CN103086355A - Synthetic method of carbon quantum dot material - Google Patents
Synthetic method of carbon quantum dot material Download PDFInfo
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- CN103086355A CN103086355A CN2013100469537A CN201310046953A CN103086355A CN 103086355 A CN103086355 A CN 103086355A CN 2013100469537 A CN2013100469537 A CN 2013100469537A CN 201310046953 A CN201310046953 A CN 201310046953A CN 103086355 A CN103086355 A CN 103086355A
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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 the 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 all is centered around on the metallic compounds such as CdS, CdSe, ZnS and HgS.But the cost of this metalloid chemicals quantum point is high, pollution is large, 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.The 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 all are unfavorable for utilization and the popularization of carbon quantum dot.Therefore, how to adopt green method, synthesize the carbon quantum dot under the reaction conditions of gentleness, 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 the carbon quanta point material simply, quickly.
Be the technical solution problem, solution of the present invention is:
A kind of method of synthetic carbon quanta point material is provided, comprises the steps:
Reductive agent and reaction substrate are put into solvent in the lump, react 2～72 hours with synthetic carbon quanta point material under 100～200 ℃; 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: the 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: the 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.
Description of drawings
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
Following illustrative example illustrates that the present invention adopts the concrete example of the synthetic carbon quanta point material of method of solvent thermal.
Embodiment 1:
At room temperature, the Methionin of 146 mg (1 mmol) and the L-AA of 1 mmol are dissolved in 2.9 g ethanol, solution is transferred in autoclave, processed 2 hours for 100 ℃.After the centrifugal suspended substance of removing bulk, the evaporation desolventizing just obtains the 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 use L-glutamic acid to replace, and can realization response obtain the carbon quanta point material equally.
Embodiment 2:
At room temperature, the phenol of 94 mg (1 mmol) and the L-AA of 10 mmol are dissolved in 18.8 g hexanaphthenes, solution is transferred in autoclave, processed 10 hours for 140 ℃.After the centrifugal suspended substance of removing bulk, the evaporation desolventizing just obtains the 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 use Resorcinol, pyrocatechol or p-methyl phenol to replace, and can realization response obtain the carbon quanta point material equally.
Embodiment 3:
At room temperature, the duct is contained 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, processed 30 hours for 160 ℃.Washing and filtering goes out meso pore silicon oxide material, just obtains in the middle of duct that the 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, with 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, the evaporation desolventizing just obtains the 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 use urea, thiocarbamide or cetyl trimethylammonium bromide to replace, and can realization response obtain the carbon quanta point material equally.
Embodiment 5:
At room temperature, the glucose of 170 mg (1 mmol) and the L-AA of 1 mmol are dissolved in 3.4g water, solution is transferred in autoclave, processed 2 hours for 100 ℃.After the centrifugal suspended substance of removing bulk, the evaporation desolventizing just obtains the carbon quanta point material.
As optional alternative, glucose also can use sucrose, cellobiose, wood sugar or fructose to replace, and can realization response obtain the carbon quanta point material equally.
At last, the thing that 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, many distortion can also be arranged.All distortion that those of ordinary skill in the art all can directly derive or associate from content disclosed by the invention all should be thought protection scope of the present invention.
Claims (6)
1. the method for a synthetic carbon quanta point material, is characterized in that, comprises the steps:
Reductive agent and reaction substrate are put into solvent in the lump, react 2～72 hours with synthetic carbon quanta point material under 100～200 ℃; 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: the duct contains the meso pore silicon oxide material of cetyl trimethylammonium bromide.
2. method according to claim 1, is characterized in that, is at room temperature the Methionin of 1 mmol and the L-AA of 1 mmol to be dissolved in 2.9 g ethanol, and solution is transferred in autoclave, processed 2 hours for 100 ℃; The centrifugal suspended substance of removing bulk evaporates desolventizing afterwards, obtains the carbon quanta point material.
3. method according to claim 1, is characterized in that, is at room temperature the phenol of 1 mmol and the L-AA of 10 mmol to be dissolved in 18.8 g hexanaphthenes, and solution is transferred in autoclave, processed 10 hours for 140 ℃; The centrifugal suspended substance of removing bulk evaporates desolventizing afterwards, obtains the carbon quanta point material.
4. method according to claim 1, it is characterized in that, at room temperature the duct to be contained the meso pore silicon oxide material of 1 mmol cetyl trimethylammonium bromide and the saccharosonic acid of 30 mmol is distributed in 200 g 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.
5. method according to claim 1, it is characterized in that, be at room temperature with 5 of the trimeric cyanamide of 1 mmol and 100 mmol, and 6-O-isopropylidene-L-AA is dissolved in 126 g water, solution is transferred in autoclave, processed 72 hours for 200 ℃; The centrifugal suspended substance of removing bulk evaporates desolventizing afterwards, obtains the carbon quanta point material.
6. method according to claim 1, is characterized in that, is at room temperature, and the glucose of 1 mmol and the L-AA of 1 mmol are dissolved in 3.4g water, and solution is transferred in autoclave, processed 2 hours for 100 ℃; The centrifugal suspended substance of removing bulk evaporates desolventizing afterwards, obtains the carbon quanta point material.
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