CN112090448A - Preparation method of ZIF-8@ g-C3N4 catalyst with zeolite structure - Google Patents

Preparation method of ZIF-8@ g-C3N4 catalyst with zeolite structure Download PDF

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CN112090448A
CN112090448A CN201910527011.8A CN201910527011A CN112090448A CN 112090448 A CN112090448 A CN 112090448A CN 201910527011 A CN201910527011 A CN 201910527011A CN 112090448 A CN112090448 A CN 112090448A
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zif
catalyst
stirring
zinc nitrate
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高时庄
侯红娟
宋俊
徐�明
韦树捷
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Baoshan Iron and Steel Co Ltd
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    • B01J31/16—Catalysts comprising hydrides, coordination complexes or organic compounds containing coordination complexes
    • B01J31/18—Catalysts comprising hydrides, coordination complexes or organic compounds containing coordination complexes containing nitrogen, phosphorus, arsenic or antimony as complexing atoms, e.g. in pyridine ligands, or in resonance therewith, e.g. in isocyanide ligands C=N-R or as complexed central atoms
    • B01J31/1805—Catalysts comprising hydrides, coordination complexes or organic compounds containing coordination complexes containing nitrogen, phosphorus, arsenic or antimony as complexing atoms, e.g. in pyridine ligands, or in resonance therewith, e.g. in isocyanide ligands C=N-R or as complexed central atoms the ligands containing nitrogen
    • B01J31/181—Cyclic ligands, including e.g. non-condensed polycyclic ligands, comprising at least one complexing nitrogen atom as ring member, e.g. pyridine
    • B01J31/1815—Cyclic ligands, including e.g. non-condensed polycyclic ligands, comprising at least one complexing nitrogen atom as ring member, e.g. pyridine with more than one complexing nitrogen atom, e.g. bipyridyl, 2-aminopyridine
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    • B01J31/16—Catalysts comprising hydrides, coordination complexes or organic compounds containing coordination complexes
    • B01J31/1691—Coordination polymers, e.g. metal-organic frameworks [MOF]
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    • B01J35/00—Catalysts, in general, characterised by their form or physical properties
    • B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
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    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
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    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
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Abstract

The invention discloses a preparation method of a ZIF-8@ g-C3N4 catalyst with a zeolite structure, which comprises the following steps: grinding urea uniformly; transferring the mixture into an alumina crucible with a cover, roasting the mixture for 2 to 4 hours at the temperature of 475-; respectively weighing barbituric acid, zinc nitrate, dimethyl imidazole and g-C3N4, dispersing g-C3N4 in a methanol solution, carrying out ultrasonic treatment, adding the barbituric acid into the mixed solution, and uniformly stirring; dissolving zinc nitrate in the mixed solution, and continuously stirring uniformly; simultaneously dissolving dimethyl imidazole in a methanol solution, and uniformly stirring; dropwise adding the dimethyl imidazole solution into the mixed solution of g-C3N4, barbituric acid and zinc nitrate under the condition of stirring, then stirring at room temperature, and standing; centrifuging, repeatedly washing with methanol and absolute ethyl alcohol, drying in vacuum, and grinding to obtain the ZIF-8@ g-C3N4 composite catalyst material. The composite photocatalyst can be separated, recovered and recycled, and the preparation method is simple, strong in controllability and easy to realize large-scale production.

Description

Preparation method of ZIF-8@ g-C3N4 catalyst with zeolite structure
Technical Field
The invention relates to the field of inorganic functional materials, relates to a catalyst for degrading organic matters in wastewater, and particularly relates to a preparation method of a zeolite structure catalyst ZIF-8@ g-C3N 4.
Background
With the increasing severity of water eutrophication problems and the increasingly strict discharge standards of ammonia nitrogen and organic matters, the technology for advanced wastewater treatment has become a subject of wide attention by domestic and foreign scholars. Wherein cold rolling mill units in the steel industry all relate to the pickling of strip steel, and acid regeneration units are designed and arranged for realizing the recycling of waste acid. Most hydrochloric acid regeneration units are provided with a silicon removal process, the problems of excessive NH3-N (NH3-N is mainly from ammonia water in the silicon removal process) and excessive organic matters (the organic matters are mainly from a flocculating agent in the silicon removal process) in the wastewater are caused when a silicon removal device runs, and the application of mature ammonia nitrogen removal and organic matter rapid degradation technology in acid-containing wastewater is not seen so far. The photocatalyst researched by the technology can effectively degrade organic matters in the wastewater, and the organic matters in the wastewater can be discharged up to the standard.
Among the technical means, photocatalysis is considered as the most promising method for solving the energy and environmental problems due to the characteristics of low energy consumption, environmental friendliness and high efficiency. Metal-organic frameworks (MOFs) are a new porous material, and have the advantages of high specific surface area, high porosity, chemical modification and the like, but the MOFs have the disadvantages of poor thermal stability and poor solvent stability, which limits the wide application thereof. Zeolite imidazole framework materials (ZIFs for short) are novel nanoporous MOFs materials with zeolite topological structures and taking imidazole or a diffractometer thereof as a ligand, have the advantages of zeolite and MOFs, and have excellent thermal stability, structural stability and adjustability of structures and functions. Therefore, the ZIF material has good application prospects in the aspects of adsorption, separation and catalysis. Among them, ZIF-8 is the most representative of ZIF materials, has large specific surface area (1400m2/g), high pore volume, good hydrothermal stability and organic solvent resistance, can be applied to a plurality of fields such as gas adsorption, separation, hydrogen storage, catalysis and the like, and is the most widely researched ZIF series materials at present.
The g-C3N4, namely the C3N4 of the graphite phase, is the most stable one of five kinds of C3N4, has a layered structure similar to graphite, is a common non-metal semiconductor material, has the advantages of no toxicity, small band gap (2.7e V) and better visible light absorption in solar spectrum, and is a novel visible light catalyst which is rapidly developed in recent years, however, the pure g-C3N4 also has the defects of limited visible light capturing capability, easy recombination of charge carriers and small specific surface area, the photocatalytic efficiency is not ideal enough, and a distance is provided from the practical industrial large-scale application.
Problems existing in the prior art:
1) organic matters in the wastewater of the acid regeneration unit mainly come from a flocculating agent in a silicon removal process, and the prior technology for removing the organic matters in the wastewater mainly adopts a chemical agent degradation method, so that secondary pollution is easily caused by the technology, and the application of the technology in the field is restricted;
2) photocatalysis is considered to be the most promising method for solving energy and environmental problems due to the characteristics of low energy consumption, environmental friendliness and high efficiency. The existing novel efficient photocatalyst g-C3N4 has the advantages of a layered structure similar to graphite and good absorption of visible light in solar spectrum, but has poor catalytic effect and low sunlight utilization rate.
201310119531.8, a porous g-C3N4 photocatalyst and a preparation method thereof, the catalytic efficiency of the obtained catalyst under visible light can reach more than 65%, and the catalyst shows better photocatalytic performance. But the catalytic efficiency of the photocatalyst is far from the production and living requirements, and further modification is needed to improve the visible light catalytic efficiency of the photocatalyst. 201510132172.9, a method for preparing CuS/g-C3N4 nanometer ball flower compound catalyst, the compound catalyst prepared by the method has extremely excellent visible light catalytic efficiency, but the compound catalyst prepared by the solvothermal method adopts acetylacetone as solvent, has toxicity, increases production cost by the solvothermal method, has small production capacity and is not easy to realize industrial production.
Disclosure of Invention
Therefore, the technical problem to be solved by the invention is to provide a preparation method of a zeolite ZIF-8@ g-C3N4 catalyst, and the preparation method of the composite visible-light-driven photocatalyst can solve the technical problems of poor catalytic effect and low sunlight utilization rate of the visible-light-driven photocatalyst prepared in the prior art.
The technical scheme of the invention is that the preparation method of the ZIF-8@ g-C3N4 catalyst with the zeolite structure comprises the following steps
1) Grinding urea uniformly;
2) transferring the uniformly ground urea powder into a crucible with a cover, roasting for 2-4h at 475-;
3) according to the mass ratio of 0.1-0.3:0.8-1.2: 1.5-2.5: 1-5 respectively weighing barbituric acid, zinc nitrate, dimethyl imidazole and g-C3N4, dispersing g-C3N4 in a methanol solution, carrying out ultrasonic treatment, adding the barbituric acid into the mixed solution, and uniformly stirring;
4) dissolving zinc nitrate in the mixed solution, and continuously stirring uniformly; simultaneously dissolving dimethyl imidazole in a methanol solution, and uniformly stirring;
5) dropwise adding the dimethyl imidazole solution into the mixed solution of g-C3N4, barbituric acid and zinc nitrate under the condition of stirring, then stirring at room temperature, and standing;
6) centrifuging, repeatedly washing with methanol and absolute ethyl alcohol, drying in vacuum, and grinding to obtain the ZIF-8@ g-C3N4 composite catalyst material.
g-C3N4, C3N4 for the graphitic phase.
The ZIF-8@ g-C3N4 catalyst belongs to a composite visible light catalyst with layered g-C3N4 loaded with ZIF-8 nano particles, and ZIF-8 grows on g-C3N4 modified by barbituric acid.
Preferably, in step 2), the temperature rise rate is 2-4 ℃/min.
According to the preparation method of the ZIF-8@ g-C3N4 catalyst with the zeolite structure, the roasting in the step 2) is preferably carried out in a muffle furnace. The crucible in the step 2) is an alumina crucible. The layer g-C3N4 is a yellow powder.
According to the preparation method of the ZIF-8@ g-C3N4 catalyst of zeolite structure of the present invention, it is preferable that the mass ratio of barbituric acid, zinc nitrate, dimethyl imidazole, and g-C3N4 in step 3) is 0.1-0.3:0.8-1: 1.8-2.1: 1-5.
More preferably, the ratio of 0.2:1:2: 1-5.
According to the preparation method of the ZIF-8@ g-C3N4 catalyst having a zeolite structure of the present invention, it is preferable that the ratio of the g-C3N4 to the methanol solution in the step 3) is 80 to 150g/150mL of methanol.
According to the preparation method of the ZIF-8@ g-C3N4 catalyst with the zeolite structure, the ratio of the dimethyl imidazole to the methanol solution in the step 4) is preferably 100-150g/150mL methanol.
According to the preparation method of the ZIF-8@ g-C3N4 catalyst with the zeolite structure, the ultrasonic treatment time in the step 3) is preferably 0.5-1 h; and 3) stirring for 0.5-2 h.
According to the preparation method of the ZIF-8@ g-C3N4 catalyst with the zeolite structure, the stirring time of the zinc nitrate in the step 4) is preferably 0.5-3 h; the stirring time of the dimethyl imidazole is 0.5-3 h.
Further, the stirring time of the zinc nitrate in the step 4) is 1-2 h; the stirring time of the dimethyl imidazole is 1-2 h.
According to the preparation method of the ZIF-8@ g-C3N4 catalyst with the zeolite structure, the step 5) is preferably stirred for 0.5 to 3 hours at room temperature and is kept still for 1 to 10 hours.
Further, stirring at room temperature for 1-2h in the step 5), and standing for 3-8 h.
Preferably, the centrifugal rotation speed of the step 6) is 800-1000 rpm; centrifuging for 5-10 min; the repeated washing times of methanol and absolute ethyl alcohol are 3-6 times.
Also provides application of the ZIF-8@ g-C3N4 catalyst prepared by the preparation method of the ZIF-8@ g-C3N4 catalyst with the zeolite structure as a visible light catalyst in degradation of organic matters in wastewater.
The preparation method comprises the steps of preparing layered g-C3N4 through a simple roasting method, and growing ZIF-8 on the g-C3N4 modified by barbituric acid through a self-assembly method to finally obtain the composite visible light catalyst with the layered g-C3N4 loaded with ZIF-8 nano particles. The composite catalyst has the characteristics of g-C3N4 visible light response and high photon-generated carrier mobility on one hand, and has the characteristics of stable ZIF-8 structure, high porosity, large specific surface area and simple preparation on the other hand. Meanwhile, under the condition of illumination, electrons generated on the g-C3N4 conduction band can migrate to the ZIF-8 conduction band, so that the recombination of photogenerated electrons and holes of the g-C3N4 is reduced. In addition, the characteristics of high porosity and high specific surface area of the ZIF-8 are utilized, so that the catalyst has more reaction active sites, and the photocatalytic performance of the composite material is greatly improved. In addition, the barbituric acid bridging is adopted, so that the transfer of a photon-generated carrier between g-C3N4 and ZIF-8 is quicker, and the photocatalytic efficiency of the composite material is further improved.
Advantageous effects
Compared with the prior art, the invention has remarkable technical progress. The ZIF-8@ g-C3N4 composite photocatalyst has a wider spectral response range, higher carrier separation efficiency and photocatalytic activity, can be separated, recovered and recycled, and is simple in preparation method, strong in controllability, easy to realize large-scale production and free of special equipment and harsh conditions.
Drawings
FIG. 1 is a PL diagram of the composite visible light catalyst ZIF-8@ g-C3N4 prepared in example 2.
FIG. 2 is an XRD pattern of the composite visible light catalyst ZIF-8@ g-C3N4 prepared in example 2.
Detailed Description
The invention will be explained in more detail below with reference to examples of embodiment and the figures, without however being limited to the examples given:
in the invention, 10mg/L methylene blue is used as a target degradation product, a 500W xenon lamp with an additional optical filter (lambda is more than 420nm) is used as a light source, and the catalytic performance of the photocatalyst is examined. Before illumination, stirring in dark for 60min to make the system reach absorption-desorption equilibrium. In the photocatalysis experiment, circulating water is used for ensuring that the temperature of the degradation system is consistent with the room temperature under the condition of illumination while stirring. 3mL of the reaction solution was taken every 15 minutes, centrifuged at 9000rpm for 5 minutes by a centrifuge, and the supernatant was filtered through a 0.22 μm filter, and the change in the concentration of methylene blue in the solution was determined from the change in absorbance at 544nm of the solution by detection using an Shimadzu UV-3600 UV spectrophotometer.
Example 1
1) 50g of urea were weighed and ground uniformly.
2) And (3) transferring the (1) into an alumina crucible with a cover, roasting in a muffle furnace for 4h at 475 ℃ under an air atmosphere, wherein the heating rate is 4 ℃/min, and then cooling to room temperature to obtain yellow powder, namely layered g-C3N 4.
3) Respectively weighing barbituric acid, zinc nitrate, dimethyl imidazole and g-C3N4 according to the mass ratio of 0.2:1:2:1, dispersing g-C3N4 in 40ml of methanol solution, carrying out ultrasonic treatment for 0.5h, then adding the barbituric acid into the mixed solution, and stirring for 0.5 h.
4) Dissolving zinc nitrate in (3) and stirring for 1 h. Meanwhile, dimethylimidazole is dissolved in 40ml of methanol solution and stirred for 1 h.
5) The dimethyl imidazole solution is added dropwise into the mixed solution of g-C3N4, barbituric acid and zinc nitrate under the stirring condition, and then stirred for 1 hour at room temperature and kept stand for 3 hours.
6) Centrifuging, repeatedly washing with methanol and absolute ethanol for 3 times, vacuum drying, and grinding to obtain the ZIF-8@ g-C3N4 composite catalyst material.
The composite visible-light-driven photocatalyst ZIF-8@ g-C3N4 prepared in the embodiment is added into methylene blue of 10mg/L in a proportion of 0.05g/100mL, and under the irradiation of simulated sunlight, a methylene blue solution can be degraded by 94% within 2 h.
Example 2
1) 50g of urea were weighed and ground uniformly.
2) Transferring the (1) into an alumina crucible with a cover, roasting in a muffle furnace for 3h at 500 ℃ under an air atmosphere, wherein the heating rate is 3 ℃/min, and then cooling to room temperature to obtain yellow powder, namely layered g-C3N 4.
3) Respectively weighing barbituric acid, zinc nitrate, dimethyl imidazole and g-C3N4 according to the mass ratio of 0.2:1:2:2.5, dispersing g-C3N4 in 40ml of methanol solution, carrying out ultrasonic treatment for 0.75h, then adding the barbituric acid into the mixed solution, and stirring for 1 h.
4) Dissolving zinc nitrate in (3) and stirring for 1 h. Meanwhile, dimethylimidazole is dissolved in 40ml of methanol solution and stirred for 1 h.
5) The dimethyl imidazole solution is dropwise added into the mixed solution of g-C3N4, barbituric acid and zinc nitrate under the stirring condition, and then stirred for 1 hour at room temperature and kept stand for 5 hours.
6) Centrifuging, repeatedly washing with methanol and absolute ethyl alcohol for 4 times, vacuum drying, and grinding to obtain the ZIF-8@ g-C3N4 composite catalyst material.
The composite visible-light-driven photocatalyst ZIF-8@ g-C3N4 prepared in the embodiment is added into 10mg/L methylene blue according to the proportion of 0.05g/100mL, and under the irradiation of simulated sunlight, the methylene blue solution can be degraded by 95% within 2 h.
Example 3
1) 50g of urea were weighed and ground uniformly.
2) Transferring the (1) into an alumina crucible with a cover, roasting for 4h in a muffle furnace at 550 ℃ under an air atmosphere, wherein the heating rate is 4 ℃/min, and then cooling to room temperature to obtain yellow powder, namely layered g-C3N 4.
3) Respectively weighing barbituric acid, zinc nitrate, dimethyl imidazole and g-C3N4 according to the mass ratio of 0.2:1:2:5, dispersing g-C3N4 in 40ml of methanol solution, carrying out ultrasonic treatment for 1h, then adding the barbituric acid into the mixed solution, and stirring for 2 h.
4) The zinc nitrate is dissolved in (3) and stirring is continued for 2 h. Meanwhile, dimethylimidazole is dissolved in 40ml of methanol solution and stirred for 2 hours.
5) The dimethyl imidazole solution is dropwise added into the mixed solution of g-C3N4, barbituric acid and zinc nitrate under the stirring condition, and then stirred for 2 hours at room temperature and kept stand for 8 hours.
6) Centrifuging, repeatedly washing with methanol and absolute ethyl alcohol for 5 times, vacuum drying, and grinding to obtain the ZIF-8@ g-C3N4 composite catalyst material.
The composite visible-light-driven photocatalyst ZIF-8@ g-C3N4 prepared in the embodiment is added into methylene blue of 10mg/L in a proportion of 0.05g/100mL, and under the irradiation of simulated sunlight, a methylene blue solution can be degraded by 93% within 2 h.

Claims (10)

1. A preparation method of a ZIF-8@ g-C3N4 catalyst with a zeolite structure is characterized by comprising the following steps: comprises the following steps
1) Grinding urea uniformly;
2) transferring the uniformly ground urea powder into a crucible with a cover, roasting for 2-4h at 475-;
3) according to the mass ratio of 0.1-0.3:0.8-1.2: 1.5-2.5: 1-5 respectively weighing barbituric acid, zinc nitrate, dimethyl imidazole and g-C3N4, dispersing g-C3N4 in a methanol solution, carrying out ultrasonic treatment, adding the barbituric acid into the mixed solution, and uniformly stirring;
4) dissolving zinc nitrate in the mixed solution, and continuously stirring uniformly; simultaneously dissolving dimethyl imidazole in a methanol solution, and uniformly stirring;
5) dropwise adding the dimethyl imidazole solution into the mixed solution of g-C3N4, barbituric acid and zinc nitrate under the condition of stirring, then stirring at room temperature, and standing;
6) centrifuging, repeatedly washing with methanol and absolute ethyl alcohol, drying in vacuum, and grinding to obtain the ZIF-8@ g-C3N4 composite catalyst material.
2. A process for preparing a ZIF-8@ g-C3N4 catalyst of zeolitic structure according to claim 1, characterized in that: and 2) roasting in a muffle furnace.
3. A process for preparing a ZIF-8@ g-C3N4 catalyst of zeolitic structure according to claim 1, characterized in that: the mass ratio of barbituric acid, zinc nitrate, dimethyl imidazole and g-C3N4 in the step 3) is 0.1-0.3:0.8-1: 1.8-2.1: 1-5.
4. A process for preparing a ZIF-8@ g-C3N4 catalyst of zeolitic structure according to claim 1, characterized in that: the ratio of the g-C3N4 to the methanol solution in step 3) is 80-150g/150mL of methanol.
5. A process for preparing a ZIF-8@ g-C3N4 catalyst of zeolitic structure according to claim 1, characterized in that: in the step 4), the ratio of the dimethyl imidazole to the methanol solution is 100-150g/150mL of methanol.
6. A process for preparing a ZIF-8@ g-C3N4 catalyst of zeolitic structure according to claim 1, characterized in that: step 3), the ultrasonic treatment time is 0.5-1 h; and 3) stirring for 0.5-2 h.
7. A process for preparing a ZIF-8@ g-C3N4 catalyst of zeolitic structure according to claim 1, characterized in that: stirring the zinc nitrate for 0.5 to 3 hours in the step 4); the stirring time of the dimethyl imidazole is 0.5-3 h.
8. A process for preparing a ZIF-8@ g-C3N4 catalyst of zeolitic structure according to claim 7, characterized in that: stirring the zinc nitrate for 1-2 hours in the step 4); the stirring time of the dimethyl imidazole is 1-2 h.
9. A process for preparing a ZIF-8@ g-C3N4 catalyst of zeolitic structure according to claim 1, characterized in that: stirring at room temperature for 0.5-3h, and standing for 1-10 h.
Further, stirring at room temperature for 1-2h in the step 5), and standing for 3-8 h.
10. The use of the ZIF-8@ g-C3N4 catalyst prepared by the process for preparing a ZIF-8@ g-C3N4 catalyst having a zeolite structure of claim 1 as a visible light catalyst in the degradation of organics in wastewater.
CN201910527011.8A 2019-06-18 2019-06-18 Preparation method of ZIF-8@ g-C3N4 catalyst with zeolite structure Pending CN112090448A (en)

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CN113354830A (en) * 2021-06-23 2021-09-07 贵州医科大学 Synthesis method and application of uniform-size ZIF-8 metal organic framework material
CN114797985A (en) * 2022-03-25 2022-07-29 哈尔滨工程大学 Flexible and recyclable C 3 N 4 ZIF-8 composite nanofiber photocatalytic film and preparation method thereof
CN115414967A (en) * 2022-08-29 2022-12-02 山东万博环境治理有限公司 Ag @ ZIF-8@ g-C 3 N 4 Composite photocatalyst and preparation method and application thereof
CN116020559A (en) * 2023-01-05 2023-04-28 南昌大学 Reusable Fenton-like catalyst ZIF-67@g-C 3 N 4 Is prepared by the method of (a) and (b)

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CN113354830A (en) * 2021-06-23 2021-09-07 贵州医科大学 Synthesis method and application of uniform-size ZIF-8 metal organic framework material
CN113354830B (en) * 2021-06-23 2022-10-21 贵州医科大学附属医院 Synthesis method and application of uniform-size ZIF-8 metal organic framework material
CN114797985A (en) * 2022-03-25 2022-07-29 哈尔滨工程大学 Flexible and recyclable C 3 N 4 ZIF-8 composite nanofiber photocatalytic film and preparation method thereof
CN115414967A (en) * 2022-08-29 2022-12-02 山东万博环境治理有限公司 Ag @ ZIF-8@ g-C 3 N 4 Composite photocatalyst and preparation method and application thereof
CN116020559A (en) * 2023-01-05 2023-04-28 南昌大学 Reusable Fenton-like catalyst ZIF-67@g-C 3 N 4 Is prepared by the method of (a) and (b)

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