CN109437155B - Method for simultaneously preparing carbon quantum dots and carbon nanospheres and product thereof - Google Patents
Method for simultaneously preparing carbon quantum dots and carbon nanospheres and product thereof Download PDFInfo
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- CN109437155B CN109437155B CN201811536356.1A CN201811536356A CN109437155B CN 109437155 B CN109437155 B CN 109437155B CN 201811536356 A CN201811536356 A CN 201811536356A CN 109437155 B CN109437155 B CN 109437155B
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Abstract
The invention discloses a method for simultaneously preparing carbon quantum dots and carbon nanospheres, which adopts glucose and sodium hydroxide as raw materials, simultaneously synthesizes and obtains the carbon quantum dots and the carbon nanospheres by a one-step simple hydrothermal method, simultaneously does not need to add any surfactant, dispersant or template, realizes green and energy-saving preparation and effectively avoids waste liquid. The method has the advantages of simple synthesis process and equipment, low cost, high efficiency, short reaction period and good repeatability, the diameter of the prepared carbon quantum dot is 5-15nm, the diameter of the carbon nanosphere is 100-300 nm, the product does not contain byproducts or waste liquid, and the industrial application prospect is wide.
Description
Technical Field
The invention relates to a preparation method of carbon quantum dots and carbon nanospheres and a product thereof, in particular to a method for simultaneously preparing the carbon quantum dots and the carbon nanospheres without adding any surfactant, dispersant or template and a product thereof; belongs to the field of nanometer material preparation.
Background
Carbon materials have been recently proved to be superior to other materials in hardness, optical characteristics, heat-resistant nanocarbon materials, radiation-resistant characteristics, chemical-resistant characteristics, electrical insulation, electrical conductivity, surface and interface characteristics, etc., and it can be said that carbon materials almost include characteristics possessed by all substances on the earth, such as hardest-softest, insulator-semiconductor-good conductor, thermal insulation-good heat conduction, total light absorption-total light transmission, etc., and thus carbon materials have wide applications in various fields.
Among many carbon materials, a representative carbon material is a carbon quantum dot, which is a novel carbon-based zero-dimensional material and has excellent optical properties, good water solubility, low toxicity, environmental friendliness, wide raw material source, low cost, good biocompatibility and other advantages, since the carbon quantum dot was first discovered, many synthetic methods including an arc discharge method, a laser ablation method, an electrochemical synthesis method, a chemical oxidation method, a combustion method, a hydrothermal synthesis method, a microwave synthesis method, a template method and the like (Guo Shao, Tang Yuan, Meng, Li, Yangwei. preparation of fluorescent carbon quantum dots and biomedical application research progress [ J ] China optics, 2018,11(03): 431-. With the intensive research on carbon quantum dots, great progress has been made in the synthesis, performance and application of carbon quantum dots. Meanwhile, the carbon quantum dots have wide raw material sources and low preparation cost, and have great advantages in the field of material preparation; the preparation method has good application prospect in the fields of medical imaging equipment, tiny light-emitting diodes, chemical sensors, photocatalytic reactions and the like (trade mark. preparation method of fluorescent carbon quantum dot material patent technology review [ J ]. metallurgy and materials, 2018,38(05):187+ 189.).
In addition to quantum dots, carbon nanospheres are a representative family of carbon materials, and have attracted the development interest of many researchers due to their high density, high strength, high specific surface area, and broad application prospects in lithium ion batteries, catalyst supports, and metal oxide hollow templates. (Lisaisaisaisai, Lifeng, Liangliang, Wang army Kai, Song Jianbo, Zhang Naihun. Process optimization research on preparation of monodisperse carbon microspheres by hydrothermal carbonization of glucose [ J ] refractory material, 2017,51(01): 32-36.).
At present, the methods for preparing the carbon quantum dots or the carbon nanospheres mainly include a hydrothermal method, a chemical vapor deposition method, a pyrolysis method and a template method, and the methods can be used for preparing the high-quality carbon quantum dots or the carbon nanospheres, but have the following defects: one preparation requires the introduction of a surfactant, a dispersant or a template (such as a template method and a pyrolysis method), the other preparation cannot realize large-scale mass production (chemical vapor deposition), and the other preparation obtains a single product and generates a large amount of waste liquid (conventional hydrothermal method) during preparation, so that pollution and waste are caused. Based on the method, the method for simultaneously synthesizing the carbon quantum dots and the carbon nanospheres is developed, any surfactant, dispersant or template is not required to be added in the preparation process, and the method for simultaneously producing the carbon quantum dots and the carbon nanospheres on a large scale is significant. Through retrieval, the related preparation methods are rarely reported at present.
Disclosure of Invention
Aiming at the defects of the preparation methods of the carbon quantum dots and the carbon nanospheres in the prior art, the invention aims to provide a method for simultaneously preparing the carbon quantum dots and the carbon nanospheres and a product thereof.
The method for simultaneously preparing the carbon quantum dots and the carbon nanospheres comprises the following steps:
(1) weighing glucose, dissolving the glucose in deionized water, adding sodium hydroxide after stirring and dissolving, continuously stirring and dissolving completely, and then adding the glucose into a hydrothermal reaction kettle, wherein the filling degree is controlled to be 60-80% of the volume of the reaction kettle; then sealing the reaction kettle, putting the reaction kettle into an oven, and heating for reaction;
(2) naturally cooling to room temperature after the reaction is finished, taking out the reaction kettle, pouring the dark brown solution in the kettle into a centrifugal tube, and centrifuging to generate an upper layer solution and a bottom precipitate;
(3) transferring the upper layer solution into a centrifugal tube, quickly freezing the upper layer solution under the action of liquid nitrogen, and then freeze-drying the frozen sample to obtain the fluorescent carbon quantum dots;
(4) dispersing the lower layer precipitate with deionized water, suction filtering with microporous filtering membrane, washing the product with deionized water to neutrality, and drying to obtain carbon nanospheres;
the method is characterized in that:
the glucose, the deionized water and the sodium hydroxide added into the hydrothermal reaction kettle in the step (1) are sequentially added in parts by weight: 1-20 parts of glucose, 100 parts of deionized water and 0.1-0.15 part of sodium hydroxide; wherein the stirring and dissolving time of the glucose added into the deionized water is not less than 30min, and the stirring time of the glucose added with the sodium hydroxide after dissolution is not less than 10 min; the conditions of the heating reaction are as follows: controlling the hydrothermal temperature at 150-220 ℃ and reacting for 5-15 h;
the centrifugation conditions of the dark brown solution in the step (2) are as follows: under the centrifugal force action of 3000 g-4000 g, centrifugally separating for 10 min-20 min;
the freeze drying conditions in the step (3) are as follows: the temperature is-70 ℃, the pressure is 5-10 Pa, and the freezing time is 24 +/-1 h;
the aperture of the microporous filter membrane in the step (4) is 40 um; the drying conditions are as follows: 50-70 ℃.
The method for simultaneously preparing the carbon quantum dots and the carbon nanospheres comprises the following steps: the glucose, the deionized water and the sodium hydroxide added into the hydrothermal reaction kettle in the step (1) preferably comprise the following components in parts by weight: 5-10 parts of glucose, 100 parts of deionized water and 0.1 part of sodium hydroxide; wherein, the stirring and dissolving time of the glucose added into the deionized water is preferably 30min +/-5 min, and the stirring time of the glucose added with the sodium hydroxide after dissolution is preferably 10min +/-5 min; the conditions for the heating reaction are preferably: controlling the hydrothermal temperature at 180-200 ℃ and reacting for 8-10 h.
Further, in the method for simultaneously preparing the carbon quantum dots and the carbon nanospheres, the method comprises the following steps: the glucose, the deionized water and the sodium hydroxide added into the hydrothermal reaction kettle in the step (1) preferably comprise the following components in parts by weight: 5 parts of glucose, 100 parts of deionized water and 0.1 part of sodium hydroxide; wherein, the stirring and dissolving time of the glucose added into the deionized water is preferably 30min, and the stirring time of the glucose added with the sodium hydroxide after dissolution is preferably 10 min; the conditions for the heating reaction are preferably: the hydrothermal temperature was controlled at 200 ℃ and the reaction was carried out for 10 hours.
The method for simultaneously preparing the carbon quantum dots and the carbon nanospheres comprises the following steps: the centrifugation conditions of the dark brown solution in the step (2) are preferably as follows: centrifuging at 3500g for 20 min.
The method for simultaneously preparing the carbon quantum dots and the carbon nanospheres comprises the following steps: the conditions for the freeze-drying in the step (3) are preferably: the temperature is-70 deg.C, the pressure is 10Pa, and the freezing time is 24 h.
The method for simultaneously preparing the carbon quantum dots and the carbon nanospheres comprises the following steps: the drying condition in the step (4) is preferably 50 ℃.
The carbon quantum dot and the carbon nanosphere prepared by the method of the invention are characterized in that: the diameter size of the carbon quantum dots is 5-15nm, the carbon quantum dots have obvious fluorescence characteristics under the action of excitation light of 320 nm-420 nm, and the corresponding emission light intensity is gradually reduced along with the increase of the wavelength of the excitation light; the carbon nanospheres have a diameter size of 100-300 nm and a monodispersity characteristic.
Wherein: the diameter of the carbon quantum dot is preferably 10m +/-2 nm; the diameter of the carbon nanoball is preferably 150nm ± 20 nm.
The invention discloses a method for simultaneously preparing carbon quantum dots and carbon nanospheres and a product thereof. The method adopts glucose and sodium hydroxide as raw materials, adopts a strategy from bottom to top, utilizes a simple hydrothermal method to synthesize and obtain the carbon quantum dots and the carbon nanospheres simultaneously, and simultaneously does not need to add any surfactant, dispersant or template, thereby realizing green and energy-saving preparation and effectively avoiding the generation of waste liquid. In the preparation method provided by the invention, the black brown solution after reaction can be separated from the upper layer solution to the maximum extent through centrifugation to obtain the carbon quantum dots, and meanwhile, the method is beneficial to cleaning of the carbon nano particles precipitated at the bottom, and really realizes energy-saving and green chemical synthesis. The invention has the advantages of simple synthesis process and equipment, low cost, high efficiency, short reaction period, good repeatability and wide industrial application prospect.
Drawings
Fig. 1 is a Transmission Electron Microscope (TEM) photograph of the prepared carbon quantum dot sample.
Fig. 2 is a fluorescence spectrum (PL) of the prepared carbon quantum dot sample.
Fig. 3 is a Scanning Electron Microscope (SEM) photograph of the prepared carbon nanoball sample.
Detailed Description
The present invention will be described in detail with reference to specific examples. The following examples are merely illustrative of the preferred embodiments of the present invention and are not intended to limit the present invention in any way, and any simple modifications, equivalent changes and modifications made to the embodiments according to the technical spirit of the present invention fall within the scope of the technical solution of the present invention.
The raw materials or reagents used in the invention are all conventional commercial products.
Example 1:
(1) weighing 5 parts by weight of glucose, dissolving the glucose in 100 parts by weight of deionized water, stirring for reaction for 30min to fully dissolve the glucose, then adding 0.1 part by weight of sodium hydroxide, continuously stirring for 10min, transferring the mixture into a hydrothermal reaction kettle after complete dissolution, controlling the filling degree to be 80% of the volume of the reaction kettle, and putting the reaction kettle into an oven. Setting the heating reaction conditions as follows: the temperature is 220 ℃, and the reaction time is 10 h.
(2) After the reaction is finished, cooling to room temperature, taking out the reaction kettle, pouring the dark brown solution in the kettle into a centrifugal tube, and carrying out centrifugal separation for 20min under the action of 3500g centrifugal force to obtain an upper layer solution and a bottom precipitate respectively.
(3) Transferring the upper layer solution into a centrifuge tube, rapidly freezing the upper layer solution under the action of liquid nitrogen, and freeze-drying the frozen sample, wherein the freeze-drying conditions are as follows: freezing for 24h at-70 ℃ under the pressure of 10Pa, and drying to obtain fluorescent carbon quantum dots; and dispersing the lower-layer precipitate by deionized water again, then performing suction filtration by using a 40-micron microporous filter membrane, washing the product to be neutral by using the deionized water, and drying at 50 ℃ to obtain the carbon nanospheres.
The obtained carbon quantum dot sample was observed with a transmission electron microscope model JEM 2100F manufactured by JEOL (see FIG. 1 for the result); as can be seen from FIG. 1, the prepared carbon quantum dots have diameters of 8 to 12nm and uniform particle sizes.
The obtained carbon quantum dot sample solution was subjected to fluorescence property analysis using a fluorescence spectrometer F-7000 manufactured by Hitachi corporation (see the result in FIG. 2); as can be seen from FIG. 2, the prepared carbon quantum dots have remarkable fluorescence characteristics under the action of excitation light of 320nm to 420 nm; and the corresponding emission light intensity is gradually reduced along with the increase of the excitation light wavelength, and the emission light wavelength is increased along with the increase of the excitation light wavelength, so that the carbon quantum dot has the typical fluorescence characteristic.
The obtained carbon nanoball sample was observed by a scanning electron microscope of S-4800 model manufactured by Hitachi corporation of Japan (see FIG. 3 for the result); as can be seen from FIG. 3, the carbon nanospheres have a size of 120-150 nm and a certain monodispersity.
Example 2:
(1) weighing 1 part of glucose by weight, dissolving the glucose in 100 parts of deionized water, stirring for reaction for 25min to fully dissolve the glucose, adding 0.1 part of sodium hydroxide, continuously stirring for 8min, transferring the mixture into a hydrothermal reaction kettle after complete dissolution, controlling the filling degree to be 60% of the volume of the reaction kettle, and putting the reaction kettle into an oven. Setting the heating reaction conditions as follows: the temperature is 150 ℃, and the reaction time is 5-15 h.
(2) After the reaction is finished, cooling to room temperature, taking out the reaction kettle, pouring the dark brown solution in the kettle into a centrifuge tube, and carrying out centrifugal separation for 10min under the action of 3000g of centrifugal force to obtain an upper layer solution and a bottom precipitate respectively.
(3) Transferring the upper solution into a centrifugal tube, quickly freezing the upper solution under the action of liquid nitrogen, and freeze-drying the frozen sample, wherein the freeze-drying conditions are as follows: freezing for 20h at-70 ℃ and under the pressure of 8Pa, and drying to obtain fluorescent carbon quantum dots; and dispersing the lower-layer precipitate by deionized water again, then carrying out suction filtration by a 40-micron microporous filter membrane, washing the product to be neutral by the deionized water, and drying at 50 ℃ to obtain the carbon nanospheres.
Example 3:
(1) weighing 20 parts by weight of glucose, dissolving the glucose in 100 parts by weight of deionized water, stirring for reaction for 35min to fully dissolve the glucose, adding 0.15 part by weight of sodium hydroxide, continuously stirring for 15min, introducing the mixture into a hydrothermal reaction kettle after complete dissolution, controlling the filling degree to be 80% of the volume of the reaction kettle, and putting the reaction kettle into an oven. Setting the heating reaction conditions as follows: the temperature is 220 ℃, and the reaction time is 15 h.
(2) After the reaction is finished, cooling to room temperature, taking out the reaction kettle, pouring the dark brown solution in the kettle into a centrifugal tube, and carrying out centrifugal separation for 20min under the action of 4000g of centrifugal force to respectively obtain an upper layer solution and a bottom precipitate.
(3) And (3) introducing the upper solution into a centrifugal tube, rapidly freezing under the action of liquid nitrogen, and freeze-drying the frozen sample, wherein the freeze-drying conditions are as follows: freezing for 25h at-70 ℃ and under the pressure of 10Pa, and drying to obtain fluorescent carbon quantum dots; and dispersing the lower-layer precipitate by deionized water again, then carrying out suction filtration by a 40-micron microporous filter membrane, washing the product to be neutral by the deionized water, and drying at 70 ℃ to obtain the carbon nanospheres.
Example 4:
(1) weighing 10 parts by weight of glucose, dissolving the glucose in 100 parts by weight of deionized water, stirring for reaction for 30min to fully dissolve the glucose, adding 0.1 part by weight of sodium hydroxide, continuously stirring for 10min, introducing the mixture into a hydrothermal reaction kettle after complete dissolution, controlling the filling degree to be 70% of the volume of the reaction kettle, and putting the reaction kettle into an oven. Setting the heating reaction conditions as follows: the temperature is 180 ℃, and the reaction time is 8 h.
(2) After the reaction is finished, cooling to room temperature, taking out the reaction kettle, pouring the dark brown solution in the reaction kettle into a centrifugal tube, and carrying out centrifugal separation for 15min under the action of 3800g of centrifugal force to obtain an upper layer solution and a bottom precipitate respectively.
(3) Transferring the upper solution into a centrifugal tube, quickly freezing the upper solution under the action of liquid nitrogen, and freeze-drying the frozen sample, wherein the freeze-drying conditions are as follows: freezing for 24h at-70 ℃ and 5Pa, and drying to obtain fluorescent carbon quantum dots; and dispersing the lower-layer precipitate by deionized water again, then carrying out suction filtration by a 40-micron microporous filter membrane, washing the product to be neutral by the deionized water, and drying at 60 ℃ to obtain the carbon nanospheres.
Claims (3)
1. A method for simultaneously preparing carbon quantum dots and carbon nanospheres comprises the following steps:
(1) weighing glucose, dissolving the glucose in deionized water, adding sodium hydroxide after stirring and dissolving, continuously stirring and dissolving completely, and then adding the glucose into a hydrothermal reaction kettle, wherein the filling degree is controlled to be 60-80% of the volume of the reaction kettle; then sealing the reaction kettle, putting the reaction kettle into an oven, and heating for reaction;
(2) naturally cooling to room temperature after the reaction is finished, taking out the reaction kettle, pouring the dark brown solution in the kettle into a centrifugal tube, and centrifuging to generate an upper layer solution and a bottom precipitate; wherein the centrifugation conditions of the dark brown solution are: under the action of a centrifugal force of 3000 g-4000 g, performing centrifugal separation for 10 min-20 min;
(3) transferring the upper layer solution into a centrifugal tube, quickly freezing the upper layer solution under the action of liquid nitrogen, and then freeze-drying the frozen sample to obtain the fluorescent carbon quantum dots; wherein the conditions of freeze-drying are: the temperature is-70 ℃, the pressure is 5-10 Pa, and the freezing time is 24 +/-1 h;
(4) dispersing the lower layer precipitate with deionized water, suction filtering with microporous filtering membrane, washing the product with deionized water to neutrality, and drying to obtain carbon nanospheres; wherein the pore size of the microporous filter membrane is 40 um; the drying conditions are as follows: 50-70 ℃;
the method is characterized in that:
the glucose, the deionized water and the sodium hydroxide added into the hydrothermal reaction kettle in the step (1) are sequentially added in parts by weight: 1-20 parts of glucose, 100 parts of deionized water and 0.1-0.15 part of sodium hydroxide; wherein the stirring and dissolving time of the glucose added into the deionized water is not less than 30min, and the stirring time of the glucose added with the sodium hydroxide after dissolution is not less than 10 min; the conditions of the heating reaction are as follows: controlling the hydrothermal temperature at 150-220 ℃ and reacting for 5-15 h.
2. The method for simultaneously preparing the carbon quantum dots and the carbon nanospheres according to claim 1, wherein the method comprises the following steps: the glucose, the deionized water and the sodium hydroxide added into the hydrothermal reaction kettle in the step (1) are sequentially added in parts by weight: 5-10 parts of glucose, 100 parts of deionized water and 0.1 part of sodium hydroxide; wherein the stirring and dissolving time of the glucose added into the deionized water is 30min +/-5 min, and the stirring time of the glucose added with the sodium hydroxide after dissolution is 10min +/-5 min; the conditions of the heating reaction are as follows: controlling the hydrothermal temperature at 180-200 ℃ and reacting for 8-10 h.
3. The method for simultaneously preparing the carbon quantum dots and the carbon nanospheres according to claim 2, wherein the method comprises the following steps: the glucose, the deionized water and the sodium hydroxide added into the hydrothermal reaction kettle in the step (1) are sequentially added in parts by weight: 5 parts of glucose, 100 parts of deionized water and 0.1 part of sodium hydroxide; wherein the stirring and dissolving time of the glucose added into the deionized water is 30min, and the stirring time of the glucose added with the sodium hydroxide after dissolution is 10 min; the conditions of the heating reaction are as follows: the hydrothermal temperature was controlled at 200 ℃ and the reaction was carried out for 10 hours.
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| CN102745669A (en) * | 2012-07-18 | 2012-10-24 | 中国人民解放军军事医学科学院卫生装备研究所 | Method for preparing photoluminescence carbon quantum dot |
| CN103771391A (en) * | 2014-01-21 | 2014-05-07 | 中国计量学院 | Preparation method of water-soluble carbon nanoparticles having fluorescent properties |
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| CN102745669A (en) * | 2012-07-18 | 2012-10-24 | 中国人民解放军军事医学科学院卫生装备研究所 | Method for preparing photoluminescence carbon quantum dot |
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