CN112756005A - Monoatomic Ag loaded nitrogen doped TiO2Catalyst, its preparation and use - Google Patents
Monoatomic Ag loaded nitrogen doped TiO2Catalyst, its preparation and use Download PDFInfo
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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
- B01J27/24—Nitrogen compounds
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/34—Chemical or biological purification of waste gases
- B01D53/74—General processes for purification of waste gases; Apparatus or devices specially adapted therefor
- B01D53/86—Catalytic processes
- B01D53/8668—Removing organic compounds not provided for in B01D53/8603 - B01D53/8665
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- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/08—Heat treatment
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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
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/16—Reducing
- B01J37/18—Reducing with gases containing free hydrogen
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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
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/34—Irradiation by, or application of, electric, magnetic or wave energy, e.g. ultrasonic waves ; Ionic sputtering; Flame or plasma spraying; Particle radiation
- B01J37/341—Irradiation by, or application of, electric, magnetic or wave energy, e.g. ultrasonic waves ; Ionic sputtering; Flame or plasma spraying; Particle radiation making use of electric or magnetic fields, wave energy or particle radiation
- B01J37/343—Irradiation by, or application of, electric, magnetic or wave energy, e.g. ultrasonic waves ; Ionic sputtering; Flame or plasma spraying; Particle radiation making use of electric or magnetic fields, wave energy or particle radiation of ultrasonic wave energy
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2258/00—Sources of waste gases
- B01D2258/06—Polluted air
Abstract
The invention particularly relates to nitrogen-doped TiO loaded with monoatomic Ag2The preparation method of the catalyst comprises the following steps: dissolving a titanium source in an organic solvent to obtain a solution A; dissolving a silver source and a nitrogen source in a mixed solvent of water, acid and an organic solvent to obtain a solution B; dropwise adding the solution B into the solution A under the action of an ultrasonic instrument, and continuing to perform ultrasonic treatment for 1-5 hours after the solution B is completely dropwise added to form stable gel; drying the gel in a constant temperature drying ovenObtaining dry gel, grinding the dry gel into powder, placing the powder in a hydrogen atmosphere furnace for high-temperature roasting to obtain the monoatomic Ag-loaded nitrogen-doped nano TiO2A catalyst. The preparation method is simple and controllable, and the prepared catalyst can efficiently remove formaldehyde at normal temperature under the conditions of light/no light, so that the formaldehyde is converted into completely nontoxic carbon dioxide and water; after long-time operation, the catalytic degradation capability of the catalyst for formaldehyde is almost not attenuated, which shows that the catalyst has very good stability.
Description
Technical Field
The invention belongs to the technical field of catalytic materials and environmental protection, and particularly relates to a nitrogen-doped TiO loaded with monoatomic Ag2A preparation method of the catalyst and application thereof in degrading formaldehyde at normal temperature.
Background
Formaldehyde is a main air pollutant with high indoor toxicity, and the short-term contact with the formaldehyde can stimulate eyes, nasal cavities and respiratory tracts to cause anaphylactic reaction; prolonged exposure to formaldehyde increases the likelihood of leukemia, nasopharyngeal carcinoma, breast cancer, and death. The world health organization international agency for the study of cancer has defined formaldehyde as a class of carcinogens. Therefore, how to remove formaldehyde in the room with high efficiency is necessary. In the prior art, a large number of novel green environment-friendly purification materials continuously appear for improving the indoor air environment. The photocatalyst has a better air purification function, and after being excited by visible light or ultraviolet light, the photocatalyst particles generate active substances on the surfaces, so that the photocatalyst can perform oxidation or reduction reaction on a target object, and has the effects of removing pollutants, purifying air, resisting bacteria, removing dust, preventing fog and other environmental purifications. At present, the main component of the photocatalyst is titanium dioxide, which can generate electric charge under the irradiation of sunlight or ultraviolet rays in an illumination light source, and the electric charge reacts with water molecules and oxygen molecules in the air to generate negative oxygen ions and hydroxyl radicals, and the substances have strong oxidizing capability and have the effects of degrading organic matters, sterilizing and the like. But TiO 22Is a wide-band gap semiconductor, can only absorb ultraviolet light with the sunlight capacity of about 4 percent, and simultaneously TiO2The generated photo-generated electrons and holes have low migration efficiency, resulting in TiO2The quantum efficiency is low.
Nitrogen doped TiO2Can reduce TiO2The forbidden band width of h is reduced+-e-Thereby increasing TiO2The utilization rate of sunlight is improved, and the photocatalytic activity of the photocatalyst is improved. The monatomic catalyst is a novel catalyst based on an atomic-level metal active componentGreat advantages are shown in maximizing the number of active sites, enhancing selectivity to target products, increasing intrinsic catalytic activity and reducing the amount of noble metals used. By combining nitrogen-doped titanium dioxide with a monoatomic noble metal, TiO enhancement can be achieved2The normal-temperature catalytic activity of the photocatalyst is expected to be used for the high-efficiency catalytic degradation of formaldehyde.
There is no prior literature report of monatomic noble metal/nitrogen-doped titanium dioxide as a catalyst for the oxidative degradation of formaldehyde.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide simple and controllable nitrogen-doped TiO loaded with monoatomic Ag2A method for preparing the catalyst. The catalyst prepared by the method can realize the efficient removal of formaldehyde at normal temperature under the conditions of light/no light, and can convert the formaldehyde into completely nontoxic carbon dioxide and water.
In order to achieve the purpose, the technical scheme of the invention is as follows:
monoatomic Ag-loaded nitrogen-doped TiO2The preparation method of the catalyst is characterized by comprising the following steps:
(1) dissolving a titanium source in an organic solvent to obtain a solution A;
(2) dissolving a silver source and a nitrogen source in a mixed solvent of water, acid and an organic solvent to obtain a solution B;
(3) dropwise adding the solution B into the solution A under the action of an ultrasonic instrument, and continuing to perform ultrasonic treatment for 1-5 hours after the solution B is completely dropwise added to form stable gel;
(4) drying the gel obtained in the step (4) in a constant-temperature drying oven to obtain dry gel, grinding the dry gel into powder, and placing the powder in a hydrogen atmosphere furnace for high-temperature roasting to obtain the monoatomic Ag-loaded nitrogen-doped nano TiO2A catalyst.
Preferably, the ratio of the titanium source to the organic solvent substance in the step (1) is (0.01-1): 1.
Preferably, the mass ratio of the water, the acid and the organic solvent in the step (2) is (0.1-10): (0.1-1): 1.
preferably, in the step (3), the solution B is dripped into the solution A, and the amount ratio of the nitrogen source, the silver source and the titanium source is controlled to be (0.1-10): (0.01-1): 1.
preferably, the titanium source in step (1) is any one or a mixture of more than one of tetramethyl titanate, tetraethyl titanate, tetraisopropyl titanate, n-butyl titanate, tetraisobutyl titanate, titanium tetrachloride and titanium sulfate.
Preferably, the silver source in step (2) is any one or a mixture of more than one of silver nitrate, silver acetate and silver acetylacetonate.
Preferably, the nitrogen source in step (2) is any one or a mixture of more than one of ammonium carbonate, urea, triethylamine or ammonium acetate.
Preferably, the acid in step (2) is one or a mixture of more than one of glacial acetic acid, hydrochloric acid or nitric acid.
Preferably, the organic solvent in steps (1) and (2) is any one or a mixture of more than one of methanol, ethanol, isopropanol, ethylene glycol and glycerol.
Preferably, the temperature of the ultrasonic treatment in the step (3) is 0-25 ℃, and the ultrasonic frequency is 50-100 HZ.
Preferably, the dropping speed in the step (3) is 1-10 mL/min.
Preferably, in the step (4), the drying temperature is 50-100 ℃, and the drying time is 6-24 hours.
Preferably, the roasting temperature in the step (4) is 300-500 ℃, and the roasting time is 0.5-6 h.
The catalyst prepared by the method is used for formaldehyde catalytic oxidation reaction to remove formaldehyde. The invention utilizes Ag loaded nitrogen-doped TiO dispersed at atomic level2The catalyst is used for catalyzing and oxidizing formaldehyde, and formaldehyde with a certain concentration is converted into completely nontoxic carbon dioxide and water under the conditions of normal temperature, light and no light.
Compared with the prior art, the invention has the following beneficial effects:
1. the preparation method is simple and easy to implement, and is easy to realize large-scale production.
2. Hair brushCatalysts doped with non-metallic N into TiO2Lattice, formation of Ti-O-N structure, reduction of TiO2The forbidden band width is reduced from 3.25eV to 3.10eV, and the charge transfer rate is increased to h+And e-The recombination probability is greatly reduced, thereby increasing TiO2The absorption of visible light improves the photocatalytic activity; the Ag with the atomic scale size has high efficient atom utilization rate, can efficiently activate oxygen molecules in the air, can convert formaldehyde into completely nontoxic carbon dioxide and water under the condition of no light, and can form a synergistic effect with the nitrogen-doped nano titanium dioxide under the condition of light, so that the degradation efficiency of the formaldehyde is improved.
3. The catalyst has stable performance, and the ability of the catalyst for catalyzing and degrading formaldehyde is almost not attenuated after the catalyst runs for a long time.
Detailed Description
The present invention will be described in further detail with reference to specific embodiments.
The monoatomic Ag-loaded nitrogen-doped TiO of the invention2The preparation method of the catalyst is characterized by comprising the following steps:
(1) dissolving a titanium source in an organic solvent to obtain a solution A;
(2) dissolving a silver source and a nitrogen source in a mixed solvent of water, acid and an organic solvent to obtain a solution B;
(3) dropwise adding the solution B into the solution A under the action of an ultrasonic instrument, and continuing to perform ultrasonic treatment for 1-5 hours after the solution B is completely dropwise added to form stable gel;
(4) drying the gel obtained in the step (4) in a constant-temperature drying oven to obtain dry gel, grinding the dry gel into powder, and placing the powder in a hydrogen atmosphere furnace for high-temperature roasting to obtain the monoatomic Ag-loaded nitrogen-doped nano TiO2A catalyst.
Preferably, the ratio of the titanium source to the organic solvent substance in the step (1) is (0.01-1): 1.
Preferably, the mass ratio of the water, the acid and the organic solvent in the step (2) is (0.1-10): (0.1-1): 1.
preferably, in the step (3), the solution B is dripped into the solution A, and the amount ratio of the nitrogen source, the silver source and the titanium source is controlled to be (0.1-10): (0.01-1): 1.
preferably, the titanium source in step (1) is any one or a mixture of more than one of tetramethyl titanate, tetraethyl titanate, tetraisopropyl titanate, n-butyl titanate, tetraisobutyl titanate, titanium tetrachloride and titanium sulfate.
Preferably, the silver source in step (2) is any one or a mixture of more than one of silver nitrate, silver acetate and silver acetylacetonate.
Preferably, the nitrogen source in step (2) is any one or a mixture of more than one of ammonium carbonate, urea, triethylamine or ammonium acetate.
Preferably, the acid in step (2) is one or a mixture of more than one of glacial acetic acid, hydrochloric acid or nitric acid.
Preferably, the organic solvent in steps (1) and (2) is any one or a mixture of more than one of methanol, ethanol, isopropanol, ethylene glycol and glycerol.
Preferably, the temperature of the ultrasonic treatment in the step (3) is 0-25 ℃, and the ultrasonic frequency is 50-100 HZ.
Preferably, the dropping speed in the step (3) is 1-10 mL/min.
Preferably, in the step (4), the drying temperature is 50-100 ℃, and the drying time is 6-24 hours.
Preferably, the roasting temperature in the step (4) is 300-500 ℃, and the roasting time is 0.5-6 h.
The monoatomic Ag-loaded nitrogen-doped TiO prepared by the method2The catalyst can convert formaldehyde into completely nontoxic carbon dioxide and water under the conditions of normal temperature, light/no light.
The following examples are provided to further illustrate the embodiments of the present invention and are not intended to limit the scope of the present invention.
Example 1
(1) Dropwise adding 0.1mol of titanium tetrachloride into 0.1mol of ethanol under the action of a magnetic stirrer, fully stirring, and uniformly mixing to obtain a solution A;
(2) uniformly mixing 1mol of water, 0.1mol of hydrochloric acid and 0.1mol of glycol under the action of a magnetic stirrer to obtain a mixed solvent; under the action of a magnetic stirrer, adding 0.001mol of silver nitrate and 0.01mol of ammonium acetate, fully stirring, and uniformly mixing to obtain a solution B;
(3) dropwise adding the solution B into the solution A at a speed of 1mL/min under the action of an ultrasonic instrument (the temperature is 0 ℃, and the frequency is 50HZ), and continuing to perform ultrasonic treatment for 1h after complete dropwise addition to form stable gel;
(4) putting the gel obtained in the step (4) into a constant-temperature drying oven at 50 ℃ for drying for 24 hours to obtain dry gel, grinding the dry gel into powder, and roasting the powder in a hydrogen atmosphere furnace at 300 ℃ for 6 hours to obtain monoatomic Ag-loaded nitrogen-doped TiO2A catalyst.
Example 2
(1) Dropwise adding 0.1mol of tetraisopropyl titanate into 10mol of methanol under the action of a magnetic stirrer, fully stirring, and uniformly mixing to obtain a solution A;
(2) uniformly mixing 1mol of water, 1mol of nitric acid and 10mol of methanol under the action of a magnetic stirrer to obtain a mixed solvent; adding 0.1mol of silver acetate and 1mol of ammonium carbonate under the action of a magnetic stirrer, fully stirring, and uniformly mixing to obtain a solution B;
(3) dripping the solution B into the solution A at a speed of 10mL/min under the action of an ultrasonic instrument (the temperature is 25 ℃, the frequency is 100HZ), and continuing to perform ultrasonic treatment for 5 hours after the dripping is completed to form stable gel;
(4) putting the gel obtained in the step (4) into a constant-temperature drying oven at 100 ℃ for drying for 6h to obtain dry gel, grinding the dry gel into powder, and roasting the powder in a hydrogen atmosphere furnace at 500 ℃ for 0.5h to obtain the monoatomic Ag-loaded nitrogen-doped TiO2A catalyst.
Example 3
(1) Dropwise adding 0.1mol of tetrabutyl titanate into 1mol of ethylene glycol under the action of a magnetic stirrer, fully stirring, and uniformly mixing to obtain a solution A;
(2) uniformly mixing 1mol of water, 0.3mol of glacial acetic acid and 1mol of ethylene glycol under the action of a magnetic stirrer to obtain a mixed solvent; under the action of a magnetic stirrer, adding 0.01mol of silver acetylacetonate and 0.1mol of urea, fully stirring, and uniformly mixing to obtain a solution B;
(3) dropwise adding the solution B into the solution A at a speed of 5mL/min under the action of an ultrasonic instrument (the temperature is 20 ℃, and the frequency is 75HZ), and continuing to perform ultrasonic treatment for 2h after complete dropwise addition to form stable gel;
(4) putting the gel obtained in the step (4) into a constant-temperature drying oven at 70 ℃ for drying for 12h to obtain dry gel, grinding the dry gel into powder, and roasting the powder in a hydrogen atmosphere furnace at 350 ℃ for 4h to obtain the monoatomic Ag-loaded nitrogen-doped TiO2A catalyst.
Example 4
The catalyst prepared in the embodiment 1-3 is placed in a 3-cube standard formaldehyde test chamber for formaldehyde degradation performance test. The reaction conditions are as follows: the catalyst loading was 30g, the temperature was 25 ℃, the relative humidity was 50%, 60w energy saving lamp was a visible light source, the initial concentration of formaldehyde was 1.0g/cm3, the formaldehyde concentration in the cabin was tested after 24h, then 1mg/m3 formaldehyde was added again, after 24h operation 1mg/m3 formaldehyde was added again, after that 1mg/m3 formaldehyde was added again every 24h until formaldehyde was added again the 10 th time, and the formaldehyde concentration in the cabin was tested after 24h, the results are shown in table 1.
Table 1: performance test data under normal temperature and light conditions:
example 5
The catalyst prepared in the embodiment 1-3 is placed in a 3-cube standard formaldehyde test chamber for formaldehyde degradation performance test. The reaction conditions are as follows: the catalyst loading was 30g, the temperature was 25 ℃, the relative humidity was 50%, no light source, the initial formaldehyde concentration was 1.0g/cm3, the cabin formaldehyde concentration was tested after 24h, then 1mg/m3 formaldehyde was added again, after 24h operation 1mg/m3 formaldehyde was added again, after 24h operation 1mg/m3 formaldehyde was added again until the 10 th formaldehyde addition, after 24h cabin formaldehyde concentration was tested, the results are shown in table 2.
Table 2: performance test data under normal temperature and no light conditions:
the catalyst can realize the efficient removal of formaldehyde at normal temperature under the conditions of no light/light, and convert the formaldehyde into completely nontoxic carbon dioxide and water; after long-time operation, the catalytic degradation capability of the catalyst for formaldehyde is almost not attenuated, which shows that the catalyst has very good stability.
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art should be considered to be within the technical scope of the present invention, and the technical solutions and inventive concepts according to the present invention are equivalent or changed and shall be covered by the scope of the present invention.
Claims (10)
1. Monoatomic Ag-loaded nitrogen-doped TiO2The preparation method of the catalyst is characterized by comprising the following steps:
(1) dissolving a titanium source in an organic solvent to obtain a solution A;
(2) dissolving a silver source and a nitrogen source in a mixed solvent of water, acid and an organic solvent to obtain a solution B;
(3) dropwise adding the solution B into the solution A under the action of an ultrasonic instrument, and continuing to perform ultrasonic treatment for 1-5 hours after the solution B is completely dropwise added to form stable gel;
(4) drying the gel obtained in the step (4) in a constant-temperature drying oven to obtain dry gel, grinding the dry gel into powder, and placing the powder in a hydrogen atmosphere furnace for high-temperature roasting to obtain the monoatomic Ag-loaded nitrogen-doped nano TiO2A catalyst.
2. The method according to claim 1, wherein the ratio of the amount of the titanium source to the organic solvent substance in the step (1) is (0.01-1): 1.
3. The method according to claim 1, wherein the ratio of the amounts of the water, the acid and the organic solvent in step (2) is (0.1-10): (0.1-1): 1.
4. the preparation method according to claim 1, wherein the solution B is added dropwise to the solution A in the step (3) while controlling the mass ratio of the nitrogen source, the silver source and the titanium source to be (0.1-10): (0.01-1): 1.
5. the method according to claim 1, wherein the titanium source in step (1) is any one or a mixture of more than one of tetramethyl titanate, tetraethyl titanate, tetrapropyl titanate, tetrabutyl titanate, tetraisopropyl titanate, tetraisobutyl titanate, titanium tetrachloride and titanium sulfate; in the step (2), the silver source is any one or more of silver nitrate, silver acetate and silver acetylacetonate, the nitrogen source is any one or more of ammonium carbonate, urea, triethylamine and ammonium acetate, and the acid is one or more of glacial acetic acid, hydrochloric acid and nitric acid.
6. The preparation method according to claim 1, wherein the organic solvent in steps (1) and (2) is any one or more of methanol, ethanol, isopropanol, ethylene glycol and glycerol.
7. The preparation method according to claim 1, wherein the ultrasonic temperature in the step (3) is 0 to 25 ℃, the ultrasonic frequency is 50 to 100Hz, and the dropping speed is 1 to 10 mL/min.
8. The preparation method according to claim 1, wherein the drying temperature in the step (4) is 50-100 ℃, the drying time is 6-24 hours, the roasting temperature is 300-500 ℃, and the roasting time is 0.5-6 hours.
9. Monoatomic Ag-loaded nitrogen-doped TiO2The catalyst, which is produced by the production method according to any one of claims 1 to 8.
10. The monoatomic Ag-supported nitrogen-doped TiO according to claim 92The application of the catalyst in the catalytic oxidation of formaldehyde is characterized in that formaldehyde is converted into carbon dioxide and water under the conditions of normal temperature, light or no light.
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Citations (5)
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| CN1792437A (en) * | 2005-12-02 | 2006-06-28 | 厦门大学 | Method for loading silver nanometer particles onto nanometer titanium dioxide |
| US20140011674A1 (en) * | 2012-07-09 | 2014-01-09 | National Chi Nan University | Process of producing a titanium dioxide-based photocatalyst used for degradation of organic pollutants |
| CN104258894A (en) * | 2014-10-21 | 2015-01-07 | 南京工业大学 | Metal plate loaded TiO2 photocatalyst with visible light response effect as well as preparation and application of photocatalyst |
| CN109012739A (en) * | 2018-07-24 | 2018-12-18 | 信阳市上天梯非金属矿管理区非金属矿技术开发应用研究所 | Photochemical catalyst, organic sewage biodegrading process and device using the photochemical catalyst |
| CN110252300A (en) * | 2019-06-05 | 2019-09-20 | 北京氦舶科技有限责任公司 | Ag/MnO2Catalyst and its preparation and the application in formaldehyde is gone in room temperature |
-
2019
- 2019-11-04 CN CN201911064893.5A patent/CN112756005A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1792437A (en) * | 2005-12-02 | 2006-06-28 | 厦门大学 | Method for loading silver nanometer particles onto nanometer titanium dioxide |
| US20140011674A1 (en) * | 2012-07-09 | 2014-01-09 | National Chi Nan University | Process of producing a titanium dioxide-based photocatalyst used for degradation of organic pollutants |
| CN104258894A (en) * | 2014-10-21 | 2015-01-07 | 南京工业大学 | Metal plate loaded TiO2 photocatalyst with visible light response effect as well as preparation and application of photocatalyst |
| CN109012739A (en) * | 2018-07-24 | 2018-12-18 | 信阳市上天梯非金属矿管理区非金属矿技术开发应用研究所 | Photochemical catalyst, organic sewage biodegrading process and device using the photochemical catalyst |
| CN110252300A (en) * | 2019-06-05 | 2019-09-20 | 北京氦舶科技有限责任公司 | Ag/MnO2Catalyst and its preparation and the application in formaldehyde is gone in room temperature |
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