CN116272936A - Preparation method and application of plant photocatalyst in different shapes - Google Patents
Preparation method and application of plant photocatalyst in different shapes Download PDFInfo
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- 239000011941 photocatalyst Substances 0.000 title claims abstract description 139
- 238000002360 preparation method Methods 0.000 title claims abstract description 22
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims abstract description 74
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 58
- VXAUWWUXCIMFIM-UHFFFAOYSA-M aluminum;oxygen(2-);hydroxide Chemical compound [OH-].[O-2].[Al+3] VXAUWWUXCIMFIM-UHFFFAOYSA-M 0.000 claims abstract description 40
- 238000002156 mixing Methods 0.000 claims abstract description 40
- 239000004927 clay Substances 0.000 claims abstract description 39
- 238000001035 drying Methods 0.000 claims abstract description 39
- 239000004408 titanium dioxide Substances 0.000 claims abstract description 37
- 238000001816 cooling Methods 0.000 claims abstract description 20
- 239000008367 deionised water Substances 0.000 claims abstract description 20
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 20
- 230000000593 degrading effect Effects 0.000 claims abstract description 3
- 241000196324 Embryophyta Species 0.000 claims description 137
- 239000002243 precursor Substances 0.000 claims description 49
- 239000003795 chemical substances by application Substances 0.000 claims description 24
- 244000062748 Eupatorium adenophorum Species 0.000 claims description 20
- 238000004140 cleaning Methods 0.000 claims description 16
- 239000002245 particle Substances 0.000 claims description 16
- 238000002791 soaking Methods 0.000 claims description 16
- 239000012634 fragment Substances 0.000 claims description 15
- 238000000034 method Methods 0.000 claims description 12
- 239000007787 solid Substances 0.000 claims description 11
- 239000010936 titanium Substances 0.000 claims description 10
- 238000001354 calcination Methods 0.000 claims description 8
- 239000012153 distilled water Substances 0.000 claims description 8
- 238000000227 grinding Methods 0.000 claims description 8
- 239000012535 impurity Substances 0.000 claims description 8
- 238000007493 shaping process Methods 0.000 claims description 8
- 239000002904 solvent Substances 0.000 claims description 8
- 238000010008 shearing Methods 0.000 claims description 7
- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical compound O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 claims description 7
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 6
- 239000002002 slurry Substances 0.000 claims description 6
- 241000208838 Asteraceae Species 0.000 claims description 4
- 241000628997 Flos Species 0.000 claims description 4
- 229910021645 metal ion Inorganic materials 0.000 claims description 4
- 239000011248 coating agent Substances 0.000 claims description 3
- 238000000576 coating method Methods 0.000 claims description 3
- 239000001038 titanium pigment Substances 0.000 claims description 3
- 241001116389 Aloe Species 0.000 claims description 2
- 241000142952 Hamamelidaceae Species 0.000 claims description 2
- 241000208680 Hamamelis mollis Species 0.000 claims description 2
- 241000756137 Hemerocallis Species 0.000 claims description 2
- 241000234280 Liliaceae Species 0.000 claims description 2
- 241000234435 Lilium Species 0.000 claims description 2
- 235000011399 aloe vera Nutrition 0.000 claims description 2
- 229910052719 titanium Inorganic materials 0.000 claims description 2
- 239000007788 liquid Substances 0.000 claims 5
- 244000208060 Lawsonia inermis Species 0.000 claims 1
- 239000000975 dye Substances 0.000 abstract 1
- 241000234282 Allium Species 0.000 description 24
- 235000002732 Allium cepa var. cepa Nutrition 0.000 description 24
- 239000000463 material Substances 0.000 description 18
- 230000015556 catabolic process Effects 0.000 description 17
- 238000006731 degradation reaction Methods 0.000 description 17
- PYWVYCXTNDRMGF-UHFFFAOYSA-N rhodamine B Chemical compound [Cl-].C=12C=CC(=[N+](CC)CC)C=C2OC2=CC(N(CC)CC)=CC=C2C=1C1=CC=CC=C1C(O)=O PYWVYCXTNDRMGF-UHFFFAOYSA-N 0.000 description 17
- 229940043267 rhodamine b Drugs 0.000 description 17
- 238000006243 chemical reaction Methods 0.000 description 13
- 150000002500 ions Chemical class 0.000 description 11
- 230000001699 photocatalysis Effects 0.000 description 10
- 230000000694 effects Effects 0.000 description 9
- 230000003197 catalytic effect Effects 0.000 description 8
- 238000005070 sampling Methods 0.000 description 6
- 239000011148 porous material Substances 0.000 description 4
- 238000000870 ultraviolet spectroscopy Methods 0.000 description 4
- 244000151012 Allium neapolitanum Species 0.000 description 3
- 240000002853 Nelumbo nucifera Species 0.000 description 3
- 235000006508 Nelumbo nucifera Nutrition 0.000 description 3
- 235000006510 Nelumbo pentapetala Nutrition 0.000 description 3
- 238000002835 absorbance Methods 0.000 description 3
- 238000005119 centrifugation Methods 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 3
- 238000001514 detection method Methods 0.000 description 3
- 239000003344 environmental pollutant Substances 0.000 description 3
- 238000002474 experimental method Methods 0.000 description 3
- 231100000719 pollutant Toxicity 0.000 description 3
- 239000010453 quartz Substances 0.000 description 3
- 230000035484 reaction time Effects 0.000 description 3
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 3
- 238000001179 sorption measurement Methods 0.000 description 3
- KKEYFWRCBNTPAC-UHFFFAOYSA-N Terephthalic acid Chemical compound OC(=O)C1=CC=C(C(O)=O)C=C1 KKEYFWRCBNTPAC-UHFFFAOYSA-N 0.000 description 2
- 238000005286 illumination Methods 0.000 description 2
- 239000012621 metal-organic framework Substances 0.000 description 2
- 239000013206 MIL-53 Substances 0.000 description 1
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 description 1
- 229910010413 TiO 2 Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- LHQLJMJLROMYRN-UHFFFAOYSA-L cadmium acetate Chemical compound [Cd+2].CC([O-])=O.CC([O-])=O LHQLJMJLROMYRN-UHFFFAOYSA-L 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- YUKQRDCYNOVPGJ-UHFFFAOYSA-N thioacetamide Chemical compound CC(N)=S YUKQRDCYNOVPGJ-UHFFFAOYSA-N 0.000 description 1
- DLFVBJFMPXGRIB-UHFFFAOYSA-N thioacetamide Natural products CC(N)=O DLFVBJFMPXGRIB-UHFFFAOYSA-N 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
- 239000002351 wastewater Substances 0.000 description 1
Classifications
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J21/00—Catalysts comprising the elements, oxides, or hydroxides of magnesium, boron, aluminium, carbon, silicon, titanium, zirconium, or hafnium
- B01J21/06—Silicon, titanium, zirconium or hafnium; Oxides or hydroxides thereof
- B01J21/063—Titanium; Oxides or hydroxides thereof
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J21/00—Catalysts comprising the elements, oxides, or hydroxides of magnesium, boron, aluminium, carbon, silicon, titanium, zirconium, or hafnium
- B01J21/18—Carbon
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/06—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of zinc, cadmium or mercury
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- 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
-
- 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
-
- 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
- C02F2101/308—Dyes; Colorants; Fluorescent agents
-
- 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
- C02F2101/38—Organic compounds containing nitrogen
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2305/00—Use of specific compounds during water treatment
- C02F2305/10—Photocatalysts
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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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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Organic Chemistry (AREA)
- Materials Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Health & Medical Sciences (AREA)
- Toxicology (AREA)
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- Hydrology & Water Resources (AREA)
- Environmental & Geological Engineering (AREA)
- Water Supply & Treatment (AREA)
- Catalysts (AREA)
Abstract
The invention discloses a preparation method and application of plant photocatalysts with different shapes, and belongs to the technical field of photocatalysts. The invention prepares plants into plant photocatalysts; adding clay, titanium dioxide and pseudo-boehmite into a plant photocatalyst, uniformly mixing, adding deionized water, uniformly mixing, preparing into different shapes, drying to remove water, and roasting for 2-24 hours at 450-900 ℃; cooling to room temperature to obtain plant photocatalysts in different shapes. The preparation method of the plant photocatalyst with different shapes is simple and can be used for degrading dyes.
Description
The application is a divisional application of a patent application No. 201910742386.6, and a patent application of a preparation method and an application of plant photocatalysts with different shapes.
Technical Field
The invention relates to a preparation method and application of plant photocatalysts with different shapes, and belongs to the technical field of photocatalysts.
Background
The treatment efficiency of the dye pollutant is low, the cost is high, secondary pollution is possibly caused, and at present, the photocatalyst of the dye pollutant mainly comprises Metal Organic Framework (MOF) materials such as Ti-MIL-125, uiO-66 and the like; semiconductor materials, e.g. TiO 2 CdS, znO, etc. There are also relatively complex composite materials. The preparation method of the CdS/MIL-53 (Fe) visible light catalyst uses ferric trichloride, terephthalic acid, N-dimethylformamide, cadmium acetate, thioacetamide and the like as precursors, and the photocatalyst has good photocatalytic activity, but has the advantages of complex preparation steps, more procedures and environmental protection.
Disclosure of Invention
Aiming at the treatment problem of dye pollutants in the prior art, the invention provides a preparation method and application of plant photocatalysts in different shapes.
The preparation method of the plant photocatalyst with different shapes comprises the following specific steps:
(1) Preparing plant into plant photocatalyst;
(2) Adding clay, titanium dioxide and pseudo-boehmite into the plant photocatalyst in the step (1), uniformly mixing, adding deionized water, uniformly mixing, preparing into different shapes, drying to remove water, and roasting for 2-24 hours at the temperature of 450-900 ℃; cooling to room temperature to obtain plant photocatalysts in different shapes;
(3) Uniformly mixing clay, titanium dioxide, pseudo-boehmite and deionized water, preparing into different shapes, drying to remove water, and roasting at 450-900 ℃ for 2-24 hours to obtain a precursor; adding silica sol into the plant photocatalyst in the step (1), uniformly mixing to obtain slurry, coating the surface of the precursor with the slurry, drying to remove water, and roasting for 2-24 hours at the temperature of 450-900 ℃; cooling to room temperature to obtain plant photocatalysts in different shapes.
The plant photocatalyst prepared from the plants in the step (1) comprises the following specific steps of
1) Soaking and cleaning the plant template in distilled water, and shearing the plant template into tissue fragments with the length of 0.5-1 cm;
2) Shaping and impurity removing pretreatment are carried out on plant template tissue fragments, and template agents are obtained through drying;
3) Soaking a template agent in a precursor solution for 6-48 h, and obtaining a plant template photocatalyst through cleaning, drying, calcining and grinding; wherein the precursor solution contains one or more metal ions of Ti, zn, cu, fe, cd, the concentration of the metal ions in the precursor solution is 0.1-100 g/L, the solvent of the precursor solution is water or ethanol, and the liquid-solid ratio mL of the precursor solution and the template agent is (100-10): 1.
The plant in the step (1) is a lily plant, an asteraceae plant or a witch hazel plant.
Further, the plants of the family Liliaceae are herba Alii Fistulosi, aloe or flos Hemerocallis, the plants of the family Compositae are Eupatorium Adenophorum or flos Chrysanthemi, and the plants of the family Hamamelidaceae are herba Calthae or Lawsoniae.
The step (2) is spherical, strip-shaped, sheet-shaped or block-shaped.
The mass ratio of the clay, the titanium dioxide, the pseudo-boehmite and the plant photocatalyst in the step (2) is (100-10), the mass ratio of the pseudo-boehmite to the plant photocatalyst is (20-2), and the mass ratio of the pseudo-boehmite to the plant photocatalyst is (20-2).
Preferably, the particle size of the titanium dioxide is 25-80 nm.
The mass ratio of the clay, the titanium pigment and the pseudo-boehmite in the step (3) is (5.5-10), the mass ratio of the clay, the titanium pigment and the pseudo-boehmite is (0-5.5), the liquid-solid ratio of the silica sol and the plant photocatalyst is (0-5.5), the mg is 100:1-10, and the mass ratio of the precursor and the plant photocatalyst is (1-50), and the mass ratio of the precursor and the plant photocatalyst is (2-1).
The application of the plant photocatalyst in degrading dye.
The method for evaluating the catalytic degradation activity of the plant photocatalyst comprises the following steps:
ultraviolet light is used as a reaction light source, a photocatalyst is added each time, the initial concentration of dye (rhodamine B) is 10mg/L, the illumination time is 4 hours, and an ultraviolet-visible spectrophotometer is used for detecting the concentration of rhodamine B.
The invention has the beneficial effects that:
(1) The plant photocatalyst has no toxic precursor, and the preparation process is simple and easy to implement;
(2) The plant photocatalyst has high-efficiency photocatalytic capability, the initial concentration of dye (rhodamine B) in 50mL of wastewater is 10mg/L, 1 photocatalyst is added, the illumination time is 4 hours, and the degradation efficiency of the dye (rhodamine B) can reach 92.7%.
Detailed Description
The invention will be described in further detail with reference to specific embodiments, but the scope of the invention is not limited to the description.
Comparative example 1: uniformly mixing clay, titanium dioxide and pseudo-boehmite, adding 50mL of deionized water, uniformly mixing, preparing into spheres with the particle size of 1cm, drying to remove water, and roasting for 2 hours at the temperature of 450 ℃; cooling to room temperature to obtain spherical photocatalyst; wherein the mass ratio of the clay to the titanium dioxide to the pseudo-boehmite is 11:11:2:11.
Example 1:
the preparation method of the onion stalk spherical photocatalyst comprises the following steps:
(1) Preparing plant (fistular onion stalk) into a plant photocatalyst; wherein the plant (fistular onion stalk) is prepared into plant photocatalyst by the following steps
1) Soaking and cleaning plant (Bulbus Allii Fistulosi) in distilled water, and cutting into tissue segments with length of 0.5-1 cm;
2) Shaping and impurity removing pretreatment are carried out on plant (fistular onion stalk) tissue fragments, and template agents are obtained after drying;
3) Soaking a template agent in Ti precursor solution (the concentration of Ti ions is 5g/L, the solvent is water, the liquid-solid ratio of the precursor solution to the template agent is 50:1) for 6 hours, and cleaning, drying, calcining and grinding to obtain a plant template photocatalyst;
(2) Adding clay, titanium dioxide and pseudo-boehmite into the plant photocatalyst in the step (1), uniformly mixing, adding 50mL of deionized water, uniformly mixing, preparing into spheres with the particle size of 1cm, drying to remove water, and roasting for 2 hours at the temperature of 450 ℃; cooling to room temperature to obtain the onion stalk spherical photocatalyst; wherein the mass ratio of the clay, the titanium dioxide, the pseudo-boehmite and the plant photocatalyst is 22:22:4:22:1;
the preparation method of the green onion spherical photocatalyst comprises the following steps:
(1) Preparing plant (green onion) into a plant photocatalyst; wherein the plant (green onion) is prepared into plant photocatalyst by the following steps
1) Soaking and cleaning a plant template (green onion) in distilled water, and shearing the plant template into tissue fragments with the length of 0.5-1 cm;
2) Shaping and impurity removing pretreatment are carried out on plant template tissue fragments, and template agents are obtained through drying;
3) Soaking a template agent in a precursor solution for 24 hours, and obtaining a plant template photocatalyst through cleaning, drying, calcining and grinding; wherein the precursor solution contains Ti ions, the concentration of the Ti ions in the precursor solution is 20g/L, the solvent of the precursor solution is water, and the liquid-solid ratio mL of the precursor solution and the template agent is 50:1;
(2) Adding clay, titanium dioxide and pseudo-boehmite into the plant photocatalyst in the step (1), uniformly mixing, adding 50mL of deionized water, uniformly mixing, preparing into spheres with the particle size of 1cm, drying to remove water, and roasting for 2 hours at the temperature of 450 ℃; cooling to room temperature to obtain the green onion spherical photocatalyst; wherein the mass ratio of the clay, the titanium dioxide, the pseudo-boehmite and the plant photocatalyst is 22:22:4:22:1;
the preparation method of the green onion stalk mixed spherical photocatalyst comprises the following steps:
(1) Preparing plants (green onion and white onion) into a plant photocatalyst; wherein the mass ratio of the green onion to the fistular onion stalk is 2:1, and the specific steps of preparing the plant photocatalyst from plants (green onion and fistular onion stalk) are (1) preparing the plant photocatalyst from plants (green onion); wherein the plant (green onion) is prepared into plant photocatalyst by the following steps
1) Soaking and cleaning a plant template (green onion and white onion) in distilled water, and shearing the plant template into tissue fragments with the length of 0.5-1 cm;
2) Shaping and impurity removing pretreatment are carried out on plant template tissue fragments, and template agents are obtained through drying;
3) Soaking a template agent in a precursor solution for 48 hours, and obtaining a plant template photocatalyst through cleaning, drying, calcining and grinding; wherein the precursor solution contains Ti ions, the concentration of the Ti ions in the precursor solution is 20g/L, the solvent of the precursor solution is water, and the liquid-solid ratio mL of the precursor solution and the template agent is 50:1;
(2) Adding clay, titanium dioxide and pseudo-boehmite into the plant photocatalyst in the step (1), uniformly mixing, adding 50mL of deionized water, uniformly mixing, preparing into spheres with the particle size of 1cm, drying to remove water, and roasting for 2 hours at the temperature of 450 ℃; cooling to room temperature to obtain the spherical photocatalyst of the green onion and the white onion; wherein the mass ratio of the clay, the titanium dioxide, the pseudo-boehmite and the plant photocatalyst is 22:22:4:22:1;
the method for testing the catalytic degradation activity of the plant photocatalyst comprises the following steps:
the visible light catalytic activity of the material is tested by selecting a rhodamine B (RhB) degradation system; in each set of experiments, 0.01-5g of material and 50-1000mL of RhB solution (10 mg/L) were placed in 50mL of quartz and stirred for reaction; dark reaction is carried out for 0.5 to 6 hours to lead the material to reach adsorption equilibrium, and then the material reacts for 4 hours under the irradiation of ultraviolet light; sampling at fixed reaction time intervals, sampling 3mL each time, and collecting the reaction solution by centrifugation for detection; the absorbance of the collected reaction solution at 554nm was measured by using an ultraviolet-visible spectrophotometer.
The degradation effect of the onion stalk spherical photocatalyst, the onion green spherical photocatalyst and the onion green onion stalk mixed spherical photocatalyst on the dye (rhodamine B) is shown in table 1,
TABLE 1 degradation efficiency
From table 1, the biological template is photocatalytic to replicate the multi-stage pore canal and morphology structure of the template, and meanwhile, the self-doping of C, si and other elements is realized in the preparation process, so that the photocatalytic performance of the material is effectively improved.
Comparative example 2: uniformly mixing clay, titanium dioxide and pseudo-boehmite, adding 75mL of deionized water, uniformly mixing, preparing into spheres with the particle size of 1.5cm, drying to remove water, and roasting at 600 ℃ for 5 hours; cooling to room temperature to obtain spherical photocatalyst; wherein the mass ratio of the clay to the titanium dioxide to the pseudo-boehmite is 5.5:5.5:1:5.5.
Example 2:
preparation method of eupatorium adenophorum spherical photocatalyst
(1) Preparing plant (Eupatorium adenophorum) into plant photocatalyst; wherein the plant (Eupatorium adenophorum Spreng) is prepared into plant photocatalyst by the following steps
1) Soaking and cleaning a plant template (Eupatorium adenophorum) in distilled water, and shearing the plant template into tissue fragments with the length of 0.5-1 cm;
2) Shaping and impurity removing pretreatment are carried out on plant template tissue fragments, and template agents are obtained through drying;
3) Soaking a template agent in a precursor solution for 12 hours, and obtaining a plant template photocatalyst through cleaning, drying, calcining and grinding; wherein the precursor solution contains Zn ions, the concentration of the Zn ions in the precursor solution is 0.4g/L, the solvent of the precursor solution is water, and the liquid-solid ratio mL of the precursor solution and the template agent is 80:1;
(2) Adding clay, titanium dioxide and pseudo-boehmite into the plant photocatalyst in the step (1), uniformly mixing, adding 75mL of deionized water, uniformly mixing, preparing into spheres with the particle size of 1.5cm, drying to remove water, and roasting for 5 hours at the temperature of 600 ℃; cooling to room temperature to obtain spherical photocatalyst of Eupatorium adenophorum, denoted as spherical photocatalyst A; wherein the mass ratio of the clay to the titanium dioxide to the pseudo-boehmite to the plant photocatalyst is 5.5:5.5:1:5.5:0.05;
(3) Adding clay, titanium dioxide and pseudo-boehmite into the plant photocatalyst in the step (1), uniformly mixing, adding 75mL of deionized water, uniformly mixing, preparing into spheres with the particle size of 1.5cm, drying to remove water, and roasting for 5 hours at the temperature of 600 ℃; cooling to room temperature to obtain spherical photocatalyst of Eupatorium adenophorum, denoted as spherical photocatalyst B; wherein the mass ratio of the clay, the titanium dioxide, the pseudo-boehmite and the plant photocatalyst is 5.5:5.5:1:5.5:0.1;
(4) Adding clay, titanium dioxide and pseudo-boehmite into the plant photocatalyst in the step (1), uniformly mixing, adding 75mL of deionized water, uniformly mixing, preparing into spheres with the particle size of 1.5cm, drying to remove water, and roasting for 5 hours at the temperature of 600 ℃; cooling to room temperature to obtain spherical photocatalyst of Eupatorium adenophorum, denoted as spherical photocatalyst C; wherein the mass ratio of the clay, the titanium dioxide, the pseudo-boehmite and the plant photocatalyst is 5.5:5.5:1:5.5:0.15;
(5) Adding clay, titanium dioxide and pseudo-boehmite into the plant photocatalyst in the step (1), uniformly mixing, adding 75mL of deionized water, uniformly mixing, preparing into spheres with the particle size of 1.5cm, drying to remove water, and roasting for 5 hours at the temperature of 600 ℃; cooling to room temperature to obtain spherical photocatalyst of Eupatorium adenophorum, denoted as spherical photocatalyst D; wherein the mass ratio of the clay, the titanium dioxide, the pseudo-boehmite and the plant photocatalyst is 5.5:5.5:1:5.5:0.25;
(6) Adding clay, titanium dioxide and pseudo-boehmite into the plant photocatalyst in the step (1), uniformly mixing, adding 75mL of deionized water, uniformly mixing, preparing into spheres with the particle size of 1.5cm, drying to remove water, and roasting for 5 hours at the temperature of 600 ℃; cooling to room temperature to obtain spherical photocatalyst of Eupatorium adenophorum, denoted as spherical photocatalyst E; wherein the mass ratio of the clay, the titanium dioxide, the pseudo-boehmite and the plant photocatalyst is 5.5:5.5:1:5.5:0.5;
the method for testing the catalytic degradation activity of the plant photocatalyst comprises the following steps:
the visible light catalytic activity of the material is tested by selecting a rhodamine B (RhB) degradation system; in each set of experiments, 0.01-5g of material and 50-1000mL of RhB solution (10 mg/L) were placed in 50mL of quartz and stirred for reaction; dark reaction is carried out for 0.5 to 6 hours to lead the material to reach adsorption equilibrium, and then the material reacts for 4 hours under the irradiation of ultraviolet light; sampling at fixed reaction time intervals, sampling 3mL each time, and collecting the reaction solution by centrifugation for detection; measuring absorbance of the collected reaction solution at 554nm by using an ultraviolet-visible spectrophotometer;
the degradation effect of the eupatorium adenophorum spherical photocatalyst on the dye (rhodamine B) is shown in table 2,
TABLE 2 degradation efficiency of spherical photocatalyst of Eupatorium adenophorum Spreng
From table 2, the biological template is photocatalytic to replicate the multi-stage pore canal and morphology structure of the template, and meanwhile, the self-doping of C, si and other elements is realized in the preparation process, so that the photocatalytic performance of the material is effectively improved.
Comparative example 3: uniformly mixing clay, titanium dioxide and pseudo-boehmite, adding 50mL of deionized water, uniformly mixing, preparing into spheres with the particle size of 2cm, drying to remove water, and roasting at 900 ℃ for 3 hours; cooling to room temperature to obtain spherical photocatalyst; wherein the mass ratio of the clay to the titanium dioxide to the pseudo-boehmite is 5.5:5.5:1:5.5.
Example 3:
preparation method of horseshoe-shaped spherical photocatalyst
(1) Preparing plant (horseshoe lotus) into plant photocatalyst; wherein the plant (horseshoe lotus) is prepared into plant photocatalyst by the following steps
1) Soaking and cleaning a plant template (horseshoe lotus) in distilled water, and shearing the plant template into tissue fragments with the length of 0.5-1 cm;
2) Shaping and impurity removing pretreatment are carried out on plant template tissue fragments, and template agents are obtained through drying;
3) Soaking a template agent in a precursor solution for 16 hours, and obtaining a plant template photocatalyst through cleaning, drying, calcining and grinding; the precursor solution contains Cu ions, the concentration of the Cu ions in the precursor solution is 10g/L, the solvent of the precursor solution is water, and the liquid-solid ratio mL of the precursor solution and the template agent is 100:1;
(2) Adding clay, titanium dioxide and pseudo-boehmite into the plant photocatalyst in the step (1), uniformly mixing, adding 50mL of deionized water, uniformly mixing, preparing into spheres with the particle size of 2cm, drying to remove water, and roasting for 3 hours at the temperature of 900 ℃; cooling to room temperature to obtain a horseshoe-shaped spherical photocatalyst, namely a horseshoe-shaped spherical photocatalyst A; wherein the mass ratio of the clay to the titanium dioxide to the pseudo-boehmite to the plant photocatalyst is 5.5:5.5:1:5.5:0.05;
(3) Adding clay, titanium dioxide and pseudo-boehmite into the plant photocatalyst in the step (1), uniformly mixing, adding 50mL of deionized water, uniformly mixing, preparing into spheres with the particle size of 2cm, drying to remove water, and roasting for 3 hours at the temperature of 900 ℃; cooling to room temperature to obtain a horseshoe-shaped spherical photocatalyst, namely a horseshoe-shaped spherical photocatalyst B; wherein the mass ratio of the clay, the titanium dioxide, the pseudo-boehmite and the plant photocatalyst is 5.5:5.5:1:5.5:0.1;
(4) Adding clay, titanium dioxide and pseudo-boehmite into the plant photocatalyst in the step (1), uniformly mixing, adding 50mL of deionized water, uniformly mixing, preparing into spheres with the particle size of 2cm, drying to remove water, and roasting for 3 hours at the temperature of 900 ℃; cooling to room temperature to obtain a horseshoe-shaped spherical photocatalyst, namely a horseshoe-shaped spherical photocatalyst C; wherein the mass ratio of the clay, the titanium dioxide, the pseudo-boehmite and the plant photocatalyst is 5.5:5.5:1:5.5:0.15;
the method for testing the catalytic degradation activity of the plant photocatalyst is the same as that in the embodiment;
the degradation effect of horseshoe-shaped spherical photocatalyst on dye (rhodamine B) is shown in table 3,
TABLE 3 degradation efficiency of horseshoe-shaped spherical photocatalyst
From table 3, the biological template is photocatalytic to replicate the multi-stage pore canal and morphology structure of the template, and meanwhile, the self-doping of C, si and other elements is realized in the preparation process, so that the photocatalytic performance of the material is effectively improved.
Example 4: preparation method of eupatorium adenophorum strip photocatalyst
(1) Preparing plant (Eupatorium adenophorum) into plant photocatalyst; wherein the plant (Eupatorium adenophorum Spreng) is prepared into plant photocatalyst by the following steps
1) Soaking and cleaning a plant template (Eupatorium adenophorum) in distilled water, and shearing the plant template into tissue fragments with the length of 0.5-1 cm;
2) Shaping and impurity removing pretreatment are carried out on plant template tissue fragments, and template agents are obtained through drying;
3) Soaking a template agent in a precursor solution for 18h, and obtaining a plant template photocatalyst through cleaning, drying, calcining and grinding; wherein the precursor solution contains Ti ions, the concentration of the Ti ions in the precursor solution is 8g/L, the solvent of the precursor solution is ethanol, and the liquid-solid ratio mL of the precursor solution and the template agent is 30:1;
(2) Uniformly mixing 10g of clay and deionized water, preparing into strips, drying to remove water, and roasting at 900 ℃ for 2 hours to obtain a precursor; adding silica sol into the plant photocatalyst in the step (1), uniformly mixing to obtain slurry, coating the surface of the precursor with the slurry, drying to remove water, and roasting for 2 hours at 900 ℃; cooling to room temperature to obtain the eupatorium adenophorum bar photocatalyst; wherein the liquid-solid ratio mL of the silica sol to the plant photocatalyst is 50:1, and the silica sol is commercially available; the mass ratio of the precursor to the plant photocatalyst is 10:0.25;
the method for testing the catalytic degradation activity of the plant photocatalyst comprises the following steps:
the visible light catalytic activity of the material is tested by selecting a rhodamine B (RhB) degradation system; in each set of experiments, 0.01-5g of material and 50-1000mL of RhB solution (10 mg/L) were placed in 50mL of quartz and stirred for reaction; dark reaction is carried out for 0.5 to 6 hours to lead the material to reach adsorption equilibrium, and then the material reacts for 4 hours under the irradiation of ultraviolet light; sampling at fixed reaction time intervals, sampling 3mL each time, and collecting the reaction solution by centrifugation for detection; measuring absorbance of the collected reaction solution at 554nm by using an ultraviolet-visible spectrophotometer;
the degradation effect of the eupatorium adenophorum bar photocatalyst on the dye (rhodamine B) is shown in table 4,
TABLE 4 degradation efficiency of Eupatorium adenophorum strip photocatalyst
From table 4, the biological template is photocatalytic to replicate the multi-stage pore canal and morphology structure of the template, and meanwhile, the self-doping of C, si and other elements is realized in the preparation process, so that the photocatalytic performance of the material is effectively improved.
Claims (7)
1. The preparation method of the plant photocatalyst with different shapes is characterized by comprising the following specific steps:
(1) Preparing plant into plant photocatalyst; the specific steps for preparing the plant into the plant photocatalyst are as follows:
(11) Soaking and cleaning plants in distilled water, and shearing the plants into tissue fragments with the length of 0.5-1 cm;
(12) Shaping and impurity removing pretreatment are carried out on the tissue fragments, and template agents are obtained through drying;
(13) Soaking the template agent in the precursor liquid for 6-48 h, and obtaining a plant photocatalyst through cleaning, drying, calcining and grinding; the precursor liquid contains one or more metal ions of Ti, zn, cu, fe, cd, the concentration of the metal ions in the precursor liquid is 0.1-100 g/L, the solvent of the precursor liquid is water or ethanol, and the liquid-solid ratio mL of the precursor liquid and the template agent is (100-10): 1;
(2) Adding clay, titanium dioxide and pseudo-boehmite into the plant photocatalyst in the step (1), uniformly mixing, adding deionized water, uniformly mixing, preparing into different shapes, drying to remove water, and roasting for 2-24 hours at the temperature of 450-900 ℃; cooling to room temperature to obtain plant photocatalysts in different shapes;
or uniformly mixing clay, titanium dioxide, pseudo-boehmite and deionized water to prepare different shapes, drying to remove water, and roasting for 2-24 hours at 450-900 ℃ to obtain a precursor; adding silica sol into the plant photocatalyst obtained in the step (1), uniformly mixing to obtain slurry, coating the surface of the precursor with the slurry, drying to remove water, and roasting for 2-24 hours at the temperature of 450-900 ℃; cooling to room temperature to obtain plant photocatalysts in different shapes; the mass ratio of the clay to the titanium pigment to the pseudo-boehmite is (5.5-10): 0-5.5, the liquid-solid ratio of the silica sol to the plant photocatalyst is (mL: mg) is 100:1-10, and the mass ratio of the precursor to the plant photocatalyst is (1-50): 2-1.
2. The method for preparing the plant photocatalyst in different shapes according to claim 1, wherein: the plant in the step (1) is a lily plant, an asteraceae plant or a witch hazel plant.
3. The method for preparing the plant photocatalyst in different shapes according to claim 2, wherein: the plants of Liliaceae are herba Alii Fistulosi, aloe or flos Hemerocallis, the plants of Compositae are Eupatorium Adenophorum or flos Chrysanthemi, and the plants of Hamamelidaceae are herba Calthae Calophylli or Lawsonia inermis.
4. The method for preparing the plant photocatalyst in different shapes according to claim 1, wherein: the step (2) is spherical, strip-shaped, sheet-shaped or block-shaped.
5. The method for preparing the plant photocatalyst in different shapes according to claim 1, wherein: the mass ratio of the clay, the titanium dioxide, the pseudo-boehmite and the plant photocatalyst in the step (2) is (100-10): 20-2): 1.
6. The method for preparing the plant photocatalyst in different shapes according to claim 5, wherein: the particle size of the titanium dioxide is 25-80 nm.
7. Use of a plant photocatalyst prepared by the method for preparing a plant photocatalyst of different shape according to any one of claims 1 to 6 for degrading a dye.
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