CN109985613B - Preparation method and application of walnut shell organic carbon-doped titanium dioxide photocatalyst - Google Patents
Preparation method and application of walnut shell organic carbon-doped titanium dioxide photocatalyst Download PDFInfo
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- 239000011941 photocatalyst Substances 0.000 title claims abstract description 48
- 239000004408 titanium dioxide Substances 0.000 title claims abstract description 48
- 238000002360 preparation method Methods 0.000 title claims abstract description 14
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- 229910052799 carbon Inorganic materials 0.000 claims description 13
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- 239000000243 solution Substances 0.000 description 20
- XHCCWBJFZUXJBV-UHFFFAOYSA-K trisodium 2-[(2-oxido-5-sulfophenyl)diazenyl]-3,6-disulfonaphthalene-1,8-diolate Chemical compound C1=CC(=C(C=C1S(=O)(=O)O)N=NC2=C(C3=C(C=C(C=C3C=C2S(=O)(=O)O)S(=O)(=O)O)[O-])[O-])[O-].[Na+].[Na+].[Na+] XHCCWBJFZUXJBV-UHFFFAOYSA-K 0.000 description 10
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- QBZIEGUIYWGBMY-FUZXWUMZSA-N (5Z)-5-hydroxyimino-6-oxonaphthalene-2-sulfonic acid iron Chemical compound [Fe].O\N=C1/C(=O)C=Cc2cc(ccc12)S(O)(=O)=O.O\N=C1/C(=O)C=Cc2cc(ccc12)S(O)(=O)=O.O\N=C1/C(=O)C=Cc2cc(ccc12)S(O)(=O)=O QBZIEGUIYWGBMY-FUZXWUMZSA-N 0.000 description 3
- RGCKGOZRHPZPFP-UHFFFAOYSA-N alizarin Chemical compound C1=CC=C2C(=O)C3=C(O)C(O)=CC=C3C(=O)C2=C1 RGCKGOZRHPZPFP-UHFFFAOYSA-N 0.000 description 3
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- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
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- RLJMLMKIBZAXJO-UHFFFAOYSA-N lead(II) nitrate Inorganic materials [O-][N+](=O)O[Pb]O[N+]([O-])=O RLJMLMKIBZAXJO-UHFFFAOYSA-N 0.000 description 1
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- 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
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- 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
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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
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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
- C02F2101/308—Dyes; Colorants; Fluorescent agents
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Abstract
The invention relates to the technical field of visible light catalysts, in particular to a preparation method and application of a walnut shell organic carbon-doped titanium dioxide photocatalyst; the method comprises the following steps: a. dissolving titanium dioxide; b. adsorbing walnut shells and drying; c. carbonizing; TiO22The walnut shell organic carbon and lead oxide are doped, so that multiple wave-absorbing advantages are combined, and the transmissivity can reach 90.3%; the combined new photocatalyst has good reaction activity, greatly improves the utilization rate of sunlight, greatly improves the catalytic efficiency, can be recycled and has considerable application prospect.
Description
Technical Field
The invention relates to the technical field of visible light catalysts, in particular to a preparation method and application of a walnut shell organic carbon-doped titanium dioxide photocatalyst.
Background
As one of the technologies developed in recent decades and having a wide research prospect, photocatalysts have achieved great achievements in the aspects of environmental improvement and new energy development. Extensive research is carried out on the aspects of preparation, modification and the like of the photocatalyst, and the defects in the research process are continuously made up. In recent years, photocatalysts have been applied to environmental treatment for decomposing pollutants, organic pollutants and the like in water. At present, rivers and lakes in China are seriously polluted, and most pollution sources come from industrial wastewater and domestic sewage.
TiO2 is a photocatalyst, has high dye catalysis efficiency, stable chemical property, relatively mild reaction condition, no harm to human body, is very effective in degrading organic pollutants in water, has incomparable advantages of other traditional water treatment processes, and has wide application prospect. But also has disadvantages. Such as a wide forbidden band and low utilization efficiency of sunlight.
Agricultural and forestry waste resources in China are rich, byproducts of food processing such as shells and skins are buried as garbage, and wood chips, sawdust and the like generated by processing forestry products are directly discarded, so that the environment is polluted and the resources are seriously wasted. Walnut is a woody oil plant, which is planted in large areas in many areas of our country. The walnuts are sold as dry fruits before, and are directly discarded after being eaten, so that shells of the walnuts are difficult to recover. At present, the walnut is deeply processed in the food processing industry, although the processing by-product walnut shells can be systematically recycled, most of the walnut shells are still burnt or discarded, and the resource waste and the environmental pollution are caused. The main components of the walnut shell are lignin, cellulose and hemicellulose, and the walnut shell is a carbon-containing substance with higher fixed carbon and volatile content and less ash content.
Disclosure of Invention
The invention aims to solve the problem of TiO2As a photocatalyst, the technical problems of low removal rate of dye organic matters, low photocatalytic efficiency and the like exist, and the preparation method and the application of the walnut shell organic matter carbon-doped titanium dioxide photocatalyst are provided.
In order to solve the technical problems, the technical scheme adopted by the invention is as follows: the preparation method of the walnut shell organic carbon doped titanium dioxide photocatalyst comprises the following steps:
a. dissolving titanium dioxide, weighing titanium dioxide, dissolving the titanium dioxide in NaOH solution with the mass concentration of 60%, heating and refluxing, standing after the reaction is stopped, and dissolving TiO in the NaOH solution2The solid is completely dissolved, and the solution becomes white;
b. b, adsorbing walnut shells, drying, crushing, pouring the walnut shells into the white solution obtained in the step a, and adding Pb (NO) with the mass concentration of 20%3)2Stirring and dipping the solution, fully adsorbing the solution by walnut shells, carrying out suction filtration and drying to obtain an earthy yellow solid;
c. and c, carbonizing, namely putting the solid of the khaki color obtained in the step b into a high-pressure kettle, putting the high-pressure kettle into a box type high-temperature furnace, setting the temperature at 500 ℃, reacting for 3 hours, cooling the reaction, taking out the solid, changing the solid from khaki color to black color, and grinding the black solid into powder to obtain the walnut shell organic carbon doped titanium dioxide photocatalyst.
Furthermore, the mass ratio of the titanium dioxide to the walnut shells is 1: 1-5.
Further, the mass ratio of the titanium dioxide to the walnut shells is 1: 2.
Preferably, the ratio of the mass of titanium dioxide used in step a to the volume of the 60% NaOH solution is 1g:10 ml.
Further, the mass concentration of the titanium dioxide used in the step a and the mass concentration of the titanium dioxide used in the step b are 20% of Pb (NO)3)2The volume ratio of the solution is 1g to 1-5 ml.
Preferably, the mass concentration of the titanium dioxide used in step a and the mass concentration of the titanium dioxide used in step b are 20% Pb (NO)3)2The volume ratio of the solution was 5g to 13 ml.
Further, the dissolution of titanium dioxide of step a was carried out in a three-necked flask and heated in a constant temperature magnetic stirrer at a reflux temperature of 100 ℃ under reflux for 4 hours.
The invention also aims to provide the application of the photocatalyst prepared by the preparation method of the walnut shell organic carbon-doped titanium dioxide photocatalyst in decomposing pollutants and organic pollutants in water.
Compared with the prior art, the invention has the following beneficial effects:
TiO2the walnut shell organic carbon and lead oxide are doped, multiple wave-absorbing advantages are combined, and the transmissivity can reach 90.3%. The combined novel photocatalyst has good reaction activity, greatly improves the utilization rate of sunlight, greatly improves the catalytic efficiency, can be recycled and has considerable application prospect. The band gap of the titanium dioxide is about 3.0eV, when the titanium dioxide is doped with walnut shell organic carbon, the light absorption wavelength of the titanium dioxide can be expanded to be within the visible light range, and the local structure of the titanium dioxide can be changed by adding PbO, so that electrons (e) which are excited to jump to a conduction band are generated (e)-) Fall back to the cavity (h)+) The time of (a) is prolonged. Such that electrons in the conduction band and vacancies in the valence bandThe cavity has sufficient time to react with some contaminants (organic compounds, dyes, cyclic hydrocarbons, aromatics, toxic gases, aldehydes, etc.) on the surface.
Drawings
FIG. 1 shows TiO in different proportions in example 12And the catalytic degradation rate of the new photocatalyst prepared from walnut shells is shown schematically.
FIG. 2 shows the amounts of Pb (NO) used in example 23)2The solution prepared shows the catalytic degradation rate of the new photocatalyst.
Detailed Description
The present invention is further illustrated by the following specific examples.
Preparing a colored dye:
weighing 25mg of acid chrome blue K indicator, naphthol green B, acid fuchsin biological coloring agent, crystal violet and alizarin red respectively, dissolving the materials in a beaker by using 100mL of distilled water respectively, pouring the materials into a 1000mL volumetric flask respectively, adding the distilled water to the scale mark, and shaking uniformly for later use.
Preparing a peach shell organic carbon-doped titanium dioxide photocatalyst:
a、TiO2by dissolving
A clean and dry 250mL three-neck flask was taken, 5g of titanium dioxide was added, 50mL of 60% NaOH solution was used as a solvent, and the mixture was heated in a constant temperature magnetic stirrer at a reflux temperature of 100 ℃ under reflux for 4 h. After the reaction was stopped, the reaction flask was cooled to room temperature, poured into a 250ml beaker, and allowed to stand.
Experimental phenomena: TiO22The solid was completely dissolved and the solution turned white.
b. Adsorption of walnut shell
A certain amount of dried and crushed walnut shells are poured into the solution obtained in the step a, and Pb (NO) with the mass concentration of 20 percent is added3)2Stirring the solution, fully mixing the walnut shells with the solution, and soaking for half an hour to ensure that the walnut shells fully adsorb the solution. And (5) carrying out suction filtration and drying to obtain a solid in the color of khaki.
c. Carbonizing
An autoclave was taken and 30g of step b were addedThe obtained pale yellow solid was then placed in an autoclave in a box-type high-temperature furnace, and the temperature was set at 500 ℃ for 3 hours. Cooling the reaction product, taking out the solid, grinding into powder to obtain new TiO2And (5) photocatalyst for standby.
The method for measuring the catalytic performance of the peach shell organic carbon-doped titanium dioxide photocatalyst comprises the following steps:
the prepared acid chrome blue K indicator is put into a quartz cuvette, and the transmissivity (T) and the absorbance (A) of the acid chrome blue K indicator before catalysis are respectively measured to be 21.3% and 0.643 respectively. 40mL of acid chrome blue K indicator is taken by a measuring cylinder and put into a beaker, and 1g of the novel TiO prepared by the invention is taken2Placing the photocatalyst into a beaker, irradiating for 30 minutes under an ultraviolet lamp with the wavelength of 365mm, further irradiating for 1 hour under sunlight, standing, filtering by folding filter paper with hands, placing the filtrate into a quartz cuvette, and measuring the absorbance A and the transmittance T by using an ultraviolet spectrophotometer. The degradation rate of the acid chrome blue K indicator is calculated according to the formula (2-1).
In the formula, A0Is the initial absorbance; a is the absorbance after catalysis.
In the following examples 1 to 4, the preparation of the colored dye, the preparation of the peach shell organic carbon-doped titanium dioxide photocatalyst, and the measurement of the catalytic performance of the peach shell organic carbon-doped titanium dioxide photocatalyst were carried out by the methods described above.
Example 1
TiO2Determining the optimum ratio of walnut shell
Pb (NO) concentration of 20%3)210mL of solution, investigating TiO2Ratio of walnut shell to TiO (1:1, 1:2, 1:3, 1:4, 1:5)2Influence of the catalytic efficiency of the photocatalyst. The data measured after catalysis are shown in table 1 and fig. 1.
TABLE 1 TiO2The proportion of the walnut shell
As can be seen from Table 1: when TiO is present2When the ratio of the photocatalyst to the walnut shell is 1:2, the catalytic efficiency of the prepared new photocatalyst is optimal.
Example 2
Pb(NO3)2Determination of the optimum amount of
Immobilising TiO2The ratio of the content of Pb to the walnut shell was 1:2, and Pb (NO) was observed at a concentration of 20%3)2The effect of the amount of (5mL, 10mL, 15mL, 20mL, 25mL) on the catalytic efficiency of the new photocatalyst. The data measured after catalysis are shown in table 2, fig. 2:
TABLE 2 Pb (NO)3)2Amount of (A) to be used
From the trend of the graph 2, it can be seen that when Pb (NO)3)2The dosage of (A) is between 10mL and 15mL with a tendency to rise first and then fall, so the optimal dosage is between 10mL and 15 mL. Thus changing Pb (NO)3)2The optimum amount is found. Table 3 is given:
TABLE 3 Pb (NO)3)2Amount of (A) to be used
As can be seen from Table 3: when 20% of Pb (NO)3)2The catalytic efficiency is best when the amount of (C) is 13 mL.
In summary, the following steps: when the carbonization temperature is 500 ℃, the carbonization time is 3h and 20 percent of Pb (NO)3)2The dosage of the composition is 13mL and TiO2At a ratio of 1:2 with respect to the corncob, TiO2Optimum catalytic efficiency TiO of photocatalyst2The photocatalyst has the best catalytic efficiency on the acid chrome blue K indicator, and the degradation efficiency is 93.4%.
Example 3
The new photocatalyst prepared under the optimal conditions is used for catalyzing different organic dyes.
The absorbance of a colored indicator such as 25mg/L acid fuchsin shown in Table 4 was measured, and the absorbance was measured by placing each of the colored indicators in 1g of a new photocatalyst prepared under the optimum conditions, irradiating the photocatalyst under an ultraviolet lamp having a wavelength of 365nm for 30 minutes, irradiating the photocatalyst under visible light for 60 minutes, and measuring the absorbance after decomposition, respectively, and the data are shown in Table 4:
TABLE 4
As can be seen from Table 4: the acid chrome blue K indicator aqueous solution is rose red, the wavelength of the acid chrome blue K indicator aqueous solution is 620-760 nm, the crystal violet indicator aqueous solution is purple, the wavelength of the crystal violet indicator aqueous solution is 350-455 nm, the acid fuchsin aqueous solution is red, the wavelength of the acid fuchsin aqueous solution is 620-750 nm, the color of alizarin red is pink when the pH value is 5, the wavelength of the alizarin red is 360-380 nm, the naphthol green B aqueous solution is green, and the wavelength of the naphthol green B aqueous solution is 492-577 nm. Therefore, the catalyst has the best catalytic efficiency on the colored indicator with the wavelength of 620-760 nm and the worst catalytic efficiency on the colored indicator with the wavelength of 490-580 nm.
Example 4
Comparative experiment
According to TiO aspect2The proportion of the walnut shell and the walnut shell is 1:2, the carbonization temperature is 500 ℃, the carbonization time is 3 hours, and 20 percent of Pb (NO) is not added3)2The solution is obtained to obtain a black carbonized product, namely the new photocatalyst. And detecting the degradation catalytic activity of the novel photocatalyst without lead oxide doping on the acid chrome blue K indicator solution. The transmittance T after the catalysis was 49.1% and the absorbance a was 0.309. The degradation rate was calculated to be 51.9%.
From the above, it can be seen that: in the degradation of the acid chrome blue K indicator solution, the degradation rate before doping with lead oxide is 51.9%, while the degradation rate after doping with lead oxide is improved to 93.4%, and the visible doped lead oxide can improve the catalytic efficiency of the new photocatalyst.
The above examples show that: when the carbonization temperature is 500 ℃, the carbonization time is 3h and 20 percent of Pb (NO)3)2The dosage of the medicine is 13mL,TiO2When the ratio of the titanium oxide to the walnut shell is 1:2, TiO2The photocatalyst has the best catalytic efficiency, the catalyst has the best catalytic efficiency on the colored indicator with the wavelength of 620-760 nm, and the catalytic efficiency of the novel photocatalyst can be effectively improved by doping lead oxide.
Claims (7)
1. A preparation method of a walnut shell organic carbon doped titanium dioxide photocatalyst is characterized by comprising the following steps:
a. dissolving titanium dioxide, weighing titanium dioxide, dissolving the titanium dioxide in NaOH solution with the mass concentration of 60%, heating and refluxing, standing after the reaction is stopped, and dissolving TiO in the NaOH solution2The solid is completely dissolved, and the solution becomes white; dissolving titanium dioxide in a three-neck flask, heating in a constant-temperature magnetic stirrer at 100 ℃, and heating and refluxing for 4 h;
b. b, adsorbing walnut shells, drying, crushing, pouring the walnut shells into the white solution obtained in the step a, and adding Pb (NO) with the mass concentration of 20%3)2Stirring and dipping the solution, fully adsorbing the solution by walnut shells, carrying out suction filtration and drying to obtain an earthy yellow solid;
c. and c, carbonizing, namely putting the solid of the khaki color obtained in the step b into a high-pressure kettle, putting the high-pressure kettle into a box type high-temperature furnace, setting the temperature at 500 ℃, reacting for 3 hours, cooling the reaction, taking out the solid, changing the solid from khaki color to black color, and grinding the black solid into powder to obtain the walnut shell organic carbon doped titanium dioxide photocatalyst.
2. The preparation method of the walnut shell organic carbon doped titanium dioxide photocatalyst according to claim 1, wherein the mass ratio of the titanium dioxide to the walnut shell is 1: 1-5.
3. The preparation method of the walnut shell organic carbon doped titanium dioxide photocatalyst according to claim 1 or 2, wherein the mass ratio of the titanium dioxide to the walnut shell is 1: 2.
4. The method for preparing the walnut shell organic carbon doped titanium dioxide photocatalyst according to claim 3, wherein the ratio of the mass of the titanium dioxide used in the step a to the volume of the NaOH solution with the mass concentration of 60% is 1g:10 ml.
5. The method for preparing the walnut shell organic carbon doped titanium dioxide photocatalyst according to claim 4, wherein the mass concentration of the titanium dioxide used in the step a and the mass concentration of the titanium dioxide used in the step b are 20% of Pb (NO)3)2The volume ratio of the solution is 1g to 1-5 ml.
6. The method for preparing the walnut shell organic carbon doped titanium dioxide photocatalyst as claimed in claim 5, wherein the mass concentration of the titanium dioxide used in the step a and the mass concentration of the titanium dioxide used in the step b are 20% of Pb (NO)3)2The volume ratio of the solution was 5g to 13 ml.
7. The application of the photocatalyst prepared by the preparation method of the walnut shell organic carbon doped titanium dioxide photocatalyst disclosed by claim 1 in decomposing pollutants and organic pollutants in water.
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|---|---|---|---|---|
| CN105148842A (en) * | 2015-09-07 | 2015-12-16 | 河北师范大学 | Preparing method of manganese oxide-charcoal composite adsorbent |
| CN105597724A (en) * | 2015-12-15 | 2016-05-25 | 浙江工业大学 | Method for preparing magnetic-biochar-supported photocatalyst |
| CN108097252A (en) * | 2018-01-03 | 2018-06-01 | 南京工业大学 | A kind of magnetic Fe3O4/ TiO2The preparation method of catalysis material |
Family Cites Families (2)
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| JP6367633B2 (en) * | 2014-07-22 | 2018-08-01 | 国立研究開発法人物質・材料研究機構 | α-PbO2 Type Crystalline TiO2 Fine Particle Manufacturing Method |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105148842A (en) * | 2015-09-07 | 2015-12-16 | 河北师范大学 | Preparing method of manganese oxide-charcoal composite adsorbent |
| CN105597724A (en) * | 2015-12-15 | 2016-05-25 | 浙江工业大学 | Method for preparing magnetic-biochar-supported photocatalyst |
| CN108097252A (en) * | 2018-01-03 | 2018-06-01 | 南京工业大学 | A kind of magnetic Fe3O4/ TiO2The preparation method of catalysis material |
Non-Patent Citations (1)
| Title |
|---|
| PbO-Modified TiO2 Thin Films: A Route to Visible Light Photocatalysts;Davinder S. Bhachu et al.;《Langmuir》;20131219;第30卷;第624-630页 * |
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