CN113663664A - RuTe2/B-TiO2Preparation method of material and application of material in photocatalytic degradation of antibiotics - Google Patents

RuTe2/B-TiO2Preparation method of material and application of material in photocatalytic degradation of antibiotics Download PDF

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CN113663664A
CN113663664A CN202110911361.1A CN202110911361A CN113663664A CN 113663664 A CN113663664 A CN 113663664A CN 202110911361 A CN202110911361 A CN 202110911361A CN 113663664 A CN113663664 A CN 113663664A
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CN113663664B (en
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马江权
强成宏
李楠
李正萍
郭志敏
詹伟
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Changzhou University
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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
    • 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
    • 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
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    • B—PERFORMING OPERATIONS; TRANSPORTING
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    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
    • B01J27/02—Sulfur, selenium or tellurium; Compounds thereof
    • B01J27/057—Selenium or tellurium; Compounds thereof
    • B01J27/0576—Tellurium; Compounds thereof
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    • B01J35/00—Catalysts, in general, characterised by their form or physical properties
    • B01J35/60—Catalysts, in general, characterised by their form or physical properties characterised by their surface properties or porosity
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
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    • C02F1/00—Treatment of water, waste water, or sewage
    • C02F1/30—Treatment of water, waste water, or sewage by irradiation
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    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2101/00—Nature of the contaminant
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    • C02F2101/34—Organic compounds containing oxygen
    • C02F2101/345—Phenols
    • 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
    • C02F2101/36—Organic compounds containing halogen
    • 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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Abstract

The invention belongs to the field of photocatalysis, and particularly relates to RuTe2/B‑TiO2A preparation method of the material and application of the material in photocatalytic degradation of antibiotics. Firstly preparing black titanium by a sol-gel method, and then carrying out microwave method on RuTe2Synthesized and loaded on the surface of black titanium to prepare RuTe2/B‑TiO2The material is applied to photocatalytic degradation of antibiotics. RuTe loaded by the method of the invention2Efficient transfer of B-TiO as electron storage sites2The generated photogenerated electrons prevent the recombination of the photogenerated electrons and holes, and the nano-bulk B-TiO is added2Becomes loose and porous, changes the structure thereof, and has the specific surface area of 45.6m2Increase in g to 56.5m2/g, thereby increasing B-TiO2The photocatalytic degradation efficiency of the material is greatly improved2The photocatalysis capability is beneficial to realizing the utilization of clean energy sunlight.

Description

RuTe2/B-TiO2Preparation method of material and application of material in photocatalytic degradation of antibiotics
Technical Field
The invention belongs to the technical field of photocatalysis, and particularly relates to RuTe2/B-TiO2A preparation method of the material and application of the material in photocatalytic degradation of antibiotics.
Background
Over the last 30 years, a number of pharmaceutically active compounds (PhAC) have been reported as environmental pollutants, including antibiotics, analgesics, antiseptics, and other commonly used drug groups. One of the most commonly detected PhACs contains Diclofenac (DCF) (2- [ (2, 6-dichlorophenyl) amino group in sewage, sludge, surface water, ground water and even drinking water]Phenyl 4 acetic acid), a commonly used non-steroidal anti-inflammatory drug. DCF is believed to be due to the constant loading of the drug in water, mainly from sewage from municipal sewage treatment plants, at concentrations usually in pg L-1To ng L-1And thus pseudo-persistent, because of the rather persistent background concentration present in the environment.
The photocatalysis method has the advantages of mild reaction conditions, simple and convenient operation, less secondary pollution, no selectivity to pollutants and the like, is generally applied to the treatment of organic pollutants, and is an important advanced oxidation technology. TiO 22Is a commonly used photocatalyst, but TiO2The photocatalytic activity of the diclofenac sodium antibiotic substance is not high. It is reported that TiO is used2When the photocatalyst is used for carrying out photocatalytic degradation on diclofenac sodium substances, the general photocatalytic activity is shown, but the overall activity of the diclofenac sodium substances still needs to be improved.
Under the condition of illumination, B-TiO2The material is excited to generate electron-hole pairs, and the hole and the electron are respectively adsorbed on the B-TiO2The organic matter on the surface undergoes redox reaction, but the recombination efficiency of electron-hole pairs is high, so thatIt cannot effectively react with organic substances, thereby reducing photocatalytic efficiency. Therefore, the recombination of photogenerated electrons and holes is slowed down, and the B-TiO is improved2The photocatalytic activity of (A) has become the first thing of research.
Disclosure of Invention
The invention aims to provide a novel RuTe2/B-TiO2The preparation method of the material and the application of the photocatalytic degradation antibiotic DCF thereof adopt a microwave method to prepare a novel composite material photocatalyst, and the DCF photocatalytic degradation is realized under the irradiation of simulated sunlight of a xenon lamp. The aim of removing the antibiotic DCF in the medical wastewater is achieved. The application aims to prepare a novel composite material and can realize the efficient degradation of the antibiotic DCF under mild conditions.
RuTe2/B-TiO2The preparation method of the material comprises the following steps: mixing 29.14mg of sodium tellurite and 1.8-9g B-TiO2Adding powder and ethylene glycol into a beaker, stirring for 30 minutes, adding 781.5 μ L of ruthenium trichloride aqueous solution (concentration: 19.4mg/ml), stirring for 30 minutes until a suspension is formed, radiating the suspension with a microwave reactor, filtering with ultrapure water, drying in a vacuum box at 60 ℃ overnight, putting the suspension into a crucible, and putting the crucible in a tube furnace with N2Heating in atmosphere, keeping the temperature, and naturally cooling to room temperature to obtain RuTe2/B-TiO2A material.
Wherein the microwave radiation power is 600-800W, and the microwave radiation time is 1-3 minutes.
The heating temperature of the tubular furnace is 300-500 ℃, and the heat preservation time is 2 hours.
RuTe2/B-TiO2RuTe in the Material2Is 0.2 to 1 percent.
RuTe prepared by the method2/B-TiO2The material is used for photocatalytic degradation of antibiotics. The application method comprises the following steps: weighing RuTe2/B-TiO2Pouring the materials into a cylindrical glass reaction container with cooling circulation, adding 60mL of prepared antibiotic diclofenac sodium (DCF) solution, adjusting the pH value, performing dark reaction to enable the solution to reach adsorption balance, and performing reaction under sunlight.
Wherein the content of the first and second substances,RuTe2/B-TiO2the material dosage is 10-80 mg; the concentration of the DCF solution is 10-40 mg/L.
Adjusting the pH value to 3-9.1; dark reaction time is 30 min; the light reaction time is 2h under a xenon lamp with the sunlight of 250W.
The invention has the following advantages:
(1) firstly, the electrocatalytic material RuTe2Applied to photocatalysis because of narrow band gap and supported B-TiO2Then, the band gap of the photocatalyst is extended to a visible light region, so that the response range of light is enlarged, and the photocatalytic activity is improved.
(2) Microwave method for mixing RuTe2Load changes B-TiO2The structure of (2) makes it become more loose and porous, has increased its specific surface area, has strengthened adsorptivity, has improved the photocatalytic property.
Description of the drawings:
FIG. 1B-TiO in example 12And RuTe in example 22And 400 deg.C-0.5% RuTe in example 52/B-TiO2XRD pattern of the catalyst.
FIG. 2 shows B-TiO in example 12The scanning electron microscope of (1).
FIG. 3 shows RuTe in example 22The scanning electron microscope of (1).
FIG. 4 is 0.5% RuTe in example 32/B-TiO2The scanning electron microscope of (1).
FIG. 5 shows B-TiO in example 12And 0.5% RuTe in example 32/B-TiO2Nitrogen adsorption desorption profile (pore size distribution).
FIG. 6 RuTe in example 32/B-TiO2Graph of efficiency of DCF degradation at different load ratios
FIG. 7 RuTe in example 32/B-TiO2Dynamic fit plots of different load ratios degrading DCF.
FIG. 8 0.5% RuTe in example 42/B-TiO2Graph of the rate of DCF degradation at different calcination temperatures.
FIG. 9 0.5% RuTe in example 52/B-TiO2Graph of the rate at which different amounts of catalyst degrade DCF.
FIG. 10 0.5% RuTe in example 62/B-TiO2Degradation rate of the catalyst in different DCF concentrations is plotted.
FIG. 11 0.5% RuTe in example 72/B-TiO2Graph of catalyst degradation rate in DCF solutions at different pH values.
Figure 12 graph of efficiency of addition of different capture agents to degraded DCF in example 8.
FIG. 13 graph of stability-affecting efficiency of the repeat experiment in example 9.
Detailed Description
The present invention will be described in detail with reference to specific examples.
The degradation efficiency and rate are calculated according to the following formula:
R＝(C-C0)/C0*100％；V＝ln{C0/(C-C0)}
r is degradation efficiency; v: rate of degradation
C0Initial concentration
C, concentration after degradation reaction.
Example 1
Sol-gel method for preparing B-TiO2: taking two beakers, adding 300mL of ethanol and 100mL of tetrabutyl titanate into one beaker, stirring for 30 minutes, and marking a solution A; another beaker was taken and added with 40mL of glacial acetic acid, 40mL of water and 100mL of ethanol, and the solution B was marked. The solution B was slowly added to the solution A after stirring for 30 minutes and stirring was continued until a gel was formed. It was then aged in a fume hood for 12 hours. Putting the aged gel into a 120 ℃ oven until light yellow particles are formed, taking out and grinding the gel, taking out a part of the gel, pouring the part of the gel into a crucible, putting the crucible into a tube furnace, and introducing N2Keeping the heating rate of 5 ℃/min, heating to 500 ℃ and keeping for 3 hours, naturally cooling to room temperature to obtain B-TiO2。
Example 2
Synthesis of RuTe by microwave method2: adding 29.14mg of sodium tellurite and 50mL of ethylene glycol into a beaker, stirring for 30 minutes, adding 781.5 mu L of ruthenium trichloride aqueous solution (concentration: 19.4mg/mL), and stirringStirring for 30min until a suspension is formed, then irradiating the suspension with a microwave reactor 800W for 3 min, filtering with ultrapure water, placing in a vacuum box, drying overnight at 60 ℃, placing in a crucible, and placing in a tube furnace N2Heating to 400 deg.C at a heating rate of 2.5 deg.C/min in atmosphere, maintaining for 2 hr, naturally cooling to room temperature to obtain RuTe2。
Example 3
Synthesis of RuTe by microwave method2/B-TiO2: adding 29.14mg of sodium tellurite and B-TiO into a beaker2Powder, specifically 1.8g, 3.6g, 9g RuTe2The supported amount of (1%) was 0.2%, 0.5%, 50mL of ethylene glycol, stirred for 30 minutes, 781.5. mu.L of an aqueous solution of ruthenium trichloride (concentration: 19.4mg/mL) was further added, stirred for 30 minutes until a suspension was formed, the suspension was irradiated with 800W of a microwave reactor for 3 minutes, filtered with ultrapure water, placed in a vacuum box at 60 ℃ for overnight drying, placed in a crucible, and placed in a tube furnace with N in a N tube furnace2Heating at 400 deg.C at a heating rate of 2.5 deg.C/min in atmosphere for 2 hr, and naturally cooling to room temperature.
Weighing catalyst RuTe2/B-TiO220mg of the solution is poured into a cylindrical glass reaction vessel with a cooling cycle, 60mL of the prepared 20mg/L DCF solution is added, the pH value is adjusted to 7, and the reaction is performed in a dark environment for 30 minutes to reach the adsorption equilibrium. And starting a 250W xenon lamp to react for 2h under sunlight, sampling every 20 minutes, and carrying out liquid phase detection. The results are as follows:
load ratio 0.2％RuTe2/B-TiO2 0.5％RuTe2/B-TiO 2 1％RuTe2/B-TiO2
Efficiency of degradation 88.6％ 95.2％ 88.9％
Example 4
The best load ratio of 0.5% RuTe in example 32/B-TiO2Adding 29.14mg of sodium tellurite and 3.6g B-TiO into a beaker2The powder, 50mL of ethylene glycol, was stirred for 30 minutes, 781.5. mu.L of an aqueous ruthenium trichloride solution (concentration: 19.4mg/mL) was added thereto, and further stirred for 30 minutes until a suspension was formed, and then the suspension was irradiated with 800W of a microwave reactor for 3 minutes, filtered with ultrapure water, dried in a vacuum oven at 60 ℃ overnight, and then put into a crucible, and N was added in a tube furnace2Heating at a heating rate of 2.5 ℃/min at 300-500 ℃ for 2 hours in the atmosphere, naturally cooling to room temperature, and finally obtaining 0.5 percent of RuTe at different calcination temperatures2/B-TiO2。
20mg of the catalyst is weighed respectively and poured into a cylindrical glass reaction vessel with a cooling cycle, 60mL of the prepared 20mg/L DCF solution is added, the pH value is adjusted to 7, and the reaction is carried out in a dark environment for 30 minutes to reach the adsorption equilibrium. And starting a 250W xenon lamp to react for 2h under sunlight, sampling every 20 minutes, and carrying out liquid phase detection. The results are as follows:
calcination temperature 300℃ 400℃ 500℃
Efficiency of degradation 86.8％ 95.2％ 83％
Example 5
The best load ratio of 0.5% RuTe in example 32/B-TiO2And the best calcination temperature in example 4 is 400 ℃, 10mg, 20mg, 40mg and 80mg of the catalyst are weighed respectively and poured into a cylindrical glass reaction vessel with a cooling circulation, 60mL of DCF solution with the concentration of 20mg/L is added, the pH value is adjusted to 7, and the mixture is dark and reacted for 30 minutes to reach the adsorption equilibrium. And starting a 250W xenon lamp to react for 2 hours under the sunlight, sampling every 30 minutes, and carrying out liquid phase detection. The results are as follows:
amount of catalyst 10mg 20mg 40mg 80mg
Efficiency of degradation 79.7％ 95.2％ 91.8％ 76.2％
Example 6
The best load ratio of 0.5% RuTe in example 32/B-TiO2Weighing 20mg, pouring into a cylindrical glass reaction container with a cooling cycle, adding 60mL of DCF solution with different concentrations of 10mg/L, 20mg/L, 30mg/L and 40mg/L, adjusting the pH value to 7, and carrying out dark reaction for 30 minutes to ensure that the solution reaches adsorption equilibrium. And starting a 250W xenon lamp to react for 2 hours under the sunlight, sampling every 30 minutes, and carrying out liquid phase detection. The results are as follows:
DCF concentration 10mg/L 20mg/L 30mg/L 40mg/L
Efficiency of degradation 98.1％ 95.2％ 91.2％ 83.7％
Example 7
The best load ratio of 0.5% RuTe in example 32/B-TiO2Weighing 20mg, pouring into a cylindrical glass reaction container with a cooling circulation, and adding 20mg/L60mL of the DCF solution, adjusting the pH to 3.1, 5.3, 7.2 and 9.1 respectively, and carrying out dark reaction for 30 minutes to allow the solution to reach adsorption equilibrium. And starting a 250W xenon lamp to react for 2 hours under the sunlight, sampling every 30 minutes, and carrying out liquid phase detection. As a result, the degradation efficiency was 83.5% at pH 3.1, 90% at pH 5.3, 95.2% at pH 7.2, and 85.6% at pH 9.1.
pH 3.1 5.3 7.2 9.1
Efficiency of degradation 83.5％ 90％ 95.2％ 85.6％
Example 8
The best load ratio of 0.5% RuTe in example 32/B-TiO2Weighing 20mg, pouring into a cylindrical glass reaction container with a cooling cycle, adding 60mL of 20mg/L DCF solution and 0.18g of p-benzoquinone, 100 mu L of isopropanol and 0.33g of ethylene diamine tetraacetic acid as capture agents respectively, adjusting the pH value to 7, and carrying out dark reaction for 30 minutes to ensure that the adsorption equilibrium is achieved. And starting a 250W xenon lamp to react for 2 hours under the sunlight, sampling every 30 minutes, and carrying out liquid phase detection. The results are as follows:
capture agent Isopropanol (I-propanol) Ethylenediaminetetraacetic acid P-benzoquinone
Efficiency of degradation 94.6％ 94.8％ 50.3％
Example 9
The best load ratio of 0.5% RuTe in example 42/B-TiO220mg of the solution is weighed and poured into a cylindrical glass reaction vessel with a cooling cycle, 60mL of the prepared 20mg/L DCF solution is added, the pH value is adjusted to 7, and the reaction is firstly carried out in a dark environment for 30 minutes to reach the adsorption equilibrium. And starting a 250W xenon lamp to react for 2 hours under the sunlight, sampling every 30 minutes, and carrying out liquid phase detection. The catalyst after each measurement is centrifugally washed, dried and repeated for 5 times to perform a stability test, and the results are as follows:
number of times 1 2 3 4 5
Efficiency of degradation 95.2％ 92.8％ 91.1％ 92％ 92.9％
Comparative example 1
Weighing 20mg of B-TiO2The powder was poured into a glass reaction vessel with a cooling cycle, 60mL of a 20mg/L DCF solution was added, the pH was adjusted to 7, and the mixture was allowed to react in the dark for 30 minutes to reach adsorption equilibrium. And starting a 250W xenon lamp to react for 2h under sunlight, sampling every 20 minutes, and carrying out liquid phase detection. As a result, B-TiO2The degradation efficiency of (2) was 80%.
TABLE 1
Figure BDA0003203737200000081
Comparative example 2
Hydrothermal synthesis of RuTe2: adding 29.14mg of sodium tellurite and 50mL of ethylene glycol into a high-pressure hydrothermal kettle, stirring for 30 minutes, adding 781.5 mu L of ruthenium trichloride aqueous solution (the concentration: 19.4mg/mL), reacting at 180 ℃ for 12 hours, naturally cooling to room temperature, finding that no black precipitate is generated in the ruthenium trichloride aqueous solution, and continuously trying for different reaction times for 18 hours, 24 hours and 36 hours to obtain black RuTe2。

Claims (9)

1. RuTe2/B-TiO2Material, characterized in that said RuTe2/B-TiO2RuTe in the Material2The mass ratio of the load is 0.2-1%.
2. RuTe2/B-TiO2The preparation method of the material is characterized by comprising the following steps: sodium tellurite, B-TiO2Adding powder and ethylene glycol into a beaker, stirring for 30 minutes, adding aqueous solution of ruthenium trichloride, stirring for another 30 minutes until suspension is formed, radiating the suspension by using a microwave reactor, filtering by using ultrapure water, placing the suspension into a vacuum box, drying at 60 ℃ overnight, placing the suspension into a crucible, and placing the crucible in a tube furnace N2Heating in atmosphere, keeping the temperature, and naturally cooling to room temperature to obtain RuTe2/B-TiO2A material.
3. The RuTe of claim 22/B-TiO2The preparation method of the material is characterized in that 29.14mg of sodium tellurite and B-TiO are added21.8-9g of powder, 781.5 μ L of aqueous solution of ruthenium trichloride, concentration of aqueous solution of ruthenium trichloride: 19.4 mg/ml.
4. The RuTe of claim 22/B-TiO2The preparation method of the material is characterized in that the microwave radiation power is 600-800W, and the microwave radiation time is 1-3 minutes.
5. The RuTe of claim 22/B-TiO2The preparation method of the material is characterized in that the heating temperature of the tubular furnace is 300-500 ℃, and the heat preservation time is 2 hours.
6. A RuTe according to claim 12/B-TiO2Use of a material, characterized in that said RuTe2/B-TiO2The material is used for photocatalytic degradation of antibiotics.
7. The RuTe of claim 62/B-TiO2The application of the material is characterized in that the application method comprises the following steps: weighing RuTe2/B-TiO2Pouring the materials into a cylindrical glass reaction container with cooling circulation, adding 60mL of prepared antibiotic diclofenac sodium (DCF) solution, adjusting the pH value, performing dark reaction to enable the solution to reach adsorption balance, and performing reaction under sunlight.
8. The RuTe of claim 72/B-TiO2Use of a material, characterized in that said RuTe2/B-TiO2The material dosage is 10-80 mg; the concentration of the DCF solution is 10-40 mg/L.
9. The RuTe of claim 72/B-TiO2The application of the material is characterized in that the pH value is adjusted to 3-9.1; dark reaction time is 30 min; the light reaction time is 2h under a xenon lamp with the sunlight of 250W.
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