CN113086970B - Method for simply preparing temperature-resistant salt-tolerant carbon dots - Google Patents

Method for simply preparing temperature-resistant salt-tolerant carbon dots Download PDF

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CN113086970B
CN113086970B CN202110417628.1A CN202110417628A CN113086970B CN 113086970 B CN113086970 B CN 113086970B CN 202110417628 A CN202110417628 A CN 202110417628A CN 113086970 B CN113086970 B CN 113086970B
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temperature
citric acid
carbon dots
salt
acid
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CN113086970A (en
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吴文婷
吴涵
戴彩丽
卢常河
赵青山
吴一宁
张庭威
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China University of Petroleum East China
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    • C01B32/00—Carbon; Compounds thereof
    • C01B32/15—Nano-sized carbon materials
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y20/00—Nanooptics, e.g. quantum optics or photonic crystals
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
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    • 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 simply preparing temperature-resistant salt-tolerant carbon points, which comprises the following steps: dissolving citric acid and isethionic acid in water, reacting in a microwave reactor, performing ultrasonic dispersion, suction filtration, dialysis and drying to obtain the carbon dots. The carbon dots prepared by the method have strong adaptability to high-temperature and high-salinity environments and high fluorescence intensity. The carbon dots have the advantages of low raw material cost, simple preparation method and short preparation time. These advantages make it promising for mass production and application to industrial production.

Description

Method for simply preparing temperature-resistant salt-tolerant carbon dots
Technical Field
The invention belongs to the technical field of carbon dot preparation, and particularly relates to a method for simply preparing temperature-resistant salt-resistant carbon dots.
Background
Carbon Dots (CDs) refer to spherical-like Carbon nanoparticles having a size below 10 nm. Compared with the traditional semiconductor quantum dots, the CDs have the advantages of excellent optical performance, small size and the like, and also have the advantages of low cytotoxicity, good biocompatibility, easiness in large-scale synthesis and functional modification, low preparation cost, mild reaction conditions and the like. CDs surfaces also possess a wide variety of water-soluble functional groups, such as amino, hydroxyl, and carboxyl groups, which facilitate dispersion in polar solvents and subsequent functional modification. Currently, CDs have some excellent properties, such as good fluorescence properties and good biocompatibility, and have been used in the field of biological imaging.
However, CDs also have some defects, and the small particle size of the particles enables the surface energy of carbon dots to be larger, so that the particles are not easy to exist stably, have poor adaptability to high-temperature and high-salt environments and are easy to generate an agglomeration phenomenon.
Disclosure of Invention
This section is for the purpose of summarizing some aspects of embodiments of the invention and to briefly introduce some preferred embodiments. In this section, as well as in the abstract and the title of the invention of this application, simplifications or omissions may be made to avoid obscuring the purpose of the section, the abstract and the title, and such simplifications or omissions are not intended to limit the scope of the invention.
As one aspect of the invention, the invention provides a method for simply preparing temperature-resistant and salt-tolerant carbon points, which is characterized by comprising the following steps: the method comprises the following steps: dissolving citric acid and isethionic acid in water, reacting in a microwave reactor, performing ultrasonic dispersion, suction filtration, dialysis and drying to obtain the carbon dots.
As an optimal scheme of the simple preparation method of the temperature-resistant salt-tolerant carbon dots, the method comprises the following steps: the molar ratio of the citric acid to the hydroxyethyl sulfonic acid is 1: 1.
as an optimal scheme of the simple preparation method of the temperature-resistant salt-tolerant carbon dots, the method comprises the following steps: and in the ultrasonic dispersion, the ultrasonic power is 80-150 Hz, and the ultrasonic time is 15-25 min.
As an optimal scheme of the simple preparation method of the temperature-resistant salt-tolerant carbon dots, the method comprises the following steps: the reaction is carried out in a microwave reactor, and the microwave power is 700W.
As a preferred scheme of the method for simply preparing the temperature-resistant salt-resistant carbon dots, the method comprises the following steps: the reaction is carried out in a microwave reactor for 5 min.
As an optimal scheme of the simple preparation method of the temperature-resistant salt-tolerant carbon dots, the method comprises the following steps: dissolving citric acid and isethionic acid in water, wherein in order to dissolve the citric acid in the water, ultrasonic waves are used for fully dissolving the citric acid, and then the isethionic acid is added for fully dissolving the citric acid by ultrasonic waves.
As an optimal scheme of the simple preparation method of the temperature-resistant salt-tolerant carbon dots, the method comprises the following steps: the filtration was carried out by filtration through a 0.22 μm filter paper.
As a preferred scheme of the method for simply preparing the temperature-resistant salt-resistant carbon dots, the method comprises the following steps: and the dialysis is to dialyze the filtrate after suction filtration for 72 hours in a dialysis bag with the molecular weight cutoff of 3500 Da.
As an optimal scheme of the simple preparation method of the temperature-resistant salt-tolerant carbon dots, the method comprises the following steps: the drying is carried out for 24-48 h at 50-60 ℃.
The invention has the beneficial effects that: the carbon dots prepared by the method have strong adaptability to high-temperature and high-salt environments and high fluorescence intensity. The carbon dots have the advantages of low raw material cost, simple preparation method and short preparation time. These advantages make it promising for mass production and application to industrial production.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings needed to be used in the description of the embodiments will be briefly introduced below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and it is obvious for those skilled in the art to obtain other drawings based on these drawings without inventive exercise. Wherein:
FIG. 1 is a TEM image of S-CD (a-b);
FIG. 2 is a UV-vis diagram of S-CD;
FIG. 3 is a graph of (left) S-CD solution stability in saline solution; (right) graph showing that the S-CD solution remains stable at 83 ℃;
FIG. 4 is a PL intensity contrast plot of S-CD solutions under different conditions;
FIG. 5 is a PL spectrum of an S-CD solution and an O-CD solution at the same excitation wavelength.
Detailed Description
In order to make the aforementioned objects, features and advantages of the present invention comprehensible, embodiments accompanied with examples are described in detail below.
In the following description, numerous specific details are set forth in order to provide a thorough understanding of the present invention, but the present invention may be practiced in other ways than those specifically described and will be readily apparent to those of ordinary skill in the art without departing from the spirit of the present invention, and therefore the present invention is not limited to the specific embodiments disclosed below.
Furthermore, reference herein to "one embodiment" or "an embodiment" means that a particular feature, structure, or characteristic described in connection with the embodiment is included in at least one implementation of the invention. The appearances of the phrase "in one embodiment" in various places in the specification are not necessarily all referring to the same embodiment, nor are separate or alternative embodiments mutually exclusive of other embodiments.
Example 1:
weighing 0.96g of citric acid, dissolving in 25mL of deionized water, performing ultrasonic treatment to fully dissolve the citric acid, adding 0.6306g of hydroxyethyl sulfonic acid, performing ultrasonic treatment to fully dissolve the citric acid, placing the solution in a microwave reactor, heating for 5min under the power of 700W, naturally cooling to room temperature, taking out the obtained liquid, performing ultrasonic treatment for 20min at the ultrasonic power of 100Hz, performing suction filtration by using 0.22 mu m filter paper, taking the filtrate, dialyzing in a dialysis bag with the molecular weight cutoff of 3500Da for 72h, and drying at 60 ℃ for 48h to obtain solid powder, namely the carbon dots S-CDs.
Testing the temperature resistance and salt tolerance of S-CDs:
and (3) preparing a NaCl solution with the molar concentration of 2.0mol/L, dropwise adding the solution into the prepared carbon dot solution, standing for 24 hours, clarifying the solution before and after dropwise adding, avoiding obvious precipitation and obvious change of PL strength, and showing the PL strength test result in figure 4, which shows that the carbon dot shows high stability under the condition of high salt.
The carbon dot solution is placed in an oven at 83 ℃ for heating, the solution is clear before and after heating, no obvious phenomenon occurs, and the PL strength has no obvious change, which shows that the carbon dot has high stability under the high-temperature condition.
The carbon dots prepared by the method have the advantages of strong adaptability to high-temperature and high-salt environments, high fluorescence intensity, low cost of raw materials, simple and convenient preparation method and short preparation time, and are expected to be produced in a large scale and applied to industrial production.
Study example 1:
0.96g of citric acid was weighed, dissolved in 25mL of deionized water, and sufficiently dissolved by sonication, and then 0.7207g of sulfosalicylic acid was added and sufficiently dissolved by sonication. The solution was heated in a microwave reactor at 700W for 5 min. And naturally cooling to room temperature, taking out the obtained liquid, performing ultrasonic treatment for 20min at the ultrasonic power of 100Hz, performing suction filtration by using 0.22 mu m filter paper, taking the filtrate, dialyzing for 72h, and drying at 60 ℃ for 48h to obtain solid powder, namely O-CDs.
According to the test conditions in example 1, NaCl solution with the same concentration is added dropwise and left standing for the same time, and the solution becomes slightly turbid after the dropwise addition. And (3) placing the equivalent carbon dot solution in an oven at 83 ℃ for heating, wherein the heated solution is turbid, which shows that the temperature-resistant and salt-tolerant carbon dots cannot be prepared by using citric acid and sulfosalicylic acid as raw materials.
The results of the PL intensity (fluorescence intensity) measurements are shown in the O-CDs curve in FIG. 5.
Study example 2:
0.90g of glucose is weighed, dissolved in 25mL of deionized water, and is fully dissolved by ultrasonic waves, and then 0.6306g of isethionic acid is added, and is fully dissolved by ultrasonic waves. The solution was heated in a microwave reactor at 700W for 5 min. And naturally cooling to room temperature, taking out the obtained liquid, performing ultrasonic treatment for 20min at the ultrasonic power of 100Hz, performing suction filtration by using 0.22 mu m filter paper, taking the filtrate, dialyzing for 72h, and drying at 60 ℃ for 48h to obtain solid powder, namely SO-CDs.
According to the test conditions in example 1, NaCl solution with the same concentration is added dropwise and left standing for the same time, and the solution becomes turbid after the dropwise addition. And (3) placing the equivalent carbon dot solution in an oven at 83 ℃ for heating, wherein the heated solution is turbid, which shows that the temperature-resistant and salt-tolerant carbon dots cannot be prepared by adopting glucose and isethionic acid as raw materials.
Study example 3:
0.90g of glucose was weighed, dissolved in 25mL of deionized water, and sufficiently dissolved by sonication, and then 0.7207g of sulfosalicylic acid was added and sufficiently dissolved by sonication. The solution was heated in a microwave reactor at 700W for 5 min. And naturally cooling to room temperature, taking out the obtained liquid, dispersing the obtained liquid in deionized water by ultrasonic treatment for 20min, carrying out suction filtration by using filter paper with the diameter of 0.22 mu m, taking the filtrate, dialyzing for 72h, and drying at 60 ℃ for 48h to obtain solid powder, namely OH-CDs. However, the sample particles were large and carbon dots of conventional particle size could not be produced.
According to the test conditions in example 1, NaCl solution with the same concentration is added dropwise and left standing for the same time, and the solution becomes very turbid obviously after the dropwise addition. And (3) placing the equivalent carbon dot solution in an oven at 80 ℃ for heating, wherein the heated solution is turbid, which shows that the temperature-resistant and salt-tolerant carbon dots cannot be prepared by adopting glucose and sulfosalicylic acid as raw materials.
Study example 4:
weighing 0.96g of citric acid, dissolving in 25mL of deionized water, performing ultrasonic treatment to fully dissolve the citric acid, adding 0.6306g of ethyl sulfonic acid, performing ultrasonic treatment to fully dissolve the ethyl sulfonic acid, placing the solution in a microwave reactor, heating for 5min under the power of 700W, naturally cooling to room temperature, taking out the obtained liquid, performing ultrasonic treatment for 20min at the ultrasonic power of 100Hz, performing suction filtration by using 0.22 mu m filter paper, taking the filtrate, dialyzing in a dialysis bag with the molecular weight cutoff of 3500Da for 72h, and drying at 60 ℃ for 48h to obtain solid powder, namely the carbon dots S-O-CDs.
According to the test conditions in example 1, NaCl solution with the same concentration is added dropwise and left standing for the same time, and the solution becomes slightly turbid after the dropwise addition. And (3) placing the equivalent carbon dot solution in an oven at 80 ℃ for heating, wherein the heated solution is turbid, which shows that the temperature-resistant and salt-tolerant carbon dots cannot be prepared by using citric acid and ethyl sulfonic acid as raw materials.
Study example 5:
weighing 0.6705g (5mM) of DL-malic acid, dissolving in 25mL of deionized water, performing ultrasonic treatment to fully dissolve the DL-malic acid, then adding 5mM of ethylsulfonic acid, performing ultrasonic treatment to fully dissolve the DL-malic acid, placing the solution in a microwave reactor, heating for 5min under the power of 700W, naturally cooling to room temperature, taking out the obtained liquid, performing ultrasonic treatment for 20min under the ultrasonic power of 100Hz, performing suction filtration by using 0.22 mu m filter paper, taking the filtrate, dialyzing in a dialysis bag with the molecular weight cutoff of 3500Da for 72h, and drying at 60 ℃ for 48h to obtain solid powder, namely the carbon dots S-O-O-CDs.
According to the test conditions in example 1, NaCl solution with the same concentration is added dropwise and left standing for the same time, and the solution becomes slightly turbid after the dropwise addition. And (3) placing the equivalent carbon dot solution in an oven at 80 ℃ for heating, wherein the heated solution is slightly turbid.
Study example 6:
weighing 0.96g of citric acid, dissolving in 25mL of deionized water, performing ultrasonic treatment to fully dissolve the citric acid, adding 0.6306g of hydroxyethyl sulfonic acid, performing ultrasonic treatment to fully dissolve the citric acid, transferring the solution into a 50mL stainless steel autoclave with a polytetrafluoroethylene lining, reacting in an oven at 180 ℃ for 10h, naturally cooling to room temperature, taking out the obtained liquid, performing ultrasonic treatment for 20min, performing suction filtration by using 0.22 mu m filter paper, dialyzing the filtrate in a dialysis bag with molecular weight cutoff of 3500Da for 72h, and drying at 60 ℃ for 48h to obtain solid particles which are large and cannot prepare carbon dots with conventional particle sizes.
According to the test conditions in example 1, NaCl solution with the same concentration is added dropwise and left standing for the same time, and the solution becomes slightly turbid after the dropwise addition. And (3) placing the equivalent carbon dot solution in an oven at 83 ℃ for heating, wherein the heated solution is slightly turbid.
Study example 7:
weighing 0.96g of citric acid, dissolving in 25mL of deionized water, performing ultrasonic treatment to fully dissolve the citric acid, adding 0.6306g of hydroxyethyl sulfonic acid, performing ultrasonic treatment to fully dissolve the citric acid, placing the solution in a microwave reactor, heating for 5min under 800W power, naturally cooling to room temperature, taking out the obtained sample, and observing that more black solids are generated, which indicates that the reactant is excessively carbonized in the reaction system and cannot obtain corresponding carbon dots.
In conclusion, the carbon dots prepared by the method have strong adaptability to high-temperature and high-salt environments and high fluorescence intensity. The carbon dots have the advantages of low raw material cost, simple preparation method and short preparation time. These advantages make it promising for mass production and application to industrial production.
It should be noted that the above-mentioned embodiments are only for illustrating the technical solutions of the present invention and not for limiting, and although the present invention has been described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that modifications or equivalent substitutions may be made on the technical solutions of the present invention without departing from the spirit and scope of the technical solutions of the present invention, which should be covered by the claims of the present invention.

Claims (8)

1. A method for simply preparing temperature-resistant salt-tolerant carbon dots is characterized by comprising the following steps: the method comprises the following steps: dissolving citric acid and isethionic acid in water, reacting in a microwave reactor, and performing ultrasonic dispersion, suction filtration, dialysis and drying to obtain carbon dots; the reaction is carried out in a microwave reactor, and the microwave power is 700W.
2. The simple method for preparing the temperature and salt resistant carbon points according to claim 1, which comprises the following steps: the molar ratio of the citric acid to the hydroxyethyl sulfonic acid is 1: 1.
3. the simple method for preparing temperature and salt resistant carbon points according to claim 1 or 2, which is characterized in that: and in the ultrasonic dispersion, the ultrasonic power is 80-150 Hz, and the ultrasonic time is 15-25 min.
4. The simple method for preparing the temperature and salt resistant carbon points according to claim 3, which comprises the following steps: the reaction is carried out in a microwave reactor for 5 min.
5. The simple method for preparing temperature and salt resistant carbon points according to claim 1 or 2, characterized in that: dissolving citric acid and isethionic acid in water, wherein in order to dissolve the citric acid in the water, ultrasonic waves are used for fully dissolving the citric acid, and then the isethionic acid is added for fully dissolving the citric acid by ultrasonic waves.
6. The simple method for preparing temperature and salt resistant carbon points according to claim 1 or 2, which is characterized in that: the filtration was carried out by filtration through a 0.22 μm filter paper.
7. The simple method for preparing temperature and salt resistant carbon points according to claim 1 or 2, which is characterized in that: and (3) dialyzing the filtrate after suction filtration for 72 hours in a dialysis bag with the molecular weight cutoff of 3500 Da.
8. The simple method for preparing temperature and salt resistant carbon points according to claim 1 or 2, which is characterized in that: the drying is carried out for 24-48 h at 50-60 ℃.
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