CN109876845B - M-g-C3N4Preparation method and application of/rGOA composite adsorption visible light catalytic material - Google Patents
M-g-C3N4Preparation method and application of/rGOA composite adsorption visible light catalytic material Download PDFInfo
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Abstract
The invention provides M-g-C3N4The preparation method and the application of the/rGOA composite adsorption visible light catalytic material comprise the following steps: 1) adding melamine into deionized water at the temperature of 80-90 ℃, cooling to room temperature, adding hydrochloric acid, stirring, and evaporating and drying to obtain melamine hydrochloride, wherein the molar ratio of the melamine to the hydrochloric acid is 1: 0.5-1: 2; putting melamine hydrochloride into a muffle furnace, keeping the temperature at 500 ℃ for 2h, then heating to 520 ℃ for 2h, cooling and grinding to obtain M-g-C3N4(ii) a 2) Mixing M-g-C3N4Adding into deionized water for ultrasonic treatment; adding graphene oxide; adding a certain mass of sodium bisulfite into the graphene oxide mixed solution, carrying out ultrasonic treatment and heating to obtain hydrogel, removing impurity ions from the hydrogel, and carrying out freeze drying. The composite material obtained by the method can effectively adsorb and degrade organic dyes and antibiotics.
Description
Technical Field
The invention relates to the technical field of environment and chemistry, in particular to M-g-C3N4Preparation method and application of/rGOA composite adsorption visible light catalytic material.
Background
Organic dye pollution is one of important sources of water environment pollution, and with the rapid development of the world industry, particularly in developing countries, the annual yield of the organic dye is 7 multiplied by 105t, is widely used in the industries of paper making, leather processing, textile dyeing, cosmetics, pharmaceutical manufacturing, and the like. Is one in ChinaIn large countries for producing and using antibiotics, various antibiotics such as amoxicillin, cefotaxime sodium and the like are detected in environmental water at present. The existing methods for solving the problem of organic pollution of dyes, antibiotics and the like comprise biodegradation, physical and chemical adsorption, advanced oxidation, visible light catalysis and the like. The visible light catalysis method can save energy and degrade organic pollution, so the method has attracted extensive attention.
Graphite phase carbon nitride (g-C)3N4) As a non-metal catalyst, the adjustable band gap width is 1.8-2.7 eV, the physical and chemical properties are stable, the catalyst is non-toxic and pollution-free, the visible light response range is wide, and the catalyst has good catalytic activity under the condition of visible light. Graphene Oxide Aerogels (GOAs) as a new carbon material have received attention from more and more researchers due to their characteristics of large specific surface area, low density, high elasticity and strong adsorption. The larger specific surface area not only can provide attachment sites for the powder photocatalytic material, but also has good adsorption capacity, and in addition, the good conductivity can improve the transfer efficiency of electrons and effectively inhibit the recombination of electrons and holes. Compared with two-dimensional graphene, the graphene has the characteristics of easy recovery and repeated use. In addition, the three-dimensional graphene aerogel can control the shape, size and density of the aerogel by controlling the concentration of graphene oxide and the shape of the reactor. Therefore, a three-dimensional graphene aerogel composite material which can be used for efficiently adsorbing visible light to catalytically degrade organic wastewater and can be better applied to practical engineering is needed.
Disclosure of Invention
The invention provides M-g-C3N4A preparation method and application of a/rGOA composite adsorption visible light catalytic material, which aim to solve the problems.
In order to achieve the purpose, the invention adopts the following technical scheme.
The invention provides M-g-C3N4The preparation method of the/rGOA composite adsorption visible light catalytic material comprises the following steps:
(1)M-g-C3N4the preparation of (1):
at 80 deg.CAdding melamine into deionized water at the temperature of 90 ℃ below zero, cooling the solution to room temperature, adding a certain amount of hydrochloric acid into the solution, continuously stirring, wherein the molar ratio of the melamine to the hydrochloric acid is 1: 0.5-1: 2, uniformly stirring, and evaporating and drying to obtain melamine hydrochloride; putting the melamine hydrochloride into a muffle furnace, heating to 500 ℃ and keeping for 2h, then heating to 520 ℃ and keeping for 2h, and finally cooling and grinding to obtain light yellow M-g-C3N4；
(2)M-g-C3N4Preparation of rGOA:
mixing a certain amount of said M-g-C3N4Adding into deionized water, and performing ultrasonic treatment to obtain M-g-C3N4Mixing the solution; for the M-g-C3N4Adding a certain amount of graphene oxide into the mixed solution to obtain a graphene mixed solution; adding a certain mass of sodium bisulfite into the graphene mixed solution, and performing ultrasonic treatment again until the mixture is uniformly mixed; heating for 2.5-3.0 h at 95 ℃ by using an air drying oven to obtain hydrogel, removing impurity ions from the hydrogel, and freeze-drying to obtain M-g-C3N4the/rGOA composite adsorption visible light catalytic material.
Preferably, the molar ratio of melamine to hydrochloric acid is 1: 1.
Preferably, M-g-C3N4And the mass ratio of the graphene oxide to the graphene oxide is (2:9) - (6: 9).
Preferably, M-g-C3N4The mass ratio of the graphene oxide to the graphene oxide is 3:9
Preferably, the graphene oxide in the step (2) is prepared by a modified Hummers method.
Preferably, the adding amount of the sodium bisulfite in the step (2) is 6-7 mg/mL.
Preferably, the evaporation drying in the step (1) adopts a forced air drying oven for drying at a constant temperature of 80 ℃.
In another aspect of the invention, M-g-C is used3N4M-g-C prepared by method of/rGOA composite adsorption visible light catalytic material3N4rGOA composite adsorption visible light catalytic material for sewage treatment of organic dye and antibioticAnd (3) adsorbing the organic dye and the antibiotic and performing visible light catalytic degradation.
From M-g-C of the invention described above3N4The preparation method and application of the/rGOA composite adsorption visible light catalytic material can be seen that the M-g-C obtained by the method of the invention3N4Under the condition of visible light irradiation, the/rGOA composite material has the structure of M-g-C3N4The generated photoelectrons can be rapidly transferred to the rGO sheet layer through a plurality of electron transfer channels, so that the recombination of electron-hole pairs is effectively inhibited, and the catalytic performance of the photocatalyst is fully exerted; the composite material has a macroscopic three-dimensional structure which is not only g-C3N4Provides attachment sites, provides adsorption sites for pollutants and is easy to recycle. The composite material has higher catalytic efficiency for degrading dye wastewater than that of pure M-g-C3N4Is easier to recycle, and is beneficial to the recycling of environment and energy; good mechanical compression resistance, excellent cycle performance and simple production process.
Additional aspects and advantages of the invention will be set forth in part in the description which follows, and in part will be obvious from the description, or may be learned by practice of the invention.
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 are 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 creative efforts.
FIG. 1 shows rGOA, M-g-C3N4、M-g-C3N4SEM pictures of/rGOA composite adsorption visible light catalytic material, (a, b) are SEM pictures of rGOA, and (C) is M-g-C3N4SEM picture of/rGOA composite adsorption visible light catalytic material, wherein (d) is M-g-C3N4SEM picture of (1);
FIG. 2 shows M-g-C3N4The x-ray diffraction pattern of the/rGOA composite adsorption visible light catalytic material;
FIG. 3 shows M-g-C3N4BET diagram of/rGOA composite adsorption visible light catalytic material;
FIG. 4 shows M-g-C3N4The adsorption degradation trend graph of the/rGOA composite adsorption visible light catalytic material on the antibiotics is shown;
FIG. 5 shows M-g-C3N4The absorption result diagram of the/rGOA composite absorption visible light catalytic material on the dye;
FIG. 6 shows M-g-C3N4A visible light catalysis result diagram of the/rGOA composite adsorption visible light catalysis material to the dye;
FIG. 7 shows M-g-C3N4A circulating experiment result diagram of catalyzing and degrading dye by the/rGOA composite adsorption visible light catalytic material.
Detailed Description
Reference will now be made in detail to embodiments of the present invention, examples of which are illustrated in the accompanying drawings, wherein like reference numerals refer to the same or similar elements or elements having the same or similar function throughout. The embodiments described below with reference to the accompanying drawings are illustrative only for the purpose of explaining the present invention, and are not to be construed as limiting the present invention.
As used herein, the singular forms "a", "an", "the" and "the" are intended to include the plural forms as well, unless the context clearly indicates otherwise. It will be further understood that the terms "comprises" and/or "comprising," when used in this specification, specify the presence of stated features, integers, steps, and/or operations, but do not preclude the presence or addition of one or more other features, integers, steps, and/or operations. It should be understood that the term "and/or" as used herein includes any and all combinations of one or more of the associated listed items.
It will be understood by those skilled in the art that, unless otherwise defined, all terms (including 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. It will be further understood that terms, such as those defined in commonly used dictionaries, should be interpreted as having a meaning that is consistent with their meaning in the context of the prior art and will not be interpreted in an idealized or overly formal sense unless expressly so defined herein.
To facilitate an understanding of embodiments of the present invention, several specific embodiments are described below in conjunction with the accompanying drawings.
Examples
This example provides M-g-C3N4The preparation method of the/rGOA (mesoporous graphite phase carbon nitride/reduced graphene oxide aerogel) composite adsorption visible light catalytic material comprises the following steps:
firstly, adding melamine into deionized water at the temperature of 80-90 ℃, after the temperature of the solution is cooled to room temperature, adding 37% hydrochloric acid (the molar ratio of the melamine to the hydrochloric acid is 1:1) under magnetic stirring, continuously stirring for 30min, and then putting the mixture into a forced air drying oven at the temperature of 80 ℃ for evaporation and drying to obtain melamine hydrochloride;
putting melamine hydrochloride into a crucible with a cover, heating to 500 ℃ at a heating rate of 20 ℃/min in an atmosphere type muffle furnace and keeping for 2h, and then heating to 520 ℃ at a heating rate of 4 ℃/min and keeping for 2 h; cooling and grinding to obtain light yellow M-g-C3N4。
60mg of the thus-obtained M-g-C3N4Adding into deionized water, and performing ultrasonic treatment for 150 min; then adding Graphene Oxide (GO) to prepare 60mL (M-g-C) of water solution with GO concentration of 3.0mg/mL3N4And graphene oxide in a mass ratio of 3: 9); weighing 512mg NaHSO3Adding into the above water solution, performing ultrasonic treatment for 20min, and mixing; after the ultrasonic treatment is finished, the hydrogel is moved into a blast drying oven, heated for 2.5 hours at the temperature of 95 ℃ to obtain hydrogel, the hydrogel is soaked for 6 hours by using deionized water, water is changed every 2 hours in the soaking period, and the hydrogel is cleaned to remove impurity ions; finally, the mixture is frozen and dried by a freezing dryer to obtain M-g-C3N4the/rGOA composite adsorption visible light catalytic material. FIG. 1 shows rGOA, M-g-C3N4、M-g-C3N4SEM picture of/rGOA composite adsorption visible light catalytic material: FIG. 1(a, b) shows rGOASEM images with different multiples, wherein the rGOA (reduced graphene oxide aerogel) is composed of a two-dimensional rGO (reduced graphene oxide) lamellar structure, the diagram (b) is a clearer reaction hole structure, and the M-g-C structure can be seen in the diagram (d) of FIG. 13N4A lamellar block structure. FIG. 1(C) rGOA layer with scale-like protrusions, illustrating two-dimensional sheet-like M-g-C3N4Adhesion to rGOA. And the corresponding layered structure, as well as pore structure, can be seen in fig. 1(C), so that the recombination of M-g-C3N4 with rGOA does not destroy the original structure of rGOA.
FIG. 2 shows M-g-C3N4The x-ray diffraction pattern of the/rGOA composite adsorption visible light catalytic material is as follows: referring to FIG. 2, M-g-C3N4Two relatively obvious diffraction peaks of 13.1 degrees and 27.2 degrees appear, and the diffraction peak of 13.1 degrees corresponds to g-C3N4The (100) crystal face periodically repeated in the surface in the structure, and the 27.2-degree diffraction peak corresponds to the (002) crystal face stacked between conjugated layers. The presence of crystal plane (100) indicates g-C3N4Planar attachment of the medium triazine units. A wider diffraction peak corresponding to a loosely packed (002) crystal face, M-g-C, can be observed at 22.6 degrees for single-phase rGOA3N4M-g-C in/rGOA composite aerogel3N4The diffraction peak at 13.1 ℃ disappeared to show that g-C3N4The crystal structure is changed in the compounding process because GO is subjected to M-g-C in the hydrothermal reaction process3N4With rGO, g-C3N4The diffraction peak at 27.2 ° was also clearly observed, indicating that the two were successfully combined.
FIG. 3 shows M-g-C3N4BET diagram of/rGOA composite adsorption visible light catalytic material: from FIG. 3(a), M-g-C can be seen3N4、rGOA、M-g-C3N4the/rGOA composite adsorption visible light catalytic material has a large hysteresis loop, which according to IUPAC belongs to the type IV adsorption-desorption isotherm, caused by the porous structure present in the sample. Thus, the adsorption characteristics of nitrogen were poor for the three samples at P/P0 ═ 0.45 to 1.00, and the hysteresis cycle indicated the presence of porosity, indicating M-g-C3N4Porosity is present. From FIG. 3 (b)) As can be seen, M-g-C3N4The pore diameter of (A) is mainly distributed at 2-50nm, and the medium and large pores are less. The pore diameter of rGOA is 2-5nm, and the pore diameter is M-g-C3N4The pore diameter of the/rGOA hybrid is 2-8nm, which shows that the composite material of the embodiment of the invention keeps the original porous structure.
M-g-C obtained by adopting the embodiment of the invention3N4the/rGOA composite adsorption visible light catalytic material can still recover to the original shape under the pressure which is 1600 times of the self weight, and has good mechanical property.
Simultaneously, according to the steps, the following mass ratio of M-g-C is prepared3N4the/rGOA composite adsorption visible light catalytic material: M-g-C3N4：GO＝6:9、M-g-C3N：GO＝5:9、M-g-C3N4：GO＝4:9、M-g-C3N4: GO 2:9 for application experiments.
Application example 1
100mg of M-g-C were added separately3N4rGOA composite material (M-g-C)3N4And graphene oxide in a mass ratio of 3:9) were dispersed in an aqueous solution of amoxicillin (50mL, 2mg/L) and cefotaxime sodium antibiotic (50mL, 2mg/L) under magnetic stirring, and after dispersion, the solution was adsorbed for 30min in the dark. Then, the solution was irradiated with visible light of 300W xenon lamp with a wavelength of 420nm or less, and 3mL of the solution was collected every 10min and subjected to centrifugal filtration to analyze the concentration of the antibiotic. All experiments are repeated for three times, and the accuracy of the experiments is ensured. FIG. 4 is a graph showing the adsorption degradation tendency of the composite material to antibiotics. Referring to fig. 4, in the dark adsorption stage, adsorption of two antibiotics is about 50% in 30min, and after visible light irradiation for 60min, the removal rate of cefotaxime sodium (CFX) reaches 83.5% and the removal rate of Amoxicillin (AMX) reaches 80%, indicating that the composite material has a good removal effect on antibiotics.
Application example 2
The performance of the sample was evaluated by the adsorption and visible light degradation performance of rhodamine B in water at room temperature. The different proportions (M-g-C) prepared in advance3N4：GO＝6:9、M-g-C3N：GO＝5:9、M-g- C3N4：GO＝4:9、M-g-C3N4：GO＝3:9、M-g-C3N4: GO 2:9), M-g-C3N4The rGOA and the rhodamine B solution (20mg/L, 100mL) are respectively added into a 250mL glass container, and the adsorption performance of the sample is directly expressed under the dark condition; the glass container is placed under 300W xenon lamp irradiation with the wavelength below 420nm filtered, and the adsorption and light degradation capability of the sample is expressed. Taking 3mL of solution every 20min, and measuring the concentration of the rhodamine B solution at 551nm by using an ultraviolet spectrophotometer. FIG. 5 shows M-g-C3N4The absorption result diagram of the/rGOA composite absorption visible light catalytic material on the dye; FIG. 6 shows M-g-C3N4A visible light catalysis result diagram of the/rGOA composite adsorption visible light catalysis material to the dye; referring to FIG. 5, when M-g-C3N4: M-g-C with GO being 3:93N4the/rGOA composite material has the dye adsorption removal rate of 79 percent in 80min under the dark condition; as can be seen in FIG. 6, after 80min under visible light irradiation, M-g-C3N4: the removal rate of the dye by the synergy of the absorption of M-g-C3N4/rGOA composite material with GO being 3:9 and visible light reaches 95%.
With M-g-C3N4: M-g-C with GO being 3:93N4And after the adsorption experiment carried out on the/rGOA composite material is finished, taking out the composite aerogel, desorbing the composite aerogel in absolute ethyl alcohol for 1.5h, soaking the composite aerogel in deionized water for 30min to remove the absolute ethyl alcohol, drying the composite aerogel for repeated use, circulating the photocatalysis experiment, and detecting the stability of the sample. FIG. 7 shows M-g-C3N4Referring to fig. 7, a result chart of a cycle experiment of catalyzing and degrading dye by using/rGOA composite adsorption visible light catalytic material shows that the composite material is treated and recycled after being used, and M-g-C3N4With rGOA at 3:9 to give M-g-C3N4the/rGOA composite adsorption visible photocatalytic material ring was used five times. The result shows that after the rhodamine B is recycled for five times, the rhodamine B removing effect still reaches 90%, so that the sample has good stability.
It will be appreciated by those skilled in the art that the foregoing types of applications are merely exemplary, and that other types of applications, whether presently existing or later to be developed, that may be suitable for use with the embodiments of the present invention, are also intended to be encompassed within the scope of the present invention and are hereby incorporated by reference.
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any changes or substitutions that can be easily conceived by those skilled in the art within the technical scope of the present invention are included in the scope of the present invention. Therefore, the protection scope of the present invention shall be subject to the protection scope of the claims.
Claims (1)
1. M-g-C3N4The application method of the/rGOA composite adsorption visible light catalytic material is characterized by comprising the following steps:
(1)M-g-C3N4the preparation of (1):
adding melamine into deionized water at the temperature of 80-90 ℃, after the temperature of the solution is cooled to room temperature, adding 37% hydrochloric acid under magnetic stirring, wherein the molar ratio of the melamine to the hydrochloric acid is 1:1, continuously stirring for 30min, and putting the mixture into a forced air drying oven at the temperature of 80 ℃ for evaporation drying to obtain melamine hydrochloride;
putting melamine hydrochloride into a crucible with a cover, heating to 500 ℃ at a heating rate of 20 ℃/min in an atmosphere type muffle furnace and keeping for 2h, and then heating to 520 ℃ at a heating rate of 4 ℃/min and keeping for 2 h; cooling and grinding to obtain light yellow M-g-C3N4；
(2)M-g-C3N4Preparation of rGOA:
60mg of the thus-obtained M-g-C3N4Adding into deionized water, and performing ultrasonic treatment for 150 min; graphene oxide GO is added to prepare 60mL of aqueous solution with GO concentration of 3.0mg/mL, M-g-C3N4The mass ratio of the graphene oxide to the graphene oxide is 3: 9; weighing 512mg NaHSO3Adding into the above water solution, performing ultrasonic treatment for 20min, and mixing; after the ultrasonic treatment is finished, the aqueous solution is moved into a blast drying oven, heated for 2.5 hours at the temperature of 95 ℃ to obtain hydrogel, and the hydrogel is soaked in deionized water for 6 hoursChanging water every 2h, and cleaning to obtain the hydrogel with impurity ions removed; finally, the hydrogel is freeze-dried by a freeze dryer to obtain M-g-C3N4the/rGOA compound absorbs visible light catalytic materials;
100mg of M-g-C were added separately3N4Dispersing the/rGOA composite material into 50mL, 2mg/L amoxicillin and 50mL, 2mg/L cefotaxime sodium antibiotic aqueous solution under magnetic stirring, placing the solution under dark condition for adsorbing for 30min after dispersion, placing the solution under 300W xenon lamp visible light irradiation with the wavelength below 420nm, taking 3mL solution every 10min, carrying out centrifugal filtration, and carrying out antibiotic concentration analysis;
the graphene oxide in the step (2) is prepared by a modified Hummers method.
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