CN107128897A - A kind of carbon quantum dot and preparation method thereof - Google Patents
A kind of carbon quantum dot and preparation method thereof Download PDFInfo
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- CN107128897A CN107128897A CN201710335432.1A CN201710335432A CN107128897A CN 107128897 A CN107128897 A CN 107128897A CN 201710335432 A CN201710335432 A CN 201710335432A CN 107128897 A CN107128897 A CN 107128897A
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- quantum dot
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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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- C01P2004/04—Particle morphology depicted by an image obtained by TEM, STEM, STM or AFM
Abstract
The present invention relates to a kind of carbon quantum dot and preparation method thereof.Its technical scheme is：By catalyst: the mass ratio of isobutylene maleic acid anhydride copolymer is (0.00045 ~ 0.015): 1 dispensing, mixing, by gained mixture: the mass ratio of deionized water is 1: (8 ~ 12) dispensing, mixing, 5 ~ 15min of magnetic agitation, is dried, and mixed powder is made.The mixed powder is placed in crucible, 0.5 ~ 3h is incubated under the conditions of argon gas atmosphere and 250 ~ 700 DEG C, carbon quantum dot presoma is made.By the carbon quantum dot presoma: polyethylene glycol: the mass ratio of deionized water is 3: (1 ~ 2): (8 ~ 12), the carbon quantum dot presoma and the polyethylene glycol are added in deionized water, mixing, centrifugation, remove supernatant, sediment is dried, carbon quantum dot is made.The present invention has that technique is simple, reaction condition gentle, the characteristics of and production cost low not high to equipment requirement；Prepared carbon quantum dot good dispersion, shape is homogeneous and particle diameter is small, there is preferable application prospect.
Description
Technical field
The invention belongs to technology of quantum dots field.Specifically related to a kind of carbon quantum dot and preparation method thereof.
Background technology
Carbon quantum dot is as a kind of new carbon nanomaterial, and similar with various metal quantum points, carbon quantum dot is in illumination
In the case of can also emit a brilliant light.Therefore, carbon quantum dot is in biology sensor, medical imaging devices and small luminous
Have wide practical use in the fields such as diode.
High-temperature synthesis is one of technique prepared by carbon quantum dot, of great interest.A kind of " system of carbon quantum dot
Preparation Method and its application " (CN104592993B) patented technology, using macromolecular chitosan as raw material, is synthesized using microwave high-temperature method
Carbon quantum dot.But this method is needed in preparation process using microwave heating, higher to equipment requirement.A kind of " carbon quantum dot
Preparation method " (CN106276861A) patented technology, first with PA sodium modified hydrotalcite, then forge by high temperature
Carbon quantum dot is made in the process such as burning and pickling.It is higher to there is calcining heat in this method, and acid cleaning process needs nitrogen to be protection gas
Deng, therefore complex process and cost are high.
At present, the preparation of carbon quantum dot there are the technological deficiencies such as high synthesis temperature, complex process and cost height mostly.
The content of the invention
It is contemplated that overcoming prior art defect, it is therefore an objective to provide that a kind of technique is simple, reaction condition is gently produced into
The preparation method of this low carbon quantum dot；The carbon quantum dot good dispersion that is prepared with this method, shape is homogeneous and particle diameter is small, has
Preferable application prospect.
To achieve the above object, the step of the technical solution adopted in the present invention is:
Step 1: by catalyst: the mass ratio of isobutyiene-maieic anhydride copolymer is (0.00045 ~ 0.015): 1, urged described
Agent and isobutyiene-maieic anhydride copolymer mixing, obtain mixture, then by the mixture: the matter of deionized water
Amount is than being 1: (8 ~ 12), the mixture and deionized water mixing, 5 ~ 15min of magnetic agitation, and mixed solution is made.
Step 2: the mixed solution is placed in baking oven, 6 ~ 8h is dried under the conditions of 50 ~ 110 DEG C, mixed powder is made
Body.
Step 3: the mixed powder is placed in crucible, it is incubated 0.5 under the conditions of argon gas atmosphere and 250 ~ 700 DEG C ~
3h, is made carbon quantum dot presoma.
Step 4: by the carbon quantum dot presoma: polyethylene glycol: the mass ratio of deionized water is 3: (1 ~ 2): (8 ~
12), the carbon quantum dot presoma and the polyethylene glycol are added in deionized water, mixed, centrifugation removes supernatant, will
Sediment is dried, and carbon quantum dot is made.
The catalyst is manganese chloride or is manganese sulfate, and the manganese chloride and the manganese sulfate are that analysis is pure.
The isobutyiene-maieic anhydride copolymer is technical pure.
Due to using above-mentioned technical proposal, the present invention has following good effect compared with prior art:
1st, catalyst safety of the present invention is nontoxic；The isobutyiene-maieic anhydride copolymer used using carbon, hydrogen and oxygen as
Main, nitrogen content is very low, smaller to staff and environmental hazard.
2nd, the mass ratio of the of the invention catalyst used and the isobutyiene-maieic anhydride copolymer used for (0.00045 ~
0.015): 1, catalyst amount is few, and production cost is low, is adapted to industrialization large-scale production.
3rd, catalyst and isobutyiene-maieic anhydride copolymer are added in deionized water by the present invention, magnetic agitation, are done
It is dry, it is subsequently placed in crucible, is incubated under the conditions of argon gas atmosphere and 250 ~ 700 DEG C, carbon quantum dot presoma is made；Again will be described
Carbon quantum dot presoma and polyethylene glycol are mixed in deionized water, centrifugation, remove supernatant, sediment is dried, and carbon is made
Quantum dot.Therefore technique is simple, reaction condition is gentle, not high to equipment requirement.
The present invention uses catalysis method, and the good dispersion of prepared carbon quantum dot, shape are homogeneous, particle diameter distribution is narrow.
Therefore, the present invention has that technique is simple, reaction condition gentle, to the spy that equipment requirement is not high and production cost is low
Point；Prepared carbon quantum dot good dispersion, shape is homogeneous and particle diameter is small, there is preferable application prospect.
Brief description of the drawings
Fig. 1 schemes for a kind of TEM of carbon quantum dot prepared by the present invention；
Fig. 2 is the high power TEM figures of the carbon quantum dot shown in Fig. 1.
Embodiment
The present invention is described further with reference to the accompanying drawings and detailed description, not to the limit of its protection domain
System.
It is first that the raw material Unify legislation involved by present embodiment is as follows to avoid repeating, no longer gone to live in the household of one's in-laws on getting married in embodiment
State：
The catalyst is pure to analyze.
The isobutyiene-maieic anhydride copolymer is technical pure.
Embodiment 1
A kind of carbon quantum dot and preparation method thereof.The step of preparation method is：
Step 1: by catalyst: the mass ratio of isobutyiene-maieic anhydride copolymer is (0.00045 ~ 0.0023): 1, will be described
Catalyst and isobutyiene-maieic anhydride copolymer mixing, obtain mixture, then by the mixture: deionized water
Mass ratio is 1: (8 ~ 12), the mixture and deionized water mixing, 5 ~ 15min of magnetic agitation, and mixed solution is made.
Step 2: the mixed solution is placed in baking oven, 6 ~ 8h is dried under the conditions of 50 ~ 110 DEG C, mixed powder is made
Body.
Step 3: the mixed powder is placed in crucible, 2 ~ 3h is incubated under the conditions of argon gas atmosphere and 250 ~ 400 DEG C,
Carbon quantum dot presoma is made.
Step 4: by the carbon quantum dot presoma: polyethylene glycol: the mass ratio of deionized water is 3: (1.5 ~ 2): (8 ~
12), the carbon quantum dot presoma and the polyethylene glycol are added in deionized water, mixed, centrifugation removes supernatant, will
Sediment is dried, and carbon quantum dot is made.
The catalyst is manganese chloride.
Embodiment 2
A kind of carbon quantum dot and preparation method thereof.The step of preparation method is：
Step 1: by catalyst: the mass ratio of isobutyiene-maieic anhydride copolymer is (0.00045 ~ 0.00275): 1, will be described
Catalyst and isobutyiene-maieic anhydride copolymer mixing, obtain mixture, then by the mixture: deionized water
Mass ratio is 1: (8 ~ 12), the mixture and deionized water mixing, 5 ~ 15min of magnetic agitation, and mixed solution is made.
Step 2: the mixed solution is placed in baking oven, 6 ~ 8h is dried under the conditions of 50 ~ 110 DEG C, mixed powder is made
Body.
Step 3: the mixed powder is placed in crucible, 2 ~ 3h is incubated under the conditions of argon gas atmosphere and 250 ~ 400 DEG C,
Carbon quantum dot presoma is made.
Step 4: by the carbon quantum dot presoma: polyethylene glycol: the mass ratio of deionized water is 3: (1.5 ~ 2): (8 ~
12), the carbon quantum dot presoma and the polyethylene glycol are added in deionized water, mixed, centrifugation removes supernatant, will
Sediment is dried, and carbon quantum dot is made.
The catalyst is manganese sulfate.
Embodiment 3
A kind of carbon quantum dot and preparation method thereof.The step of preparation method is：
Step 1: by catalyst: the mass ratio of isobutyiene-maieic anhydride copolymer is (0.0023 ~ 0.007): 1, urged described
Agent and isobutyiene-maieic anhydride copolymer mixing, obtain mixture, then by the mixture: the matter of deionized water
Amount is than being 1: (8 ~ 12), the mixture and deionized water mixing, 5 ~ 15min of magnetic agitation, and mixed solution is made.
Step 2: the mixed solution is placed in baking oven, 6 ~ 8h is dried under the conditions of 50 ~ 110 DEG C, mixed powder is made
Body.
Step 3: the mixed powder is placed in crucible, 1 ~ 2h is incubated under the conditions of argon gas atmosphere and 400 ~ 550 DEG C,
Carbon quantum dot presoma is made.
Step 4: by the carbon quantum dot presoma: polyethylene glycol: the mass ratio of deionized water is 3: (1.3 ~ 1.8): (8
~ 12), and the carbon quantum dot presoma and the polyethylene glycol are added in deionized water, mixed, centrifugation removes supernatant, will
Sediment is dried, and carbon quantum dot is made.
The catalyst is manganese chloride.
Embodiment 4
A kind of carbon quantum dot and preparation method thereof.The step of preparation method is：
Step 1: by catalyst: the mass ratio of isobutyiene-maieic anhydride copolymer is (0.00275 ~ 0.008): 1, urged described
Agent and isobutyiene-maieic anhydride copolymer mixing, obtain mixture, then by the mixture: the matter of deionized water
Amount is than being 1: (8 ~ 12), the mixture and deionized water mixing, 5 ~ 15min of magnetic agitation, and mixed solution is made.
Step 2: the mixed solution is placed in baking oven, 6 ~ 8h is dried under the conditions of 50 ~ 110 DEG C, mixed powder is made
Body.
Step 3: the mixed powder is placed in crucible, 1 ~ 2h is incubated under the conditions of argon gas atmosphere and 400 ~ 550 DEG C,
Carbon quantum dot presoma is made.
Step 4: by the carbon quantum dot presoma: polyethylene glycol: the mass ratio of deionized water is 3: (1.3 ~ 1.8): (8
~ 12), and the carbon quantum dot presoma and the polyethylene glycol are added in deionized water, mixed, centrifugation removes supernatant, will
Sediment is dried, and carbon quantum dot is made.
The catalyst is manganese sulfate.
Embodiment 5
A kind of carbon quantum dot and preparation method thereof.The step of preparation method is：
Step 1: by catalyst: the mass ratio of isobutyiene-maieic anhydride copolymer is (0.007 ~ 0.0115): 1, urged described
Agent and isobutyiene-maieic anhydride copolymer mixing, obtain mixture, then by the mixture: the matter of deionized water
Amount is than being 1: (8 ~ 12), the mixture and deionized water mixing, 5 ~ 15min of magnetic agitation, and mixed solution is made.
Step 2: the mixed solution is placed in baking oven, 6 ~ 8h is dried under the conditions of 50 ~ 110 DEG C, mixed powder is made
Body.
Step 3: the mixed powder is placed in crucible, it is incubated 0.5 under the conditions of argon gas atmosphere and 550 ~ 700 DEG C ~
1.5h, is made carbon quantum dot presoma.
Step 4: by the carbon quantum dot presoma: polyethylene glycol: the mass ratio of deionized water is 3: (1 ~ 1.5): (8 ~
12), the carbon quantum dot presoma and the polyethylene glycol are added in deionized water, mixed, centrifugation removes supernatant, will
Sediment is dried, and carbon quantum dot is made.
The catalyst is manganese chloride.
Embodiment 6
A kind of carbon quantum dot and preparation method thereof.The step of preparation method is：
Step 1: by catalyst: the mass ratio of isobutyiene-maieic anhydride copolymer is (0.008 ~ 0.015): 1, by the catalysis
Agent and isobutyiene-maieic anhydride copolymer mixing, obtain mixture, then by the mixture: the quality of deionized water
Than for 1: (8 ~ 12), the mixture and deionized water are mixed, 5 ~ 15min of magnetic agitation, mixed solution is made.
Step 2: the mixed solution is placed in baking oven, 6 ~ 8h is dried under the conditions of 50 ~ 110 DEG C, mixed powder is made
Body.
Step 3: the mixed powder is placed in crucible, it is incubated 0.5 under the conditions of argon gas atmosphere and 550 ~ 700 DEG C ~
1.5h, is made carbon quantum dot presoma.
Step 4: by the carbon quantum dot presoma: polyethylene glycol: the mass ratio of deionized water is 3: (1 ~ 1.5): (8 ~
12), the carbon quantum dot presoma and the polyethylene glycol are added in deionized water, mixed, centrifugation removes supernatant, will
Sediment is dried, and carbon quantum dot is made.
The catalyst is manganese sulfate.
Present embodiment has following good effect compared with prior art:
1st, the catalyst safety that present embodiment is used is nontoxic；The isobutyiene-maieic anhydride copolymer used is with carbon, hydrogen
Based on oxygen, nitrogen content is very low, smaller to staff and environmental hazard.
2nd, the catalyst and the mass ratio of the isobutyiene-maieic anhydride copolymer used that present embodiment is used for
(0.00045 ~ 0.015): 1, catalyst amount is few, and production cost is low, is adapted to industrialization large-scale production.
3rd, catalyst and isobutyiene-maieic anhydride copolymer are added in deionized water by present embodiment, magnetic force
Stirring, dries, is subsequently placed in crucible, is incubated under the conditions of argon gas atmosphere and 250 ~ 700 DEG C, and carbon quantum dot presoma is made；
The carbon quantum dot presoma and polyethylene glycol are mixed in deionized water again, centrifuged, supernatant is removed, sediment is dried
It is dry, carbon quantum dot is made.Therefore technique is simple, reaction condition is gentle, not high to equipment requirement.
Present embodiment uses the carbon quantum dot of catalysis method preparation as depicted in figs. 1 and 2, and Fig. 1 is the institute of the present embodiment 3
A kind of TEM figures of the carbon quantum dot prepared, Fig. 2 schemes for the high power TEM of carbon quantum dot shown in Fig. 1.It can be seen that from Fig. 1 and Fig. 2
It is about 2nm using the carbon quantum dot diameter prepared by this method, and good dispersion, shape are homogeneous and particle diameter is small.
Therefore, present embodiment has that technique is simple, reaction condition gentle, and production cost not high to equipment requirement
Low the characteristics of；Prepared carbon quantum dot good dispersion, shape is homogeneous and particle diameter is small, there is preferable application prospect.
Claims (4)
1. a kind of preparation method of carbon quantum dot, it is characterised in that be the step of the preparation method:
Step 1: by catalyst: the mass ratio of isobutyiene-maieic anhydride copolymer is (0.00045 ~ 0.015): 1, urged described
Agent and isobutyiene-maieic anhydride copolymer mixing, obtain mixture, then by the mixture: the matter of deionized water
Amount is than being 1: (8 ~ 12), the mixture and deionized water mixing, 5 ~ 15min of magnetic agitation, and mixed solution is made；
Step 2: the mixed solution is placed in baking oven, 6 ~ 8h is dried under the conditions of 50 ~ 110 DEG C, mixed powder is made；
Step 3: the mixed powder is placed in crucible, 0.5 ~ 3h, system are incubated under the conditions of argon gas atmosphere and 250 ~ 700 DEG C
Obtain carbon quantum dot presoma；
Step 4: by the carbon quantum dot presoma: polyethylene glycol: the mass ratio of deionized water is 3: (1 ~ 2): (8 ~ 12), will
The carbon quantum dot presoma and the polyethylene glycol are added in deionized water, are mixed, and centrifugation removes supernatant, by sediment
Drying, is made carbon quantum dot.
2. the preparation method of carbon quantum dot according to claim 1, it is characterised in that the catalyst is manganese chloride or is
Manganese sulfate, the manganese chloride and the manganese sulfate are that analysis is pure.
3. the preparation method of carbon quantum dot according to claim 1, it is characterised in that the isobutyiene-maieic anhydride copolymerization
Thing is technical pure.
4. a kind of carbon quantum dot, it is characterised in that the carbon quantum dot is the carbon according to any one of claim 1 ~ 3
Carbon quantum dot prepared by the preparation method of quantum dot.
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Citations (1)
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|---|---|---|---|---|
| US20170058056A1 (en) * | 2015-08-27 | 2017-03-02 | The Florida State University Research Foundation, Inc. | Multifunctional and multicoordinating amphiphilic polymer ligands for interfacing semiconducting, magnetic, and metallic nanocrystals with biological systems |
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| US20170058056A1 (en) * | 2015-08-27 | 2017-03-02 | The Florida State University Research Foundation, Inc. | Multifunctional and multicoordinating amphiphilic polymer ligands for interfacing semiconducting, magnetic, and metallic nanocrystals with biological systems |
Non-Patent Citations (1)
| Title |
|---|
| ANGELINA CAYUELA ET AL.: "One-Step Synthesis and Characterization of N‑Doped Carbon Nanodots for Sensing in Organic Media", 《ANAL. CHEM.》 * |
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Granted publication date: 20190412 |