CN103086355B - Synthetic method of carbon quantum dot material - Google Patents
Synthetic method of carbon quantum dot material Download PDFInfo
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- CN103086355B CN103086355B CN201310046953.7A CN201310046953A CN103086355B CN 103086355 B CN103086355 B CN 103086355B CN 201310046953 A CN201310046953 A CN 201310046953A CN 103086355 B CN103086355 B CN 103086355B
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Abstract
The invention relates to the technical field of inorganic synthesis, and aims to provide a synthetic method of a carbon quantum dot material. The method is characterized in that a reducing agent and a reaction substrate are put in a solvent and react at 100-200DEG C for 2-72h to synthesize the carbon quantum dot material; the molar ratio of the reducing agent to the reaction substrate is 1-100; and the mass ratio of the solvent to the reaction substrate is 20-1000. The method is simple and effective, adopts a solvothermal synthesis process to substitute traditional tedious synthetic processes, adopts an organic matter to substitute traditional expensive substances as a carbon precursor and adopts L-ascorbic acid and its analogues as the reducing agent. The whole process of the method has the advantages of high efficiency, environmental protection and low cost.
Description
Technical field
The present invention relates to inorganic synthetic technical field, specially refer to a kind of new environmental protection cheaply method synthesize carbon quanta point material.
Background technology
Quanta point material is due to the special property of himself, and at biology, electricity and optical field have a wide range of applications.At present, the research majority for quanta point material is all centered around on the metallic compounds such as CdS, CdSe, ZnS and HgS.But the cost of this metalloid chemicals quantum point is high, it is large to pollute, toxicity is large, and this has limited their widespread use greatly.In recent years, carbon material was because the character such as its low cost, low pollution have caused everybody extensive concern.Carbon quanta point material also becomes a popular research topic.The method of synthetic carbon quanta point material has many, and these methods are mainly around synthetic carbon matrix precursor, surface passivation and carbonization, and three steps of functionalization are carried out.In these steps, high temperature cabonization, acid treatment etc. are all necessary treatment condition, and presoma and the passivator of carbon are expensive, and whole experimentation is loaded down with trivial details, and energy consumption is high, and these are all unfavorable for utilization and the popularization of carbon quantum dot.Therefore, how to adopt green method, under gentle reaction conditions, synthesize carbon quantum dot, become a significant challenge in this field.
Summary of the invention
The technical problem to be solved in the present invention is, overcomes deficiency of the prior art, and a kind of method that synthetic carbon quanta point material is provided is to realize green, to prepare carbon quanta point material simply, quickly.
For technical solution problem, solution of the present invention is:
A kind of method that synthetic carbon quanta point material is provided, comprises the steps:
Reductive agent and reaction substrate are put into solvent in the lump, at 100～200 ℃, react 2～72 hours to synthesize carbon quanta point material; The mol ratio of described reductive agent and reaction substrate is 1～100, and the mass ratio of solvent and reaction substrate is 20～1000; Described reductive agent is L-AA, saccharosonic acid or 5,6-O-isopropylidene-L-AA; Described solvent is water, hexanaphthene or ethanol;
Described reaction substrate is any one of the following stated: carboritride organism: trimeric cyanamide, urea, thiocarbamide or cetyl trimethylammonium bromide; Or carbohydrate: glucose, sucrose, cellobiose, wood sugar or fructose; Or oxygen-bearing organic matter: phenol, Resorcinol, pyrocatechol or p-methyl phenol; Or amino acid: Methionin or L-glutamic acid; Or contain organic silica material: duct contains the meso pore silicon oxide material of cetyl trimethylammonium bromide.
Beneficial effect of the present invention is:
The present invention is simply effective, adopts the synthetic method of solvent thermal to replace traditional loaded down with trivial details synthetic method, adopts organism to replace traditional expensive material as carbon matrix precursor, adopts L-AA and similar substance thereof as reductive agent.Whole process is efficient, green, with low cost.
Accompanying drawing explanation
Fig. 1 is the transmission electron microscope photo of carbon quanta point material synthetic in embodiment 1.
Fig. 2 is the transmission electron microscope photo of carbon quanta point material synthetic in embodiment 2.
Fig. 3 is the transmission electron microscope photo of carbon quanta point material synthetic in embodiment 3.
Fig. 4 is the XPS spectrum figure of the C1s of carbon quanta point material synthetic in embodiment 4.
Fig. 5 is the XPS spectrum figure of the N1s of carbon quanta point material synthetic in embodiment 4.
Embodiment
Illustrative example, illustrates that the present invention adopts the concrete example of the synthetic carbon quanta point material of method of solvent thermal below.
Embodiment 1:
At room temperature, the L-AA of the Methionin of 146 mg (1 mmol) and 1 mmol is dissolved in 2.9 g ethanol, solution is transferred in autoclave, process 2 hours for 100 ℃.After the centrifugal suspended substance of removing bulk, evaporation, except desolventizing, just obtains carbon quanta point material.Fig. 1 has provided the transmission electron microscope photo of carbon quanta point material synthetic under this condition.
As optional alternative, Methionin also can be used L-glutamic acid to replace, and can realization response obtain carbon quanta point material equally.
Embodiment 2:
At room temperature, the L-AA of the phenol of 94 mg (1 mmol) and 10 mmol is dissolved in 18.8 g hexanaphthenes, solution is transferred in autoclave, process 10 hours for 140 ℃.After the centrifugal suspended substance of removing bulk, evaporation, except desolventizing, just obtains carbon quanta point material.Fig. 2 has provided the transmission electron microscope photo of carbon quanta point material synthetic under this condition.
As optional alternative, phenol also can be used Resorcinol, pyrocatechol or p-methyl phenol to replace, and can realization response obtain carbon quanta point material equally.
Embodiment 3:
At room temperature, duct is contained to cetyl trimethylammonium bromide, and (content is 1 mmol, quality is 365mg) meso pore silicon oxide material (MCM-41) and the saccharosonic acid of 30 mmol be distributed in 200 g water, mixture is transferred in autoclave, process 30 hours for 160 ℃.Washing and filtering goes out meso pore silicon oxide material, just obtains in the middle of duct that carbon quantum dot is dispersed in silicon oxide.Fig. 3 has provided the transmission electron microscope photo of carbon quanta point material synthetic under this condition.
Embodiment 4:
At room temperature, by 5 of the trimeric cyanamide of 126 mg (1 mmol) and 100 mmol, 6-O-isopropylidene-L-AA is dissolved in 126 g water, and solution is transferred in autoclave, processes 72 hours for 200 ℃.After the centrifugal suspended substance of removing bulk, evaporation, except desolventizing, just obtains carbon quanta point material.Fig. 4,5 has provided C1s and N1s x-ray photoelectron power spectrum (XPS) figure of carbon quanta point material synthetic under this condition, shows that sample has abundant nitrogen-containing group.
As optional alternative, trimeric cyanamide also can be used urea, thiocarbamide or cetyl trimethylammonium bromide to replace, and can realization response obtain carbon quanta point material equally.
Embodiment 5:
At room temperature, the L-AA of the glucose of 170 mg (1 mmol) and 1 mmol is dissolved in 3.4g water, solution is transferred in autoclave, process 2 hours for 100 ℃.After the centrifugal suspended substance of removing bulk, evaporation, except desolventizing, just obtains carbon quanta point material.
As optional alternative, glucose also can be used sucrose, cellobiose, wood sugar or fructose to replace, and can realization response obtain carbon quanta point material equally.
Finally, the thing also should be noted that, what more than enumerate is only specific embodiments of the invention.Obviously, the invention is not restricted to above examples of implementation, can also have many distortion.All distortion that those of ordinary skill in the art all can directly derive or associate from content disclosed by the invention, all should think protection scope of the present invention.
Claims (3)
1. a method for synthetic carbon quanta point material, is characterized in that, is at room temperature the L-AA of the phenol of 1mmol and 10mmol to be dissolved in 18.8g hexanaphthene, and solution is transferred in autoclave, processes 10 hours for 140 ℃; Centrifugal suspended substance evaporation afterwards of removing bulk, except desolventizing, obtains carbon quanta point material.
2. the method for a synthetic carbon quanta point material, it is characterized in that, at room temperature duct to be contained to the meso pore silicon oxide material of 1mmol cetyl trimethylammonium bromide and the saccharosonic acid of 30mmol to be distributed in 200g water, mixture is transferred in autoclave, processed 30 hours for 160 ℃; Washing and filtering goes out meso pore silicon oxide material, obtains being dispersed in the carbon quanta point material in the duct of silicon oxide.
3. the method for a synthetic carbon quanta point material, it is characterized in that, be at room temperature by 5 of the trimeric cyanamide of 1mmol and 100mmol, and 6-O-isopropylidene-L-AA is dissolved in 126g water, solution is transferred in autoclave, processed 72 hours for 200 ℃; Centrifugal suspended substance evaporation afterwards of removing bulk, except desolventizing, obtains carbon quanta point material.
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Cited By (1)
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| CN106829919A (en) * | 2017-01-05 | 2017-06-13 | 江南大学 | A kind of method that carbon quantum dot is synthesized based on ascorbic acid and urea microwave reaction |
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| CN106829919A (en) * | 2017-01-05 | 2017-06-13 | 江南大学 | A kind of method that carbon quantum dot is synthesized based on ascorbic acid and urea microwave reaction |
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