CN117963892B - Method for preparing carbon quantum dots by taking inorganic salt as reaction medium and application - Google Patents
Method for preparing carbon quantum dots by taking inorganic salt as reaction medium and application Download PDFInfo
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- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 title claims abstract description 105
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- 238000000034 method Methods 0.000 title claims abstract description 24
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- 238000002360 preparation method Methods 0.000 claims abstract description 10
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims description 54
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- 239000011780 sodium chloride Substances 0.000 claims description 28
- JAUCIKCNYHCSIR-UHFFFAOYSA-M sodium;2-cyanoacetate Chemical compound [Na+].[O-]C(=O)CC#N JAUCIKCNYHCSIR-UHFFFAOYSA-M 0.000 claims description 17
- FDRCDNZGSXJAFP-UHFFFAOYSA-M sodium chloroacetate Chemical compound [Na+].[O-]C(=O)CCl FDRCDNZGSXJAFP-UHFFFAOYSA-M 0.000 claims description 11
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- 239000000126 substance Substances 0.000 claims description 10
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- 239000004202 carbamide Substances 0.000 claims description 9
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- CDBYLPFSWZWCQE-UHFFFAOYSA-L sodium carbonate Substances [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 8
- REYJJPSVUYRZGE-UHFFFAOYSA-N Octadecylamine Chemical compound CCCCCCCCCCCCCCCCCCN REYJJPSVUYRZGE-UHFFFAOYSA-N 0.000 claims description 7
- WQZGKKKJIJFFOK-VFUOTHLCSA-N beta-D-glucose Chemical compound OC[C@H]1O[C@@H](O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-VFUOTHLCSA-N 0.000 claims description 7
- 238000000926 separation method Methods 0.000 claims description 7
- 235000018417 cysteine Nutrition 0.000 claims description 6
- XUJNEKJLAYXESH-UHFFFAOYSA-N cysteine Natural products SCC(N)C(O)=O XUJNEKJLAYXESH-UHFFFAOYSA-N 0.000 claims description 6
- 238000001728 nano-filtration Methods 0.000 claims description 5
- JTNCEQNHURODLX-UHFFFAOYSA-N 2-phenylethanimidamide Chemical compound NC(=N)CC1=CC=CC=C1 JTNCEQNHURODLX-UHFFFAOYSA-N 0.000 claims description 4
- XUJNEKJLAYXESH-REOHCLBHSA-N L-Cysteine Chemical compound SC[C@H](N)C(O)=O XUJNEKJLAYXESH-REOHCLBHSA-N 0.000 claims description 4
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 claims description 4
- 229910000343 potassium bisulfate Inorganic materials 0.000 claims description 4
- 229910000029 sodium carbonate Inorganic materials 0.000 claims description 4
- 229910052938 sodium sulfate Inorganic materials 0.000 claims description 4
- 235000011152 sodium sulphate Nutrition 0.000 claims description 4
- 239000012528 membrane Substances 0.000 claims description 3
- 230000035484 reaction time Effects 0.000 claims description 3
- JRBPAEWTRLWTQC-UHFFFAOYSA-N dodecylamine Chemical compound CCCCCCCCCCCCN JRBPAEWTRLWTQC-UHFFFAOYSA-N 0.000 claims description 2
- 239000005416 organic matter Substances 0.000 abstract description 16
- 238000006862 quantum yield reaction Methods 0.000 abstract description 12
- 239000000463 material Substances 0.000 abstract description 4
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 abstract description 3
- 229910052799 carbon Inorganic materials 0.000 abstract description 2
- 230000003197 catalytic effect Effects 0.000 abstract description 2
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- 238000001000 micrograph Methods 0.000 description 4
- XMWGSPLTTNCSMB-UHFFFAOYSA-M sodium;2-hydroxypropane-1,2,3-tricarboxylic acid;chloride Chemical class [Na+].[Cl-].OC(=O)CC(O)(C(O)=O)CC(O)=O XMWGSPLTTNCSMB-UHFFFAOYSA-M 0.000 description 4
- PAYRUJLWNCNPSJ-UHFFFAOYSA-N Aniline Chemical compound NC1=CC=CC=C1 PAYRUJLWNCNPSJ-UHFFFAOYSA-N 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
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- XDTMQSROBMDMFD-UHFFFAOYSA-N Cyclohexane Chemical compound C1CCCCC1 XDTMQSROBMDMFD-UHFFFAOYSA-N 0.000 description 1
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- 238000001506 fluorescence spectroscopy Methods 0.000 description 1
- 229910021389 graphene Inorganic materials 0.000 description 1
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- 229910010272 inorganic material Inorganic materials 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
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- -1 sodium cyanoacetate-sodium chloride Chemical compound 0.000 description 1
- 239000007790 solid phase Substances 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/15—Nano-sized carbon materials
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J21/00—Catalysts comprising the elements, oxides, or hydroxides of magnesium, boron, aluminium, carbon, silicon, titanium, zirconium, or hafnium
- B01J21/18—Carbon
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
- C09K11/08—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials
- C09K11/65—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing carbon
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Abstract
The invention discloses a method for preparing carbon quantum dots by taking inorganic salts as reaction media and application thereof, belonging to the technical field of carbon catalytic materials. The preparation method comprises the following steps: dissolving an organic matter and inorganic salt in a solvent, and removing the solvent to obtain an inorganic-organic compound; and heating the inorganic-organic compound at 180-210 ℃ for reaction to obtain the carbon quantum dot. The carbon quantum dots prepared by the method have uniform size distribution, the relative fluorescence quantum yield of the carbon quantum dots can be controlled to be about 3 nm, the relative fluorescence quantum yield of the carbon quantum dots can reach 34.13%, and the fluorescence emission wavelength can be regulated and controlled between 370 nm and 500 nm. The method for preparing the carbon quantum dots by using the inorganic salt as the reaction medium can be applied to high-valued treatment of the organic pollution chemical waste salt, and realizes the purification of the inorganic salt while converting the organic matters in the waste salt to prepare the high-value carbon quantum dots, wherein the purity of the obtained inorganic salt is more than 99%.
Description
Technical Field
The invention belongs to the technical field of carbon catalytic materials, and particularly relates to a method for preparing carbon quantum dots by taking inorganic salts as reaction media and application thereof.
Background
The carbon quantum dot has the advantages of easy surface modification, good water solubility, high photobleaching resistance, low toxicity and good biocompatibility, and is widely applied to the fields of biological imaging, ion detection, photoelectrocatalysis, fluorescence imaging, light emitting diodes and the like. The carbon quantum dot has the characteristics of fluorescence performance, biocompatibility, high light stability, adjustable optical property and the like, and has great application potential in the field of photocatalysis. The carbon quantum dots are generally prepared from citric acid, glucose, amino acid, aniline and other small molecules through four stages of dehydration, polymerization, carbonization and passivation, the main method adopted is a hydrothermal method or a solvothermal method, the reaction time is different from several hours to more than ten hours, a high-pressure environment is required, and the problems of difficult control of the reaction process, uneven size distribution of the prepared carbon quantum dots and the like exist. In order to solve the problems, researchers use inorganic salt as a template agent to synthesize polymer coating quantum dots with single dispersion, high quantum yield and good light stability in a high-temperature molten state, but the preparation process needs to be carried out at 800-1000 ℃ and has high energy consumption.
Disclosure of Invention
Aiming at the defects existing in the prior art, the invention provides a solid-phase method for synthesizing carbon quantum dots by taking inorganic salts as reaction media, wherein organic matters and inorganic salts are dissolved, dispersed and evaporated to remove solvents to obtain inorganic-organic compounds, the inorganic salts in the compounds wrap the organic matters to form a micro-reactor, then the organic matters are subjected to dehydration condensation, carbonization and other reactions in the micro-reactor to be converted into the carbon quantum dots under the heating condition of 180-210 ℃, and the separation of the inorganic salts and the carbon quantum dots is realized by means of nanofiltration/extraction separation and the like, so that the fluorescent carbon quantum dots with adjustable high-purity inorganic salts and fluorescence emission wavelength and higher quantum yield can be obtained. In addition, the invention also provides a high-valued treatment method of the organic pollution chemical waste salt based on the method for preparing the fluorescent carbon quantum dots by using the inorganic salt as the reaction medium solid phase method.
In order to achieve the above purpose, the present invention provides the following technical solutions:
a method for preparing carbon quantum dots by taking inorganic salts as reaction medium comprises the following steps:
heating and reacting the inorganic-organic compound at 180-210 ℃ to obtain the carbon quantum dot;
The inorganic-organic compound is obtained by dissolving an organic substance and an inorganic salt in a solvent and removing the solvent;
or the inorganic-organic compound is obtained by dissolving organic pollution chemical waste salt in a solvent and removing the solvent;
Or the inorganic-organic compound is obtained by dissolving organic pollution chemical waste salt and organic matters in a solvent together and removing the solvent;
in the three preparation modes of the inorganic-organic compound, the organic matters in the inorganic-organic compound are one or more of citric acid, glucose, sodium chloroacetate, sodium cyanoacetate, cysteine, o-phenylenediamine, urea, dodecyl amine, octadecylamine and octadecylamine derivatives; the inorganic salt in the inorganic-organic compound is one or more of sodium chloride, sodium sulfate, sodium carbonate and potassium bisulfate.
Preferably, the mass fraction of the organic in the inorganic-organic compound is 4-50%.
Preferably, the heating reaction time is 1-3 hours.
Preferably, the heating reaction is followed by a separation step comprising:
when the carbon quantum dots generated by the heating reaction are water-soluble carbon quantum dots, dissolving the product after the heating reaction in water, and separating the water-soluble carbon quantum dots and inorganic salts through a nanofiltration membrane; when the carbon quantum dots generated by the heating reaction are oil-soluble carbon quantum dots, dissolving the product after the heating reaction by using a good solvent of the oil-soluble carbon quantum dots, centrifuging, and separating to obtain the oil-soluble carbon quantum dots.
The beneficial technical effects of the invention are as follows:
(1) The method for preparing the carbon quantum dots by using the inorganic salt as a reaction medium provided by the invention takes a micro-reactor formed by solid-phase inorganic salt as a reaction medium to realize the conversion of organic matters to the carbon quantum dots, and the reaction process is carried out under normal pressure, and has the advantages of high reaction rate and low energy consumption.
(2) The carbon quantum dots prepared by the method have uniform size distribution, the relative fluorescence quantum yield of the carbon quantum dots can be controlled to be about 3 nm, the relative fluorescence quantum yield of the carbon quantum dots can reach 34.13%, and the fluorescence emission wavelength can be regulated and controlled between 370 nm and 500 nm.
(3) The method for preparing the carbon quantum dots by using the inorganic salt as the reaction medium can be applied to high-valued treatment of the organic pollution chemical waste salt, and realizes the purification of the inorganic salt while converting the organic matters in the waste salt to prepare the high-value carbon quantum dots, wherein the purity of the obtained inorganic salt is more than 99%.
Drawings
Fig. 1 is an XRD pattern of sodium chloride, citric acid and sodium chloride milled mixtures and citric acid-sodium chloride complexes of example 1.
Fig. 2 shows fluorescence excitation spectra and fluorescence emission spectra of the carbon quantum dots prepared in example 1, wherein a is a carbon quantum dot prepared from citric acid, B is a carbon quantum dot prepared from glucose, C is a carbon quantum dot prepared from sodium chloroacetate, D is a carbon quantum dot prepared from sodium cyanoacetate, F is a carbon quantum dot prepared from cysteine, and E is a carbon quantum dot prepared from o-phenylenediamine.
Fig. 3 is a fluorescence emission spectrum of the carbon quantum dot prepared in example 2.
Fig. 4 is a fluorescence emission spectrum of the carbon quantum dots prepared in example 3 and example 4.
Fig. 5 is a fluorescence emission spectrum of the carbon quantum dot prepared in example 5.
Fig. 6 is a fluorescence emission spectrum of the carbon quantum dot prepared in example 6.
Fig. 7 is a fluorescence emission spectrum of the carbon quantum dot prepared in example 7.
Fig. 8 is a fluorescence emission spectrum and an ultraviolet lamp irradiation pattern of the carbon quantum dot solution prepared in example 8, wherein a is a fluorescence emission spectrum of the carbon quantum dot prepared in example 8, and B is an ultraviolet lamp irradiation pattern of the carbon quantum dot solution.
Fig. 9 is a transmission electron microscope image of the carbon quantum dot prepared in example 9, wherein a is a carbon quantum dot transmission electron microscope image with a scale of 50 nm, B is a carbon quantum dot transmission electron microscope image with a scale of 10nm, C is a carbon quantum dot transmission electron microscope image with a scale of 5nm, and D is a prepared carbon quantum dot lattice fringe pattern.
Detailed Description
Various exemplary embodiments of the invention will now be described in detail, which should not be considered as limiting the invention, but rather as more detailed descriptions of certain aspects, features and embodiments of the invention. It is to be understood that the terminology used herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention.
In addition, for numerical ranges in this disclosure, it is understood that each intermediate value between the upper and lower limits of the ranges is also specifically disclosed. Every smaller range between any stated value or stated range, and any other stated value or intermediate value within the stated range, is also encompassed within the invention. The upper and lower limits of these smaller ranges may independently be included or excluded in the range.
Unless otherwise defined, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. Although only preferred methods and materials are described herein, any methods and materials similar or equivalent to those described herein can be used in the practice or testing of the present invention.
As used herein, the terms "comprising," "including," "having," "containing," and the like are intended to be inclusive and mean an inclusion, but not limited to.
Example 1
Taking sodium chloride as inorganic salt, and taking the carbon quantum dot prepared by the organic matter accounting for 10% of the total mass of the inorganic salt and the organic matter as an example:
(1) Preparation of organic-sodium chloride complex: respectively weighing organic matters (citric acid, glucose, sodium chloroacetate, sodium cyanoacetate, cysteine and o-phenylenediamine) and sodium chloride according to the mass ratio of the organic matters of 10%, mixing and dissolving the organic matters and the sodium chloride in water to prepare an aqueous solution with the mass concentration of 10%, and removing the water by adopting an evaporation mode after the organic matters and the sodium chloride are completely dissolved to obtain the organic matter-sodium chloride compound. To demonstrate the "microreactor" formed by sodium chloride to organic matter in the above-described resulting composite, an X-ray diffractometer was used to analyze sodium chloride, citric acid, a mixture of citric acid and sodium chloride and a citric acid-sodium chloride composite using an organic matter as citric acid, and the results are shown in fig. 1. It is evident that only the characteristic diffraction peaks of sodium chloride, but not of citric acid, were observed in the prepared citric acid-sodium chloride complex, indicating that sodium chloride forms a "microreactor" for the inclusion of citric acid in the prepared citric acid-sodium chloride complex.
(2) Preparation of carbon quantum dots: heating the organic matter-sodium chloride compound obtained in the step (1) for 1h at 200 ℃ to obtain a mixture of the carbon quantum dots and sodium chloride, dissolving the mixture, and separating sodium chloride by nanofiltration to obtain the carbon quantum dots containing no or little salt; the fluorescence excitation spectrum and the fluorescence emission spectrum of the carbon quantum dot solution are shown in fig. 2, wherein A is a carbon quantum dot prepared by taking citric acid as a raw material, B is a carbon quantum dot prepared by taking glucose as a raw material, C is a carbon quantum dot prepared by taking sodium chloroacetate as a raw material, D is a carbon quantum dot prepared by taking sodium cyanoacetate as a raw material, F is a carbon quantum dot prepared by taking cysteine as a raw material, and E is a carbon quantum dot prepared by taking o-phenylenediamine as a raw material. As can be seen from fig. 2, the fluorescence emission wavelengths corresponding to citric acid, glucose, sodium chloroacetate, sodium cyanoacetate, cysteine and o-phenylenediamine are 455 nm, 430 nm, 435 nm, 410 nm, 410 nm and 370 nm, respectively, and stokes shift can reach 100nm.
Example 2
Taking sodium chloride as inorganic salt, sodium cyanoacetate as organic substance, and the mass of the sodium cyanoacetate accounts for 20% -50% of the total mass of the inorganic salt and the organic substance, for example, the carbon quantum dot is prepared:
The organic matter in example 1 is fixed as sodium cyanoacetate, the inorganic salt is still sodium chloride, the mass ratio of the sodium cyanoacetate is respectively adjusted to 20%,30%,40% and 50%, and the rest of reaction conditions are unchanged, so that the fluorescence emission spectrum of the obtained carbon quantum dot is shown in figure 3. As can be seen from fig. 3, the fluorescence emission wavelength of the prepared carbon quantum dots was 410 nm, and the relative fluorescence quantum yields of the prepared carbon quantum dot solutions were 8.37%,10.63%,10.95% and 10.67%, respectively, as measured by the measurement method described in the group standard "graphene quantum dot blue light emission relative fluorescence quantum yield measurement molecular fluorescence spectrometry (T/CSTM 00197-2021)".
Example 3
Taking sodium chloride as inorganic salt, citric acid and urea as organic matters, wherein the organic matters account for 10 percent of the total mass of the inorganic salt and the organic matters, and preparing the carbon quantum dots is exemplified:
The organic matter in the embodiment 1 is adjusted to be a mixture of citric acid and urea, wherein the mass ratio of the citric acid to the urea is 1.2:1, other reaction conditions are unchanged, and the fluorescence emission spectrum of the obtained carbon quantum dot is shown in fig. 4. As can be seen from FIG. 4, the fluorescence emission wavelength thereof was 442 nm, and the relative fluorescence quantum yield measured according to the method described in example 2 was 20.78%.
Example 4
Taking potassium bisulfate as inorganic salt, citric acid and urea as organic matters, wherein the organic matters account for 10 percent of the total mass of the inorganic salt and the organic matters, the preparation of the carbon quantum dot is exemplified:
The inorganic salt in the example 3 is replaced by potassium bisulfate, other reaction conditions are unchanged, and the fluorescence emission spectrum of the prepared carbon quantum dot is shown in figure 4. As can be seen from FIG. 4, the fluorescence emission wavelength was 436 nm, and the relative fluorescence quantum yield was 22.32% as measured by the method described in example 2.
Example 5
Taking sodium carbonate as inorganic salt, glucose and urea as organic matters, and preparing carbon quantum dots by taking 10% of the total mass of the inorganic salt and the organic matters as an example:
The inorganic salt in the example 3 is replaced by sodium carbonate, the organic matter is replaced by a mixture of glucose and urea, wherein the mass ratio of the glucose to the urea is 1:1, and other reaction conditions are unchanged, so that the fluorescence emission spectrum of the obtained carbon quantum dot is shown in figure 5. As can be seen from fig. 5, the fluorescence emission wavelength is 430 nm.
Example 6
Taking sodium sulfate as inorganic salt and o-phenylenediamine as organic substance, wherein the organic substance accounts for 4% of the total mass of the inorganic salt and the organic substance, for example, the carbon quantum dot is prepared:
The inorganic salt in example 1 was replaced with sodium sulfate, the organic matter was determined to be o-phenylenediamine, the organic matter mass ratio was adjusted to 4%, and the fluorescence emission spectrum of the prepared carbon quantum dots was shown in fig. 6. As can be seen from FIG. 6, the fluorescence emission wavelength was 500 nm, and the relative fluorescence quantum yield measured as described in example 2 was 34.13%.
Example 7
Taking sodium chloride as inorganic salt and sodium cyanoacetate as organic substance, wherein the organic substance accounts for 10% of the total mass of the inorganic salt and the organic substance, and preparing the carbon quantum dots at different temperatures is exemplified by:
The organic matter in example 1 was determined as sodium cyanoacetate, and the prepared sodium cyanoacetate-sodium chloride complex was heated at 180 ℃, 190 ℃ and 210 ℃ for 1 hour to prepare carbon quantum dots, and other reaction conditions were unchanged, so that the fluorescence emission patterns of the prepared carbon quantum dots were shown in fig. 7. As can be seen from FIG. 7, the fluorescence emission wavelengths were 384 nm, 386 nm and 410 nm, respectively, and the relative fluorescence quantum yields were 11.42%,11.25% and 10.89% as measured in the method described in example 2.
Example 8
The preparation method comprises the steps of taking organic pollution chemical waste salt containing sodium chloroacetate, sodium cyanoacetate and sodium chloride as raw materials, adding nonpolar organic matter octadecylamine into the raw materials, and carrying out high-value treatment to prepare the oil-soluble carbon quantum dots, wherein the preparation method comprises the following steps:
Mixing organic pollution chemical waste salt containing sodium chloroacetate, sodium cyanoacetate and sodium chloride with nonpolar organic matter octadecylamine, preparing to enable the mass ratio of organic matter to inorganic salt and organic matter mixture to be 8%, wherein the octadecylamine is dissolved by ethanol firstly and then mixed with waste salt aqueous solution to enable the mass concentration of the organic matter and the inorganic salt to be 10%. Other process conditions for preparing the oil-soluble carbon quantum dots are the same as those in example 1, and the prepared carbon quantum dots are a mixture of the oil-soluble carbon quantum dots and inorganic salts. And then, cyclohexane is adopted to dissolve, wash and centrifugally separate the mixture to obtain supernatant, and the oil-soluble carbon quantum dots are dissolved in the supernatant, and the fluorescence emission spectrum is shown in figure 8. As can be seen from fig. 8, the oil-soluble carbon quantum dot solution exhibited significant fluorescence. The centrifugal separation solid is inorganic salt sodium chloride, and the purity of the centrifugal separation solid is more than 99 percent through testing.
Example 9
The preparation of water-soluble carbon quantum dots by using organic pollution chemical waste salt containing sodium chloroacetate, sodium cyanoacetate and sodium chloride as raw materials through high-valued treatment is exemplified by:
Organic pollution chemical waste salt containing sodium chloroacetate, sodium cyanoacetate and sodium chloride (wherein the mass ratio of the sodium chloroacetate to the sodium cyanoacetate in the waste salt is 6%) is dissolved in water to prepare aqueous solution with the concentration of 10%, the aqueous solution is evaporated to remove water to obtain an organic-inorganic compound, other process conditions for preparing the carbon quantum dots are the same as those of example 1, a mixture of the water-soluble carbon quantum dots and the sodium chloride is prepared, then the water-soluble carbon quantum dots and the sodium chloride are separated by a nanofiltration membrane, the aqueous solution of the separated carbon quantum dots is sampled, and the prepared carbon quantum dots are subjected to transmission electron microscopy characterization, and the result is shown in figure 9. The results of fig. 9 show that the carbon quantum dots were uniformly distributed (a in fig. 9) and the particle diameter was about 3 nm (B and C in fig. 9), and that the lattice spacing was 0.25 nm (D in fig. 9) by calculating the interplanar spacing using Digital Micrograph software.
The above embodiments are only illustrative of the preferred embodiments of the present invention and are not intended to limit the scope of the present invention, and various modifications and improvements made by those skilled in the art to the technical solutions of the present invention should fall within the protection scope defined by the claims of the present invention without departing from the design spirit of the present invention.
Claims (3)
1. The method for preparing the carbon quantum dots by taking the inorganic salt as the reaction medium is characterized by comprising the following steps of:
heating and reacting the inorganic-organic compound at 180-210 ℃ to obtain the carbon quantum dot;
The inorganic-organic compound is obtained by dissolving an organic substance and an inorganic salt in a solvent and removing the solvent;
or the inorganic-organic compound is obtained by dissolving organic pollution chemical waste salt in a solvent and removing the solvent;
Or the inorganic-organic compound is obtained by dissolving organic pollution chemical waste salt and organic matters in a solvent together and removing the solvent;
In the three preparation modes of the inorganic-organic compound, the organic matters in the inorganic-organic compound are one or more of citric acid, glucose, sodium chloroacetate, sodium cyanoacetate, cysteine, o-phenylenediamine, urea, dodecyl amine, octadecylamine and octadecylamine derivatives; the inorganic salt in the inorganic-organic compound is one or more of sodium chloride, sodium sulfate, sodium carbonate and potassium bisulfate; the mass fraction of the organic in the inorganic-organic compound is 4-50%; the solvent is water.
2. The method for preparing carbon quantum dots by using inorganic salts as reaction media according to claim 1, wherein the heating reaction time is 1-3 hours.
3. The method for preparing carbon quantum dots by using inorganic salts as reaction media according to any one of claims 1 to 2, wherein the method further comprises a separation step after the heating reaction, the separation step comprising:
when the carbon quantum dots generated by the heating reaction are water-soluble carbon quantum dots, dissolving the product after the heating reaction in water, and separating the water-soluble carbon quantum dots and inorganic salts through a nanofiltration membrane; when the carbon quantum dots generated by the heating reaction are oil-soluble carbon quantum dots, dissolving the product after the heating reaction by using a good solvent of the oil-soluble carbon quantum dots, centrifuging, and separating to obtain the oil-soluble carbon quantum dots.
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