CN115364839A - Preparation of visible light response TiO at low temperature 2 Method for preparing photocatalyst - Google Patents
Preparation of visible light response TiO at low temperature 2 Method for preparing photocatalyst Download PDFInfo
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- CN115364839A CN115364839A CN202211077836.2A CN202211077836A CN115364839A CN 115364839 A CN115364839 A CN 115364839A CN 202211077836 A CN202211077836 A CN 202211077836A CN 115364839 A CN115364839 A CN 115364839A
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- 238000000034 method Methods 0.000 title claims abstract description 27
- 239000011941 photocatalyst Substances 0.000 title claims abstract description 18
- 230000004298 light response Effects 0.000 title claims abstract description 13
- 238000002360 preparation method Methods 0.000 title claims description 16
- 229910010413 TiO 2 Inorganic materials 0.000 claims abstract description 17
- 238000006243 chemical reaction Methods 0.000 claims abstract description 17
- 239000004698 Polyethylene Substances 0.000 claims abstract description 16
- 239000004372 Polyvinyl alcohol Substances 0.000 claims abstract description 16
- -1 polyethylene Polymers 0.000 claims abstract description 16
- 229920000573 polyethylene Polymers 0.000 claims abstract description 16
- 229920002451 polyvinyl alcohol Polymers 0.000 claims abstract description 16
- 238000003756 stirring Methods 0.000 claims abstract description 13
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims abstract description 10
- 239000002071 nanotube Substances 0.000 claims abstract description 10
- 229910052760 oxygen Inorganic materials 0.000 claims abstract description 10
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- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 10
- 238000011049 filling Methods 0.000 claims abstract description 6
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- 230000001699 photocatalysis Effects 0.000 claims description 11
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 claims description 6
- 238000010438 heat treatment Methods 0.000 claims description 5
- 230000009467 reduction Effects 0.000 claims description 5
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 claims description 4
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 3
- 229910052739 hydrogen Inorganic materials 0.000 claims description 3
- 239000001257 hydrogen Substances 0.000 claims description 3
- 238000004519 manufacturing process Methods 0.000 claims description 3
- 238000013033 photocatalytic degradation reaction Methods 0.000 claims description 3
- 239000001569 carbon dioxide Substances 0.000 claims description 2
- 229910002092 carbon dioxide Inorganic materials 0.000 claims description 2
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- 230000008569 process Effects 0.000 abstract description 8
- 230000015572 biosynthetic process Effects 0.000 abstract description 6
- 238000003786 synthesis reaction Methods 0.000 abstract description 6
- 238000009776 industrial production Methods 0.000 abstract description 3
- 238000011031 large-scale manufacturing process Methods 0.000 abstract description 2
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 22
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 16
- 239000003054 catalyst Substances 0.000 description 7
- 239000004408 titanium dioxide Substances 0.000 description 7
- 230000008859 change Effects 0.000 description 5
- 230000002950 deficient Effects 0.000 description 4
- 239000003638 chemical reducing agent Substances 0.000 description 3
- RAXXELZNTBOGNW-UHFFFAOYSA-N imidazole Natural products C1=CNC=N1 RAXXELZNTBOGNW-UHFFFAOYSA-N 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 238000007146 photocatalysis Methods 0.000 description 3
- 239000010936 titanium Substances 0.000 description 3
- CIWBSHSKHKDKBQ-JLAZNSOCSA-N Ascorbic acid Chemical compound OC[C@H](O)[C@H]1OC(=O)C(O)=C1O CIWBSHSKHKDKBQ-JLAZNSOCSA-N 0.000 description 2
- 238000004435 EPR spectroscopy Methods 0.000 description 2
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 2
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- 238000003837 high-temperature calcination Methods 0.000 description 1
- 150000004678 hydrides Chemical class 0.000 description 1
- 231100000053 low toxicity Toxicity 0.000 description 1
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- JMANVNJQNLATNU-UHFFFAOYSA-N oxalonitrile Chemical compound N#CC#N JMANVNJQNLATNU-UHFFFAOYSA-N 0.000 description 1
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- 229910052724 xenon Inorganic materials 0.000 description 1
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 description 1
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J21/00—Catalysts comprising the elements, oxides, or hydroxides of magnesium, boron, aluminium, carbon, silicon, titanium, zirconium, or hafnium
- B01J21/06—Silicon, titanium, zirconium or hafnium; Oxides or hydroxides thereof
- B01J21/063—Titanium; Oxides or hydroxides thereof
-
- B01J35/39—
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- B01J35/40—
-
- 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
- B01J37/12—Oxidising
- B01J37/14—Oxidising with gases containing free oxygen
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G23/00—Compounds of titanium
- C01G23/04—Oxides; Hydroxides
- C01G23/047—Titanium dioxide
- C01G23/053—Producing by wet processes, e.g. hydrolysing titanium salts
-
- 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
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/80—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70
- C01P2002/84—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70 by UV- or VIS- data
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/04—Particle morphology depicted by an image obtained by TEM, STEM, STM or AFM
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/10—Particle morphology extending in one dimension, e.g. needle-like
- C01P2004/13—Nanotubes
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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
-
- 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 relates to a method for preparing TiO responding to visible light at low temperature 2 A method of photocatalyst comprising the steps of: (1) Weighing a defined amount of H 2 TiO 3 Placing the nanotube in a container, then adding polyethylene and polyvinyl alcohol, and uniformly stirring; (2) Filling the container with oxygen, and transferring to water at 30-80 deg.CHeating while stirring in a bath, and reacting for 3-15 days; (3) After the reaction is finished, the polyethylene and the polyvinyl alcohol are removed to obtain the visible light response TiO 2 . The method greatly simplifies the synthesis process, makes the reaction conditions milder, improves the synthesis quality, reduces the process cost and provides possibility for industrial and large-scale production.
Description
Technical Field
The invention relates to a titanium-based photocatalystThe technical field of preparation methods, in particular to preparation of visible light response TiO at low temperature 2 A method of photocatalyst.
Background
TiO 2 The material has become the most widely studied photocatalyst in various applications, compared to other semiconductor materials, tiO 2 There are several advantages in photocatalytic reactions, such as abundance, low toxicity, chemical and thermal stability, and high resistance to photo-corrosion. Due to these characteristics, they are widely used in the field of photocatalysis. But it also has the inevitable disadvantage of having a wide band gap (3,2 eV) making it applicable only in the ultraviolet region (less than 390 nm), which results in a serious shortage (less than 5%) of solar energy utilization. Therefore, how to expand the light absorption range is a key problem to be solved. The existing means include metal doping, non-metal doping, and semiconductor doping, however, these methods have a disadvantage in that the introduced dopant often becomes a charge carrier recombination center, resulting in a decrease in photocatalytic activity.
Compared to the above approaches, recent studies have shown that in TiO 2 In which Ti is introduced 3+ Or O-vacancy, can extend light absorption into the visible region by suppressing the recombination effect. By reaction on TiO 2 The introduction of defects can change the titanium dioxide from the original white color to other colors that can utilize more light energy, and prior studies have synthesized titanium dioxide in black or other colors (e.g., yellow, blue, green, brown). TiO accompanied by color change 2 The characteristics of narrow forbidden band, strong photocatalysis performance and the like can be presented. The methods for synthesizing black titanium dioxide are commonly adopted at present and comprise the following steps: (1) The reduced titanium dioxide is obtained by regulating and controlling the temperature or the pressure under the hydrogen atmosphere. (2) Black titanium dioxide can be obtained under mild conditions in the presence of hydrides. And (3) annealing under an argon atmosphere. (4) Using active metal or organic matter (such as imidazole and ascorbic acid) as reducing agent. And (5) preparing by adopting an electrochemical reduction method. In addition to the reduction method, an oxidation method may be used, in which the photoresponse range is changed by changing the valence of titanium. Go toThe above method can achieve the purpose of introducing defects, but in a specific implementation process, the reaction conditions are harsh (such as high temperature and high pressure), high in danger, special reaction equipment, specific reagents and the like are required. This greatly increases the difficulty of implementation and also increases the difficulty of large-scale industrial production. Publication No. CN 114345393A discloses a preparation method of defective titanium dioxide/ultrathin carbon nitride/defective titanium dioxide Z-type heterojunction photocatalyst, wherein defective TiO is obtained by reduction with strong reducing agent 2 ，
Thus, how to perform defective TiO in a simpler and more efficient manner 2 Is currently based on TiO 2 One of the very pressing problems in the field of photocatalysis. The above-mentioned processes, although capable of achieving the intended purpose, are complex to operate, impose certain requirements on equipment and reagents and present certain risks. The method has important practical significance in exploring the visible light response TiO2 which is simpler, has low energy consumption and is easy to implement, and the method is especially provided.
Disclosure of Invention
In order to solve the problems that other oxidants or reducing agents are required to be added in the synthesis process and the reaction conditions are harsh (such as high temperature, high pressure, high temperature calcination and the like) in the existing preparation method, the invention provides a method for simplifying the synthesis process, saving the cost and producing TiO in large batch 2 Possible routes to photocatalysts.
In order to achieve the purpose, the invention adopts the technical scheme that:
preparation of visible light response TiO at low temperature 2 A method of photocatalyst comprising the steps of:
(1) Weighing a certain amount of H 2 TiO 3 Placing the nanotube in a container, adding polyethylene and polyvinyl alcohol, and uniformly stirring;
(2) Filling oxygen into the container, transferring the container to a water bath at the temperature of 30-80 ℃, heating while stirring, and reacting for 3-15 days;
(3) After the reaction is finished, the polyethylene and the polyvinyl alcohol are removed to obtain the visible light response TiO 2 。
Preferably, the step (1) is performed by H 2 TiO 3 The mass ratio of the nanotube to the polyethylene to the polyvinyl alcohol is 1.
The preferable scheme is that the water bath temperature in the step (2) is 50 ℃.
TiO obtained by the preparation method 2 The photocatalyst is applied to the fields of photocatalytic hydrogen production, photocatalytic reduction of carbon dioxide, photocatalytic degradation of wastewater and removal of indoor formaldehyde.
The invention has the beneficial effects of providing a strategy for improving the photocatalytic performance and enriching TiO 2 The preparation method of the photocatalytic material greatly simplifies the synthesis process, makes the reaction conditions milder, improves the synthesis quality, reduces the process cost and provides possibility for industrial and large-scale production.
Description of the drawings:
FIG. 1 is a diagram of visible light responsive TiO of the present invention 2 A TEM image of (B);
FIG. 2 is TiO 2 Ultraviolet and visible absorption spectrum of (1);
FIG. 3 shows TiO before and after the reaction 2 EPR spectrum contrast diagram of photocatalyst;
FIG. 4 shows TiO before and after the reaction 2 Graph comparing the performance of photocatalyst in degrading RhB.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Referring to fig. 1-4, the present invention provides the following embodiments:
example 1
Preparation of TiO responsive to visible light 2 The photocatalyst preparation method comprises the following steps:
1. weigh 0.5g H 2 TiO 3 Adding the nanotube into a 250 ml three-mouth beaker, then adding 0.05g of polyethylene and 0.05g of polyvinyl alcohol, and uniformly stirring;
2. filling oxygen into the beaker, transferring the beaker into a water bath at the temperature of 30 ℃, heating the beaker while stirring, and reacting the beaker for 3 days;
3. after the reaction is finished, the polyethylene and the polyvinyl alcohol are removed to obtain the visible light response TiO 2 。
As shown in FIG. 1, tiO can be seen 2 The catalyst is in a tubular structure and has certain aggregation, and the diameter of the nanotube is about 5-10nm.
Example 2
Preparation of TiO responsive to visible light 2 The photocatalyst preparation method comprises the following steps:
1. weigh 0.5g H 2 TiO 3 Adding the nanotube into a 250 ml three-mouth beaker, then adding 0.5g of polyethylene and 0.5g of polyvinyl alcohol, and uniformly stirring;
2. filling oxygen into the beaker, transferring the beaker into a water bath at 50 ℃, heating the beaker while stirring, and reacting the beaker for 15 days;
3. after the reaction is finished, the polyethylene and the polyvinyl alcohol are removed to obtain the visible light response TiO 2 。
Starting material H 2 TiO 3 The nanotube is white, and after polyethylene and polyvinyl alcohol are added and reacted, the color of the obtained catalyst is obviously changed from the original white color to the yellow color. This change in color may mean a change in the internal structure of the catalyst and also a change in the photoresponse range of the catalyst.
Example 3
Preparation of TiO responsive to visible light 2 The photocatalyst preparation method comprises the following steps:
1. weigh 0.5g H 2 TiO 3 Adding the nanotube into a 250 ml three-mouth beaker, then adding 0.2g of polyethylene and 0.4g of polyvinyl alcohol, and uniformly stirring;
2. filling oxygen into the beaker, transferring the beaker into a water bath at 80 ℃, heating while stirring, and reacting for 10 days;
3. after the reaction is complete, the polyethylene is removed andthe visible light response TiO can be obtained by polyvinyl alcohol 2 。
The invention can realize the consumption at low temperature by means of oxygen transfer in the catalyst, and can realize the consumption in TiO 2 Oxygen vacancy is formed inside, thereby achieving the aim of TiO 2 Modifying and modifying to improve the photocatalytic performance.
By TiO in FIG. 2 2 The ultraviolet visible absorption spectrum of (A) shows that, in the range of 400-600 nm, the synthesized TiO 2 The light response range of the photocatalyst is obviously enhanced. In other words, after the reaction, the corresponding capacity and range of the photocatalyst in the visible light region have been greatly enhanced.
Further characterization by EPR spectroscopy to determine the presence of oxygen vacancies in the reacted sample, as shown in FIG. 3, shows that the reacted TiO 2 Produce a strong EPR signal, whereas the pre-reacted TiO 2 No signal was observed for the sample, so it can be concluded that the reaction was followed at TiO 2 Oxygen vacancies were introduced into the samples.
Experimental example:
to examine the photocatalytic degradation performance of the sample, 0.05g of the catalyst obtained in example 3 was weighed into a 100ml beaker, and then 100ml of secondary water and 400 μ L of a preconfigured RhB solution were added, respectively. Transferring the mixed solution into a dark box of the reactor, opening the condensed water, and starting stirring. Dark treatment for 30 min. The xenon lamp was turned on, samples were taken at different times and the absorbance of each sample was measured by an ultraviolet-visible spectrophotometer, and the performance was plotted and analyzed, the results of which are shown in fig. 4.
As can be seen from fig. 4, the performance of the catalyst is greatly improved after the reaction with the polyethylene and the polyvinyl alcohol. When the reaction time reached 90 min, about 95% of the dye had been degraded. Under the same conditions, the degradation rate of the starting material is only about 50%.
Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that various changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.
Claims (4)
1. Preparation of visible light response TiO at low temperature 2 A method of photocatalyst, comprising the steps of:
(1) Weighing a defined amount of H 2 TiO 3 Placing the nanotube in a container, then adding polyethylene and polyvinyl alcohol, and uniformly stirring;
(2) Filling oxygen into the container, transferring the container into a water bath at the temperature of 30-80 ℃, heating while stirring, and reacting for 3-15 days;
(3) After the reaction is finished, the polyethylene and the polyvinyl alcohol are removed to obtain the visible light response TiO 2 。
2. The method of claim 1, wherein: h in step (1) 2 TiO 3 The mass ratio of the nanotube to the polyethylene to the polyvinyl alcohol is 1.
3. The method of claim 1, wherein: the temperature of the water bath in the step (2) is 50 ℃.
4. TiO obtained by the production method according to any one of claims 1 to 3 2 The photocatalyst is applied to the fields of photocatalytic hydrogen production, photocatalytic reduction of carbon dioxide, photocatalytic degradation of wastewater and removal of indoor formaldehyde.
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