CN109701664A - A kind of Ag/AgBr@ZIF-8 composite photo-catalyst and its preparation method and application - Google Patents
A kind of Ag/AgBr@ZIF-8 composite photo-catalyst and its preparation method and application Download PDFInfo
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Abstract
It is the composite photo-catalyst prepared for organic pollutants degradation and the requirement handled the present invention relates to a kind of Ag/AgBr@ZIF-8 composite photo-catalyst and its preparation method and application.Composite photo-catalyst of the invention is the Ag/AgBr@ZIF-8 composite photo-catalyst using zinc nitrate hexahydrate, 2-methylimidazole, silver nitrate and potassium bromide as raw material, through one-step method preparation.It is characterized using X-ray powder diffraction (XRD), solid ultraviolet specrophotometer (UV-vis) and specific surface area and lacunarity analysis (BET), and the catalytic performance of the composite photo-catalyst of preparation is investigated, bisphenol-A in the organic pollutants that can effectively degrade and Congo red.Method for preparing catalyst of the present invention is simple, reaction condition is mild, simple process, environmental-friendly.
Description
Technical field
The invention belongs to photocatalyst technology field, in particular to a kind of Ag/AgBr@ZIF-8 composite photo-catalyst and its
Preparation method and application.
Background technique
Since Fujishima in 1972 and Honda report photochemical catalyzing phenomenon since, photocatalysis technology gradually at
One of the emphasis studied for domestic and international researchers.Photocatalysis technology is to generate to have Strong oxdiative under light illumination using light-sensitive material
Property active group, can direct oxidation organic pollutant so that it is degraded to small molecule acid or water and CO2, so that reaching degradation has
The purpose of machine pollutant.Usually, catalysis material big, the light that solve band gap width of high activity and stability is designed and developed
The problems such as raw charge transfer rate and low utilization rate.
Argentiferous halide is a kind of important light-sensitive semiconductor material and is widely used in the fields such as photograph, but itself by
Photoetch is more serious.Generally by AgX(X=Cl, Br, I) particulate load to solid carrier, such as Bi2WO6、MCM-41、TiO2With
Al2O3Deng the rate of transform of Lai Tigao photo-generated carrier.In addition, the size of Ag/AgX mixture particle in the synthesis process
It will affect the power of catalyst activity.Zeolite imidazole ester frame structure material (ZIFs) is metal-organic framework material
(MOFs) can lead to the functional material of more outstanding porous and physicochemical stability as the carrier of AgX in race
The hole of via materials effectively limits the growth of AgX nanoparticle and the excessive aggregation in forming process.Nowadays have AgX
The report being carried in MOFs, such as by heterogeneous precipitation method by ZnCl2It is pre-mixed with ZIF-8, adds AgNO3Solution system
Ag/AgCl/ZIF-8 catalyst (J. Alloy. Compd., 693 (2017) 543-549； Appl. Catal. B, 202
(2017) 64-71), also there is the Ag/AgCl@MIL-53-Fe composite photo-catalyst prepared under DMF system by solvent thermal reaction
(Appl. Catal. B-Environ., 224(2018) and 38-45).Gao Shutao etc. is reported through NaCl and AgNO3Solution system
Standby Ag/AgCl/ZIF-8 catalyst, shown in degradation of dye rhodamine B higher catalytic activity (RSC Adv., 4
(2014) 61736-61742).In this context, the Ag/AgBr@ZIF-8 complex light that we are prepared for high activity and stability is urged
Agent, and be applied in the Study on degradation of organic pollutant.
Summary of the invention
The purpose of the present invention is being directed to the situation of background technique, provide a kind of Ag/AgBr@ZIF-8 composite photo-catalyst and
Preparation method and application.
The technical solution for realizing the aim of the invention is as follows: a kind of Ag/AgBr@ZIF-8 composite photo-catalyst is with zeolite miaow
Azoles ester framework material ZIF-8 is carrier, Ag and AgBr particle is the composite photo-catalyst that active component is constituted.
The specific surface area of Ag/AgBr@ZIF-8 composite photo-catalyst of the present invention is up to 1020 m2/g。
Ag/AgBr@ZIF-8 composite photo-catalyst of the present invention, the mass percentage of the Ag are 0.01~2.0
%。
As a general technical idea, the present invention also provides the systems of the Ag/AgBr@ZIF-8 composite photo-catalyst
Preparation Method, comprising the following steps:
It (1) by 2-methylimidazole and concentrated ammonia liquor is in molar ratio at room temperature that 1:10 ~ 30 are mixed evenly to obtain clear solution；
It (2) by zinc nitrate hexahydrate and concentrated ammonia liquor is in molar ratio at room temperature that the mixing of 1:20 ~ 60 obtains clear solution；
(3) a certain amount of AgNO3It is dissolved in step (2) acquired solution and is uniformly mixing to obtain clear solution；
(4) clear solution by step (3) preparation is added in step (1) acquired solution, stirs evenly, and is 20 ~ 80 in temperatureoC reacts 1 ~ 6 hour；
(5) solution prepared by the 0.4 mol/L KBr aqueous solution to step (4) of certain volume is added dropwise with 0.05 mL/min of speed
In, it is 20 ~ 80 in temperature after KBr solution is added dropwiseoC reacts 10 ~ 26 hours.First alcohol and water is used after reaction
Ag/AgBr@ZIF-8 composite photo-catalyst is prepared in each centrifuge washing 3 times, filtering, drying at room temperature.
A kind of preparation method of Ag/AgBr@ZIF-8 photochemical catalyst, it is characterised in that: the 2- methyl of step (1)
The molar ratio of imidazoles and the zinc nitrate hexahydrate of step (2) is 2:1.AgNO described in step (3)3Nitre is hydrated with step (2) six
The molar ratio of sour zinc is 1 ~ 30:100.KBr described in step (4) and AgNO described in step (3)3Molar ratio be 1 ~ 3:
1。
As same technical concept of the invention, the present invention also provides the Ag/AgBr@ZIF-8 composite photocatalysts
Agent is applied to Visible Light Induced Photocatalytic organic pollutant.
Application of the present invention, organic pollutant are divided into bisphenol-A and Congo red, and the concentration of the bisphenol-A is 0.04 ~
0.08 mmol L-1, Congo red concentration is 3 ~ 8 ppm.
Application of the present invention, when organic pollutant is bisphenol-A, it is characterised in that: the pH value of the bisphenol-A aqueous solution
It is 7~11, it is preferred that pH=11.
Compared with the existing technology, the present invention has the following advantages: (1) present invention with zinc nitrate hexahydrate, 2-methylimidazole,
AgNO3It is raw material with KBr, the Ag/AgBr@ZIF-8 composite photo-catalyst prepared by one-step method, preparation process is simple, and condition is easy
Control, raw material is simple and easy to get, at low cost, and the by-product for having pollution to environment will not be generated in preparation process.(2) this hair is used
Bright method disperses photochemical catalyst Ag and AgBr particle in the inside of zeolitic imidazolate framework material, effectively reduces photoproduction
The recombination rate of carrier.(3) composite photo-catalyst of the invention is in photocatalytic degradation bisphenol-A and Congo red experiment, bisphenol-A
Degradation rate up to 92 %, Congo red degradation rate illustrates that the higher visible light catalytic of the composite photo-catalyst is living up to 78 %
Property.
Detailed description of the invention
Fig. 1 is the XRD comparison diagram of Ag/AgBr@ZIF-8 composite photo-catalyst and synthesis ZIF-8 material of the invention；
Fig. 2 is the outer comparison diagram of solid violet of Ag/AgBr@ZIF-8 composite photo-catalyst and synthesis ZIF-8 material of the invention；
Fig. 3 is the BET comparison diagram of Ag/AgBr@ZIF-8 composite photo-catalyst and synthesis ZIF-8 material of the invention；
Fig. 4 is that the light degradation that Ag/AgBr@ZIF-8 composite photocatalyst for degrading bisphenol-A of the invention is influenced by bisphenol A concentration is dynamic
Mechanical equation map；
Fig. 5 is the light degradation property that Ag/AgBr@ZIF-8 composite photocatalyst for degrading bisphenol-A of the invention is influenced by solution ph
Map；
Fig. 6 is the Congo red light degradation influenced by Congo red concentration of Ag/AgBr@ZIF-8 composite photocatalyst for degrading of the invention
Performance atlas.
Specific embodiment
In order to make technological means of the invention be easier to understand, it is further described below combined with specific embodiments below, but
The implementation of the present invention is not limited to this.
Embodiment 1
(1) 20 mmol 2-methylimidazoles are dissolved in 15 mL concentrated ammonia liquors at room temperature and are mixed evenly to obtain clear solution；
(2) at room temperature by 10 mmol zinc nitrate hexahydrates be dissolved in 15 mL concentrated ammonia liquors in molar ratio in be mixed obtain clarifying it is molten
Liquid；
(3) by 1.0 mmol AgNO3It is dissolved in step (2) acquired solution and is uniformly mixing to obtain clear solution；
(4) clear solution by step (3) preparation is added in step (1) acquired solution, stirs evenly, 20oC, reaction 3 are small
When；
(5) it is added dropwise with 0.05 mL/min of speed in solution prepared by the 0.4 mol/L KBr aqueous solution to step (4) of 4 mL, drop
It is 20 in temperature after adding KBr aqueous solution oC, react 16 hours.It uses each centrifuge washing of first alcohol and water 3 times after reaction,
Ag/AgBr@ZIF-8 composite photo-catalyst is prepared in filtering, drying.
Embodiment 2
The present embodiment prepares Ag/AgBr@ZIF-8 photochemical catalyst by the identical mode of embodiment 1, and difference is only that in step (3)
AgNO3Molal quantity be changed to 0.5 mmol.The volume of KBr solution is changed to 2.1 mL in step (5).
Embodiment 3
The present embodiment prepares Ag/AgBr@ZIF-8 photochemical catalyst by the identical mode of embodiment 1, and difference is only that in step (3)
AgNO3Molal quantity be changed to 0.8 mmol.The volume of KBr solution is changed to 3.3 mL in step (5).
Embodiment 4
The present embodiment prepares Ag/AgBr@ZIF-8 photochemical catalyst by the identical mode of embodiment 1, and difference is only that in step (3)
AgNO3Molal quantity be changed to 1.2 mmol.The volume of KBr solution is changed to 4.2 mL in step (5).
Embodiment 5
The present embodiment prepares Ag/AgBr@ZIF-8 photochemical catalyst by the identical mode of embodiment 1, and difference is only that in step (3)
AgNO3Molal quantity be changed to 1.5 mmol.The volume of KBr solution is changed to 4.6 mL in step (5).
Embodiment 6
The present embodiment prepares Ag/AgBr@ZIF-8 photochemical catalyst by the identical mode of embodiment 1, and difference is only that in step (3)
AgNO3Molal quantity be changed to 1.2 mmol.The volume of KBr solution is changed to 4.2 mL in step (5).
The application of Ag/AgBr@ZIF-8 composite photo-catalyst prepared by the embodiment of the present invention 1 in degradation bisphenol-A, specifically
Application method are as follows:
Ag/AgBr@ZIF-8 composite photo-catalyst prepared by the embodiment 1 of 30 mg is weighed, being added to 100 mL concentration is 0.04
mmol L-1, pH=11(pass through 0.1 mol L-1NaOH adjust) bisphenol-A aqueous solution in, in the dark stir 1 ~ 10 hour.So
Afterwards under the irradiation using 250 W xenon lamps as analog light source, the H of 0.1 mL is pipetted using pipette2O2, illumination reaction 10 hours, point
Not in 0 minute, 2 hours, 4 hours, 6 hours, 8 hours, 10 hours 1.5 mL of sampling, and through 0.45 um filtering with microporous membrane, lead to
Cross bisphenol A concentration in high performance liquid chromatograph measurement sample.Resulting photocatalysis performance is as shown in Figure 4.
Embodiment 7
The present embodiment is degraded bisphenol-A by the identical mode of embodiment 2, and difference is only that the concentration of bisphenol-A aqueous solution is 0.06
mmol L-1.Resulting photocatalysis performance is as shown in Figure 4.
Embodiment 8
The present embodiment is degraded bisphenol-A by the identical mode of embodiment 2, and difference is only that the concentration of bisphenol-A aqueous solution is 0.08
mmol L-1.Resulting photocatalysis performance is as shown in Figure 4.
Embodiment 9
The present embodiment is degraded bisphenol-A by the identical mode of embodiment 2, and difference is only that pH=9 of bisphenol-A aqueous solution.Resulting light
Catalytic performance is as shown in Figure 5.
Embodiment 10
The present embodiment is degraded bisphenol-A by the identical mode of embodiment 2, and difference is only that the pH of bisphenol-A aqueous solution is not adjusted.Gained
Photocatalysis performance it is as shown in Figure 5.
Embodiment 11
The application of Ag/AgBr@ZIF-8 composite photo-catalyst prepared by the embodiment of the present invention 1 in degradation is Congo red, concrete application
Method are as follows:
Ag/AgBr@ZIF-8 composite photo-catalyst prepared by the embodiment 1 of 30 mg is weighed, being added to 100 mL concentration is 3
Ppm, pH=11(pass through 0.1 mol L-1NaOH adjust) Congo red aqueous solution in, in the dark stir 1 ~ 10 hour.Then exist
Using 250 W xenon lamps to pipette the H of 0.1 mL using pipette under the irradiation of analog light source2O2, illumination reaction 3 hours, respectively 0
Minute, 30 minutes, 1 hour, 2 hours, 3 hours 1.5 mL of sampling are measured Congo red dense in sample by ultraviolet specrophotometer
Degree.Resulting photocatalysis performance is as shown in Figure 6.
Embodiment 12
The present embodiment degrade by the identical mode of embodiment 7 it is Congo red, difference be Congo red aqueous solution concentration be 5 ppm,
And sample time is 0 minute, 30 minutes, 1 hour, 2 hours, 3 hours, 5 hours.Resulting photocatalysis performance is as shown in Figure 6.
Embodiment 13
The present embodiment degrade by the identical mode of embodiment 7 it is Congo red, difference be Congo red aqueous solution concentration be 8 ppm,
And sample time is 0 minute, 30 minutes, 2 hours, 6 hours, 8 hours.Resulting photocatalysis performance is as shown in Figure 6.
X-ray diffraction analysis is carried out to Ag/AgBr@ZIF-8 composite photo-catalyst prepared by embodiment 1, outside solid violet
The characterization such as spectrophotometer, specific surface area and lacunarity analysis.
Referring to Fig. 1: the XRD spectra of Ag/AgBr@ZIF-8 composite photo-catalyst prepared by the present invention and template ZIF-8 material
Unanimously, show that they have consistent crystal structure, and be the spy that AgBr is observed in 33.1 ° and 44.5 ° of positions in 2Theta
Peak is levied, illustrates that Ag/AgBr is successfully carried in zeolitic imidazolate framework material by infusion process of the invention.
Referring to fig. 2: the solid violet of Ag/AgBr@ZIF-8 composite photo-catalyst prepared by the present invention and synthesis ZIF-8 material
Outer comparison observes the characteristic peak of AgBr in 698 nm and in 710 positions nm, illustrates infusion process of the invention successfully by Ag/
AgBr is carried in zeolitic imidazolate framework material.
Referring to Fig. 3: BET pairs of Ag/AgBr@ZIF-8 composite photo-catalyst prepared by the present invention and synthesis ZIF-8 material
Than showing to be introduced into the duct of ZIF-8 with Ag/AgBr, specific surface area is reduced therewith, is 1020 m2/g。
Claims (7)
1. a kind of Ag/AgBr@ZIF-8 composite photo-catalyst, it is characterised in that: the Ag/AgBr@ZIF-8 composite photo-catalyst
Using ZIF-8 as carrier, Ag and AgBr particle is the composite photo-catalyst that active component is constituted.
2. Ag/AgBr@ZIF-8 composite photo-catalyst according to claim 1, it is characterised in that: the Ag/AgBr@
The specific surface area of ZIF-8 composite photo-catalyst is up to 1020 m2/g。
3. Ag/AgBr@ZIF-8 composite photo-catalyst according to claim 1, it is characterised in that: the quality hundred of the Ag
Dividing content is 0.01 ~ 2.0 %.
4. a kind of preparation method of Ag/AgBr@ZIF-8 composite photo-catalyst as described in claim 1, it is characterised in that: institute
State preparation process the following steps are included:
It (1) by 2-methylimidazole and concentrated ammonia liquor is in molar ratio at room temperature that 1:10 ~ 30 are mixed evenly to obtain clear solution；
It (2) by zinc nitrate hexahydrate and concentrated ammonia liquor is in molar ratio at room temperature that the mixing of 1:20 ~ 60 obtains clear solution；
(3) a certain amount of AgNO3It is dissolved in step (2) acquired solution and is uniformly mixing to obtain clear solution；
(4) clear solution by step (3) preparation is added in step (1) acquired solution, stirs evenly, and is 20 ~ 80 in temperatureoC reacts 1 ~ 6 hour；
(5) solution prepared by the 0.4 mol/L KBr aqueous solution to step (4) of certain volume is added dropwise with 0.05 mL/min of speed
In, it is 20 ~ 80 in temperature after KBr solution is added dropwiseoC reacts 10 ~ 26 hours；
It uses each centrifuge washing of first alcohol and water 3 times after reaction, filtering, drying are prepared Ag/AgBr ZIF-8 complex light and urge
Agent；
A kind of preparation method of Ag/AgBr@ZIF-8 photochemical catalyst, it is characterised in that: the 2-methylimidazole of step (1)
Molar ratio with the zinc nitrate hexahydrate of step (2) is 2:1；AgNO described in step (3)3With step (3) zinc nitrate hexahydrate
Molar ratio be 1 ~ 30:100；KBr described in step (4) and AgNO described in step (3)3Molar ratio be 1 ~ 3:1.
5. a kind of application of Ag/AgBr@ZIF-8 composite photo-catalyst as described in claim 1, it is characterised in that: the Ag/
AgBr@ZIF-8 composite photo-catalyst is applied to Visible Light Induced Photocatalytic organic pollutant.
6. application according to claim 5, it is characterised in that: the organic pollutant is respectively bisphenol-A and Congo red, double
The concentration of phenol A is 0.04 ~ 0.08 mmol L-1, Congo red concentration is 3 ~ 8 ppm.
7. application according to claim 5, it is characterised in that: the organic pollutant is bisphenol-A, and the pH value of aqueous solution is
7 ~ 11。
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Cited By (3)
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| CN110270376A (en) * | 2019-07-18 | 2019-09-24 | 深圳市深港产学研环保工程技术股份有限公司 | Photocatalysis sponge and its preparation method and application for removing algae and water |
| CN111266068A (en) * | 2020-03-04 | 2020-06-12 | 大连理工大学 | Micro-reactor of nano-structure micro-channel substrate grafted with supported catalyst and preparation method thereof |
| CN111450858A (en) * | 2020-04-11 | 2020-07-28 | 天津工业大学 | Composite photocatalyst Ag/AgCl @ Co3O4Preparation method of (1) and composite photocatalyst prepared by using same |
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| CN111266068B (en) * | 2020-03-04 | 2021-08-06 | 大连理工大学 | Micro-reactor of nano-structure micro-channel substrate grafted with supported catalyst and preparation method thereof |
| CN111450858A (en) * | 2020-04-11 | 2020-07-28 | 天津工业大学 | Composite photocatalyst Ag/AgCl @ Co3O4Preparation method of (1) and composite photocatalyst prepared by using same |
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