CN104888858A - Ternary efficient compound visible light photocatalytic material and preparation method thereof - Google Patents
Ternary efficient compound visible light photocatalytic material and preparation method thereof Download PDFInfo
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- CN104888858A CN104888858A CN201510266687.8A CN201510266687A CN104888858A CN 104888858 A CN104888858 A CN 104888858A CN 201510266687 A CN201510266687 A CN 201510266687A CN 104888858 A CN104888858 A CN 104888858A
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Abstract
The invention discloses a ternary efficient compound visible light photocatalytic material and a preparation method and application thereof. The preparation method is characterized by comprising the following steps: preparing N-K2Ti4O9 and g-C3N4 by a forging method, preparing an N-K2Ti4O9/g-C3N4 binary composite material via electrostatic attraction, and further synthesizing an N-K2Ti4O9/g-C3N4/UiO-66 ternary efficient compound visible light photocatalytic catalyst via self-assembling by a solvothermal method. According to the invention, the characteristics of good visible light response of N-K2Ti4O9, high conduction electron hole capacity of g-C3N4 and high MOF material adsorption amount of UiO-66 are utilized; the ternary compound light catalyst synthesized by integrating the advantages of N-K2Ti4O9, g-C3N4 and UiO-66 has obviously reinforced activity of performing photocatalytic degradation on organic dye under visible light under the effect of compound promoted photogenerated charge separation, and has wide application prospect in the field of photocatalysis.
Description
Technical field
The invention belongs to material preparation, visible light photocatalysis technology, field of environment protection, be specifically related to ternary high-efficiency composite photocatalyst N-K
2ti
4o
9/ g-C
3n
4the application of the preparation of/UiO-66 and under visible light catalytic degradation organic pollutants.
Background technology
Current energy shortage, problem of environmental pollution more and more cause the concern of people, the challenge that the Faced In Sustainable Development of human society is huge.Photocatalysis technology is a kind of novel process technology of degraded environmental contaminants, there is the advantages such as low-carbon (LC), cleaning, environmental protection, therefore be a kind of desirable route solving the energy, environmental problem, but the photochemical catalysts such as traditional titanium dioxide are due to shortcomings such as band gap are high, photo-generate electron-hole recombination rate is fast, limit the practical application of photocatalysis technology, how preparing efficient photochemical catalyst is then the key issue that photocatalysis technology application needs solve.
Potassium titanate (K
2ti
4o
9) be generally considered a kind of material reliably, the performances such as, stable in properties, material nontoxic because of it are easy to get, photoelectric property is unique.But due to its band-gap energy higher (3.2-3.4eV), by ultraviolet excitation, can only therefore improve its photocatalytic activity significant with the range of application widening associated materials.By nitrogen-doping to K
2ti
4o
9in (be labeled as " N-K
2ti
4o
9") be a kind of common method reducing band gap, after doping, photocatalytic activity is improved, but N-K
2ti
4o
9little etc. low bandgap semiconductor ubiquity specific area, the defects such as photo-generate electron-hole recombination rate is fast are existed to hydrophobic organic compound absorption difference and homogenous material, and limit the further raising of its photocatalysis performance.G-C
3n
4it is the polymer be made up of triazine unit, it is non-metal semiconductive, its heat endurance and chemical stability stronger, there is delocalization conjugatedπbond (effectively can conduct photo-generated carrier), the degraded etc. of photocatalytic water and organic pollution is mainly used in visible light catalytic reaction, but g-C
3n
4the shortcomings such as it is little that photochemical catalyst also exists specific area, and photo-generated carrier compound is serious.Research finds, to g-C
3n
4carry out acid treatment and can improve its specific area, promote separation of charge.And g-C
3n
4make its positively charged through its nitrogen-atoms of peracid treatment is protonated, easily and other electronegative materials be effectively combined with each other by electrostatic attraction.Metal organic frame (metal-organic framework, being called for short MOF) material is the novel porous materials just causing extensive concern in recent ten years, be the coordination polymer by the multiple tooth organic ligand such as oxygen, nitrogen and transition metal ions self assembly, (specific area of most MOF is at 1000m to have king-sized specific area
2/ more than g, is greater than conventional porous material).Its uncovered through duct is conducive to the contaminant molecule in Adsorption Concentration environment to the surface of material and inside.Wherein UiO-66 is Zr
iVwith a kind of MOF material that terephthalic acid (TPA) complexation reaction is formed, there is specific area and adsorbance large, the advantages such as physics and chemistry stable in properties.In view of the absorption property of UiO-66 excellence, loaded to other materials surface and formed composite construction, the adsorption photochemical catalysis performance of material can be improved.
The present invention is in conjunction with N-K
2ti
4o
9visible light-responded good, g-C
3n
4the advantage that conduction electron hole ability is strong, MOF adsorption capacities of materials is large, the N-K prepared
2ti
4o
9/ g-C
3n
4/ UiO-66 trielement composite material has higher absorption property, can effectively be separated photoproduction electron-hole pair, has the visible light photocatalysis active significantly strengthened.
Summary of the invention
The object of this invention is to provide a kind of N-K
2ti
4o
9/ g-C
3n
4/ UiO-66 ternary high efficiency composition visible-light photocatalyst and preparation method thereof, to overcome the defect of single catalysis material existence and to promote photogenerated charge centrifugation by compound, its preparation method is simple, and the photocatalysis effect of rhodamine B degradation is remarkable.
For achieving the above object, the present invention adopts following technical scheme:
Ternary high efficiency composition visible-light photocatalyst of the present invention, its feature is: described ternary high efficiency composition visible-light photocatalyst is by N-K
2ti
4o
9, g-C
3n
4form with UiO-66 compound, be designated as N-K
2ti
4o
9/ g-C
3n
4/ UiO-66.
The preparation method of ternary high efficiency composition visible-light photocatalyst of the present invention, its feature is:
(1) by K
2cO
3with TiO
21:9 ~ 4:9 mixes and grinds evenly in molar ratio, then at 400 ~ 1000 DEG C of calcining 4 ~ 10h, finally naturally cools to room temperature, obtains K
2ti
4o
9;
By K
2ti
4o
9after urea in mass ratio 1:5 ~ 3:5 mixing, at 300 ~ 500 DEG C of calcining 3 ~ 6h, then naturally cool to room temperature, obtain N-K
2ti
4o
9;
By N-K
2ti
4o
9joining concentration is in the sodium oxalate water solution of 0.10 ~ 0.30mol/L, stirs, ultrasonic, then filters, washs, dry, grinding, obtains pretreatment N-K
2ti
4o
9;
(2) melamine is calcined 3 ~ 8h at 400 ~ 600 DEG C, be then cooled to room temperature, grinding, obtain g-C
3n
4;
By described g-C
3n
4joining concentration is in the salpeter solution of 0.5 ~ 2.0mol/L, and is incubated 6h at 135 DEG C, by the washing of gained sample to neutral, dry, obtains pretreatment g-C
3n
4;
(3) by pretreatment N-K that step (1) obtains
2ti
4o
9with the pretreatment g-C that step (2) obtains
3n
4be mixed in ethanol for 1:2 ~ 7:2 in mass ratio, then stir 20 ~ 40h, filter, washing, dry, obtain N-K
2ti
4o
9/ g-C
3n
4binary composite;
(4) by N-K that step (3) obtains
2ti
4o
9/ g-C
3n
4binary composite and ZrCl
41:2 ~ 7:2 joins in DMF in mass ratio, then adds terephthalic acid (TPA) and benzoic acid (terephthalic acid (TPA), ZrCl
4be 0.64:1:10 with benzoic mass ratio), transfer them at 100 ~ 150 DEG C of reaction 18 ~ 32h in polytetrafluoroethylene (PTFE) reactor after ultrasonic 30min, products therefrom after filtration, washing, dry, namely obtain N-K
2ti
4o
9/ g-C
3n
4/ UiO-66 ternary high efficiency composition visible-light photocatalyst.
The invention also discloses the application of above-mentioned ternary high efficiency composition visible-light photocatalyst as the catalyst of organic pollution in the Photocatalytic Activity for Degradation aqueous solution.
Beneficial effect of the present invention is embodied in:
(1) the present invention is first by composite photo-catalyst N-K
2ti
4o
9/ g-C
3n
4/ UiO-66 is applied to photocatalysis field, and be a kind of photochemical catalyst of novel degradable organic pollutant, preparation method is simple, and visible light catalytic efficiency is high, has broad application prospects in photocatalysis field;
(2) the present invention prepares N-K by the electrostatic attraction of modifying induction
2ti
4o
9/ g-C
3n
4binary composite, and then utilize complexation reaction to assemble preparation N-K
2ti
4o
9/ g-C
3n
4/ UiO-66 trielement composite material, for cooperative photocatalysis purification organic pollutants;
(3) the present invention is in conjunction with N-K
2ti
4o
9visible light-responded good, lamelliform g-C
3n
4easy and other materials combines and conduction electron hole ability is strong, and the advantage that UiO-66 adsorbance is large, compound not only increases the specific area of catalyst, also improves separative efficiency and the photocatalysis efficiency of photo-generated carrier.
Accompanying drawing explanation
Fig. 1 is N-K of the present invention
2ti
4o
9, g-C
3n
4with UiO-66, N-K
2ti
4o
9/ g-C
3n
4binary composite and N-K
2ti
4o
9/ g-C
3n
4the XRD figure of/UiO-66 (3:2) ternary high efficiency composition visible-light photocatalyst;
Fig. 2 is UiO-66 (a) of the present invention, N-K
2ti
4o
9(b), g-C
3n
4(c) and N-K
2ti
4o
9/ g-C
3n
4the TEM figure of/UiO-66 (3:2) ternary high efficiency composition visible-light photocatalyst (d);
Fig. 3 is N-K of the present invention
2ti
4o
9, g-C
3n
4, UiO-66, N-K
2ti
4o
9/ g-C
3n
4binary composite and N-K
2ti
4o
9/ g-C
3n
4/ UiO-66 (3:2) ternary high efficiency composition visible-light photocatalyst is to the visible light catalytic design sketch of rhodamine B;
Fig. 4 is the N-K of different proportion of the present invention
2ti
4o
9/ g-C
3n
4/ UiO-66 ternary high efficiency composition visible-light photocatalyst is to the visible light catalytic design sketch of rhodamine B.
Detailed description of the invention
Enumerate embodiment below and further illustrate the present invention.
Embodiment 1
The present embodiment prepares N-K as follows
2ti
4o
9/ g-C
3n
4/ UiO-66 ternary high efficiency composition visible-light photocatalyst:
1, N-K
2ti
4o
9preparation
By 6.6g K
2cO
3with 12.0g TiO
2mortar is put in (mol ratio is 1:3) mixing, after grinding fully, powder is put into crucible, at 150 DEG C, calcines 2h, be then warming up to 960 DEG C, and calcining 10h, after cooling, obtains K
2ti
4o
9;
By 1.0g K
2ti
4o
9mix in 15g ethanol with 2.0g urea, then heat solvent evaporation, move to 400 DEG C of calcining 4h in Muffle furnace, cooling, washing, drying obtain N-K
2ti
4o
9.Gained N-K
2ti
4o
9xRD figure as shown in Figure 1, TEM figure as shown in Fig. 2 (b).
2, N-K
2ti
4o
9pretreatment
The N-K that step 1 is obtained
2ti
4o
9join the sodium oxalate water solution (0.22molL of 100mL
-1) in, stir 2h, after ultrasonic 1h, filter, washing, 70 DEG C of dry 5h, obtain pretreatment N-K after grinding
2ti
4o
9.
3, g-C
3n
4preparation
5.0g melamine is put into crucible, moves in Muffle furnace and be heated to 520 DEG C with the programming rate of 3 DEG C per minute, and be incubated 4 hours, be then cooled to room temperature, grinding, obtain g-C
3n
4.Gained g-C
3n
4xRD figure as shown in Figure 1, TEM figure as shown in Fig. 2 (c).
4, g-C
3n
4nitrogen protonated
The g-C that step 3 is obtained
3n
4put into nitric acid (0.5molL
-1) in solution, move in polytetrafluoroethylene (PTFE) reactor and be incubated 6h at 135 DEG C.Take out sample, by sample washing to neutral, 70 DEG C of dry 5h, obtain pretreatment g-C
3n
4.
5, N-K
2ti
4o
9/ g-C
3n
4the preparation of binary composite photo-catalyst
By the pretreatment N-K of gained in 1.0g step 2
2ti
4o
9with the pretreatment g-C of gained in 0.5g step 4
3n
4mix and blend 24h in 50mL ethanolic solution, filters, and washing, drying obtains N-K
2ti
4o
9/ g-C
3n
4binary composite.Gained N-K
2ti
4o
9/ g-C
3n
4the XRD figure of binary composite as shown in Figure 1.
6, N-K
2ti
4o
9/ g-C
3n
4the preparation of/UiO-66 ternary high efficiency composition visible-light photocatalyst
Take the N-K prepared in 0.080g step 5
2ti
4o
9/ g-C
3n
4binary composite, 0.053g ZrCl
4, 0.034g terephthalic acid (TPA) and 0.530g benzoic acid join in the DMF of 42ml, then transfer them to 120 DEG C of reaction 24h in 50mL polytetrafluoroethylene (PTFE) reactor after ultrasonic 30min, be then cooled to room temperature, filter and use DMF and CHCl
3for several times, drying under reduced pressure obtains ternary high efficiency composition visible-light photocatalyst N-K in each washing
2ti
4o
9/ g-C
3n
4/ UiO-66 (3:2) (i.e. N-K
2ti
4o
9/ g-C
3n
4binary composite and ZrCl
4mass ratio be 3:2).
As shown in Figure 1, TEM figure is as shown in Fig. 2 (d) for the XRD figure of products therefrom.
For carrying out the contrast of photocatalysis performance, the present embodiment has also prepared UiO-66 as follows:
Take 0.053g ZrCl
4(0.227mmol), 0.034g terephthalic acid (TPA) (0.227mmol) and 0.530g benzoic acid (4.344mmol) join the N of 25ml, in dinethylformamide, then 120 DEG C of reaction 24h in 30ml polytetrafluoroethylene (PTFE) reactor are transferred them to after ultrasonic 30min, be cooled to room temperature after reacted, filter and use DMF and CHCl
3for several times, drying under reduced pressure obtains UiO-66 in each washing.As shown in Figure 1, TEM figure is as shown in Fig. 2 (a) for the XRD figure of gained UiO-66.
For exploring N-K
2ti
4o
9/ g-C
3n
4the application of/UiO-66 degradable organic pollutant, contrasts N-K simultaneously
2ti
4o
9, g-C
3n
4, UiO-66, N-K
2ti
4o
9/ g-C
3n
4binary composite and N-K
2ti
4o
9/ g-C
3n
4/ UiO-66 is as photocatalysis performance during catalyst, do following test: get each catalyst 20mg, join in the rhodamine B aqueous solution of 100mL 10mg/L, dark place absorption 12h reaches balance, then open light source and carry out photocatalysis experiment, whole experiment makes catalyst and solution mix by air-blowing, uses recirculated cooling water to maintain temperature of reactor constant.After sampling, filtered by 0.22 μm of filter, absorbance measures on Shimadzu UV 2550 ultraviolet-uisible spectrophotometer.Result as shown in Figure 3, binary N-K
2ti
4o
9/ g-C
3n
4composite is better than the photocatalysis performance of pure material, ternary N-K
2ti
4o
9/ g-C
3n
4the photocatalysis effect of/UiO-66 composite is best.
Embodiment 2
The present embodiment prepares N-K by the mode that embodiment 1 is identical
2ti
4o
9/ g-C
3n
4/ UiO-66 ternary high efficiency composition visible-light photocatalyst, difference is only N-K in step 6
2ti
4o
9/ g-C
3n
4the quality of binary composite changes 0.027g into.Products therefrom N-K
2ti
4o
9/ g-C
3n
4/ UiO-66 (1:2) photocatalysis performance as shown in Figure 4.
Embodiment 3
The present embodiment prepares N-K by the mode that embodiment 1 is identical
2ti
4o
9/ g-C
3n
4/ UiO-66 ternary high efficiency composition visible-light photocatalyst, difference is only N-K in step 6
2ti
4o
9/ g-C
3n
4the quality of binary composite changes 0.035g into.Products therefrom N-K
2ti
4o
9/ g-C
3n
4/ UiO-66 (2:3) photocatalysis performance as shown in fig. 4.
Embodiment 4
The present embodiment prepares N-K by the mode that embodiment 1 is identical
2ti
4o
9/ g-C
3n
4/ UiO-66 ternary high efficiency composition visible-light photocatalyst, difference is only N-K in step 6
2ti
4o
9/ g-C
3n
4the quality of binary composite changes 0.053g into.Products therefrom N-K
2ti
4o
9/ g-C
3n
4/ UiO-66 (1:1) photocatalysis performance as shown in fig. 4.
Embodiment 5
The present embodiment prepares N-K by the mode that embodiment 1 is identical
2ti
4o
9/ g-C
3n
4/ UiO-66 ternary high efficiency composition visible-light photocatalyst, difference is only N-K in step 6
2ti
4o
9/ g-C
3n
4the quality of binary composite changes 0.106g into.Products therefrom N-K
2ti
4o
9/ g-C
3n
4/ UiO-66 (2:1) photocatalysis performance as shown in fig. 4.
Comparative example 1 ~ 5 is known by N-K
2ti
4o
9/ g-C
3n
4and ZrCl
4according to different quality than the N-K prepared
2ti
4o
9/ g-C
3n
4/ UiO-66 ternary high efficiency composition visible-light photocatalyst all has good photocatalysis performance, works as N-K simultaneously
2ti
4o
9/ g-C
3n
4and ZrCl
4mass ratio when being 3:2 composite photocatalysis performance best.
Claims (5)
1. a ternary high efficiency composition visible-light photocatalyst, is characterized in that: described ternary high efficiency composition visible-light photocatalyst is by N-K
2ti
4o
9, g-C
3n
4form with UiO-66 compound, be designated as N-K
2ti
4o
9/ g-C
3n
4/ UiO-66.
2. a preparation method for ternary high efficiency composition visible-light photocatalyst according to claim 1, is characterized in that comprising the following steps:
(1) by K
2cO
3with TiO
21:9 ~ 4:9 mixes and grinds evenly in molar ratio, then at 400 ~ 1000 DEG C of calcining 4 ~ 10h, finally naturally cools to room temperature, obtains K
2ti
4o
9;
By K
2ti
4o
9after urea in mass ratio 1:5 ~ 3:5 mixing, at 300 ~ 500 DEG C of calcining 3 ~ 6h, then naturally cool to room temperature, obtain N-K
2ti
4o
9;
By N-K
2ti
4o
9join in sodium oxalate water solution, stir, ultrasonic, then filter, wash, dry, grinding, obtain pretreatment N-K
2ti
4o
9;
(2) melamine is calcined 3 ~ 8h at 400 ~ 600 DEG C, be then cooled to room temperature, grinding, obtain g-C
3n
4;
By described g-C
3n
4join in salpeter solution, and be incubated 6h at 135 DEG C, by the washing of gained sample to neutral, dry, obtain pretreatment g-C
3n
4;
(3) by pretreatment N-K that step (1) obtains
2ti
4o
9with the pretreatment g-C that step (2) obtains
3n
4be mixed in ethanol for 1:2 ~ 7:2 in mass ratio, then stir 20 ~ 40h, filter, washing, dry, obtain N-K
2ti
4o
9/ g-C
3n
4binary composite;
(4) by N-K that step (3) obtains
2ti
4o
9/ g-C
3n
4binary composite and ZrCl
41:2 ~ 7:2 joins N in mass ratio, in dinethylformamide, then add terephthalic acid (TPA) and benzoic acid, transfer them to after ultrasonic 30min in polytetrafluoroethylene (PTFE) reactor at 100 ~ 150 DEG C of reaction 18 ~ 32h, products therefrom after filtration, washing, dry, namely obtain N-K
2ti
4o
9/ g-C
3n
4/ UiO-66 ternary high efficiency composition visible-light photocatalyst;
Wherein terephthalic acid (TPA), ZrCl
4be 0.64:1:10 with benzoic mass ratio.
3. preparation method according to claim 2, is characterized in that: described in step (1), the concentration of sodium oxalate water solution is 0.10 ~ 0.30mol/L.
4. preparation method according to claim 2, is characterized in that: in step (2), the concentration of nitric acid is 0.5 ~ 2.0mol/L.
5. an application for ternary high efficiency composition visible-light photocatalyst according to claim 1, is characterized in that: for the catalyst as organic pollution in the Photocatalytic Activity for Degradation aqueous solution.
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| CN108160120A (en) * | 2016-04-25 | 2018-06-15 | 项敬来 | A kind of compounded visible light photocatalyst Ag2CO3/TiO2/UIO-66-(COOH)2And organic matter degradation application |
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| CN109395777A (en) * | 2018-04-12 | 2019-03-01 | 常州大学 | A kind of Three-element composite photocatalyst BiOI@UIO-66 (NH2)@g-C3N4Preparation method |
| CN109046424B (en) * | 2018-08-09 | 2021-02-19 | 武汉科技大学 | UiO-66-NH for high-efficiency hydrogen production2/TiO2/Ti3C2Composite photocatalyst and preparation method thereof |
| CN109046424A (en) * | 2018-08-09 | 2018-12-21 | 武汉科技大学 | A kind of UiO-66-NH of highly effective hydrogen yield2/TiO2/Ti3C2Composite photo-catalyst and preparation method thereof |
| CN109046425A (en) * | 2018-08-13 | 2018-12-21 | 山东交通学院 | Composite photo-catalyst TiO derived from a kind of MOF base2/g-C3N4Preparation method |
| CN109590022A (en) * | 2018-12-13 | 2019-04-09 | 常州大学 | Stratiform UiO-66/g-C3N4The preparation method and application of/Ag composite material |
| CN109589934A (en) * | 2018-12-13 | 2019-04-09 | 常州大学 | It is adjusted based on benzoic acid and chloroform activates the method and adsorption applications for preparing UiO-66 |
| CN109847786B (en) * | 2019-03-06 | 2021-12-21 | 常州大学 | Preparation method and application of Z-type photocatalyst MgAlLDH/CN-H |
| CN109847786A (en) * | 2019-03-06 | 2019-06-07 | 常州大学 | A kind of preparation method and application of Z-type photochemical catalyst MgAlLDH/CN-H |
| CN110064433A (en) * | 2019-05-08 | 2019-07-30 | 上海应用技术大学 | A kind of composite photo-catalyst and preparation method thereof |
| CN110776049A (en) * | 2019-11-18 | 2020-02-11 | 湖南大学 | Method for treating organic wastewater by activating peroxymonosulfate with functionalized zirconium-based metal organic framework/protonated carbon nitride composite material |
| CN111558389A (en) * | 2020-05-13 | 2020-08-21 | 燕山大学 | BiVO4Protonated g-C3N4AgI ternary composite photocatalyst and preparation method thereof |
| CN111558389B (en) * | 2020-05-13 | 2022-04-01 | 燕山大学 | BiVO4Protonated g-C3N4AgI ternary composite photocatalyst and preparation method thereof |
| CN115608400A (en) * | 2022-10-12 | 2023-01-17 | 金宏气体股份有限公司 | Catalyst, preparation method and application thereof |
| CN115608400B (en) * | 2022-10-12 | 2024-04-02 | 金宏气体股份有限公司 | Catalyst, preparation method and application thereof |
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