CN106566543A - Carbon nano dot with adjustable light emission in visible-region whole spectral coverage and preparation method thereof - Google Patents
Carbon nano dot with adjustable light emission in visible-region whole spectral coverage and preparation method thereof Download PDFInfo
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Abstract
The invention provides a preparation method of a carbon nano dot with adjustable light emission in visible-region whole spectral coverage. The preparation method comprises the following steps of dissolving citric acid and urea in a reactive solvent to carry out a solvothermal reaction, so as to obtain the carbon nano dot, wherein the reactive solvent comprises one or multiple of protonic solvents which are mutually soluble with water and/or non-protonic solvents which are mutually soluble with the water and the water; the mixing ratio of the water to the one or the multiple of the protonic solvents which are mutually soluble with the water and/or the non-protonic solvents which are mutually soluble with the water is 0 to 100 percent; and the mixing ratio of the protonic solvents which are mutually soluble with the water to the non-protonic solvents which are mutually soluble with the water is 0 to 100 percent. By using the preparation method, in a solvothermal condition, through regulating the mixing ratio of the water to the protonic solvents and the non-protonic solvents, which can be mutually soluble with the water, the carbon nano dot with the adjustable light emission in the visible-region whole spectral coverage can be prepared. The problem that a light-emitting band gap of the carbon nano dot is difficult to regulate and control is solved.
Description
Technical field
The invention belongs to technical field of nano material, and in particular to a kind of full spectral coverage in visual field light adjustable carbon nano dot and
Its preparation method.
Background technology
Carbon nano dot (Carbon dots, CDots) is a kind of carbon nanomaterial of novel light-emitting, and it is because steady with fluorescence
It is qualitative it is high, without optical flare, exciting light spectrum width and it is continuous, launch wavelength is tunable, good biocompatibility, low toxin, quilt
It is considered as the potential succedaneum of organic dyestuff and semiconductor-quantum-point.But at present most of carbon point fluorescent emission concentrate on indigo plant
Light and green light band, but the High Efficiency Luminescence of gold-tinted and red spectral band is still difficult to.Because its luminescence mechanism is still not clear,
The not clear luminous band gap for how regulating and controlling carbon point.Prior art is passively to separate acquisition visual field by the method for column chromatography
In the range of multicolor fluorescence carbon point, however, also without clear and definite preparation method adjust carbon nano dot in the range of the full spectral coverage in visual field
Fluorescent emission.
The content of the invention
In view of this, the technical problem to be solved in the present invention is to provide a kind of full spectral coverage in visual field to light adjustable carbon nanometer
Point and preparation method thereof, the preparation method that the present invention is provided can prepare the full spectral coverage in visual field and light adjustable carbon nano dot.
The preparation method of adjustable carbon nano dot the invention provides a kind of full spectral coverage in visual field lights, comprises the following steps：
Citric acid and carbamide are dissolved in reaction dissolvent carries out solvent thermal reaction, obtains carbon nano dot；
The reaction dissolvent includes in protonic solvent and/or non-protonic solvent miscible with water miscible with water
Plant or various and water；
One or more and water in the protonic solvent miscible with water and/or non-protonic solvent miscible with water
Mixed proportion be 0～100%；
The mixed proportion of the protonic solvent miscible with water and non-protonic solvent miscible with water is 0～100%.
Preferably, organic solvent or carboxylic organic molten of the protonic solvent miscible with water selected from hydroxyl
Agent.
Preferably, the protonic solvent miscible with water is in methanol, ethanol, ethylene glycol, glycerol, acetic acid and oxalic acid
One or more；
Preferably, the non-protonic solvent miscible with water is selected from dimethyl sulfoxide (DMSO), N, N- dimethyl formyls
One or more in amine (DMF), dimethyl acetylamide, acetonitrile and acetone.
Preferably, the non-protonic solvent miscible with water is selected from DMSO and/or DMF.
Preferably, the reaction dissolvent that the reaction dissolvent is formed selected from water with DMF, the reaction dissolvent that water is formed with DMSO,
The reaction dissolvent that the reaction dissolvent that DMSO, DMF and water are formed, the reaction dissolvent that water is formed with glycerol, glycerol and DMF are formed with water
Or the reaction dissolvent that one or more in glycerol, acetic acid, DMSO and DMF is formed with water.
Preferably, the citric acid and the mass ratio of carbamide are 1：(1～3).
Preferably, the temperature of the solvent thermal reaction is 120～200 DEG C, and the time of the solvent thermal reaction is 2～8 little
When.
Preferably, after solvent thermal reaction is carried out, also include the product is washed and is dried.
The full spectral coverage in visual field that method prepares is prepared as above lights adjustable carbon nanometer present invention also offers a kind of
Point.
Compared with prior art, the preparation side of adjustable carbon nano dot the invention provides a kind of full spectral coverage in visual field lights
Method, comprises the following steps：Citric acid and carbamide are dissolved in reaction dissolvent carries out solvent thermal reaction, obtains carbon nano dot；Institute
State reaction dissolvent including one or more in protonic solvent and/or non-protonic solvent miscible with water miscible with water with
And water；One or more in the water and protonic solvent miscible with water and/or non-protonic solvent miscible with water
Mixed proportion is 0～100%；The mixed proportion of the protonic solvent miscible with water and non-protonic solvent miscible with water
For 0～100%.The present invention under the conditions of solvent thermal, by adjusting water and the protonic solvent that can dissolve each other therewith and aprotic
The mixed proportion of solvent, can prepare the full spectral coverage in visual field and light adjustable carbon nano dot.Solve the luminous band gap of carbon nano dot
It is difficult to the problem for regulating and controlling.
Description of the drawings
Fig. 1 be embodiment 16 prepare fluorescence nano carbon point daylight (on) and ultraviolet light (under) under the conditions of optics shine
Piece；
Fig. 2 is the fluorescence spectrum under the original solution of the fluorescent carbon nano dot that embodiment 16 is prepared is excited at 365 nanometers；
Fig. 3 is the transmission electron microscope of fluorescent carbon nano dot CDot 1, CDot 4 prepared by embodiment 16 and CDot 7
And high resolution transmission electron microscopy (HRTEM) photo and its particle diameter statistic histogram (TEM)；
Fig. 4 is the atomic force micrograph (AFM) of the carbon nano dot CDot 4 prepared in embodiment 16；
Fig. 5 is the X-ray photoelectron spectroscopic analysis of nano-sized carbon point CDot 1, CDot 4 and CDot 7 prepared by embodiment 16
(XPS) figure；
Fig. 6 is the absorption spectrum of fluorescent carbon aqueous nanodot solutions prepared by embodiment 16 and optimum emission spectrum.
Specific embodiment
The preparation method of adjustable carbon nano dot the invention provides a kind of full spectral coverage in visual field lights, it is characterised in that bag
Include following steps：
Citric acid and carbamide are dissolved in reaction dissolvent carries out solvent thermal reaction, obtains carbon nano dot；
The reaction dissolvent includes in protonic solvent and/or non-protonic solvent miscible with water miscible with water
Plant or various and water；
One or more and water in the protonic solvent miscible with water and/or non-protonic solvent miscible with water
Mixed proportion be 0～100%；
The mixed proportion of the protonic solvent miscible with water and non-protonic solvent miscible with water is 0～100%.
The present invention is changed by the protonic solvent that adjust water and can dissolve each other therewith and the mixed proportion of non-protonic solvent
The polarity of the reaction dissolvent under the conditions of solvent thermal, lights adjustable carbon nano dot such that it is able to prepare the full spectral coverage in visual field.
The present invention is first dissolved in citric acid and carbamide in reaction dissolvent, wherein, the reaction dissolvent includes mutual with water
One or more and water in molten protonic solvent and/or non-protonic solvent miscible with water.
In the present invention, organic solvent or carboxylic organic of the protonic solvent miscible with water selected from hydroxyl
One or more in solvent, preferably methanol, ethanol, ethylene glycol, glycerol, acetic acid and oxalic acid.
The non-protonic solvent miscible with water is selected from DMSO, DMF, dimethyl acetylamide, acetonitrile and acetone
Plant or various, preferably DMSO and/or DMF.
In certain specific embodiments of the invention, the reaction dissolvent that the reaction dissolvent is formed selected from water with DMF, water
The reaction dissolvent formed with DMSO, the reaction dissolvent that DMSO, DMF and water are formed, the reaction dissolvent that water is formed with glycerol, glycerol and
The reaction dissolvent that one or more in DMF and the reaction dissolvent or glycerol, acetic acid, DMSO and DMF of water formation is formed with water.
In the present invention, in the water and protonic solvent miscible with water and/or non-protonic solvent miscible with water
One or more of mixed proportion be 0～100%, it is preferred that the protonic solvent miscible with water and/or miscible with water
Non-protonic solvent in be preferably (0～8) with the volume ratio of water one or more：(0～2), is zero when the two is different.
The mixed proportion of the protonic solvent miscible with water and non-protonic solvent miscible with water is 0～100%,
Preferably, the mass ratio of protonic solvent miscible with water and non-protonic solvent miscible with water is (0～3)：(0～6).
By adjust water and protonic solvent miscible with water and/or one kind in non-protonic solvent miscible with water or
Various mixed proportions is further to affect finally to carry out what solvent thermal reaction was obtained such that it is able to adjust the polarity of reaction dissolvent
The color of carbon nano dot.
In the present invention, the citric acid and the mass ratio of carbamide are 1：(1～3), some in the present invention are embodied as
In example, the citric acid is 1 with the mass ratio of carbamide：1, in other embodiments of the present invention, the citric acid and carbamide
Mass ratio be 1：2, in other embodiments of the present invention, the citric acid is 1 with the mass ratio of carbamide：3.
The citric acid is preferably (2～4g) with the gross mass of carbamide with the volume ratio of the reaction dissolvent：(5～
15ml), more preferably (2～4g)：(10ml).
The temperature of the solvent thermal reaction is 120～200 DEG C, preferably 140～180 DEG C；The solvent thermal reaction when
Between be 2～8 hours, preferably 4～6 hours.In the present invention, the solvent thermal reaction is preferably in steel lining polytetrafluoroethyl-ne alkene reaction
React in kettle, reaction condition is to carry out reacting by heating under airtight condition.
In the present invention, after solvent thermal reaction is carried out, also include being purified the product.
The present invention does not have particular restriction to the method for purification of the product, preferably carries out as follows：
1) reactant liquor and ethanol are mixed, after vibration, the method mix homogeneously of ultrasound, centrifugation removes upper strata
After liquid, it is precipitated；
2) precipitation and ethanol are mixed, centrifugation removes supernatant liquid, is precipitated；
3) by step 2) the precipitation repeat step 2 that obtains), till supernatant liquid is as clear as crystal, after being washed
Carbon nano dot.
Wherein, the rotating speed of the centrifugation is preferably 6000～9000 revs/min, more preferably 8000 revs/min；It is described from
The time of the heart be 4-8 minutes, preferably 5 minutes.
Carbon nano dot after the washing is dried, carbon nano dot is obtained.Wherein, to be preferably vacuum cold for the drying
Lyophilizing is dry.Preferably, the freeze temperature is preferably -45 DEG C to -55 DEG C, more preferably -50 DEG C；The freeze-drying time is preferably
24～48 hours, more preferably 36 hours.
Present invention also offers a kind of full spectral coverage in visual field prepared using above-mentioned preparation method is lighted, adjustable carbon is received
Nanodot.
According to above-mentioned preparation method, by the reaction dissolvent for adjusting the opposed polarity for obtaining, navy blue, indigo plant can be obtained
Color, cyan, green, yellow, the fluorescent carbon nano dot of orange or red.The carbon nanodot fluorescence emission peak is arrived at 440 nanometers
Between 640 nanometers, with the good characteristics of luminescence and water solublity, also, the carbon nano dot is a kind of nontoxic, low cost
And the fluorescent material of environmental protection.Can be widely applied for chemistry, biological and material science.
For a further understanding of the present invention, the full spectral coverage in visual field that the present invention is provided is lighted with reference to embodiment adjustable
Carbon nano dot and preparation method thereof is illustrated, and protection scope of the present invention is not limited by the following examples.
The reaction raw materials citric acid and carbamide that the present invention is used is all from Shanghai Mike's woods biochemical technology company limited, reaction
Solvent glycerin, acetic acid, DMSO, DMF are all from Aladdin reagent company limited, and all raw materials and reagent are directly used, without the need for
Purification processes.
Embodiment 1
Using 3g citric acids and 6g carbamide, as reaction raw materials, used as reaction raw materials, (reaction raw materials mixed proportion is 1：2) it is, molten
Solution obtains colourless well-illuminated solution in the reaction dissolvent of 30ml.Wherein, the mixed solution of the reaction dissolvent water and DMF, its
In, the volume ratio of water and DMF is reacted according to the ratio shown in table 1 in reaction dissolvent.
By in the colourless transparent solution steel lining ptfe autoclave, airtight heating is carried out under conditions of 160 DEG C
Solvent thermal reaction 4 hours, obtains reaction mixture；
The reaction mixture is mixed with 60 milliliters of ethanol, is centrifuged 5 minutes with 8000 revs/min of rotating speed；In removal
Layer liquid (removes the reactant and reaction dissolvent of remnants), precipitation is dissolved in into repeated centrifugation 3 times in 60 milliliters of ethanol, to upper liquid
Till body is more thorough, precipitation, lyophilizing are taken, freeze temperature is -50 DEG C, and freeze-drying time is 36 hours, obtains fluorescent carbon nano dot.
The fluorescence nano carbon point is excited and launch wavelength detection, 1 is the results are shown in Table, table 1 be reaction raw materials and
Product detection result.
The reaction raw materials of table 1 and product detection result
Embodiment 2
Using 3g citric acids and 3g carbamide, as reaction raw materials, used as reaction raw materials, (reaction raw materials mixed proportion is 1：1) it is, molten
Solution obtains colourless well-illuminated solution in the reaction dissolvent of 30ml.Wherein, the mixed solution of the reaction dissolvent water and DMF, its
In, the volume ratio of water and DMF is reacted according to the ratio shown in table 2 in reaction dissolvent.
By in the colourless transparent solution steel lining ptfe autoclave, airtight heating is carried out under conditions of 160 DEG C
Solvent thermal reaction 4 hours, obtains reaction mixture；
The reaction mixture is mixed with 60 milliliters of ethanol, is centrifuged 5 minutes with 8000 revs/min of rotating speed；In removal
Layer liquid (removes the reactant and reaction dissolvent of remnants), precipitation is dissolved in into repeated centrifugation 3 times in 60 milliliters of ethanol, to upper liquid
Till body is more thorough, precipitation, lyophilizing are taken, freeze temperature is -50 DEG C, and freeze-drying time is 36 hours, obtains fluorescent carbon nano dot.
The fluorescence nano carbon point is excited and launch wavelength detection, 2 are the results are shown in Table, table 2 be reaction raw materials and
Product detection result.
The reaction raw materials of table 2 and product detection result
Embodiment 3
Using 3g citric acids and 9g carbamide, as reaction raw materials, used as reaction raw materials, (reaction raw materials mixed proportion is 1：3) it is, molten
Solution obtains colourless well-illuminated solution in the reaction dissolvent of 30ml.Wherein, the mixed solution of the reaction dissolvent water and DMF, its
In, the volume ratio of water and DMF is reacted according to the ratio shown in table 3 in reaction dissolvent.
By in the colourless transparent solution steel lining ptfe autoclave, airtight heating is carried out under conditions of 160 DEG C
Solvent thermal reaction 4 hours, obtains reaction mixture；
The reaction mixture is mixed with 60 milliliters of ethanol, is centrifuged 5 minutes with 8000 revs/min of rotating speed；In removal
Layer liquid (removes the reactant and reaction dissolvent of remnants), precipitation is dissolved in into repeated centrifugation 3 times in 60 milliliters of ethanol, to upper liquid
Till body is more thorough, precipitation, lyophilizing are taken, freeze temperature is -50 DEG C, and freeze-drying time is 36 hours, obtains fluorescent carbon nano dot.
The fluorescence nano carbon point is excited and launch wavelength detection, 3 are the results are shown in Table, table 3 be reaction raw materials and
Product detection result.
The reaction raw materials of table 3 and product detection result
Embodiment 4
Using 3g citric acids and 6g carbamide, as reaction raw materials, used as reaction raw materials, (reaction raw materials mixed proportion is 1：2) it is, molten
Solution obtains colourless well-illuminated solution in the reaction dissolvent of 30-40ml.Wherein, the mixed solution of the reaction dissolvent water and DMF,
Wherein, the volume ratio of water and DMF is reacted according to the ratio shown in table 4 in reaction dissolvent.
By in the colourless transparent solution steel lining ptfe autoclave, airtight heating is carried out under conditions of 120 DEG C
Solvent thermal reaction 4 hours, obtains reaction mixture；
The reaction mixture is mixed with 60 milliliters of ethanol, is centrifuged 5 minutes with 8000 revs/min of rotating speed；In removal
Layer liquid (removes the reactant and reaction dissolvent of remnants), precipitation is dissolved in into repeated centrifugation 3 times in 60 milliliters of ethanol, to upper liquid
Till body is more thorough, precipitation, lyophilizing are taken, freeze temperature is -50 DEG C, and freeze-drying time is 36 hours, obtains fluorescent carbon nano dot.
The fluorescence nano carbon point is excited and launch wavelength detection, 4 are the results are shown in Table, table 4 be reaction raw materials and
Product detection result.
The reaction raw materials of table 4 and product detection result
Embodiment 5
Using 3g citric acids and 6g carbamide, as reaction raw materials, used as reaction raw materials, (reaction raw materials mixed proportion is 1：2) it is, molten
Solution obtains colourless well-illuminated solution in the reaction dissolvent of 30ml.Wherein, the mixed solution of the reaction dissolvent water and DMF, its
In, the volume ratio of water and DMF is reacted according to the ratio shown in table 5 in reaction dissolvent.
By in the colourless transparent solution steel lining ptfe autoclave, airtight heating is carried out under conditions of 180 DEG C
Solvent thermal reaction 4 hours, obtains reaction mixture；
The reaction mixture is mixed with 60 milliliters of ethanol, is centrifuged 5 minutes with 8000 revs/min of rotating speed；In removal
Layer liquid (removes the reactant and reaction dissolvent of remnants), precipitation is dissolved in into repeated centrifugation 3 times in 60 milliliters of ethanol, to upper liquid
Till body is more thorough, precipitation, lyophilizing are taken, freeze temperature is -50 DEG C, and freeze-drying time is 36 hours, obtains fluorescent carbon nano dot.
The fluorescence nano carbon point is excited and launch wavelength detection, 5 are the results are shown in Table, table 5 be reaction raw materials and
Product detection result.
The reaction raw materials of table 5 and product detection result
Embodiment 6
Using 3g citric acids and 6g carbamide, as reaction raw materials, used as reaction raw materials, (reaction raw materials mixed proportion is 1：2) it is, molten
Solution obtains colourless well-illuminated solution in the reaction dissolvent of 30ml.Wherein, the mixed solution of the reaction dissolvent water and DMF, its
In, the volume ratio of water and DMF is reacted according to the ratio shown in table 6 in reaction dissolvent.
By in the colourless transparent solution steel lining ptfe autoclave, airtight heating is carried out under conditions of 160 DEG C
Solvent thermal reaction 2 hours, obtains reaction mixture；
The reaction mixture is mixed with 60 milliliters of ethanol, is centrifuged 5 minutes with 8000 revs/min of rotating speed；In removal
Layer liquid (removes the reactant and reaction dissolvent of remnants), precipitation is dissolved in into repeated centrifugation 3 times in 60 milliliters of ethanol, to upper liquid
Till body is more thorough, precipitation, lyophilizing are taken, freeze temperature is -50 DEG C, and freeze-drying time is 36 hours, obtains fluorescent carbon nano dot.
The fluorescence nano carbon point is excited and launch wavelength detection, 6 are the results are shown in Table, table 6 be reaction raw materials and
Product detection result.
The reaction raw materials of table 6 and product detection result
Embodiment 7
Using 3g citric acids and 6g carbamide, as reaction raw materials, used as reaction raw materials, (reaction raw materials mixed proportion is 1：2) it is, molten
Solution obtains colourless well-illuminated solution in the reaction dissolvent of 30ml.Wherein, the mixed solution of the reaction dissolvent water and DMF, its
In, the volume ratio of water and DMF is reacted according to the ratio shown in table 7 in reaction dissolvent.
By in the colourless transparent solution steel lining ptfe autoclave, airtight heating is carried out under conditions of 160 DEG C
Solvent thermal reaction 8 hours, obtains reaction mixture；
The reaction mixture is mixed with 60 milliliters of ethanol, is centrifuged 5 minutes with 8000 revs/min of rotating speed；In removal
Layer liquid (removes the reactant and reaction dissolvent of remnants), precipitation is dissolved in into repeated centrifugation 3 times in 60 milliliters of ethanol, to upper liquid
Till body is more thorough, precipitation, lyophilizing are taken, freeze temperature is -50 DEG C, and freeze-drying time is 36 hours, obtains fluorescent carbon nano dot.
The fluorescence nano carbon point is excited and launch wavelength detection, 7 are the results are shown in Table, table 7 be reaction raw materials and
Product detection result.
The reaction raw materials of table 7 and product detection result
Embodiment 8
Using 3g citric acids and 3g carbamide, as reaction raw materials, used as reaction raw materials, (reaction raw materials mixed proportion is 1：1) it is, molten
Solution obtains colourless well-illuminated solution in the reaction dissolvent of 30ml.Wherein, the reaction dissolvent is molten for the mixing of water, DMSO and DMF
Liquid, wherein, the volume ratio of water, DMSO and DMF is reacted according to the ratio shown in table 8 in reaction dissolvent.
By in the colourless transparent solution steel lining ptfe autoclave, airtight heating is carried out under conditions of 160 DEG C
Solvent thermal reaction 4 hours, obtains reaction mixture；
The reaction mixture is mixed with 60 milliliters of ethanol, is centrifuged 5 minutes with 8000 revs/min of rotating speed；In removal
Layer liquid (removes the reactant and reaction dissolvent of remnants), precipitation is dissolved in into repeated centrifugation 3 times in 60 milliliters of ethanol, to upper liquid
Till body is more thorough, precipitation, lyophilizing are taken, freeze temperature is -50 DEG C, and freeze-drying time is 36 hours, obtains fluorescent carbon nano dot.
The fluorescence nano carbon point is excited and launch wavelength detection, 8 are the results are shown in Table, table 8 be reaction raw materials and
Product detection result.
The reaction raw materials of table 8 and product detection result
Embodiment 9
Using 3g citric acids and 6g carbamide, as reaction raw materials, used as reaction raw materials, (reaction raw materials mixed proportion is 1：2) it is, molten
Solution obtains colourless well-illuminated solution in the reaction dissolvent of 30ml.Wherein, the reaction dissolvent is molten for the mixing of water, DMSO and DMF
Liquid, wherein, the volume ratio of water, DMSO and DMF is reacted according to the ratio shown in table 9 in reaction dissolvent.
By in the colourless transparent solution steel lining ptfe autoclave, airtight heating is carried out under conditions of 160 DEG C
Solvent thermal reaction 4 hours, obtains reaction mixture；
The reaction mixture is mixed with 60 milliliters of ethanol, is centrifuged 5 minutes with 8000 revs/min of rotating speed；In removal
Layer liquid (removes the reactant and reaction dissolvent of remnants), precipitation is dissolved in into repeated centrifugation 3 times in 60 milliliters of ethanol, to upper liquid
Till body is more thorough, precipitation, lyophilizing are taken, freeze temperature is -50 DEG C, and freeze-drying time is 36 hours, obtains fluorescent carbon nano dot.
The fluorescence nano carbon point is excited and launch wavelength detection, 9 are the results are shown in Table, table 9 be reaction raw materials and
Product detection result.
The reaction raw materials of table 9 and product detection result
Embodiment 10
Using 3g citric acids and 9g carbamide, as reaction raw materials, used as reaction raw materials, (reaction raw materials mixed proportion is 1：3) it is, molten
Solution obtains colourless well-illuminated solution in the reaction dissolvent of 30ml.Wherein, the reaction dissolvent is molten for the mixing of water, DMSO and DMF
Liquid, wherein, the volume ratio of water, DMSO and DMF is reacted according to the ratio shown in table 10 in reaction dissolvent.
By in the colourless transparent solution steel lining ptfe autoclave, airtight heating is carried out under conditions of 160 DEG C
Solvent thermal reaction 4 hours, obtains reaction mixture；
The reaction mixture is mixed with 60 milliliters of ethanol, is centrifuged 5 minutes with 8000 revs/min of rotating speed；In removal
Layer liquid (removes the reactant and reaction dissolvent of remnants), precipitation is dissolved in into repeated centrifugation 3 times in 60 milliliters of ethanol, to upper liquid
Till body is more thorough, precipitation, lyophilizing are taken, freeze temperature is -50 DEG C, and freeze-drying time is 36 hours, obtains fluorescent carbon nano dot.
The fluorescence nano carbon point is excited and launch wavelength detection, 10 are the results are shown in Table, table 10 be reaction raw materials with
And product detection result.
The reaction raw materials of table 10 and product detection result
Embodiment 11
Using 3g citric acids and 6g carbamide, as reaction raw materials, used as reaction raw materials, (reaction raw materials mixed proportion is 1：2) it is, molten
Solution obtains colourless well-illuminated solution in the reaction dissolvent of 30ml.Wherein, the reaction dissolvent is molten for the mixing of water, DMSO and DMF
Liquid, wherein, the volume ratio of water, DMSO and DMF is reacted according to the ratio shown in table 11 in reaction dissolvent.
By in the colourless transparent solution steel lining ptfe autoclave, airtight heating is carried out under conditions of 120 DEG C
Solvent thermal reaction 4 hours, obtains reaction mixture；
The reaction mixture is mixed with 60 milliliters of ethanol, is centrifuged 5 minutes with 8000 revs/min of rotating speed；In removal
Layer liquid (removes the reactant and reaction dissolvent of remnants), precipitation is dissolved in into repeated centrifugation 3 times in 60 milliliters of ethanol, to upper liquid
Till body is more thorough, precipitation, lyophilizing are taken, freeze temperature is -50 DEG C, and freeze-drying time is 36 hours, obtains fluorescent carbon nano dot.
The fluorescence nano carbon point is excited and launch wavelength detection, 11 are the results are shown in Table, table 11 be reaction raw materials with
And product detection result.
The reaction raw materials of table 11 and product detection result
Embodiment 12
Using 3g citric acids and 6g carbamide, as reaction raw materials, used as reaction raw materials, (reaction raw materials mixed proportion is 1：2) it is, molten
Solution obtains colourless well-illuminated solution in the reaction dissolvent of 30ml.Wherein, the reaction dissolvent is molten for the mixing of water, DMSO and DMF
Liquid, wherein, the volume ratio of water, DMSO and DMF is reacted according to the ratio shown in table 12 in reaction dissolvent.
By in the colourless transparent solution steel lining ptfe autoclave, airtight heating is carried out under conditions of 180 DEG C
Solvent thermal reaction 4 hours, obtains reaction mixture；
The reaction mixture is mixed with 60 milliliters of ethanol, is centrifuged 5 minutes with 8000 revs/min of rotating speed；In removal
Layer liquid (removes the reactant and reaction dissolvent of remnants), precipitation is dissolved in into repeated centrifugation 3 times in 60 milliliters of ethanol, to upper liquid
Till body is more thorough, precipitation, lyophilizing are taken, freeze temperature is -50 DEG C, and freeze-drying time is 36 hours, obtains fluorescent carbon nano dot.
The fluorescence nano carbon point is excited and launch wavelength detection, 12 are the results are shown in Table, table 12 be reaction raw materials with
And product detection result.
The reaction raw materials of table 12 and product detection result
Embodiment 13
Using 3g citric acids and 6g carbamide, as reaction raw materials, used as reaction raw materials, (reaction raw materials mixed proportion is 1：2) it is, molten
Solution obtains colourless well-illuminated solution in the reaction dissolvent of 30ml.Wherein, the reaction dissolvent is molten for the mixing of water, DMSO and DMF
Liquid, wherein, the volume ratio of water, DMSO and DMF is reacted according to the ratio shown in table 13 in reaction dissolvent.
By in the colourless transparent solution steel lining ptfe autoclave, airtight heating is carried out under conditions of 160 DEG C
Solvent thermal reaction 2 hours, obtains reaction mixture；
The reaction mixture is mixed with 60 milliliters of ethanol, is centrifuged 5 minutes with 8000 revs/min of rotating speed；In removal
Layer liquid (removes the reactant and reaction dissolvent of remnants), precipitation is dissolved in into repeated centrifugation 3 times in 60 milliliters of ethanol, to upper liquid
Till body is more thorough, precipitation, lyophilizing are taken, freeze temperature is -50 DEG C, and freeze-drying time is 36 hours, obtains fluorescent carbon nano dot.
The fluorescence nano carbon point is excited and launch wavelength detection, 13 are the results are shown in Table, table 13 be reaction raw materials with
And product detection result.
The reaction raw materials of table 13 and product detection result
Embodiment 14
Using 3g citric acids and 6g carbamide, as reaction raw materials, used as reaction raw materials, (reaction raw materials mixed proportion is 1：2) it is, molten
Solution obtains colourless well-illuminated solution in the reaction dissolvent of 30ml.Wherein, the reaction dissolvent is molten for the mixing of water, DMSO and DMF
Liquid, wherein, the volume ratio of water, DMSO and DMF is reacted according to the ratio shown in table 14 in reaction dissolvent.
By in the colourless transparent solution steel lining ptfe autoclave, airtight heating is carried out under conditions of 160 DEG C
Solvent thermal reaction 8 hours, obtains reaction mixture；
The reaction mixture is mixed with 60 milliliters of ethanol, is centrifuged 5 minutes with 8000 revs/min of rotating speed；In removal
Layer liquid (removes the reactant and reaction dissolvent of remnants), precipitation is dissolved in into repeated centrifugation 3 times in 60 milliliters of ethanol, to upper liquid
Till body is more thorough, precipitation, lyophilizing are taken, freeze temperature is -50 DEG C, and freeze-drying time is 36 hours, obtains fluorescent carbon nano dot.
The fluorescence nano carbon point is excited and launch wavelength detection, 14 are the results are shown in Table, table 14 be reaction raw materials with
And product detection result.
The reaction raw materials of table 14 and product detection result
Embodiment 15
Using 3g citric acids and 3g carbamide, as reaction raw materials, used as reaction raw materials, (reaction raw materials mixed proportion is 1：1) it is, molten
Solution obtains colourless well-illuminated solution in the reaction dissolvent of 30ml.Wherein, the reaction dissolvent is molten for the mixing of water, glycerol and DMF
Liquid, wherein, the volume ratio of water, glycerol and DMF is reacted according to the ratio shown in table 15 in reaction dissolvent.
By in the colourless transparent solution steel lining ptfe autoclave, airtight heating is carried out under conditions of 160 DEG C
Solvent thermal reaction 4 hours, obtains reaction mixture；
The reaction mixture is mixed with 60 milliliters of ethanol, is centrifuged 5 minutes with 8000 revs/min of rotating speed；In removal
Layer liquid (removes the reactant and reaction dissolvent of remnants), precipitation is dissolved in into repeated centrifugation 3 times in 60 milliliters of ethanol, to upper liquid
Till body is more thorough, precipitation, lyophilizing are taken, freeze temperature is -50 DEG C, and freeze-drying time is 36 hours, obtains fluorescent carbon nano dot.
The fluorescence nano carbon point is excited and launch wavelength detection, 15 are the results are shown in Table, table 15 be reaction raw materials with
And product detection result.
The reaction raw materials of table 15 and product detection result
Embodiment 16
Using 3g citric acids and 6g carbamide, as reaction raw materials, used as reaction raw materials, (reaction raw materials mixed proportion is 1：2) it is, molten
Solution obtains colourless well-illuminated solution in the reaction dissolvent of 30ml.Wherein, the reaction dissolvent is molten for the mixing of water, glycerol and DMF
Liquid, wherein, the volume ratio of water, glycerol and DMF is reacted according to the ratio shown in table 16 in reaction dissolvent.
By in the colourless transparent solution steel lining ptfe autoclave, airtight heating is carried out under conditions of 160 DEG C
Solvent thermal reaction 4 hours, obtains reaction mixture, the i.e. original solution of fluorescence nano carbon point；
The reaction mixture is mixed with 60 milliliters of ethanol, is centrifuged 5 minutes with 8000 revs/min of rotating speed；In removal
Layer liquid (removes the reactant and reaction dissolvent of remnants), precipitation is dissolved in into repeated centrifugation 3 times in 60 milliliters of ethanol, to upper liquid
Till body is more thorough, precipitation, lyophilizing are taken, freeze temperature is -50 DEG C, and freeze-drying time is 36 hours, obtains fluorescent carbon nano dot.
Optics is carried out under conditions of daylight and uviol lamp to the original solution of the above-mentioned fluorescence nano carbon point for preparing
Take pictures, as a result see Fig. 1, Fig. 1 be the fluorescence nano carbon point for preparing of embodiment 16 daylight (on) and ultraviolet light (under) under the conditions of
Optical photograph.Wherein, 7 quartz colorimetric utensils of Fig. 1 middle and upper parts point hold respectively the fluorescence nano carbon point of CDot1～CDot7
Original solution optical photograph in the sunlight, from left to right respectively CDot 1, CDot 2, CDot 3, CDot 4, CDot 5,
CDot6、CDot 7；7 quartz colorimetric utensils of lower part are the original solution of the fluorescence nano carbon point of CDot1～CDot7 ultraviolet
Optical photograph under the conditions of lamp, from left to right respectively CDot1, CDot 2, CDot 3, CDot 4, CDot 5, CDot 6,
CDot 7.As shown in Figure 1, the nano-sized carbon point that the present invention is prepared has the good characteristics of luminescence, under the conditions of uviol lamp, can
So that navy blue, blueness, cyan, green, yellow, orange, redness is presented.
The original solution of the above-mentioned fluorescence nano carbon point for preparing is carried out into fluoroscopic examination in the case where 365nm is excited, is as a result seen
Fig. 2, Fig. 2 are the fluorescence spectrum under the original solution of the fluorescent carbon nano dot that embodiment 16 is prepared is excited at 365 nanometers.
The above-mentioned fluorescent carbon nano dot for preparing is carried out into transmission electron microscope (TEM) and high-resolution transmitted electron is aobvious
Micro mirror is observed, and carries out particle diameter statistics, as a result sees that Fig. 3, Fig. 3 are fluorescent carbon nano dot CDot 1, CDot prepared by embodiment 16
4 and CDot 7 transmission electron microscope (TEM) and high resolution transmission electron microscopy (HRTEM) photo and its particle diameter statistics are directly
Fang Tu.Wherein, a：CDot 1；b：CDot 4；c：CDot 7.From the figure 3, it may be seen that the chi of carbon nano dot that the present invention is prepared
It is very little between 0～10 nanometer, and be 0.
Atomic force microscopy observation is carried out to the above-mentioned fluorescent carbon nano dot (CDot 4) for preparing, Fig. 4, Fig. 4 is as a result seen
The atomic force micrograph (AFM) of the carbon nano dot CDot 4 to prepare in embodiment 16.As shown in Figure 4, the particle diameter of CDot 4
For 2～5 nanometers
X-ray photoelectron spectroscopic analysis are carried out to the above-mentioned nano-sized carbon point CDot 1, CDot 4 and CDot 7 for preparing
(XPS), as a result see that Fig. 5, Fig. 5 are the x-ray photoelectron of nano-sized carbon point CDot 1, CDot 4 and CDot 7 prepared by embodiment 16
Energy spectrum analysiss (XPS) figure, wherein, a：Quan Pu；b：Oxygen element is composed.
The fluorescence nano carbon point of above-mentioned preparation is excited and is determined with launch wavelength detection and fluorescence quantum efficiency, knot
Fruit sees respectively Fig. 6 and Biao 16, and table 16 is reaction raw materials and product detection result.Fig. 6 is that fluorescent carbon prepared by embodiment 16 is received
The absorption spectrum of nanodot aqueous solution and optimum emission spectrum.
The reaction raw materials of table 16 and product detection result
Embodiment 17
Using 3g citric acids and 9g carbamide, as reaction raw materials, used as reaction raw materials, (reaction raw materials mixed proportion is 1：3) it is, molten
Solution obtains colourless well-illuminated solution in the reaction dissolvent of 30ml.Wherein, the reaction dissolvent is molten for the mixing of water, glycerol and DMF
Liquid, wherein, the volume ratio of water, glycerol and DMF is reacted according to the ratio shown in table 17 in reaction dissolvent.
By in the colourless transparent solution steel lining ptfe autoclave, airtight heating is carried out under conditions of 160 DEG C
Solvent thermal reaction 4 hours, obtains reaction mixture；
The reaction mixture is mixed with 60 milliliters of ethanol, is centrifuged 5 minutes with 8000 revs/min of rotating speed；In removal
Layer liquid (removes the reactant and reaction dissolvent of remnants), precipitation is dissolved in into repeated centrifugation 3 times in 60 milliliters of ethanol, to upper liquid
Till body is more thorough, precipitation, lyophilizing are taken, freeze temperature is -50 DEG C, and freeze-drying time is 36 hours, obtains fluorescent carbon nano dot.
The fluorescence nano carbon point is excited and launch wavelength detection, 17 are the results are shown in Table, table 17 be reaction raw materials with
And product detection result.
The reaction raw materials of table 17 and product detection result
Embodiment 18
Using 3g citric acids and 6g carbamide, as reaction raw materials, used as reaction raw materials, (reaction raw materials mixed proportion is 1：2) it is, molten
Solution obtains colourless well-illuminated solution in the reaction dissolvent of 30ml.Wherein, the reaction dissolvent is molten for the mixing of water, glycerol and DMF
Liquid, wherein, the volume ratio of water, glycerol and DMF is reacted according to the ratio shown in table 18 in reaction dissolvent.
By in the colourless transparent solution steel lining ptfe autoclave, airtight heating is carried out under conditions of 120 DEG C
Solvent thermal reaction 4 hours, obtains reaction mixture；
The reaction mixture is mixed with 60 milliliters of ethanol, is centrifuged 5 minutes with 8000 revs/min of rotating speed；In removal
Layer liquid (removes the reactant and reaction dissolvent of remnants), precipitation is dissolved in into repeated centrifugation 3 times in 60 milliliters of ethanol, to upper liquid
Till body is more thorough, precipitation, lyophilizing are taken, freeze temperature is -50 DEG C, and freeze-drying time is 36 hours, obtains fluorescent carbon nano dot.
The fluorescence nano carbon point is excited and launch wavelength detection, 18 are the results are shown in Table, table 18 be reaction raw materials with
And product detection result.
The reaction raw materials of table 18 and product detection result
Embodiment 19
Using 3g citric acids and 6g carbamide, as reaction raw materials, used as reaction raw materials, (reaction raw materials mixed proportion is 1：2) it is, molten
Solution obtains colourless well-illuminated solution in the reaction dissolvent of 30ml.Wherein, the reaction dissolvent is molten for the mixing of water, glycerol and DMF
Liquid, wherein, the volume ratio of water, glycerol and DMF is reacted according to the ratio shown in table 19 in reaction dissolvent.
By in the colourless transparent solution steel lining ptfe autoclave, airtight heating is carried out under conditions of 180 DEG C
Solvent thermal reaction 4 hours, obtains reaction mixture；
The reaction mixture is mixed with 60 milliliters of ethanol, is centrifuged 5 minutes with 8000 revs/min of rotating speed；In removal
Layer liquid (removes the reactant and reaction dissolvent of remnants), precipitation is dissolved in into repeated centrifugation 3 times in 60 milliliters of ethanol, to upper liquid
Till body is more thorough, precipitation, lyophilizing are taken, freeze temperature is -50 DEG C, and freeze-drying time is 36 hours, obtains fluorescent carbon nano dot.
The fluorescence nano carbon point is excited and launch wavelength detection, 19 are the results are shown in Table, table 19 be reaction raw materials with
And product detection result.
The reaction raw materials of table 19 and product detection result
Embodiment 20
Using 3g citric acids and 6g carbamide, as reaction raw materials, used as reaction raw materials, (reaction raw materials mixed proportion is 1：2) it is, molten
Solution obtains colourless well-illuminated solution in the reaction dissolvent of 30ml.Wherein, the reaction dissolvent is molten for the mixing of water, glycerol and DMF
Liquid, wherein, the volume ratio of water, glycerol and DMF is reacted according to the ratio shown in table 20 in reaction dissolvent.
By in the colourless transparent solution steel lining ptfe autoclave, airtight heating is carried out under conditions of 160 DEG C
Solvent thermal reaction 2 hours, obtains reaction mixture；
The reaction mixture is mixed with 60 milliliters of ethanol, is centrifuged 5 minutes with 8000 revs/min of rotating speed；In removal
Layer liquid (removes the reactant and reaction dissolvent of remnants), precipitation is dissolved in into repeated centrifugation 3 times in 60 milliliters of ethanol, to upper liquid
Till body is more thorough, precipitation, lyophilizing are taken, freeze temperature is -50 DEG C, and freeze-drying time is 36 hours, obtains fluorescent carbon nano dot.
The fluorescence nano carbon point is excited and launch wavelength detection, 20 are the results are shown in Table, table 20 be reaction raw materials with
And product detection result.
The reaction raw materials of table 20 and product detection result
Embodiment 21
Using 3g citric acids and 6g carbamide, as reaction raw materials, used as reaction raw materials, (reaction raw materials mixed proportion is 1：2) it is, molten
Solution obtains colourless well-illuminated solution in the reaction dissolvent of 30ml.Wherein, the reaction dissolvent is molten for the mixing of water, glycerol and DMF
Liquid, wherein, the volume ratio of water, glycerol and DMF is reacted according to the ratio shown in table 21 in reaction dissolvent.
By in the colourless transparent solution steel lining ptfe autoclave, airtight heating is carried out under conditions of 160 DEG C
Solvent thermal reaction 4 hours, obtains reaction mixture；
The reaction mixture is mixed with 60 milliliters of ethanol, is centrifuged 5 minutes with 8000 revs/min of rotating speed；In removal
Layer liquid (removes the reactant and reaction dissolvent of remnants), precipitation is dissolved in into repeated centrifugation 3 times in 60 milliliters of ethanol, to upper liquid
Till body is more thorough, precipitation, lyophilizing are taken, freeze temperature is -50 DEG C, and freeze-drying time is 36 hours, obtains fluorescent carbon nano dot.
The fluorescence nano carbon point is excited and launch wavelength detection, 21 are the results are shown in Table, table 21 be reaction raw materials with
And product detection result.
The reaction raw materials of table 21 and product detection result
Embodiment 22
Using 3g citric acids and 3g carbamide, as reaction raw materials, used as reaction raw materials, (reaction raw materials mixed proportion is 1：1) it is, molten
Solution obtains colourless well-illuminated solution in the reaction dissolvent of 30ml.Wherein, the reaction dissolvent be water, glycerol, acetic acid, DMSO and
The mixed solution of DMF, wherein, the volume ratio of water, glycerol, acetic acid, DMSO and DMF is according to the ratio shown in table 22 in reaction dissolvent
Example is reacted.
By in the colourless transparent solution steel lining ptfe autoclave, airtight heating is carried out under conditions of 160 DEG C
Solvent thermal reaction 4 hours, obtains reaction mixture；
The reaction mixture is mixed with 60 milliliters of ethanol, is centrifuged 5 minutes with 8000 revs/min of rotating speed；In removal
Layer liquid (removes the reactant and reaction dissolvent of remnants), precipitation is dissolved in into repeated centrifugation 3 times in 60 milliliters of ethanol, to upper liquid
Till body is more thorough, precipitation, lyophilizing are taken, freeze temperature is -50 DEG C, and freeze-drying time is 36 hours, obtains fluorescent carbon nano dot.
The fluorescence nano carbon point is excited and launch wavelength detection, 22 are the results are shown in Table, table 22 be reaction raw materials with
And product detection result.
The reaction raw materials of table 22 and product detection result
Embodiment 23
Using 3g citric acids and 6g carbamide, as reaction raw materials, used as reaction raw materials, (reaction raw materials mixed proportion is 1：2) it is, molten
Solution obtains colourless well-illuminated solution in the reaction dissolvent of 30ml.Wherein, the reaction dissolvent be water, glycerol, acetic acid, DMSO and
The mixed solution of DMF, wherein, the volume ratio of water, glycerol, acetic acid, DMSO and DMF is according to the ratio shown in table 23 in reaction dissolvent
Example is reacted.
By in the colourless transparent solution steel lining ptfe autoclave, airtight heating is carried out under conditions of 160 DEG C
Solvent thermal reaction 4 hours, obtains reaction mixture；
The reaction mixture is mixed with 60 milliliters of ethanol, is centrifuged 5 minutes with 8000 revs/min of rotating speed；In removal
Layer liquid (removes the reactant and reaction dissolvent of remnants), precipitation is dissolved in into repeated centrifugation 3 times in 60 milliliters of ethanol, to upper liquid
Till body is more thorough, precipitation, lyophilizing are taken, freeze temperature is -50 DEG C, and freeze-drying time is 36 hours, obtains fluorescent carbon nano dot.
The fluorescence nano carbon point is excited and launch wavelength detection, 23 are the results are shown in Table, table 23 be reaction raw materials with
And product detection result.
The reaction raw materials of table 23 and product detection result
Embodiment 24
Using 3g citric acids and 9g carbamide, as reaction raw materials, used as reaction raw materials, (reaction raw materials mixed proportion is 1：3) it is, molten
Solution obtains colourless well-illuminated solution in the reaction dissolvent of 30ml.Wherein, the reaction dissolvent be water, glycerol, acetic acid, DMSO and
The mixed solution of DMF, wherein, the volume ratio of water, glycerol, acetic acid, DMSO and DMF is according to the ratio shown in table 24 in reaction dissolvent
Example is reacted.
By in the colourless transparent solution steel lining ptfe autoclave, airtight heating is carried out under conditions of 160 DEG C
Solvent thermal reaction 4 hours, obtains reaction mixture；
The reaction mixture is mixed with 60 milliliters of ethanol, is centrifuged 5 minutes with 8000 revs/min of rotating speed；In removal
Layer liquid (removes the reactant and reaction dissolvent of remnants), precipitation is dissolved in into repeated centrifugation 3 times in 60 milliliters of ethanol, to upper liquid
Till body is more thorough, precipitation, lyophilizing are taken, freeze temperature is -50 DEG C, and freeze-drying time is 36 hours, obtains fluorescent carbon nano dot.
The fluorescence nano carbon point is excited and launch wavelength detection, 24 are the results are shown in Table, table 24 be reaction raw materials with
And product detection result.
The reaction raw materials of table 24 and product detection result
Embodiment 25
Using 3g citric acids and 6g carbamide, as reaction raw materials, used as reaction raw materials, (reaction raw materials mixed proportion is 1：2) it is, molten
Solution obtains colourless well-illuminated solution in the reaction dissolvent of 30ml.Wherein, the reaction dissolvent be water, glycerol, acetic acid, DMSO and
The mixed solution of DMF, wherein, the volume ratio of water, glycerol, acetic acid, DMSO and DMF is according to the ratio shown in table 25 in reaction dissolvent
Example is reacted.
By in the colourless transparent solution steel lining ptfe autoclave, airtight heating is carried out under conditions of 120 DEG C
Solvent thermal reaction 4 hours, obtains reaction mixture；
The reaction mixture is mixed with 60 milliliters of ethanol, is centrifuged 5 minutes with 8000 revs/min of rotating speed；In removal
Layer liquid (removes the reactant and reaction dissolvent of remnants), precipitation is dissolved in into repeated centrifugation 3 times in 60 milliliters of ethanol, to upper liquid
Till body is more thorough, precipitation, lyophilizing are taken, freeze temperature is -50 DEG C, and freeze-drying time is 36 hours, obtains fluorescent carbon nano dot.
The fluorescence nano carbon point is excited and launch wavelength detection, 25 are the results are shown in Table, table 25 be reaction raw materials with
And product detection result.
The reaction raw materials of table 25 and product detection result
Embodiment 26
Using 3g citric acids and 6g carbamide, as reaction raw materials, used as reaction raw materials, (reaction raw materials mixed proportion is 1：2) it is, molten
Solution obtains colourless well-illuminated solution in the reaction dissolvent of 30ml.Wherein, the reaction dissolvent be water, glycerol, acetic acid, DMSO and
The mixed solution of DMF, wherein, the volume ratio of water, glycerol, acetic acid, DMSO and DMF is according to the ratio shown in table 26 in reaction dissolvent
Example is reacted.
By in the colourless transparent solution steel lining ptfe autoclave, airtight heating is carried out under conditions of 180 DEG C
Solvent thermal reaction 4 hours, obtains reaction mixture；
The reaction mixture is mixed with 60 milliliters of ethanol, is centrifuged 5 minutes with 8000 revs/min of rotating speed；In removal
Layer liquid (removes the reactant and reaction dissolvent of remnants), precipitation is dissolved in into repeated centrifugation 3 times in 60 milliliters of ethanol, to upper liquid
Till body is more thorough, precipitation, lyophilizing are taken, freeze temperature is -50 DEG C, and freeze-drying time is 36 hours, obtains fluorescent carbon nano dot.
The fluorescence nano carbon point is excited and launch wavelength detection, 26 are the results are shown in Table, table 26 be reaction raw materials with
And product detection result.
The reaction raw materials of table 26 and product detection result
Embodiment 27
Using 3g citric acids and 6g carbamide, as reaction raw materials, used as reaction raw materials, (reaction raw materials mixed proportion is 1：3) it is, molten
Solution obtains colourless well-illuminated solution in the reaction dissolvent of 30ml.Wherein, the reaction dissolvent be water, glycerol, acetic acid, DMSO and
The mixed solution of DMF, wherein, the volume ratio of water, glycerol, acetic acid, DMSO and DMF is according to the ratio shown in table 27 in reaction dissolvent
Example is reacted.
By in the colourless transparent solution steel lining ptfe autoclave, airtight heating is carried out under conditions of 160 DEG C
Solvent thermal reaction 2 hours, obtains reaction mixture；
The reaction mixture is mixed with 60 milliliters of ethanol, is centrifuged 5 minutes with 8000 revs/min of rotating speed；In removal
Layer liquid (removes the reactant and reaction dissolvent of remnants), precipitation is dissolved in into repeated centrifugation 3 times in 60 milliliters of ethanol, to upper liquid
Till body is more thorough, precipitation, lyophilizing are taken, freeze temperature is -50 DEG C, and freeze-drying time is 36 hours, obtains fluorescent carbon nano dot.
The fluorescence nano carbon point is excited and launch wavelength detection, 27 are the results are shown in Table, table 27 be reaction raw materials with
And product detection result.
The reaction raw materials of table 27 and product detection result
Embodiment 28
Using 3g citric acids and 6g carbamide, as reaction raw materials, used as reaction raw materials, (reaction raw materials mixed proportion is 1：2) it is, molten
Solution obtains colourless well-illuminated solution in the reaction dissolvent of 30ml.Wherein, the reaction dissolvent be water, glycerol, acetic acid, DMSO and
The mixed solution of DMF, wherein, the volume ratio of water, glycerol, acetic acid, DMSO and DMF is according to the ratio shown in table 28 in reaction dissolvent
Example is reacted.
By in the colourless transparent solution steel lining ptfe autoclave, airtight heating is carried out under conditions of 160 DEG C
Solvent thermal reaction 8 hours, obtains reaction mixture；
The reaction mixture is mixed with 60 milliliters of ethanol, is centrifuged 5 minutes with 8000 revs/min of rotating speed；In removal
Layer liquid (removes the reactant and reaction dissolvent of remnants), precipitation is dissolved in into repeated centrifugation 3 times in 60 milliliters of ethanol, to upper liquid
Till body is more thorough, precipitation, lyophilizing are taken, freeze temperature is -50 DEG C, and freeze-drying time is 36 hours, obtains fluorescent carbon nano dot.
The fluorescence nano carbon point is excited and launch wavelength detection, 28 are the results are shown in Table, table 28 be reaction raw materials with
And product detection result.
The reaction raw materials of table 28 and product detection result
The above is only the preferred embodiment of the present invention, it is noted that for the ordinary skill people of the art
For member, under the premise without departing from the principles of the invention, some improvements and modifications can also be made, these improvements and modifications also should
It is considered as protection scope of the present invention.
Claims (10)
1. a kind of full spectral coverage in visual field lights the preparation method of adjustable carbon nano dot, it is characterised in that comprise the following steps：
Citric acid and carbamide are dissolved in reaction dissolvent carries out solvent thermal reaction, obtains carbon nano dot；
The reaction dissolvent include protonic solvent and/or non-protonic solvent miscible with water miscible with water in one kind or
Various and water；
One or more in the protonic solvent miscible with water and/or non-protonic solvent miscible with water and water it is mixed
Composition and division in a proportion example is 0～100%；
The mixed proportion of the protonic solvent miscible with water and non-protonic solvent miscible with water is 0～100%.
2. preparation method according to claim 1, it is characterised in that the protonic solvent miscible with water is selected from containing hydroxyl
The organic solvent of base or carboxylic organic solvent.
3. preparation method according to claim 1, it is characterised in that the protonic solvent miscible with water is selected from first
One or more in alcohol, ethanol, ethylene glycol, glycerol, acetic acid and oxalic acid.
4. preparation method according to claim 1, it is characterised in that the non-protonic solvent miscible with water is selected from two
One or more in methyl sulfoxide, N,N-dimethylformamide, dimethyl acetylamide, acetonitrile and acetone.
5. preparation method according to claim 1, it is characterised in that the non-protonic solvent miscible with water is selected from two
Methyl sulfoxide and/or N,N-dimethylformamide.
6. preparation method according to claim 1, it is characterised in that the reaction dissolvent is selected from water and N, N- dimethyl methyl
The reaction dissolvent that amide is formed, the reaction dissolvent that water and dimethyl sulfoxide are formed, dimethyl sulfoxide, DMF with
The reaction that the reaction dissolvent that water is formed, the reaction dissolvent that water is formed with glycerol, glycerol and DMF are formed with water
The reaction that one or more in solvent or glycerol, acetic acid, dimethyl sulfoxide and N,N-dimethylformamide is formed with water is molten
Agent.
7. preparation method according to claim 1, it is characterised in that the citric acid is 1 with the mass ratio of carbamide：(1～
3)。
8. preparation method according to claim 1, it is characterised in that the temperature of the solvent thermal reaction is 120～200
DEG C, the time of the solvent thermal reaction is 2～8 hours.
9. preparation method according to claim 1, it is characterised in that after solvent thermal reaction is carried out, also include institute
State product to be purified.
10. the full spectral coverage in visual field that a kind of preparation method as claimed in any one of claims 1 to 9 wherein is prepared lights adjustable
Carbon nano dot.
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