CN108101022A - A kind of method that carbon quantum dot is prepared using fennel seeds as raw material - Google Patents
A kind of method that carbon quantum dot is prepared using fennel seeds as raw material Download PDFInfo
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- CN108101022A CN108101022A CN201711448330.7A CN201711448330A CN108101022A CN 108101022 A CN108101022 A CN 108101022A CN 201711448330 A CN201711448330 A CN 201711448330A CN 108101022 A CN108101022 A CN 108101022A
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Abstract
A kind of method using fennel seeds as raw material preparation carbon quantum dot is to be added to fennel seeds in hydrothermal reaction kettle together with ultra-pure water to carry out hydro-thermal reaction, after hydro-thermal reaction, naturally cool to 20 25 DEG C, then pour out the reaction solution in hydrothermal reaction kettle, then through centrifuge, filter, be freeze-dried and etc. obtain carbon quantum dot material.The raw material of the present invention for preparing is environmentally protective, cheap and easy to get.Used hydrothermal synthesis of carbon quanta point material have many advantages, such as it is green, easy, quick, efficient, be convenient on a large scale prepare and industrialized production.Prepared carbon quantum dot material has the series of advantages such as preferable water solubility, high-purity, dispersiveness, size uniformity, high stability, has huge application potential in fields such as biomarker, bio-imaging, drug conveying, analysis detection, sensing, catalysis, the energy and environmental protection.
Description
Technical field
The invention belongs to field of material synthesis technology, and in particular to a kind of side that carbon quantum dot is prepared using fennel seeds as raw material
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
It is 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 many 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 for the first time 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 electric arc electric discharge, laser ablation, with
And the methods of electrochemical oxidation, carries out broken cutting, forms the carbon quantum dot of small size.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 that 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, environmental-friendly raw material are found, utilize the method rapid batch system being simple and efficient
Standby 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,
Biomass resource for the green of carbon nanomaterial is prepared, that is, has expanded the application field of biomass resource, and has protected ring
Border, therefore have broad application prospects.At present, some on biomass resource prepare carbon quantum dot reports, 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 have using fennel seeds also at present
The relevant report of the new carbons such as carbon quantum dot is prepared for raw material.
The content of the invention
It is an object of the invention to provide a kind of methods that carbon quantum dot is prepared using fennel seeds as raw material.
The purpose of the present invention is what is realized by following technical measures：
A kind of method that carbon quantum dot is prepared using fennel seeds as raw material, which is characterized in that it is to comprise the following steps to be made：It will be small
Fennel is added in hydrothermal reaction kettle and is sealed together with ultra-pure water, is then placed in baking oven or Muffle furnace, and set temperature is
When 150-250 DEG C of progress hydro-thermal reaction 4-48 is small, 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 through centrifuge, filter, be freeze-dried and etc. obtain carbon quantum dot material.
Further, the mass volume ratio of above-mentioned fennel seeds and ultra-pure water（g/ml）For 1:10 ~ 60, the centrifugation step is to adopt
It is carried out with gradient centrifugation, places reaction liquid into 3000 ~ 5000r/min in low speed centrifuge first and centrifuge 5 ~ 30 minutes, receive
Collect the supernatant liquor in centrifuge tube, place it in 10000 ~ 16000r/min in supercentrifuge and centrifuge 5 ~ 30 minutes, receive again
Collect centrifuge tube in supernatant liquor to get.
Further, above-mentioned filtering is by the supernatant after centrifugation, first with 0.45 μm of cellulose mixture fat water system micropore
Membrane filtration is collected 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 get.
Further, above-mentioned freeze-drying is that precooling 6 ~ 13 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 2 ~ 5 are small, then add in and waits to do
Dry carbon quantum dot freezing liquid starts to vacuumize freeze-drying, and vacuum degree is below 20Pa, and freeze-drying temperature is -52 ~ -59
DEG C, when sublimation drying is 26 ~ 50 small, by the product after vacuum freeze drying further in vacuum drying oven, vacuum
Below degree -0.1MPa, to get carbon quantum dot when 65-75 DEG C of drying 40-53 of temperature is small.
The beneficial effects of the present invention are：
A kind of method that carbon quantum dot is prepared using fennel seeds as raw material of the present invention, the used raw material for preparing is environmentally protective, inexpensive
It is easy to get.Used hydrothermal synthesis of carbon quanta point material has many advantages, such as green, easy, quick, efficient, is convenient for advising greatly
The preparation of mould and industrialized production., it is necessary to raw material by reasonably selecting raw material, appropriate design in preparation process of the present invention
Proportioning, it is accurate to control high temperature and pressure hydro-thermal reaction parameter, filtered using level, the drying of gradient centrifugation, multiprogramization the methods of and
Technology means just can ensure that and carbon quantum dot material in high yield be prepared by raw material of fennel seeds, if control is bad
Full-flow process prepared by carbon quantum dot, on the one hand will cause to cannot get carbon quantum dot material, on the other hand can cause to occur
The phenomenon that carbon quantum dot yield is too low.Carbon quantum dot material prepared by the present invention has preferable water solubility, high-purity, disperses
Property good, size uniformity, high stability, the series of advantages such as in high yield, in biomarker, bio-imaging, drug conveying, analysis
There is huge application potential in the fields such as detection, sensing, catalysis, the energy and environmental protection.
Description of the drawings
Fig. 1 is the transmission electron microscope picture of 1 gained carbon quantum dot of embodiment.
Fig. 2 is the transmission electron microscope picture of 2 gained carbon quantum dot of embodiment.
Fig. 3 is the transmission electron microscope picture of 3 gained carbon quantum dot of embodiment.
Fig. 4 is the transmission electron microscope picture of 4 gained carbon quantum dot of embodiment.
Fig. 5 is a kind of process flow chart that carbon quantum dot is prepared using fennel seeds as raw material.
Specific embodiment
The present invention is specifically described below by embodiment, it is necessary to which indicated herein is that following embodiment is 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, to the modifications or substitutions that the method for the present invention, step or condition are made, all belong to the scope of the present invention.
Embodiment 1
Fennel seeds are cleaned, are dried, weighs 1.0 grams of dry fennel seeds and 55 milliliters of ultra-pure waters, is added in water heating kettle, drying
When 180 DEG C of hydro-thermals 12 are small in case, after hydro-thermal reaction, water heating kettle is taken out, naturally cools to 20 DEG C, it is anti-then to pour out hydro-thermal
Answer the reaction solution in kettle；It is separated 30 minutes by the rotating speed low-speed centrifugal of 3000r/min, collects supernatant liquor, be further continued for using
The rotating speed of 16000r/min is centrifuged at a high speed 5 minutes, collects supernatant liquor again；Successively using 0.45 micron, 0.22 micron,
0.1 micron of cellulose mixture fat（Water system）Miillpore filter is filtered purifying, obtains carbon quantum dot solution.To carbon quantum dot solution
It is sampled and is positioned over Cord blood in 4 DEG C of refrigerators, setting-out is observed for 1 year, it is found that carbon quantum dot solution still never degenerates, illustrated institute
Obtaining carbon quantum dot has excellent water solubility, is capable of the scattered of stable and uniform in water.
Then when by carbon quantum dot solution, precooling 6 is small in refrigerator, the freezing liquid for the carbon quantum dot freezed；It opens
Freeze drier when -60 DEG C of precoolings 2 are small, then adds in carbon quantum dot freezing liquid to be dried, starts to vacuumize to freeze and do
Dry, vacuum degree is below 20Pa, and freeze-drying temperature is -52 DEG C, when sublimation drying is 50 small, obtains carbon quantum dot material
Material, then by the product after vacuum freeze drying further in vacuum drying oven when 65 DEG C of drying 53 of temperature are small.
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 of discovery 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.It can be seen that institute of the present invention
Obtaining carbon quantum dot has the series of advantages such as preferable water solubility, high-purity, dispersiveness, size uniformity, high stability.
Embodiment 2
Fennel seeds are cleaned, are dried, weighs 2.5 grams of dry fennel seeds and 70 milliliters of ultra-pure waters, is added in water heating kettle, drying
When 150 DEG C of hydro-thermals 48 are small in case, after hydro-thermal reaction, water heating kettle is taken out, naturally cools to 25 DEG C, it is anti-then to pour out hydro-thermal
Answer the reaction solution in kettle；It is separated 25 minutes by the rotating speed low-speed centrifugal of 3500r/min, collects supernatant liquor, be further continued for using
The rotating speed of 14000r/min is centrifuged at a high speed 8 minutes, collects supernatant liquor again；Successively using 0.45 micron, 0.22 micron,
0.1 micron of cellulose mixture fat（Water system）Miillpore filter is filtered purifying, obtains carbon quantum dot solution.To carbon quantum dot solution
It is sampled and is positioned over Cord blood in 4 DEG C of refrigerators, setting-out is observed for 1 year, it is found that carbon quantum dot solution still never degenerates, illustrated institute
Obtaining carbon quantum dot has excellent water solubility, is capable of the scattered of stable and uniform in water.
Then when by carbon quantum dot solution, precooling 13 is small in refrigerator, the freezing liquid for the carbon quantum dot freezed；It opens
Freeze drier is opened, when -60 DEG C of precoolings 5 are small, then adds in carbon quantum dot freezing liquid to be dried, starts to vacuumize to freeze and do
Dry, vacuum degree is below 20Pa, and freeze-drying temperature is -53 DEG C, when sublimation drying is 40 small, will pass through vacuum refrigeration
Dried product further in vacuum drying oven, when 65 DEG C of drying 40 are small, obtains carbon quantum dot 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 of discovery 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.It can be seen that institute of the present invention
Obtaining carbon quantum dot has the series of advantages such as preferable water solubility, high-purity, dispersiveness, size uniformity, high stability.
Embodiment 3
Fennel seeds are cleaned, are dried, weighs 3.0 grams of dry fennel seeds and 70 milliliters of ultra-pure waters, is added in water heating kettle, drying
When 210 DEG C of hydro-thermals 10 are small in case, after hydro-thermal reaction, water heating kettle is taken out, naturally cools to 22 DEG C, it is anti-then to pour out hydro-thermal
Answer the reaction solution in kettle；It is separated 15 minutes by the rotating speed low-speed centrifugal of 4000r/min, collects supernatant liquor, be further continued for using
The rotating speed of 12000r/min is centrifuged at a high speed 15 minutes, collects supernatant liquor again；Successively using 0.45 micron, it is 0.22 micro-
Rice, 0.1 micron of cellulose mixture fat（Water system）Miillpore filter filter membrane is filtered purifying, obtains carbon quantum dot solution.To carbon amounts
Son point solution, which is sampled, is positioned over Cord blood in 4 DEG C of refrigerators, and setting-out is observed for 1 year, it is found that carbon quantum dot solution is still constant
Matter illustrates that gained carbon quantum dot has excellent water solubility, is 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；It opens
Freeze drier is opened, when -60 DEG C of precoolings 3 are small, then adds in carbon quantum dot freezing liquid to be dried, starts to vacuumize to freeze and do
Dry, vacuum degree is below 20Pa, and freeze-drying temperature is -55 DEG C, when sublimation drying is 36 small, will be done by vacuum refrigeration
Product after dry obtains nitrogen-doped carbon quanta point material when further 70 DEG C of drying 45 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 of discovery 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.It can be seen that institute of the present invention
Obtaining carbon quantum dot has the series of advantages such as preferable water solubility, high-purity, dispersiveness, size uniformity, high stability.
Embodiment 4
Fennel seeds are cleaned, are dried, weighs 3.5 grams of dry fennel seeds and 75 milliliters of ultra-pure waters, is added in water heating kettle, drying
When 250 DEG C of hydro-thermals 4 are small in case, after hydro-thermal reaction, water heating kettle is taken out, naturally cools to 23 DEG C, it is anti-then to pour out hydro-thermal
Answer the reaction solution in kettle；It is separated 5 minutes by the rotating speed low-speed centrifugal of 5000r/min, collects supernatant liquor, be further continued for using
The rotating speed of 10000r/min is centrifuged at a high speed 30 minutes, collects supernatant liquor again；Successively using 0.45 micron, it is 0.22 micro-
Rice, 0.1 micron of cellulose mixture fat（Water system）Miillpore filter filter membrane is filtered purifying, obtains carbon quantum dot solution.To carbon amounts
Son point solution, which is sampled, is positioned over Cord blood in 4 DEG C of refrigerators, and setting-out is observed for 1 year, it is found that carbon quantum dot solution is still constant
Matter illustrates that gained carbon quantum dot has excellent water solubility, is capable of the scattered of stable and uniform in water.
Then when by carbon quantum dot solution, precooling 11 is small in refrigerator, the freezing liquid for the carbon quantum dot freezed；It opens
Freeze drier is opened, when -60 DEG C of precoolings 4 are small, then adds in carbon quantum dot freezing liquid to be dried, starts to vacuumize to freeze and do
Dry, vacuum degree is below 20Pa, and freeze-drying temperature is -59 DEG C, when sublimation drying is 26 small.It will be done by vacuum refrigeration
Product after dry obtains nitrogen-doped carbon quanta point material when further 72 DEG C of drying 43 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 of discovery 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.It can be seen that institute of the present invention
Obtaining carbon quantum dot has the series of advantages such as preferable water solubility, high-purity, dispersiveness, size uniformity, high stability.
Claims (4)
- A kind of 1. method that carbon quantum dot is prepared using fennel seeds as raw material, which is characterized in that it is to include getting off step to be made：It will Fennel seeds are added in hydrothermal reaction kettle and are sealed together with ultra-pure water, are then placed in baking oven or Muffle furnace, and set temperature is When 150-250 DEG C of progress hydro-thermal reaction 4-48 is small, 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 through centrifuge, filter, be freeze-dried and etc. obtain carbon quantum dot material.
- 2. a kind of method that carbon quantum dot is prepared using fennel seeds as raw material as described in claim 1, which is characterized in that above-mentioned small The mass volume ratio of fennel and ultra-pure water（g/ml）For 1:10 ~ 60, the centrifugation step is carried out using gradient centrifugation, first It first places reaction liquid into 3000 ~ 5000r/min in low speed centrifuge to centrifuge 5 ~ 30 minutes, collects the supernatant liquor in centrifuge tube, It places it in 10000 ~ 16000r/min in supercentrifuge to centrifuge 5 ~ 30 minutes, collects the supernatant liquor in centrifuge tube again, To obtain the final product.
- A kind of 3. method that carbon quantum dot is prepared using fennel seeds as raw material as described in claim 1, which is characterized in that above-mentioned mistake Filter is by the supernatant after centrifugation, is first filtered with 0.45 μm of cellulose mixture fat water system miillpore filter, collects filtrate, then use 0.22 μm of cellulose mixture fat water system miillpore filter filtering, collects filtrate, finally micro- with 0.1 μm of cellulose mixture fat water system Hole membrane filtration, collect filtrate to get.
- 4. a kind of method that carbon quantum dot is prepared using fennel seeds as raw material as described in claim 1, which is characterized in that above-mentioned cold It is lyophilized it is dry be by the aqueous solution of carbon quantum dot precooling 6 ~ 13 is small in freezer compartment of refrigerator when, the carbon quantum dot freezed it is cold Freeze liquid；Freeze drier is opened, when -60 DEG C of precoolings 2 ~ 5 are small, carbon quantum dot freezing liquid to be dried then added in, starts to take out Vacuum freeze drying, vacuum degree are below 20Pa, and freeze-drying temperature is -52 ~ -59 DEG C, and sublimation drying is small for 26 ~ 50 When, by the product after vacuum freeze drying further in vacuum drying oven, below vacuum degree -0.1MPa, 65-75 DEG C of temperature To get carbon quantum dot when drying 40-53 is small.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111204737A (en) * | 2020-03-12 | 2020-05-29 | 新余学院 | Preparation method of carbon quantum dots |
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| CN104531147A (en) * | 2014-12-30 | 2015-04-22 | 太原理工大学 | Method for quickly preparing carbon quantum dots emitting blue light and carbon quantum dots emitting green light |
| CN105152157A (en) * | 2015-09-15 | 2015-12-16 | 郑州大学 | Method for preparing solid light-emitting carbon point |
| CN107043097A (en) * | 2017-01-20 | 2017-08-15 | 西南大学 | Method and its carbon point and the application of carbon point are prepared by mushroom |
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2017
- 2017-12-27 CN CN201711448330.7A patent/CN108101022A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104531147A (en) * | 2014-12-30 | 2015-04-22 | 太原理工大学 | Method for quickly preparing carbon quantum dots emitting blue light and carbon quantum dots emitting green light |
| CN105152157A (en) * | 2015-09-15 | 2015-12-16 | 郑州大学 | Method for preparing solid light-emitting carbon point |
| CN107043097A (en) * | 2017-01-20 | 2017-08-15 | 西南大学 | Method and its carbon point and the application of carbon point are prepared by mushroom |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111204737A (en) * | 2020-03-12 | 2020-05-29 | 新余学院 | Preparation method of carbon quantum dots |
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Application publication date: 20180601 |