture fat water system miillpore filter, collect filtrate, then with 0.22 μm Cellulose mixture fat water system miillpore filter filtering, collect filtrate, finally with 0.1 μm of cellulose mixture fat water system miillpore filter Filtering, collects filtrate, to obtain the final product.
- 4. a kind of method with cypress shell synthesis nitrogen-doped carbon quantum dot as claimed in claim 1, it is characterised in that above-mentioned freezing is done It is dry be by the aqueous solution of carbon quantum dot precooling 8 ~ 15 is small in freezer compartment of refrigerator when, the freezing for the carbon quantum dot freezed Liquid；Freeze drier is opened, when -60 DEG C of precoolings 3 ~ 6 are small, then adds carbon quantum dot freezing liquid to be dried, starts to take out true Vacuum freecing-dry, vacuum are below 20Pa, and freeze-drying temperature is -50 ~ -59 DEG C, when sublimation drying is 28 ~ 53 small, When by the product after vacuum freeze drying, further 50-70 DEG C of drying 45-60 is small in vacuum drying oven, up to nitrogen-doped carbon Quantum dot.
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| CN108975309A (en) * | 2018-09-03 | 2018-12-11 | 南京林业大学 | The method and its application of Water-soluble carbon quantum dot and fluorescent ink are prepared using cyanobacteria |
| CN109336087A (en) * | 2018-12-26 | 2019-02-15 | 南京林业大学 | Cork oak acorn-cup base carbon quantum dot and its application on fluorescent ink are prepared using cork oak acorn-cup |
| CN109504377A (en) * | 2018-12-26 | 2019-03-22 | 南京林业大学 | Cork oak shell base carbon quantum dot and its application on fluorescent ink are prepared using cork oak shell |
| CN109593524A (en) * | 2018-12-26 | 2019-04-09 | 南京林业大学 | Use radiation loose wire preparation Water-soluble carbon quantum dot and the method and its application of fluorescent ink |
| CN111650172A (en) * | 2020-07-17 | 2020-09-11 | 安徽大学 | Qualitative and quantitative detection method for rare earth elements based on carbon quantum dot fluorescence mechanism |
| CN112552904A (en) * | 2020-12-17 | 2021-03-26 | 中国标准化研究院 | Novel fluorescent carbon quantum dot material and synthesis method and application thereof |
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| CN108975309A (en) * | 2018-09-03 | 2018-12-11 | 南京林业大学 | The method and its application of Water-soluble carbon quantum dot and fluorescent ink are prepared using cyanobacteria |
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| CN109593524A (en) * | 2018-12-26 | 2019-04-09 | 南京林业大学 | Use radiation loose wire preparation Water-soluble carbon quantum dot and the method and its application of fluorescent ink |
| CN111650172A (en) * | 2020-07-17 | 2020-09-11 | 安徽大学 | Qualitative and quantitative detection method for rare earth elements based on carbon quantum dot fluorescence mechanism |
| CN112552904A (en) * | 2020-12-17 | 2021-03-26 | 中国标准化研究院 | Novel fluorescent carbon quantum dot material and synthesis method and application thereof |
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Application publication date: 20180413 |