CN111592882A - Method for synthesizing carbon quantum dots by using hydrolyzed polymaleic anhydride as main raw material - Google Patents

Method for synthesizing carbon quantum dots by using hydrolyzed polymaleic anhydride as main raw material Download PDF

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CN111592882A
CN111592882A CN202010501685.3A CN202010501685A CN111592882A CN 111592882 A CN111592882 A CN 111592882A CN 202010501685 A CN202010501685 A CN 202010501685A CN 111592882 A CN111592882 A CN 111592882A
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carbon quantum
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刘晓伟
王家庚
高灿柱
李小明
杨春丽
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Abstract

The invention discloses a method for synthesizing carbon quantum dots by using hydrolyzed polymaleic anhydride as a main raw material, which comprises the following steps: dissolving hydrolyzed polymaleic anhydride (HPMA) as a raw material in deionized water, and uniformly stirring; adding organic amine solution into the system, and carrying out closed hydrothermal reaction at 140-230 ℃; and after the reaction is finished, cooling and filtering the reaction solution to obtain the fluorescent carbon quantum dot solution. The fluorescent carbon quantum dots obtained by the method are in blue fluorescence emission under an ultraviolet light source, and have the advantages of good water solubility, stable chemical properties, simple synthesis method, low raw material cost and the like.

Description

Method for synthesizing carbon quantum dots by using hydrolyzed polymaleic anhydride as main raw material
Technical Field
The invention belongs to the technical field of fluorescent materials, and particularly relates to a method for synthesizing carbon quantum dots by hydrolyzing polymaleic anhydride.
Background
The preparation of Carbon Quantum Dots (CQDs) adopts two methods of top-down and bottom-up, wherein the carbon quantum dots are prepared from top to bottom and are peeled from a large-size carbon target into powder; various synthetic methods for CQDs including arc discharge, laser ablation, electrochemical methods, microwave heating, etc. have been developed, but some methods require complicated equipment or complicated treatment processes. The bottom-up preparation is self-assembled from small-sized carbon sources through weak interaction; the carbon quantum dots synthesized by the bottom-up method mostly adopt organic small molecules or oligomers as carbon sources, and commonly used organic small molecules or oligomers comprise citric acid, glucose, polyethylene glycol, urea, ionic liquid and the like. Common bottom-up synthesis methods include chemical oxidation, combustion, hydrothermal/solvothermal, microwave synthesis, template, and the like. The method has the advantages of cheap equipment and simple operation steps, and is widely applied in recent years.
CQDs is represented by sp2And sp3A conjugated system consisting of hybridized carbon atoms and a large number of oxygen-containing groups. In 2014, xu moon and the like break the wall of the apple and stir the apple into juice, and the juice is heated, filtered and centrifuged in a polytetrafluoroethylene high-pressure reaction kettle to prepare pure carbon quantum dot solution. Researchers have adopted various biological materials such as grass (Liu S et al, 2012), waste paper (Wei J et al, 2014), grape juice (Huang H et al, 2014), orange juice (Sahu S et al, 2012), etc. as carbon sources for hydrothermal synthesis of CQDs, which exhibit blue or green fluorescence. CQDs quantum yield of CQDs obtained by Zhu Georgi et al through citric acid and ethylenediamine hydrothermal treatment and dialysis is as high as 80% (patent publication No. CN 103045242A).
There are also many reports on patents for carbon quantum dots, such as: CN109896517A discloses a blue fluorescent carbon quantum dot and a preparation method and application thereof, CN109880620A discloses a preparation method and application of a green fluorescent carbon quantum dot using biomass as a precursor, and CN107502349A discloses a preparation method of a water-soluble yellow fluorescent carbon quantum dot. CQDs synthesized by adopting different raw materials have different surface functional groups and have great difference in performance, which is important connected with the application of the CQDs. Hydrolyzed polymaleic anhydride (HPMA) is a low molecular weight polyelectrolyte, and the HPMA has excellent scale inhibition performance and high temperature resistance, so the hydrolyzed polymaleic anhydride (HPMA) is widely used in low-pressure boilers, water and oil pipelines and industrial circulating cooling water. However, at present, there is no patent or literature report related to the synthesis of carbon quantum dots from low molecular materials such as polymaleic anhydride.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides a preparation method of a fluorescent carbon quantum dot with stable fluorescence performance and excellent water solubility.
The technical scheme of the invention is as follows:
a method for synthesizing carbon quantum dots by using hydrolyzed polymaleic anhydride as a main raw material comprises the following steps:
dissolving hydrolyzed polymaleic anhydride (HPMA) as a raw material in deionized water, and uniformly stirring;
adding organic amine solution into the system, and carrying out closed hydrothermal reaction at 140-230 ℃;
and after the reaction is finished, cooling and filtering the reaction solution to obtain the fluorescent carbon quantum dot solution.
According to the invention, preferably, the HPMA has a relative molecular weight of 400-800, and is a low molecular weight polyelectrolyte.
Preferably, the mass ratio of the HPMA to the deionized water is 1: (10-120).
According to the present invention, preferably, the organic amine is Ethylenediamine (EN), diethylenetriamine or triethylenetetramine.
According to the invention, the hydrothermal reaction time is preferably 5h to 50h, more preferably 10h to 36 h.
According to the invention, the mass ratio of the HPMA to the organic amine is preferably (0.3-4): 1, more preferably (0.5 to 3): 1, most preferably 2: 1.
According to the present invention, the reaction temperature of the hydrothermal reaction is preferably 140 to 230 ℃, and more preferably 180 to 230 ℃.
According to the invention, the filter membrane used for filtration has a pore size specification of
Figure BDA0002525064210000021
And (5) filtering the membrane.
According to the invention, preferably, the prepared fluorescent carbon quantum dot solution is scanned by an absorption spectrum to obtain a characteristic absorption peak of 327nm of the carbon quantum dot.
According to the invention, preferably, the prepared fluorescent carbon quantum dot solution is scanned by a 3D fluorescence spectrum to obtain the carbon quantum dot lambdaEX253nm and λEXAt 327nm, at λEMStrong fluorescence is emitted at 400 nm.
According to the present invention, a preferred embodiment comprises the steps of:
(1) 3.3333g of HPMA (Tech, 50%) is weighed and dissolved in 45.8334g of deionized water, and the mixture is stirred uniformly;
(2) 0.8333g of ethylenediamine (Tech, 99%) solution (mass ratio HPMA/EN is 2:1) is added into the system, mixed uniformly and placed in a closed hydrothermal reaction synthesis kettle;
(3) placing the reaction kettle in an oven, heating to 180 ℃, reacting for 5 hours, and naturally cooling to room temperature to obtain a brown yellow liquid;
(4) the brown yellow liquid is passed through
Figure BDA0002525064210000022
And filtering by using a microporous filtering membrane to obtain the fluorescent carbon quantum dot solution.
The invention has the beneficial effects that:
1. according to the invention, HPMA is adopted to synthesize the fluorescent carbon quantum dots, the raw materials are cheap and easy to obtain, the fluorescent carbon quantum dots contain a large amount of carboxyl structures and are easy to polymerize with amino groups, and the light intensity of the carbon quantum dots is improved; the raw materials are biodegradable, environment-friendly, low in toxicity and free of pollution; the preparation process is simple and can be mass-produced in large scale.
2. The fluorescent carbon quantum dot obtained by the invention emits blue fluorescence under an ultraviolet light source, and the carbon quantum dot lambda is obtained by scanning through a 3D fluorescence spectrumEX253nm and λEXAt 327nm, at λEMStrong fluorescence is emitted at 400 nm. 3. The fluorescent carbon quantum dot obtained by the method has good water solubility and stable chemical property, and residual chlorine cannot influence the fluorescence intensity of the carbon quantum dot within a certain concentration range; the synthetic method is simpleThe fluorescent probe has the advantages of low cost of raw materials, environmental protection, low toxicity and the like, and can be used for water body detection and the like as the fluorescent probe.
Drawings
FIG. 1 is a diagram showing the UV-VIS absorption spectrum of the fluorescent carbon quantum dot obtained in example 1.
Fig. 2 is a 3D fluorescence spectrum of the fluorescent carbon quantum dots obtained in example 1.
FIG. 3 is a standard curve of fluorescence intensity versus concentration of the fluorescent carbon quantum dots obtained in example 1.
FIG. 4 is a graph showing the influence of mass ratio (HPMA/EN) of fluorescent carbon quantum dot raw materials on the fluorescence performance of carbon quantum dots obtained in examples 1 to 5 and comparative examples 1 to 4.
FIG. 5 is a graph showing the influence of the reaction time of the fluorescent carbon quantum dots on the fluorescence properties of the carbon quantum dots obtained in examples 1 and 6 to 9.
FIG. 6 is a graph showing the influence of the reaction temperature of the fluorescent carbon quantum dots on the fluorescence properties of the carbon quantum dots obtained in example 1 and comparative examples 5 to 8.
FIG. 7 is a graph showing the interference of NaClO in test example 4 with the fluorescent carbon quantum dots obtained in example 1.
Detailed Description
In order to further explain the meaning of the present invention, the following examples are given to explain the contents of the present invention, but the contents are not limited thereto. The raw materials used in the examples are all conventional commercial products.
The HPMA (Tech, 50%) used in the examples was technical grade at a mass concentration of 50%.
Example 1
The embodiment provides a method for synthesizing carbon quantum dots by hydrolyzing polymaleic anhydride, which comprises the following steps:
2.5000g of HPMA (Tech, 50%) is weighed and dissolved in 46.2500g of deionized water, and the mixture is stirred uniformly;
adding 1.2626g of ethylenediamine (Tech, 99%) solution (the mass ratio of HPMA/EN is 1:1) into the system, uniformly mixing, and placing in a closed hydrothermal reaction synthesis kettle;
placing the reaction kettle in an oven, heating to 180 ℃, reacting for 5 hours, and naturally cooling to room temperature to obtain a brown yellow liquid;
the brown yellow liquid is passed through
Figure BDA0002525064210000031
And filtering by using a microporous filtering membrane to obtain the fluorescent carbon quantum dot solution.
Diluting the fluorescent carbon quantum dot solution, and scanning by an absorption spectrum to obtain a characteristic absorption peak of the quantum dot as 327nm (figure 1); when the fluorescent carbon quantum dot solution was further diluted, the maximum excitation wavelength of the fluorescent carbon quantum dot was 327nm and the maximum fluorescence emission wavelength was 400nm, as seen from the 3D fluorescence spectrum scan (fig. 2).
The fluorescent carbon quantum dot solution is diluted to 4ppm, 5ppm, 10ppm, 20ppm and 40ppm, the excitation wavelength (EX ═ 327nm) is set, the excitation and emission slit width is set to 5nm, the scanning speed is 12000nm/min, the photomultiplier voltage is 550V, the absolute fluorescence intensity at the position of emitted light (EM ═ 400nm) is read, a standard curve of the fluorescence intensity and the concentration is drawn (fig. 3), and the linear relation expression of the obtained standard curve is as follows: 184.018x-262.283 (R)2＝0.999)。
Example 2
The embodiment provides a method for synthesizing carbon quantum dots by hydrolyzing polymaleic anhydride, which comprises the following steps:
3.3333g of HPMA (Tech, 50%) is weighed and dissolved in 45.8334g of deionized water, and the mixture is stirred uniformly;
0.8333g of ethylenediamine (Tech, 99%) solution (mass ratio HPMA/EN is 2:1) is added into the system, mixed uniformly and placed in a closed hydrothermal reaction synthesis kettle;
placing the reaction kettle in an oven, heating to 180 ℃, reacting for 5 hours, and naturally cooling to room temperature to obtain a brown yellow liquid;
the brown yellow liquid is passed through
Figure BDA0002525064210000041
And filtering by using a microporous filtering membrane to obtain the fluorescent carbon quantum dot solution.
Example 3
The embodiment provides a method for synthesizing carbon quantum dots by hydrolyzing polymaleic anhydride, which comprises the following steps:
weighing 1.6667g HPMA (Tech, 50%) and dissolving in 46.6666g deionized water, and stirring well;
adding 1.6667g of ethylenediamine (Tech, 99%) solution (mass ratio HPMA/EN is 0.5:1) into the system, mixing uniformly, and placing in a closed hydrothermal reaction synthesis kettle;
placing the reaction kettle in an oven, heating to 180 ℃, reacting for 5 hours, and naturally cooling to room temperature to obtain a brown yellow liquid;
the brown yellow liquid is passed through
Figure BDA0002525064210000043
And filtering by using a microporous filtering membrane to obtain the fluorescent carbon quantum dot solution.
Example 4
The embodiment provides a method for synthesizing carbon quantum dots by hydrolyzing polymaleic anhydride, which comprises the following steps:
weighing 1.2500g of HPMA (Tech,50 percent) and dissolving in 46.8750g of deionized water, and uniformly stirring;
1.8750g of ethylenediamine (Tech, 99%) solution (mass ratio HPMA/EN is 0.33:1) is added into the system, mixed uniformly and placed in a closed hydrothermal reaction synthesis kettle;
placing the reaction kettle in an oven, heating to 180 ℃, reacting for 5 hours, and naturally cooling to room temperature to obtain a brown yellow liquid;
the brown yellow liquid is passed through
Figure BDA0002525064210000042
And filtering by using a microporous filtering membrane to obtain the fluorescent carbon quantum dot solution.
Example 5
The embodiment provides a method for synthesizing carbon quantum dots by hydrolyzing polymaleic anhydride, which comprises the following steps:
3.7500g of HPMA (Tech, 50%) is weighed and dissolved in 45.6250g of deionized water, and the mixture is stirred uniformly;
0.6250g of ethylenediamine (Tech, 99%) solution (mass ratio HPMA/EN is 3:1) is added into the system, mixed uniformly and placed in a closed hydrothermal reaction synthesis kettle;
placing the reaction kettle in an oven, heating to 180 ℃, reacting for 5 hours, and naturally cooling to room temperature to obtain a brown yellow liquid;
the brown yellow liquid is passed through
Figure BDA0002525064210000051
And filtering by using a microporous filtering membrane to obtain the fluorescent carbon quantum dot solution.
Example 6
The embodiment provides a method for synthesizing carbon quantum dots by hydrolyzing polymaleic anhydride, which comprises the following steps:
weighing 4.000g HPMA (Tech, 50%) and dissolving in 45.5000g deionized water, and stirring well;
adding 0.5000g of ethylenediamine (Tech, 99%) solution (the mass ratio of HPMA/EN is 4:1) into the system, uniformly mixing, and placing in a closed hydrothermal reaction synthesis kettle;
placing the reaction kettle in an oven, heating to 180 ℃, reacting for 5 hours, and naturally cooling to room temperature to obtain a brown yellow liquid;
the brown yellow liquid is passed through
Figure BDA0002525064210000052
And filtering by using a microporous filtering membrane to obtain the fluorescent carbon quantum dot solution.
Example 7
The embodiment provides a method for synthesizing carbon quantum dots by hydrolyzing polymaleic anhydride, which comprises the following steps:
2.5000g of HPMA (Tech, 50%) is weighed and dissolved in 46.2500g of deionized water, and the mixture is stirred uniformly;
adding 1.2626g of ethylenediamine (Tech, 99%) solution into the system, uniformly mixing, and placing in a closed hydrothermal reaction synthesis kettle;
placing the reaction kettle in an oven, heating to 180 ℃, reacting for 12 hours, and naturally cooling to room temperature to obtain a brown yellow liquid;
the brown yellow liquid is passed through
Figure BDA0002525064210000053
And filtering by using a microporous filtering membrane to obtain the fluorescent carbon quantum dot solution.
Example 8
The embodiment provides a method for synthesizing carbon quantum dots by hydrolyzing polymaleic anhydride, which comprises the following steps:
2.5000g of HPMA (Tech, 50%) is weighed and dissolved in 46.2500g of deionized water, and the mixture is stirred uniformly;
adding 1.2626g of ethylenediamine (Tech, 99%) solution into the system, uniformly mixing, and placing in a closed hydrothermal reaction synthesis kettle;
placing the reaction kettle in an oven, heating to 180 ℃, reacting for 18h, and naturally cooling to room temperature to obtain a brown yellow liquid;
the brown yellow liquid is passed through
Figure BDA0002525064210000054
And filtering by using a microporous filtering membrane to obtain the fluorescent carbon quantum dot solution.
Example 9
The embodiment provides a method for synthesizing carbon quantum dots by hydrolyzing polymaleic anhydride, which comprises the following steps:
2.5000g of HPMA (Tech, 50%) is weighed and dissolved in 46.2500g of deionized water, and the mixture is stirred uniformly;
adding 1.2626g of ethylenediamine (Tech, 99%) solution into the system, uniformly mixing, and placing in a closed hydrothermal reaction synthesis kettle;
placing the reaction kettle in an oven, heating to 180 ℃, reacting for 24 hours, and naturally cooling to room temperature to obtain a brown yellow liquid;
the brown yellow liquid is passed through
Figure BDA0002525064210000061
And filtering by using a microporous filtering membrane to obtain the fluorescent carbon quantum dot solution.
Example 10
The embodiment provides a method for synthesizing carbon quantum dots by hydrolyzing polymaleic anhydride, which comprises the following steps:
2.5000g of HPMA (Tech, 50%) is weighed and dissolved in 46.2500g of deionized water, and the mixture is stirred uniformly;
adding 1.2626g of ethylenediamine (Tech, 99%) solution into the system, uniformly mixing, and placing in a closed hydrothermal reaction synthesis kettle;
placing the reaction kettle in an oven, heating to 180 ℃, reacting for 36 hours, and naturally cooling to room temperature to obtain brown yellow liquid;
the brown yellow liquid is passed through
Figure BDA0002525064210000062
And filtering by using a microporous filtering membrane to obtain the fluorescent carbon quantum dot solution.
Example 11
The embodiment provides a method for synthesizing carbon quantum dots by hydrolyzing polymaleic anhydride, which comprises the following steps:
2.5000g of HPMA (Tech, 50%) is weighed and dissolved in 46.2500g of deionized water, and the mixture is stirred uniformly;
adding 1.2626g of ethylenediamine (Tech, 99%) solution into the system, uniformly mixing, and placing in a closed hydrothermal reaction synthesis kettle;
placing the reaction kettle in an oven, heating to 180 ℃, reacting for 48 hours, and naturally cooling to room temperature to obtain brown yellow liquid;
the brown yellow liquid is passed through
Figure BDA0002525064210000063
And filtering by using a microporous filtering membrane to obtain the fluorescent carbon quantum dot solution.
Example 12
The embodiment provides a method for synthesizing carbon quantum dots by hydrolyzing polymaleic anhydride, which comprises the following steps:
weighing 2.50g HPMA (Tech, 50%), dissolving in 46.25g deionized water, and stirring;
adding 1.25g of diethylenetriamine (Tech, 99%) solution into the system, uniformly mixing, and placing in a closed hydrothermal reaction synthesis kettle;
placing the reaction kettle in an oven, heating to 150 ℃, reacting for 18h, and naturally cooling to room temperature to obtain a brown yellow liquid;
the brown yellow liquid is passed through
Figure BDA0002525064210000064
And filtering by using a microporous filtering membrane to obtain the fluorescent carbon quantum dot solution.
Example 13
The embodiment provides a method for synthesizing carbon quantum dots by hydrolyzing polymaleic anhydride, which comprises the following steps:
weighing 2.50g HPMA (Tech, 50%), dissolving in 46.25g deionized water, and stirring;
adding 1.25g of triethylene tetramine (Tech, 99%) solution into the system, uniformly mixing, and placing in a closed hydrothermal reaction synthesis kettle;
placing the reaction kettle in an oven, heating to 220 ℃, reacting for 18h, and naturally cooling to room temperature to obtain a brown yellow liquid;
the brown yellow liquid is passed through
Figure BDA0002525064210000071
And filtering by using a microporous filtering membrane to obtain the fluorescent carbon quantum dot solution.
Example 14
As described in example 1, except that:
the reaction temperature was 140 ℃.
Example 15
As described in example 1, except that:
the reaction temperature was 160 ℃.
Example 16
As described in example 1, except that:
the reaction temperature was 230 ℃.
Comparative example 1
The comparative example provides a method for synthesizing carbon quantum dots from hydrolyzed polymaleic anhydride, comprising the following steps:
4.1667g of HPMA (Tech, 50%) is weighed and dissolved in 46.6666g of deionized water, and the mixture is stirred uniformly;
adding 0.4167g of ethylenediamine (Tech, 99%) solution (the mass ratio of HPMA/EN is 5:1) into the system, uniformly mixing, and placing in a closed hydrothermal reaction synthesis kettle;
placing the reaction kettle in an oven, heating to 180 ℃, reacting for 5 hours, and naturally cooling to room temperature to obtain a brown yellow liquid;
the brown yellow liquid is passed through
Figure BDA0002525064210000072
And filtering by using a microporous filtering membrane to obtain the fluorescent carbon quantum dot solution.
Comparative example 2
The comparative example provides a method for synthesizing carbon quantum dots from hydrolyzed polymaleic anhydride, comprising the following steps:
4.5454g of HPMA (Tech, 50%) is weighed and dissolved in 45.2272g of deionized water, and the mixture is stirred uniformly;
adding 0.2273g of ethylenediamine (Tech, 99%) solution (the mass ratio of HPMA/EN is 10:1) into the system, uniformly mixing, and placing in a closed hydrothermal reaction synthesis kettle;
placing the reaction kettle in an oven, heating to 180 ℃, reacting for 5 hours, and naturally cooling to room temperature to obtain a brown yellow liquid;
the brown yellow liquid is passed through
Figure BDA0002525064210000073
And filtering by using a microporous filtering membrane to obtain the fluorescent carbon quantum dot solution.
Comparative examples 3,
A method of synthesizing carbon quantum dots from hydrolyzed polymaleic anhydride as described in example 1, except that:
the reaction temperature was 120 ℃.
Test example 1
The fluorescence properties of the fluorescent carbon quantum dots obtained in examples 1 to 6 and comparative examples 1 to 2 were measured, and the results are shown in fig. 4.
As can be seen from fig. 4, the mass ratio HPMA/EN has an important influence on the fluorescence properties of the obtained carbon quantum dots, and when the mass ratio HPMA/EN exceeds 5: at 1, the fluorescence intensity of the carbon quantum dot sharply decreases. Therefore, the invention controls the mass ratio of HPMA/EN to be (0.3-4): 1, in HPMA/EN mass ratio 2: the fluorescence intensity was highest at 1.
Test example 2
The fluorescence properties of the fluorescent carbon quantum dots obtained in example 1 and examples 7 to 11 were measured, and the results are shown in fig. 5.
As can be seen from FIG. 5, the hydrothermal reaction time also has an important influence on the fluorescence performance, the reaction time is too short, the fluorescence intensity is lower when the reaction time is less than 5 hours, the fluorescence intensity is enhanced along with the increase of the reaction time, but the effect of enhancing the fluorescence intensity is not obvious when the reaction time reaches a certain time, and the reaction time is controlled to be 5 hours to 50 hours in comprehensive consideration.
Test example 3
The fluorescence properties of the fluorescent carbon quantum dots obtained in example 1, examples 14 to 16, and comparative example 3 were measured, and the results are shown in fig. 6.
As can be seen from FIG. 6, the hydrothermal reaction temperature has an important influence on the fluorescence performance, the reaction temperature is lower than 140 ℃, the fluorescence intensity is lower, and the fluorescence intensity is enhanced along with the increase of the reaction temperature in a certain temperature range, and comprehensively considered, the temperature of the invention is controlled to be 140-230 ℃.
Test example 4
The interference of NaClO on the fluorescent carbon quantum dots obtained in example 1 was tested.
Five groups of 10ppm and 20ppm carbon quantum dot solutions are prepared respectively, NaClO solutions with residual chlorine contents of 0, 1, 2, 3 and 4ppm are added, and the influence of sodium hypochlorite on the carbon quantum dots is tested, and the result is shown in FIG. 7. As can be seen from FIG. 7, the residual chlorine cannot affect the fluorescence intensity of the carbon quantum dots within a certain concentration range, indicating that the carbon quantum dots have better stability.

Claims (10)

1. A method for synthesizing carbon quantum dots by using hydrolyzed polymaleic anhydride as a main raw material comprises the following steps:
dissolving hydrolyzed polymaleic anhydride (HPMA) as a raw material in deionized water, and uniformly stirring;
adding organic amine solution into the system, and carrying out closed hydrothermal reaction at 140-230 ℃;
and after the reaction is finished, cooling and filtering the reaction solution to obtain the fluorescent carbon quantum dot solution.
2. The method for synthesizing carbon quantum dots by using hydrolyzed polymaleic anhydride as a main raw material according to claim 1, wherein the relative molecular weight of the HPMA is 400-800.
3. The method for synthesizing carbon quantum dots by using hydrolyzed polymaleic anhydride as a main raw material according to claim 1, wherein the organic amine is Ethylenediamine (EN), diethylenetriamine or triethylenetetramine.
4. The method for synthesizing the carbon quantum dots by using the hydrolyzed polymaleic anhydride as the main raw material according to claim 1, wherein the hydrothermal reaction time is 5-50 h.
5. The method for synthesizing the carbon quantum dots by using the hydrolyzed polymaleic anhydride as the main raw material according to claim 1, wherein the mass ratio of the HPMA to the organic amine is (0.3-4): 1.
6. the method for synthesizing carbon quantum dots by using hydrolyzed polymaleic anhydride as a main raw material according to claim 1, wherein the reaction temperature of the hydrothermal reaction is 140-230 ℃.
7. The method for synthesizing carbon quantum dots by using hydrolyzed polymaleic anhydride as a main raw material according to claim 1, wherein the filtration is performed by using a filter membrane with a pore size specification of
Figure FDA0002525064200000011
And (5) filtering the membrane.
8. The method for synthesizing the carbon quantum dots by using the hydrolyzed polymaleic anhydride as the main raw material according to claim 1, wherein the characteristic absorption peak of the prepared fluorescent carbon quantum dot solution is 327nm by scanning absorption spectrum.
9. The method for synthesizing carbon quantum dots by using hydrolyzed polymaleic anhydride as a main raw material according to claim 1, wherein the prepared fluorescent carbon quantum dot solution is scanned by a 3D fluorescence spectrum to obtain the carbon quantum dots lambdaEX253nm and λEXAt 327nm, at λEMStrong fluorescence is emitted at 400 nm.
10. The method for synthesizing the carbon quantum dots by using the hydrolyzed polymaleic anhydride as the main raw material according to claim 1, which is characterized by comprising the following steps:
(1) 3.3333g of HPMA (Tech, 50%) is weighed and dissolved in 45.8334g of deionized water, and the mixture is stirred uniformly;
(2) 0.8333g of ethylenediamine (Tech, 99%) solution (mass ratio HPMA/EN is 2:1) is added into the system, mixed uniformly and placed in a closed hydrothermal reaction synthesis kettle;
(3) placing the reaction kettle in an oven, heating to 180 ℃, reacting for 5 hours, and naturally cooling to room temperature to obtain a brown yellow liquid;
(4) the brown yellow liquid is passed through
Figure FDA0002525064200000021
And filtering by using a microporous filtering membrane to obtain the fluorescent carbon quantum dot solution.
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CN112794463A (en) * 2020-12-30 2021-05-14 河南清水源科技股份有限公司 Preparation method of carbon dot fluorescent tracing scale inhibitor for circulating cooling water

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