CN115779848A - Cobaltosic oxide-graphite phase carbon nitride adsorbent and preparation method and application thereof - Google Patents
Cobaltosic oxide-graphite phase carbon nitride adsorbent and preparation method and application thereof Download PDFInfo
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- 239000010439 graphite Substances 0.000 title claims abstract description 24
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- 238000001179 sorption measurement Methods 0.000 claims abstract description 33
- QGUAJWGNOXCYJF-UHFFFAOYSA-N cobalt dinitrate hexahydrate Chemical compound O.O.O.O.O.O.[Co+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O QGUAJWGNOXCYJF-UHFFFAOYSA-N 0.000 claims abstract description 28
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W10/00—Technologies for wastewater treatment
- Y02W10/30—Wastewater or sewage treatment systems using renewable energies
- Y02W10/37—Wastewater or sewage treatment systems using renewable energies using solar energy
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Abstract
The invention relates to a cobaltosic oxide-graphite phase carbon nitride adsorbent, a preparation method and application thereof, and belongs to the technical field of dye wastewater treatment. The expression of the adsorbent of the invention is: co 3 O 4 ‑g‑C 3 N 4 The material is prepared from dicyandiamide, ammonium chloride and cobalt nitrate hexahydrate. The preparation method of the adsorbent comprises the steps of uniformly grinding dicyandiamide, ammonium chloride and cobalt nitrate hexahydrate powder, annealing, cooling to room temperature, and grinding into powder to obtain the cobaltosic oxide-graphite phase carbon nitride adsorbent. The invention also provides application of the adsorbent in dye adsorption. The adsorbent of the invention has mesoporous junctions with various aperturesThe structure increases the specific surface area and provides enough active sites for the adsorption of the dye.
Description
Technical Field
The invention relates to the technical field of dye wastewater treatment, and particularly relates to a cobaltosic oxide-graphite phase carbon nitride adsorbent, and a preparation method and application thereof.
Background
With the continuous acceleration of the industrialization process, the discharge amount of industrial wastewater is increased day by day, and the types and components of the wastewater are more various and more complex than the former ones, which has serious influence on the water environment quality. Untreated industrial wastewater containing organic (dyes, aromatic phenols, pesticides, medicines, polycyclic aromatic hydrocarbons and personal care products) and inorganic (heavy metal ions) pollutants in textile, paper, pharmacy, batteries, rubber, printing, food processing, grease and the like is introduced into a water body, so that the water body is polluted, and the ecological stability of the water environment is damaged.
The dye wastewater has the characteristics of large water quantity, high chromaticity, large water quality change and the like, and is a problem to be solved in the field of industrial wastewater treatment. The dye is mainly used for coloring paper and fabrics, however, most dyes are not fixed on materials in the dyeing process but stay in solution, the dyes have high stability, are hardly biodegradable and can not be automatically degraded, if the dyes can not be treated in time, the dyes can exist in water for decades or even hundreds of years, and the consequences are very serious, so that the discharge of dye wastewater is emphasized, and a novel adsorbent is actively developed for treating the dye wastewater.
Disclosure of Invention
The invention aims to provide a cobaltosic oxide-graphite phase carbon nitride adsorbent, and a preparation method and application thereof.
In order to achieve the above purpose, the technical scheme of the invention is as follows:
the invention provides a cobaltosic oxide-graphite phase carbon nitride adsorbent, which has the expression as follows: co 3 O 4 -g-C 3 N 4 The adsorbent is prepared from dicyandiamide, ammonium chloride and cobalt nitrate hexahydrate.
Preferably, the mass ratio of dicyandiamide to ammonium chloride to cobalt nitrate hexahydrate is 4.
The adsorbent is preferably of a mesoporous structure, and the pore size of the adsorbent is mainly three pore sizes of 2.60nm, 3.60nm and 30.40 nm.
The adsorbent preferably has a total pore volume of 0.19cm 3 /g。
The above adsorbent preferably has a BET surface area of 47.82m 2 /g。
The invention also provides a preparation method of the cobaltosic oxide-graphite phase carbon nitride adsorbent, which comprises the following steps:
and uniformly grinding dicyandiamide, ammonium chloride and cobalt nitrate hexahydrate powder, annealing, cooling to room temperature, and grinding into powder to obtain the cobaltosic oxide-graphite phase carbon nitride adsorbent.
In the above production method, it is preferable that the mass ratio of the dicyandiamide, the ammonium chloride and the cobalt nitrate hexahydrate is 4.
In the above preparation method, preferably, the annealing treatment is specifically: raising the temperature to 550 ℃ at the heating rate of 5 ℃/min, and annealing for 3h at constant temperature.
The invention also provides application of the cobaltosic oxide-graphite phase carbon nitride adsorbent in dye adsorption.
In the above application, preferably, the dye is methyl orange.
The invention has the beneficial effects that:
the invention provides a cobaltosic oxide-graphite phase carbon nitride adsorbent, which comprises the following components in part by weight: (1) The N atom effectively changes the electronic property of the carbon material, is favorable for carrier migration and provides an active site. The N-rich carbon material has high adsorption performance, and the N atom with strong electronegativity can raise the pi acceptor capacity of carbon and improve the interaction with dye pi donor. (2) g-C 3 N 4 Has a defect-rich surface and contains a large amount of functional groups containing nitrogen atoms to promote nucleophilic interaction, thereby having good adsorption capacity. After the introduction of the metal oxide, the g-C is effectively expanded 3 N 4 The pi conjugated system is beneficial to adsorbing the dye with a benzene ring structure through pi-pi action; (3) Co 3 O 4 -g-C 3 N 4 The adsorbent has a mesoporous structure with various pore diameters, so that the specific surface area of the adsorbent is increased, and sufficient active sites are provided for adsorption of the dye. (4) The past literature reports that the preparation of graphite phase carbon nitride material by using single dicyandiamide is mainly used for photocatalysis technologyAfter the addition of ammonium chloride, the photocatalytic power becomes stronger. However, the invention obtains Co by introducing cobalt nitrate hexahydrate on the basis of the original method 3 O 4 -g-C 3 N 4 The performance exhibited is primarily adsorptive rather than photocatalytic applications.
The preparation method of the cobaltosic oxide-graphite phase carbon nitride adsorbent provided by the invention can be obtained by only mixing the raw materials of dicyandiamide, ammonium chloride and cobalt nitrate hexahydrate and then carrying out annealing treatment, and the preparation process is simple.
Drawings
The invention is described in further detail below with reference to the drawings and the detailed description.
FIG. 1 shows g-C 3 N 4 And Co prepared at different annealing temperatures 3 O 4 -g-C 3 N 4 The adsorption performance graph for methyl orange is shown in the specification, wherein (a) is g-C 3 N 4 And Co 3 O 4 -g-C 3 N 4 (550 ℃) adsorption performance diagram, and (b) Co prepared at 500 ℃, 550 ℃ and 600 DEG C 3 O 4 -g-C 3 N 4 (550 ℃) adsorption performance chart.
FIG. 2 shows the content of cobalt nitrate hexahydrate and the length of polymerization 3 O 4 -g-C 3 N 4 (550 ℃) graph of adsorption performance on methyl orange, wherein (a) is adsorbent Co with contents of 15%, 20% and 25% cobalt nitrate hexahydrate 3 O 4 -g-C 3 N 4 The adsorption performance chart of (b) is that of the adsorbent Co with the polymerization time of 2, 3 and 4h 3 O 4 -g-C 3 N 4 The adsorption performance of (1).
FIG. 3 shows Co prepared in example 1 3 O 4 -g-C 3 N 4 Maximum equilibrium adsorption rate for methyl orange.
FIG. 4 shows Co prepared in example 1 3 O 4 -g-C 3 N 4 SEM image of (d).
Fig. 5 is a nitrogen adsorption-desorption isotherm and pore size distribution diagram of the adsorbent prepared in example 1.
Detailed Description
The invention is described in detail below with reference to the figures and examples.
Example 1
Uniformly grinding dicyandiamide, ammonium chloride and cobalt nitrate hexahydrate powder in a mass ratio of 0.80 3 O 4 -g-C 3 N 4 。
Example 2
Uniformly grinding dicyandiamide, ammonium chloride and cobalt nitrate hexahydrate powder in a mass ratio of 0.80 3 O 4 -g-C 3 N 4 。
Example 3
Uniformly grinding dicyandiamide, ammonium chloride and cobalt nitrate hexahydrate powder in a mass ratio of 0.80 3 O 4 -g-C 3 N 4 。
Example 4
Uniformly grinding dicyandiamide, ammonium chloride and cobalt nitrate hexahydrate powder in a mass ratio of 0.85 to 0.80 3 O 4 -g-C 3 N 4 。
Example 5
Uniformly grinding dicyandiamide, ammonium chloride and cobalt nitrate hexahydrate powder in a mass ratio of 0.75 3 O 4 -g-C 3 N 4 。
Example 6
Uniformly grinding dicyandiamide, ammonium chloride and cobalt nitrate hexahydrate powder in a mass ratio of 0.80Heating for 2h, naturally cooling to room temperature in the furnace, and grinding into powder to obtain Co 3 O 4 -g-C 3 N 4 。
Example 7
Uniformly grinding dicyandiamide, ammonium chloride and cobalt nitrate hexahydrate powder in a mass ratio of 0.80 3 O 4 -g-C 3 N 4 。
Comparative example
Uniformly mixing dicyandiamide and ammonium chloride in a mass ratio of 0.80 to 0.80, annealing at a constant temperature of 550 ℃ for 3h at a heating rate of 5 ℃/min, naturally cooling to room temperature in a waiting furnace, and grinding into powder, namely g-C 3 N 4 。
Adsorption Performance test
30mg of g-C prepared in comparative example is respectively added into 20mg/L and 100mL of methyl orange solution 3 N 4 (550 ℃ C.) adsorbent Co prepared in example 1 3 O 4 -g-C 3 N 4 The (550 ℃) material adsorbs the carbon dioxide with adsorption rates of 28.75% and 94.27%, respectively (see FIG. 1 a). As can be seen from FIG. 1a, the Co prepared in example 1 after polymerization treatment 3 O 4 -g-C 3 N 4 The adsorption efficiency of the material is obviously superior to that of a pure graphite phase carbon nitride material, which fully illustrates the necessity of introducing a cobalt nitrate hexahydrate material for preparation.
30mg of the adsorbent Co prepared in example 2 and having different annealing temperatures are respectively added into 20mg/L and 100mL of methyl orange solution 3 O 4 -g-C 3 N 4 (500 ℃ C.) adsorbent Co prepared in example 1 3 O 4 -g-C 3 N 4 (550 ℃) and the Co adsorbent of example 3 3 O 4 -g-C 3 N 4 (600 ℃ C.). At 30min, the adsorption rates of 17.42%, 94.27% and 7.00% are respectively obtained (see fig. 1 b), and the optimum polymerization temperature of the material shows that the material calcined at 550 ℃ has the best adsorption performance.
The examples are respectively added into methyl orange solution with the concentration of 20mg/L and 100mL4 prepared adsorbent Co 3 O 4 -g-C 3 N 4 (15% content of cobalt nitrate hexahydrate), adsorbent Co prepared in example 1 3 O 4 -g-C 3 N 4 (cobalt nitrate hexahydrate of 20% content), adsorbent Co prepared in example 5 3 O 4 -g-C 3 N 4 The cobalt nitrate hexahydrate (550 ℃) was adsorbed, and the adsorption rates at 30min were 77.89%, 94.27% and 48.34%, respectively (see FIG. 2 a). The optimal precursor ratio is dicyandiamide: ammonium chloride: cobalt nitrate hexahydrate = 0.80.
The adsorbent Co prepared in example 6 is added into methyl orange solution of 20mg/L and 100mL respectively 3 O 4 -g-C 3 N 4 (2h) Adsorbent Co prepared in example 1 3 O 4 -g-C 3 N 4 (3h) Co adsorbent prepared in example 7 3 O 4 -g-C 3 N 4 (4h) And the adsorption rate was 66.03%, 94.27% and 57.34% at 30min (see fig. 2 b). The optimal polymerization time is 3h by optimizing the polymerization time.
Adsorbent Co prepared in example 1 3 O 4 -g-C 3 N 4 Adsorption experiment
30mg of the Co adsorbent prepared in example 1 was added to a 20 mg/L100 mL methyl orange aqueous solution 3 O 4 -g-C 3 N 4 The material is dispersed for adsorption. As is clear from the observation of the ultraviolet-visible absorption spectrum, the maximum absorption peak of the methyl orange solution was 461nm, and the absorbances at 0, 6, 12, 18, 24, and 30min at which the maximum absorption peak was read were 1.48, 0.31, 0.23, 0.18, 0.15, and 0.08, respectively, and the adsorption rates were 79.05%, 84.46%, 87.84%, 89.87%, and 94.27%, respectively. According to adsorption experiments, the methyl orange solution can be adsorbed by the adsorbent in a short time, and good adsorption performance is shown.
Adsorbent Co prepared in example 1 3 O 4 -g-C 3 N 4 Maximum equilibrium adsorption Rate experiment
Adding 50 mg/L100 mL methyl orange solution30mg of the Co adsorbent prepared in example 1 was added 3 O 4 -g-C 3 N 4 (550 ℃), sampling every 12min, ultraviolet testing for 5 times, and finally calculating that the adsorption efficiencies are 59.41%, 62.24%, 66.40%, 69.76% and 70.74%, and the equilibrium adsorption rates are 95.73, 105.83, 112.00, 115.67 and 118.83mg g -1 (see fig. 3).
Adsorbent Co prepared in example 1 3 O 4 -g-C 3 N 4 The SEM image obtained by shooting under the condition of 500nm is shown in figure 4, and as can be seen from figure 4, the cobalt nitrate hexahydrate is added into the raw materials of dicyandiamide and ammonium chloride, and the adsorbent Co obtained by thermal polymerization is obtained 3 O 4 -g-C 3 N 4 The material is formed by stacking particles with different sizes, the particle size distribution is uniform, the pore diameter of the pores is reduced, the pore size types and the number of the pores are increased, the result is consistent with the result obtained by BET, the specific surface area is greatly increased, the adsorption active sites are increased, and the adsorption capacity is enhanced.
BET characterization: adsorbent Co prepared in example 1 3 O 4 -g-C 3 N 4 The nitrogen adsorption-desorption isotherms and pore size distributions are shown in FIG. 5, and from the BET data, co is found 3 O 4 -g-C 3 N 4 The adsorbent is in a type IV adsorption-desorption isotherm and has an obvious hysteresis loop, which indicates that the adsorbent Co is 3 O 4 -g-C 3 N 4 Mesopores are present in the material. The BET surface area, the total pore volume and the average pore diameter were 47.82m 2 /g、0.19cm 3 The pore size distribution of the material shows that the adsorbent Co is at 16.24nm and/g 3 O 4 -g-C 3 N 4 The material has rich mesoporous structure, the pore sizes are mainly three pore sizes of 2.60, 3.60 and 30.40nm, the peak heights of the two pore sizes of 3.60 and 30.40nm are obviously larger than those of 2.60nm, which indicates that most pores have 3.60 or 30.40nm pore sizes, and the pores with 2.60nm pore sizes are fewer. The adsorption isotherm showed a clear upward trend, which is mainly the multilayer filling of the pores. Co 3 O 4 -g-C 3 N 4 The larger hysteresis loop indicates the larger type of aperture and the larger apertureThe distribution maps are consistent. Comparative bulk g-C 3 N 4 Has a specific surface area of 2.90m 2 G, modified Co 3 O 4 -g-C 3 N 4 The specific surface area of (a) is increased by 16.50 times. This indicates that the specific surface area of the material is significantly increased by introducing cobalt nitrate hexahydrate into the precursor, which means that the active sites are increased, thereby leading to the enhancement of the adsorption capacity.
It should be understood that the above examples are only for clarity of illustration and are not intended to limit the embodiments. Other variations and modifications will be apparent to persons skilled in the art in light of the above description. And are neither required nor exhaustive of all embodiments. And obvious variations or modifications derived therefrom are intended to be within the scope of the invention.
Claims (10)
1. The cobaltosic oxide-graphite phase carbon nitride adsorbent is characterized by comprising the following expression: co 3 O 4 -g-C 3 N 4 The adsorbent is prepared from dicyandiamide, ammonium chloride and cobalt nitrate hexahydrate.
2. The cobaltosic oxide-graphite phase carbon nitride adsorbent according to claim 1, wherein the mass ratio of dicyandiamide to ammonium chloride to cobalt nitrate hexahydrate is 4.
3. The cobaltosic oxide-graphite phase carbon nitride adsorbent according to claim 1, which is of a mesoporous structure having three pore sizes of 2.60nm, 3.60nm and 30.40 nm.
4. The cobaltosic oxide-graphite phase carbon nitride adsorbent of claim 1, wherein the total pore volume is 0.19cm 3 /g。
5. The cobaltosic oxide-graphite phase carbon nitride adsorbent of claim 1, wherein the BET surface area is 47.82m 2 /g。
6. A preparation method of a cobaltosic oxide-graphite phase carbon nitride adsorbent is characterized by comprising the following steps:
and uniformly grinding dicyandiamide, ammonium chloride and cobalt nitrate hexahydrate powder, annealing, cooling to room temperature, and grinding into powder to obtain the cobaltosic oxide-graphite phase carbon nitride adsorbent.
7. The method for preparing a cobaltosic oxide-graphite phase carbon nitride adsorbent according to claim 6, wherein the mass ratio of dicyandiamide to ammonium chloride to cobalt nitrate hexahydrate is 4.
8. The method for preparing a cobaltosic oxide-graphite phase carbon nitride adsorbent according to claim 7, wherein the annealing treatment specifically comprises: raising the temperature to 550 ℃ at the heating rate of 5 ℃/min, and annealing for 3h at constant temperature.
9. Use of the tricobalt tetraoxide-graphite phase carbon nitride adsorbent of any one of claims 1 to 5 for dye adsorption.
10. Use according to claim 9, wherein the dye is methyl orange.
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| 刘莛予;宫懿桐;赵锦;王敏;: "Co_3O_4/g-C_3N_4复合光催化剂降解罗丹明B的研究", 工业水处理, no. 02, pages 100 - 103 * |
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