CN108479740B - Carbonized bamboo fungus/nano titanium dioxide composite photocatalyst and preparation method thereof - Google Patents
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- 235000017166 Bambusa arundinacea Nutrition 0.000 title claims abstract description 53
- 235000017491 Bambusa tulda Nutrition 0.000 title claims abstract description 53
- 241001330002 Bambuseae Species 0.000 title claims abstract description 53
- 235000015334 Phyllostachys viridis Nutrition 0.000 title claims abstract description 53
- 239000011425 bamboo Substances 0.000 title claims abstract description 53
- 241000233866 Fungi Species 0.000 title claims abstract description 48
- SOQBVABWOPYFQZ-UHFFFAOYSA-N oxygen(2-);titanium(4+) Chemical compound [O-2].[O-2].[Ti+4] SOQBVABWOPYFQZ-UHFFFAOYSA-N 0.000 title claims abstract description 42
- 239000011941 photocatalyst Substances 0.000 title claims abstract description 36
- 239000002131 composite material Substances 0.000 title claims abstract description 24
- 238000002360 preparation method Methods 0.000 title claims abstract description 15
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims abstract description 40
- 239000004408 titanium dioxide Substances 0.000 claims abstract description 16
- 239000000463 material Substances 0.000 claims abstract description 8
- 239000002105 nanoparticle Substances 0.000 claims abstract description 3
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 18
- LZZYPRNAOMGNLH-UHFFFAOYSA-M Cetrimonium bromide Chemical compound [Br-].CCCCCCCCCCCCCCCC[N+](C)(C)C LZZYPRNAOMGNLH-UHFFFAOYSA-M 0.000 claims description 14
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 12
- 241001313710 Dictyophora indusiata Species 0.000 claims description 12
- 238000010438 heat treatment Methods 0.000 claims description 10
- 238000001035 drying Methods 0.000 claims description 9
- 238000000034 method Methods 0.000 claims description 9
- 229910052786 argon Inorganic materials 0.000 claims description 6
- 238000001914 filtration Methods 0.000 claims description 6
- 238000003763 carbonization Methods 0.000 claims description 3
- 238000002156 mixing Methods 0.000 claims description 3
- 238000005406 washing Methods 0.000 claims description 3
- 241001313737 Dictyophora echinovolvata Species 0.000 claims description 2
- 241000890685 Dictyophora rubrovolvata Species 0.000 claims description 2
- 238000010000 carbonizing Methods 0.000 claims description 2
- 239000011261 inert gas Substances 0.000 claims description 2
- 238000004321 preservation Methods 0.000 claims description 2
- 239000011148 porous material Substances 0.000 claims 1
- 230000001699 photocatalysis Effects 0.000 abstract description 16
- RBTBFTRPCNLSDE-UHFFFAOYSA-N 3,7-bis(dimethylamino)phenothiazin-5-ium Chemical compound C1=CC(N(C)C)=CC2=[S+]C3=CC(N(C)C)=CC=C3N=C21 RBTBFTRPCNLSDE-UHFFFAOYSA-N 0.000 abstract description 6
- 229960000907 methylthioninium chloride Drugs 0.000 abstract description 6
- 239000002994 raw material Substances 0.000 abstract description 3
- 238000013033 photocatalytic degradation reaction Methods 0.000 abstract description 2
- 239000003054 catalyst Substances 0.000 abstract 1
- 239000000523 sample Substances 0.000 description 27
- 239000007787 solid Substances 0.000 description 9
- 241001313734 Dictyophora Species 0.000 description 7
- 230000015556 catabolic process Effects 0.000 description 6
- 238000006731 degradation reaction Methods 0.000 description 6
- 239000007864 aqueous solution Substances 0.000 description 4
- 239000002086 nanomaterial Substances 0.000 description 4
- 238000000643 oven drying Methods 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 3
- 239000002245 particle Substances 0.000 description 3
- 238000007146 photocatalysis Methods 0.000 description 3
- 239000000243 solution Substances 0.000 description 3
- 238000001179 sorption measurement Methods 0.000 description 3
- 238000003756 stirring Methods 0.000 description 3
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 3
- 238000002371 ultraviolet--visible spectrum Methods 0.000 description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- 241001313708 Dictyophora phalloidea Species 0.000 description 2
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 239000013068 control sample Substances 0.000 description 2
- 230000001934 delay Effects 0.000 description 2
- 230000031700 light absorption Effects 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 230000006798 recombination Effects 0.000 description 2
- 238000005215 recombination Methods 0.000 description 2
- 230000027756 respiratory electron transport chain Effects 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 238000001354 calcination Methods 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- -1 compound nano titanium dioxide Chemical class 0.000 description 1
- 238000013329 compounding Methods 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 239000002957 persistent organic pollutant Substances 0.000 description 1
- 238000001782 photodegradation Methods 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000000634 powder X-ray diffraction Methods 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
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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
- B01J35/39—Photocatalytic properties
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- B01J21/00—Catalysts comprising the elements, oxides, or hydroxides of magnesium, boron, aluminium, carbon, silicon, titanium, zirconium, or hafnium
- B01J21/18—Carbon
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/30—Treatment of water, waste water, or sewage by irradiation
- C02F1/32—Treatment of water, waste water, or sewage by irradiation with ultraviolet light
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/40—Organic compounds containing sulfur
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
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Abstract
The invention provides a carbonized bamboo fungus/nano titanium dioxide composite photocatalyst and a preparation method thereof. The catalyst is a carbonized bamboo fungus supported nano titanium dioxide material, has a three-dimensional reticular micro-nano hierarchical structure, takes carbonized bamboo fungus as a framework, and is compounded with titanium dioxide nano particles. The carbonized bamboo fungus/nano titanium dioxide composite photocatalyst provided by the invention has a three-dimensional reticular micro-nano hierarchical structure and good photocatalytic activity, is compounded under the same conditions, shows better photocatalytic efficiency, and can be used for completing photocatalytic degradation of dye methylene blue within 30 minutes under the ultraviolet visible condition; the preparation raw materials are easy to obtain, the preparation method is simple, and the preparation method has potential application value in the fields of energy and environment.
Description
Technical Field
The invention relates to the field of environment and energy, and particularly relates to a carbonized bamboo fungus/nano titanium dioxide composite photocatalyst and a preparation method thereof.
Background
The nanometer titanium dioxide photocatalyst is shown as a high-efficiency photocatalyst in the front of people, and the technology can effectively degrade organic pollutants and is expected to utilize visible light. However, the titanium dioxide photocatalyst, as a wide bandgap semiconductor material, has a low effective absorption efficiency for light and is easy to recombine electron-hole, so that the photocatalytic activity of the titanium dioxide photocatalyst is not high.
Disclosure of Invention
The invention aims to provide a preparation method of a carbonized bamboo fungus/nano titanium dioxide composite photocatalyst with a micro-nano hierarchical structure. The photocatalyst provided by compounding the carbonized bamboo fungus and the nano titanium dioxide can obviously improve the photocatalytic performance of the compounded carbonized bamboo fungus/nano titanium dioxide composite photocatalyst.
A carbonized bamboo fungus/nano titanium dioxide composite photocatalyst is a carbonized bamboo fungus supported nano titanium dioxide material, has a three-dimensional reticular micro-nano hierarchical structure, takes carbonized bamboo fungus as a framework, and is compounded with titanium dioxide nanoparticles.
The preparation method of the carbonized bamboo fungus/nano titanium dioxide composite photocatalyst comprises the following steps:
1) primarily carbonizing natural bamboo fungus with sulfuric acid;
2) adding the sample obtained in the step 1) into a solution of Cetyl Trimethyl Ammonium Bromide (CTAB) and titanium dioxide, uniformly mixing, filtering, washing and drying;
3) and (3) carrying out heat treatment on the dried sample in the step 2) under inert gas argon to obtain the carbonized bamboo fungus/nano titanium dioxide composite photocatalyst material with a carbonized bamboo fungus skeleton structure.
According to the scheme, the dictyophora indusiata in the step 1) is a dictyophora indusiata with a three-dimensional mesh structure, such as dictyophora indusiata, dictyophora phalloidea, dictyophora echinovolvata and dictyophora rubrovolvata.
According to the scheme, the carbonization in the step 1) is to dry and stand the natural bamboo fungus in sulfuric acid, heat the natural bamboo fungus to 100-160 ℃ for a period of time, and then dry the natural bamboo fungus for later use.
According to the scheme, the heat preservation time of 100-160 ℃ in the step 1) is 2 h.
According to the scheme, the drying in the step 1) is carried out for 2 hours at the temperature of 60 ℃.
According to the scheme, in the step 1), the concentration of the sulfuric acid is 10-30 wt%.
According to the scheme: in the step 2), the concentration of the titanium dioxide in the solution of the Cetyl Trimethyl Ammonium Bromide (CTAB) and the titanium dioxide is 16.7mg/ml-50 mg/ml; cetyl trimethylammonium bromide (CTAB) at a concentration of 0.025mg/ml to 1.25 mg/ml.
According to the scheme: the heat treatment temperature in the step 3) is 500-800 ℃; the heat treatment time is 2-4 h.
Dictyophora indusiata is a fungus, and has a special net-shaped structure due to the weak light growth characteristic of the fungus. The invention adopts dictyophora as a raw material, the dictyophora is carbonized primarily by sulfuric acid, the dictyophora has the advantages of a hierarchical structure and a larger specific surface area, composite nano titanium dioxide can be well adsorbed, then Cetyl Trimethyl Ammonium Bromide (CTAB) and titanium dioxide solution are added and uniformly mixed, and then the mixture is filtered, dried and thermally treated to carry out full carbonization and crystallization, and the obtained carbonized dictyophora/nano titanium dioxide composite photocatalyst material takes carbonized dictyophora as a framework and nano titanium dioxide particles as an active center and has a micro-nano hierarchical structure. The micro-nano structure can improve the light absorption efficiency of the nano titanium dioxide, can inhibit the increase of the size of the nano titanium dioxide, increases the specific surface area, the adsorption performance and the photocatalytic performance of the composite photocatalyst, and solves the problems of poor adsorption performance, easy agglomeration, poor photocatalytic effect and the like of the granular nano titanium dioxide photocatalyst. In addition, the carbonized bamboo fungus mainly contains carbon, has stronger conductivity than the nano titanium dioxide, can play a role of an electron transfer carrier in the photocatalysis process, and effectively delays the recombination of electrons and holes, thereby enhancing the photocatalysis activity of the nano titanium dioxide.
The invention has the beneficial effects that:
(1) the carbonized bamboo fungus/nano titanium dioxide composite photocatalyst provided by the invention has a micro-nano structure and good photocatalytic activity, is compounded under the same conditions, shows better photocatalytic efficiency, and can be used for completing photocatalytic degradation of dye methylene blue within 30 minutes under the ultraviolet visible condition;
(2) the preparation raw materials are easy to obtain, the preparation method is simple, and the preparation method has potential application value in the fields of energy and environment.
Drawings
FIGS. 1a and b are SEM photographs of carbonized Dictyophora phalloidea; FIGS. 1 c-f are H-TiO2SEM photograph of @ C;
FIG. 2 is a powder X-ray diffraction pattern (XRD) of the carbonized bamboo fungus-supported nano titanium dioxide photocatalyst obtained in example 1 and comparative example 1;
FIG. 3 is an ultraviolet-visible spectrum (UV-vis) of the carbonized bamboo fungus-supported nano titanium dioxide photocatalyst obtained in example 1 under dark conditions;
FIG. 4 is a degradation curve of dye methylene blue under ultraviolet visible light for a carbonized bamboo fungus-supported nano titanium dioxide photocatalyst sample obtained in example 1;
fig. 5 is a degradation rate curve of a dye methylene blue under ultraviolet visible light for a carbonized bamboo fungus-supported nano titanium dioxide photocatalyst sample obtained in example 1;
fig. 6 is a bamboo fungus photo.
Detailed Description
For better understanding of the present invention, the following description is further illustrated with reference to the drawings and examples, but the present invention is not limited to the following examples.
Example 1
The embodiment provides a carbonized bamboo fungus supported nano titanium dioxide photocatalyst. The preparation method comprises the following steps:
1) drying natural Dictyophora Indusiata, standing in 30 ml 10% (mass concentration, the same below) concentrated sulfuric acid for 20 min, oven-drying at 130 deg.C for 2 hr, and taking out. Then put into a 60 ℃ oven, taken out after two hours, added into 40mL of aqueous solution containing 0.050g CTAB and 0.5g P25 and mixed evenly.
2) Slowly stirring to mix them uniformly. Then filtering to obtain a solid sample, putting the solid sample into a 60 ℃ oven, and taking out the solid sample after 2 hours.
3) And (3) putting the sample obtained in the step 2) into a tube furnace filled with argon, and carrying out heat treatment for 3 hours at 800 ℃. Taking out to obtain carbonized bamboo fungus composite nano titanium dioxide photocatalyst named as H-TiO2@C。
Comparative example
1) Drying natural Dictyophora Indusiata, standing in 30 ml 10% (mass concentration, the same below) concentrated sulfuric acid for 20 min, oven-drying at 130 deg.C for 2 hr, taking out, washing, and filtering. After drying, grinding into powder, adding into 40mL aqueous solution containing 0.05g CTAB and 0.5g P25, and mixing well.
2) Slowly stirring to mix them uniformly. Then filtering to obtain a solid sample, putting the solid sample into a 60 ℃ oven, and taking out the solid sample after 2 hours.
3) And (3) putting the sample obtained in the step 2) into a tube furnace filled with argon, and carrying out heat treatment for 3 hours at 800 ℃. Taking out to obtain carbonized bamboo fungus composite nano titanium dioxide photocatalyst named as M-TiO2@C。
The picture of Dictyophora Indusiata is shown in figure 6; SEM photos of the carbonized bamboo fungus are shown in figures 1a and b, and the photos show that the carbonized bamboo fungus has a micro-nano concave-convex structure on the surface, is in a three-dimensional net shape, can load and compound nano titanium dioxide particles, is favorable for electron transmission during titanium dioxide degradation, and prolongs the electron-hole separation time.
Obtaining carbonized bamboo fungus:
1) drying natural Dictyophora Indusiata, standing in 30 ml 10% (mass concentration, the same below) concentrated sulfuric acid for 20 min, oven-drying at 130 deg.C for 2 hr, and taking out. Then put into a 60 ℃ oven, taken out after two hours, added into 40mL of aqueous solution containing 0.050g CTAB and 0.5g P25 and mixed evenly.
2) Putting the sample obtained in the step 1) into a tube furnace filled with argon, and carrying out heat treatment for 3 hours at 800 ℃. Taking out to obtain carbonized bamboo fungus.
FIGS. 1 c-f are H-TiO2In SEM photograph of @ C, we can see that P25 is compounded on carbonized dictyophora, and very much P25 particle load can be found on the porous channel structure of the carbonized dictyophora.
FIG. 2 is a sample of H-TiO according to an embodiment of the present invention2The XRD pattern of @ C shows that the product of the invention is a mixture of anatase phase and rutile phase, the main peak of the rutile phase peak of the sample is enhanced, and the calcination improves TiO2The crystallinity of bamboo shoots is facilitated by high-temperature treatment, and the carbonized bamboo fungus/nano titanium dioxide composite photocatalyst with excellent performance is obtained.
FIG. 3 shows the carbonized bamboo fungus loaded nano titanium dioxide photocatalyst sample H-TiO obtained in example 12The ultraviolet-visible spectrograms of @ C (UV-vis); FIG. 4 is a graph showing the degradation curve of dye methylene blue under ultraviolet visible light for the carbonized bamboo fungus-supported nano titanium dioxide photocatalyst sample and the control sample obtained in example 1; FIG. 5 is a graph showing the degradation rate of dye methylene blue under ultraviolet visible light for the carbonized bamboo fungus-supported nano titanium dioxide photocatalyst sample and the control sample obtained in example 1; as can be seen from the graph, the concentration of the example sample and the comparative sample did not change much in the dark reaction stage, but the concentration changed greatly after the light irradiation. The final result shows that the composite photocatalytic product H-TiO with the carbonized bamboo fungus three-dimensional structure2The photocatalytic performance of @ C is greatly superior to that of a composite photocatalytic contrast sample without a micro-nano structure. The photocatalytic efficiency of the example sample was about 1.6 times that of the control, which was 2 times that of P25. The main reasons are that the three-dimensional reticular micro-nano structure can inhibit the increase of the size of the nano titanium dioxide, can improve the light absorption efficiency of the nano titanium dioxide and increase the specific surface area and the adsorption performance of the photocatalyst after the composite. In addition, the carbonized bamboo fungus mainly contains carbon, has stronger conductivity than nano titanium dioxide, can play a role of an electron transfer carrier in the photocatalysis process, effectively delays the recombination of electrons and holes, and can strengthen the effectThe photocatalytic activity of the nano titanium dioxide.
Example 2
The embodiment provides a carbonized bamboo fungus supported nano titanium dioxide photocatalyst. The preparation method comprises the following steps:
1) drying natural Dictyophora Indusiata, standing in 30 ml 15% (mass concentration, the same below) concentrated sulfuric acid for 15 min, oven drying at 120 deg.C for 2 hr, and taking out. Then put into a 60 ℃ oven, taken out after two hours, added into 40mL of aqueous solution containing 0.030gCTAB and 0.5gP25 and mixed evenly.
2) Slowly stirring to mix them uniformly. Then filtering to obtain a solid sample, putting the solid sample into a 60 ℃ oven, and taking out the solid sample after 2 hours.
3) And (3) putting the sample obtained in the step 2) into a tube furnace filled with argon for heat treatment at 700 ℃ for 4 hours. Taking out to obtain the carbonized bamboo fungus composite nano titanium dioxide photocatalyst. The photodegradation experiments show that the sample also shows excellent degradation performance, which is only slightly weaker than that of example 1 and is better than P25.
Claims (9)
1. A carbonized bamboo fungus/nano titanium dioxide composite photocatalyst is characterized in that: the nanometer titanium dioxide material is a carbonized bamboo fungus supported nanometer titanium dioxide material, has a three-dimensional reticular micro-nano hierarchical structure, takes the carbonized bamboo fungus as a framework, has a three-dimensional pore structure, and is compounded with titanium dioxide nanoparticles.
2. The preparation method of the carbonized bamboo fungus/nano titanium dioxide composite photocatalyst as claimed in claim 1, which is characterized in that: it comprises the following steps:
1) primarily carbonizing natural bamboo fungus with sulfuric acid;
2) adding the sample obtained in the step 1) into a solution of cetyl trimethyl ammonium bromide and titanium dioxide, uniformly mixing, filtering, washing and drying;
3) and (3) carrying out heat treatment on the dried sample in the step 2) under inert gas argon to obtain the carbonized bamboo fungus/nano titanium dioxide composite photocatalyst material with a carbonized bamboo fungus skeleton structure.
3. The method of claim 2, wherein: the dictyophora indusiata in the step 1) is a dictyophora indusiata with a three-dimensional mesh structure, and includes but is not limited to dictyophora indusiata, dictyophora echinovolvata and dictyophora rubrovolvata.
4. The method of claim 2, wherein: the carbonization in the step 1) is to dry and stand the natural bamboo fungus in sulfuric acid, heat the natural bamboo fungus to 100-160 ℃ for a period of time, and then dry the natural bamboo fungus for later use.
5. The method of claim 4, wherein: the heat preservation time of 100-160 ℃ in the step 1) is 2 h.
6. The method of claim 4, wherein: the drying in the step 1) is carried out for two hours at the temperature of 60 ℃.
7. The method of claim 2, wherein: in the step 1), the concentration of the sulfuric acid is 10 wt% -30 wt%.
8. The method of claim 2, wherein: in the step 2), the concentration of the titanium dioxide in the solution of the hexadecyl trimethyl ammonium bromide and the titanium dioxide is 16.7mg/mL-50 mg/mL; the concentration of cetyl trimethyl ammonium bromide is 0.025mg/mL to 1.25 mg/mL.
9. The method of claim 2, wherein: the heat treatment temperature in the step 3) is 500-800 ℃; the heat treatment time is 2-4 h.
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