CN114367275A - Ni-doped TiO prepared by taking cut tobacco stems as template2Method and use of photocatalytic materials - Google Patents
Ni-doped TiO prepared by taking cut tobacco stems as template2Method and use of photocatalytic materials Download PDFInfo
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- 239000000463 material Substances 0.000 title claims abstract description 54
- 241000208125 Nicotiana Species 0.000 title claims abstract description 45
- 235000002637 Nicotiana tabacum Nutrition 0.000 title claims abstract description 45
- 230000001699 photocatalysis Effects 0.000 title claims abstract description 35
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 claims abstract description 26
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 18
- 238000000034 method Methods 0.000 claims abstract description 18
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 claims abstract description 17
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims abstract 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 claims abstract description 15
- 229940043267 rhodamine b Drugs 0.000 claims abstract description 15
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims abstract description 12
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 11
- KBJMLQFLOWQJNF-UHFFFAOYSA-N nickel(ii) nitrate Chemical compound [Ni+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O KBJMLQFLOWQJNF-UHFFFAOYSA-N 0.000 claims abstract description 9
- 238000001354 calcination Methods 0.000 claims abstract description 8
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- SXRSQZLOMIGNAQ-UHFFFAOYSA-N Glutaraldehyde Chemical compound O=CCCCC=O SXRSQZLOMIGNAQ-UHFFFAOYSA-N 0.000 claims abstract description 6
- YHWCPXVTRSHPNY-UHFFFAOYSA-N butan-1-olate;titanium(4+) Chemical compound [Ti+4].CCCC[O-].CCCC[O-].CCCC[O-].CCCC[O-] YHWCPXVTRSHPNY-UHFFFAOYSA-N 0.000 claims abstract description 6
- 230000000593 degrading effect Effects 0.000 claims abstract description 6
- 238000002156 mixing Methods 0.000 claims abstract description 5
- 239000007787 solid Substances 0.000 claims abstract description 5
- 238000009210 therapy by ultrasound Methods 0.000 claims abstract description 4
- PXHVJJICTQNCMI-UHFFFAOYSA-N nickel Substances [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 13
- 239000000243 solution Substances 0.000 claims description 12
- 239000010936 titanium Substances 0.000 claims description 7
- 238000006243 chemical reaction Methods 0.000 claims description 6
- 238000001035 drying Methods 0.000 claims description 6
- 239000007795 chemical reaction product Substances 0.000 claims description 4
- 150000002815 nickel Chemical class 0.000 claims description 4
- 239000012266 salt solution Substances 0.000 claims description 4
- 150000003609 titanium compounds Chemical class 0.000 claims description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 4
- 238000001816 cooling Methods 0.000 claims description 3
- 239000008367 deionised water Substances 0.000 claims description 3
- 229910021641 deionized water Inorganic materials 0.000 claims description 3
- 238000005406 washing Methods 0.000 claims description 3
- 230000008569 process Effects 0.000 claims description 2
- 239000000376 reactant Substances 0.000 claims description 2
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- 235000011187 glycerol Nutrition 0.000 claims 2
- 230000000052 comparative effect Effects 0.000 description 10
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- 230000015556 catabolic process Effects 0.000 description 3
- 238000006731 degradation reaction Methods 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 238000005286 illumination Methods 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N nitrogen Substances N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 3
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 229910052757 nitrogen Inorganic materials 0.000 description 2
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- 238000007146 photocatalysis Methods 0.000 description 2
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- -1 polytetrafluoroethylene Polymers 0.000 description 2
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- 239000011148 porous material Substances 0.000 description 2
- 238000000985 reflectance spectrum Methods 0.000 description 2
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- 238000001878 scanning electron micrograph Methods 0.000 description 2
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- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000002114 nanocomposite Substances 0.000 description 1
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen(.) Chemical compound [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
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Images
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
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
- B01J23/74—Iron group metals
- B01J23/755—Nickel
-
- 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
-
- B01J35/39—
-
- 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
- C02F2305/00—Use of specific compounds during water treatment
- C02F2305/10—Photocatalysts
Abstract
The invention discloses a method for preparing Ni-doped TiO by using cut tobacco stems as a template2A method of photocatalytic material comprising the steps of: (1) soaking the cut tobacco stems with glutaraldehyde, hydrochloric acid, ethanol solution and nickel nitrate solution respectively; (2) mixing tetrabutyl titanate, isopropanol, glycerol and a tobacco stalk template for ultrasonic treatment; (3) reacting in an oven for a period of time; (4) calcining the obtained solid to obtain the Ni-doped TiO tobacco stalk template2A photocatalytic material. The invention also discloses the obtained Ni-doped TiO2Photocatalytic material and use thereofThe application of degrading rhodamine B.
Description
Technical Field
The invention belongs to the technical field of nano composite material preparation, and particularly relates to a method for preparing Ni-doped TiO by using tobacco stems as templates2A synthesis method and application of a photocatalytic material.
Background
With TiO2The semiconductor photocatalysis technology based on the solar energy has strong oxidation capability, can treat refractory toxic substances, is environment-friendly, mild in reaction condition, low in cost and free from secondary pollution, and has wide application prospect. Compared with the traditional preparation method, the biological template method can obtain a material with high-efficiency photocatalytic activity by utilizing a template with special optical properties or capable of efficiently utilizing light energy in the nature. How to further reduce TiO2The band gap of (1) is TiO to improve the utilization efficiency of sunlight2The core problem was studied.
The invention takes the tobacco stalk silk as the biological template to prepare Ni-doped TiO for the first time2Material, using the obtained Ni-doped TiO2The material can be used for carrying out photocatalytic degradation on rhodamine B under the condition of visible light, and shows excellent photocatalytic propertyCan be used.
Disclosure of Invention
The invention provides a method for preparing Ni-doped TiO by taking cut tobacco stems as a template2Method for preparing photocatalytic material and Ni-doped TiO prepared by same2Use of a photocatalytic material for the reduction of rhodamine B in visible light conditions.
The technical scheme of the invention is as follows:
the invention discloses a method for preparing Ni-doped TiO by taking cut tobacco stems as a template2A method of photocatalytic material, comprising the steps of:
(1) soaking the cut tobacco stems with glutaraldehyde, hydrochloric acid, ethanol solution with gradually increased concentration and nickel salt solution with certain concentration, and drying to obtain cut tobacco stem templates;
(2) adding a certain amount of titanium compound into isopropanol, uniformly mixing, adding a certain amount of glycerol, uniformly mixing, adding the treated tobacco stem silk template obtained in the step (1), and performing ultrasonic treatment for a period of time;
(3) reacting the reactant in the step (2) for a period of time under a sealed condition at a certain temperature, and then cooling to room temperature;
(4) separating the reaction product obtained in the step (3), washing the reaction product with deionized water and ethanol for several times respectively, drying the obtained solid, and calcining the dried solid at a certain temperature in an air atmosphere to obtain the Ni-doped TiO2Photocatalytic material (Ni-STIO)2)。
Preferably, the glutaraldehyde concentration used in step (1) is from 1 to 10% by weight, preferably 5% by weight; the hydrochloric acid concentration is 1 to 10% by weight, preferably 5% by weight; the ethanol concentration is respectively 30 wt%, 50 wt% and 90 wt%; the nickel salt solution is soluble, preferably nickel nitrate solution, and the molar ratio of Ni to Ti in the nickel nitrate solution is 0.25-0.75: 100.
Preferably, the titanium compound in the step (2) is tetrabutyl titanate, and the adding amount ratio of the tetrabutyl titanate, the isopropanol, the glycerol and the tobacco stalk template is (1-2) mL: 50 mL: 1-10 mL: 1-5 g; the ultrasonic time is 12-48 h.
Preferably, the reaction temperature of the step (3) is 100-180 ℃, and the reaction time is 12-48 h.
Preferably, the calcination temperature in step (4) is 300-600 ℃; the calcination time is 5-20 h.
The invention discloses Ni-doped TiO prepared by the method in a second aspect2A photocatalytic material.
The third aspect of the invention discloses the Ni-doped TiO2Use of a photocatalytic material for degrading rhodamine B.
The invention has the following advantages and effects:
1. using tobacco stalk filaments treated by nickel nitrate solution as a template to obtain Ni-doped TiO2A material. The doping of Ni can not only narrow the forbidden band width of the material and enhance the visible light response, but also increase the specific surface area of the material, and the material shows excellent photocatalytic activity under the condition of visible light. However, the higher the doping of Ni is, the better, and the better the rhodamine B degradation effect under the illumination condition is when the molar ratio of Ni to Ti is 0.50: 100.
2. Ni-STIO prepared by the invention2The photocatalytic material shows higher catalytic activity in the degradation of rhodamine B under visible light conditions. Ni-STIO prepared by the invention2The photocatalytic material also has wide application prospect in the fields of sewage treatment, environmental purification, solar energy conversion and utilization and the like.
3. The method starts from tobacco waste, namely cut tobacco stems, combines the characteristics of a biological template to prepare a photocatalytic material, utilizes the special appearance characteristics of the cut tobacco stems to copy the appearance of the cut tobacco stems, and regulates and controls the microstructure of the cut tobacco stems by a method of doping Ni in the material synthesis process to narrow the forbidden bandwidth of the material, so as to prepare the high-efficiency Ni-STIO2A photocatalytic material. The photocatalytic material is prepared by utilizing the tobacco stalk template, and corresponding theoretical basis and experimental evidence are provided for further exploring and constructing complex special inorganic structural materials.
Drawings
FIG. 1 shows the Ni-doped TiO tobacco stalk template prepared in example 12XRD pattern of photocatalytic material.
FIG. 2 shows the Ni-doped TiO tobacco stalk template prepared in example 12Scanning electron micrographs of photocatalytic material.
FIG. 3 shows the Ni-doped TiO tobacco stalk template prepared in example 12Transmission electron microscopy of photocatalytic material.
FIG. 4 shows the Ni-doped TiO tobacco stalk template prepared in example 12Nitrogen adsorption/desorption isotherms and pore size distribution curves of the photocatalytic material;
FIG. 5 shows the Ni-doped TiO tobacco stalk template prepared in example 12A graph of the ultraviolet-visible diffuse reflectance spectrum of the photocatalytic material;
FIG. 6 shows the Ni-doped TiO tobacco stalk template prepared in example 12Photocatalytic material 0.25Ni-STIO2(molar ratio of Ni to Ti in the material 0.25: 100), 0.5Ni-STIO2(molar ratio of Ni to Ti in the material 0.50: 100), 0.75Ni-STIO2(the molar ratio of Ni to Ti in the material is 0.75: 100); STIO obtained in comparative example 12(without Ni addition) TiO obtained in comparative example 22(smokeless stem silk template), and blank (no TiO)2) And (3) an activity comparison curve graph of degrading rhodamine B.
Detailed Description
The invention is described in detail below with reference to some specific embodiments. These examples are intended to illustrate the invention only and are not intended to limit the scope of the invention. The embodiments in the examples are merely preferred embodiments, but the present invention is not limited to the preferred embodiments.
Example 1: ni-doped TiO with cut tobacco stem template2The photocatalytic material comprises the following steps:
(1) soaking tobacco stem shreds with 5 wt% of glutaraldehyde and 5 wt% of HCl respectively, then sequentially soaking tobacco stem shreds with 30 wt%, 50 wt% and 90 wt% of ethanol solution, and drying; soaking 2g of tobacco stem shreds in 20mL of water to obtain a solution with a concentration of 0.875 × 10-3mol·L-1、1.750×10-3mol·L-1And 2.625 × 10-3mol·L-1Soaking in nickel nitrate solution for 24 hr and stoving.
(2) Respectively adding 50mL of isopropanol, 1.2mL of tetrabutyl titanate and 10mL of glycerol into a 100mL of polytetrafluoroethylene reaction kettle, uniformly stirring at room temperature, adding 2g of the cut tobacco stem template treated in the step (1), performing ultrasonic treatment for 30min, and standing for 24 h.
(3) And (3) putting the polytetrafluoroethylene reaction kettle into a stainless steel cylinder, sealing, putting into an oven, carrying out solvothermal reaction at 180 ℃ for 24 hours, and then cooling to room temperature.
(4) Filtering the product with a Buchner funnel, washing with deionized water and ethanol for 3 times respectively, drying at 60 ℃, putting into a muffle furnace, heating to 450 ℃ at a heating rate of 2 ℃/min, and calcining for 10h in an air atmosphere to obtain the tobacco stem shred template Ni-doped TiO2Material named Ni-STIO2(ii) a Is named as 0.25Ni-STIO according to different concentrations of nickel nitrate solution2，0.5Ni-STiO2，0.75Ni-STiO2TiO2Wherein S represents cut tobacco stems, 0.25Ni, 0.5Ni and 0.75Ni represent molar ratios of Ni to Ti in the material of 0.25: 100, 0.50: 100 and 0.75: 100.
FIG. 1-FIG. 5 show the obtained Ni-STIO with cut tobacco stems as the template2Characterization results of the photocatalytic material. From the XRD pattern of FIG. 1, it can be seen that the obtained Ni-STIO with cut tobacco stems template2The photocatalytic materials are all anatase phase TiO2. As can be seen from the scanning electron micrograph of FIG. 2 and the transmission electron micrograph of FIG. 3, the obtained Ni-STIO with cut tobacco stems as a template2The photocatalysis material well copies the plant tissue morphology of the tobacco stems, the sample is rougher after being doped with Ni, and the surface of the sample consists of a plurality of linear particles. As can be seen from the nitrogen adsorption/desorption isotherms and pore size distribution curves of FIG. 4 (in FIG. 4), the resulting Ni-STIO2The photocatalytic material has a mesoporous structure resulting from particle packing. As can be seen from the UV-visible diffuse reflectance spectrum curve of FIG. 5, the obtained Ni-STIO2Photocatalytic materials exhibit a degree of light absorption in the visible region.
Comparative example 1: TiO without Ni addition2Preparation of photocatalytic Material
The preparation method is the same as example 1, except that the nickel nitrate solution is not used for soaking in the step (1). To obtain TiO2Photocatalytic material, named STIO2。
Comparative example 2: TiO with no added cut tobacco stems as template2Preparation of photocatalytic Material
The preparation method is the same as example 1, except that no cut tobacco stem template is added in the step (2). To obtain TiO2Photocatalytic material, named TiO2。
0.25Ni-STIO obtained in example 12，0.5Ni-STiO2，0.75Ni-STiO2STIO obtained in comparative example 12TiO obtained in comparative example 22And the result of the experiment for photocatalytic degradation of rhodamine B in the blank is shown in FIG. 6. As can be seen from FIG. 6, the blank sample cannot degrade rhodamine B under illumination; example 1, comparative example 1 and comparative example 22The material can degrade rhodamine B under the illumination condition, but the degradation performance of the rhodamine B is different, and the Ni-STIO obtained in example 12The performance of degrading rhodamine B is best, wherein 0.5Ni-STIO2Preferably; STIO obtained in comparative example 12The performance of degrading rhodamine B is better than that of the TiO obtained in comparative example 22Degrading the performance of rhodamine B.
The principal features of the invention and advantages of the invention have been shown and described above. It will be understood by those skilled in the art that the present invention is not limited to the embodiments described above, which are merely preferred examples of the present invention, but various changes and modifications may be made without departing from the spirit and scope of the present invention, which fall within the scope of the claimed invention.
Claims (7)
1. Ni-doped TiO prepared by taking cut tobacco stems as template2A method of photocatalytic material, comprising the steps of:
(1) soaking cut tobacco stems with glutaraldehyde, hydrochloric acid, ethanol solution with gradually increased concentration and nickel salt solution with certain concentration, and drying to obtain cut tobacco stem templates;
(2) adding a certain amount of titanium compound into isopropanol, uniformly mixing, adding a certain amount of glycerol, uniformly mixing, adding the treated tobacco stem silk template obtained in the step (1), and performing ultrasonic treatment for a period of time;
(3) reacting the reactant in the step (2) for a period of time under a sealed condition at a certain temperature, and then cooling to room temperature;
(4) separating the reaction product obtained in the step (3), washing the reaction product with deionized water and ethanol for several times respectively, drying the obtained solid, and calcining the dried solid at a certain temperature in an air atmosphere to obtain the Ni-doped TiO2A photocatalytic material.
2. The method of claim 1, wherein the glutaraldehyde concentration used in step (1) is 1-10 wt.%; the concentration of hydrochloric acid is 1-10 wt%; the ethanol concentration is respectively 30 wt%, 50 wt% and 90 wt%; the nickel salt solution is nickel nitrate solution, and the molar ratio of Ni to Ti in the nickel nitrate solution is 0.25-0.75: 100.
3. The method of claim 1, wherein the titanium compound of step (2) is tetrabutyl titanate, and the tetrabutyl titanate, isopropanol, glycerin and tobacco stem template are added in a ratio of (1-2) mL: 50 mL: (1-10) mL: 1-5 g; the ultrasonic time is 12-48 h.
4. The method as claimed in claim 1, wherein the reaction temperature in step (3) is 100-180 ℃ and the reaction time is 12-48 h.
5. The method as claimed in claim 1, wherein the calcination temperature in step (4) is 300-600 ℃; the calcination time is 5-20 h.
6. Ni-doped TiO prepared according to the process of any one of claims 1 to 52A photocatalytic material.
7. The Ni-doped TiO of claim 62Use of a photocatalytic material for degrading rhodamine B.
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|---|---|---|---|---|
| CN101249952A (en) * | 2008-03-27 | 2008-08-27 | 上海交通大学 | Method for preparing self-doping nitrogen grading porous oxide by using biomass template |
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| US20180345264A1 (en) * | 2015-09-23 | 2018-12-06 | University Of Ulsan Foundation For Industry Cooperation | Photocatalyst having high visible-light activity |
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| CN113304739A (en) * | 2021-05-12 | 2021-08-27 | 云南中烟工业有限责任公司 | Method for preparing TiO by taking cut tobacco stems as template2Method and use of photocatalytic materials |
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- 2022-01-13 CN CN202210039162.0A patent/CN114367275A/en active Pending
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| CN101249952A (en) * | 2008-03-27 | 2008-08-27 | 上海交通大学 | Method for preparing self-doping nitrogen grading porous oxide by using biomass template |
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| CN113304739A (en) * | 2021-05-12 | 2021-08-27 | 云南中烟工业有限责任公司 | Method for preparing TiO by taking cut tobacco stems as template2Method and use of photocatalytic materials |
Non-Patent Citations (2)
| Title |
|---|
| ROBERTO POL ET AL.: "Ni-, Pt- and (Ni/Pt)-doped TiO2 nanophotocatalysts: A smart approach for sustainable degradation of Rhodamine B dye", 《APPLIED CATALYSIS B: ENVIRONMENTAL》, vol. 181, pages 270 - 278 * |
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