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CN115445593A - Photoelectrocatalysis material, electrochemical preparation method and application thereof - Google Patents

Photoelectrocatalysis material, electrochemical preparation method and application thereof Download PDF

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CN115445593A
CN115445593A CN202211095248.1A CN202211095248A CN115445593A CN 115445593 A CN115445593 A CN 115445593A CN 202211095248 A CN202211095248 A CN 202211095248A CN 115445593 A CN115445593 A CN 115445593A
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cts
carbon
flexible
tio
photoelectrocatalysis
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CN115445593B (en
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陈华军
席晓晶
李扬
高洁
田文杰
李冬
王锐
赵莉
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Luoyang Institute of Science and Technology
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Abstract

The invention relates to a photoelectrocatalysis material, an electrochemical preparation method and application thereof, belonging to the field of photocatalysis and photoelectrocatalysis material synthesis and comprising the following steps: the method comprises the following steps of (1) depositing amorphous carbon on the surface of a carbon fiber fabric by using methane as a carbon source and adopting a chemical vapor deposition method to prepare a flexible AC @ CTs carbon/carbon composite material; dissolving titanium sulfate and sodium nitrate in water to obtain a solution A; immersing flexible AC @ CTs carbon/carbon composite material serving as a working electrode into the solution A, and adopting a constant potential method to perform flexible AC @ CTs carbon/carbon recombinationDeposition of TiO on the surface of composite materials 2 A nanorod; the product is subjected to freeze drying and roasting to obtain the flexible TiO 2 @ AC @ CTs photocatalytic material. The method is simple and easy to implement, the process is environment-friendly, the product is easy to separate and recycle, the difficult problems of separating and recycling the powder photocatalyst are solved, and the industrial application of the photoelectrocatalysis technology is promoted.

Description

Photoelectrocatalysis material, electrochemical preparation method and application thereof
Technical Field
The invention belongs to the field of photocatalysis and synthesis of photoelectrocatalysis materials, and particularly relates to a photoelectrocatalysis material, and an electrochemical preparation method and application thereof.
Background
In the aspect of organic wastewater treatment, the solar photocatalytic technology has wide application prospect. However, the separation and recovery costs of the powdered photocatalytic material after use are high, and the design of the photocatalytic reaction apparatus is also not facilitated. The above drawbacks limit the industrial application of photocatalytic technology in the treatment of organic waste water.
Disclosure of Invention
In order to solve the difficult problems of separation and recovery of the photocatalytic material and promote the industrial application of the photocatalytic technology in the aspect of organic wastewater treatment, the invention aims at providing an electrochemical preparation method of the photocatalytic material, and aims at providing the flexible TiO prepared by the method 2 @ AC @ CTs photoelectrocatalytic material, and the third purpose is to provide the flexible TiO 2 The application of the @ AC @ CTs photoelectrocatalysis material in organic wastewater treatment. The invention adopts a simple electrochemical deposition method to assemble the traditional powder photocatalytic material and the macroscopic carbon fiber fabric into a photocatalytic and photoelectrocatalysis material which is easy to separate and recycle, thereby solving the difficult problems of separating and recycling the powder photocatalyst in the water treatment process.
The invention adopts the following specific scheme:
photoelectricity catalysisElectrochemical preparation method of chemical material, wherein the photoelectrocatalysis material is flexible TiO 2 @ AC @ CTs photocatalytic material, the method comprising the steps of:
(1) The method comprises the following steps of (1) depositing amorphous carbon on the surface of a carbon fiber fabric by using methane as a carbon source through a chemical vapor deposition method to prepare a flexible AC @ CTs carbon/carbon composite material;
(2) Dissolving titanium sulfate and sodium nitrate in deionized water to obtain a solution A;
(3) Immersing flexible AC @ CTs carbon/carbon composite material serving as a working electrode into the solution A, and depositing TiO on the surface of the flexible AC @ CTs carbon/carbon composite material by adopting a potentiostatic method 2 A nanorod;
(4) Freeze drying and roasting the electrochemical deposition product to prepare flexible TiO 2 @ AC @ CTs photocatalytic material.
The electrochemical preparation method of the photoelectrocatalysis material comprises the following steps of (1): the chemical vapor deposition is to heat a carbon fiber fabric to 900 to 1100 ℃ under the protection of 180 to 240 SCCM argon, then introduce 60 to 180 SCCM methane gas, deposit for 20 to 40 min, and naturally cool to room temperature to obtain the flexible AC @ CTs carbon/carbon composite material.
The electrochemical preparation method of the photoelectrocatalysis material comprises the following steps of (2): the mass concentration of the titanium sulfate in the solution A is 20-30 g/L, and the mass concentration of the sodium nitrate is 6-10 g/L.
The electrochemical preparation method of the photoelectrocatalysis material comprises the following steps of (3): the electrochemical deposition time is 40 to 160 min.
The electrochemical preparation method of the photoelectrocatalysis material comprises the following steps of (4): the freeze drying time is 12 to 24h; the roasting temperature is 600 to 800 ℃, the time is 2 to 4h, the roasting atmosphere is argon atmosphere, and the argon flow speed is 40 to 60SCCM.
The invention also claims the flexible TiO prepared by the electrochemical preparation method 2 @ AC @ CTs.
The invention additionally claims the flexible TiO 2 The application of the @ AC @ CTs photoelectrocatalysis material in organic wastewater treatment.
The technical scheme of the invention obtains the following beneficial technical effects:
1. the invention adopts a simple electrochemical deposition method to grow the powder photocatalytic material on the surface of the macroscopic carbon fiber fabric in a chemical epitaxial manner to prepare the flexible TiO 2 @ AC @ CTs. Compared with the traditional chemical epitaxial growth method, the electrochemical deposition method is simple and easy to implement, and no pollutant is generated in the preparation process. The preparation method has low cost and environment-friendly preparation process.
2. The electrochemical deposition strategy provided by the invention solves the difficult problems of separation and recovery of the powder photocatalyst in the actual use process, and opens up a new way for the industrial application of photocatalysis.
3. The amorphous carbon coating can promote TiO 2 The chemical epitaxial growth of the nano rod on the surface of the carbon fiber fabric improves the carbon fiber fabric and the TiO 2 The bonding strength of the nanorods.
4. Flexible TiO prepared by electrochemical deposition method 2 The @ AC @ CTs photoelectrocatalysis material has excellent photocatalysis and photoelectrocatalysis cycle performance, the photoelectrocatalysis performance is larger than the sum of photocatalysis and electrocatalysis, and the photocatalysis have synergistic effect.
Drawings
FIG. 1 is the flexible TiO of example 1 2 @ CTs photoelectrocatalytic material (a) and flexible TiO 2 SEM photograph of @ AC @ CTs photocatalytic material (b);
FIG. 2 shows the flexible TiO of examples 1, 2 and 3 2 XRD spectrum of @ AC @ CTs photoelectrocatalysis material;
FIG. 3 shows the flexible TiO of example 1 2 SEM photograph of XRD of the @ AC @ CTs photoelectrocatalysis material;
FIG. 4 shows the flexible TiO of example 2 2 SEM photograph of XRD of @ AC @ CTs photoelectrocatalysis material;
FIG. 5 shows the flexible TiO of example 3 2 SEM photograph of XRD of the @ AC @ CTs photoelectrocatalysis material;
FIG. 6 shows the flexible TiO of examples 1, 2 and 3 2 An ultraviolet-visible diffuse reflection spectrogram of the @ AC @ CTs photoelectrocatalysis material;
FIG. 7 isIn examples 1, 2 and 3, flexible TiO 2 A photoelectrochemical spectrum of the @ AC @ CTs photoelectrocatalysis material;
FIG. 8 shows the flexible TiO of examples 1, 2 and 3 2 Electrochemical impedance spectroscopy of @ AC @ CTs photoelectrocatalysis material;
FIG. 9 shows the flexible TiO of example 1 2 In the process of degrading rhodamine B through the photoelectrocatalysis of @ AC @ CTs, the ultraviolet-visible absorption spectrum of the rhodamine B at different degradation times is obtained;
FIG. 10 shows the flexible TiO of example 2 2 In the process of degrading rhodamine B through the photoelectrocatalysis of @ AC @ CTs, the ultraviolet-visible absorption spectrum of the rhodamine B at different degradation times is obtained;
FIG. 11 is the same as in example 3, wherein the flexible TiO material was used 2 In the process of degrading rhodamine B through electro-photocatalysis of @ AC @ CTs, the rhodamine B has ultraviolet-visible absorption spectrum with different degradation time.
Detailed Description
Flexible TiO 2 The electrochemical preparation method of the @ AC @ CTs photoelectrocatalysis material comprises the following steps:
(1) The method comprises the following steps of (1) depositing amorphous carbon on the surface of a carbon fiber fabric by using methane as a carbon source and adopting a chemical vapor deposition method to prepare a flexible AC @ CTs carbon/carbon composite material;
(2) Dissolving titanium sulfate and sodium nitrate in deionized water to obtain a solution A;
(3) Immersing flexible AC @ CTs carbon/carbon composite material serving as a working electrode into the solution A, and depositing TiO on the surface of the flexible AC @ CTs carbon/carbon composite material by adopting a potentiostatic method 2 A nanorod;
(4) Freeze drying and roasting the electrochemical deposition product to prepare flexible TiO 2 @ AC @ CTs.
The flexible TiO 2 An electrochemical preparation method of a @ AC @ CTs photoelectrocatalysis material comprises the following steps of (1): the chemical vapor deposition is that under the protection of 180-240 SCCM argon, the carbon fiber fabric is heated to 900-1100 ℃, then methane gas of 60-180 SCCM is introduced, the deposition time is 20-40 min, and the carbon fiber fabric is naturally cooled to the room temperature, so that the flexible AC @ CTs carbon/carbon composite material is obtained.
The flexible TiO 2 Electrochemical method of @ AC @ CTs photoelectrocatalysis materialThe preparation method is characterized in that in the step (2): the mass concentration of the titanium sulfate in the solution A is 20-30 g/L, and the mass concentration of the sodium nitrate is 6-10 g/L.
The flexible TiO 2 The electrochemical preparation method of the @ AC @ CTs photoelectrocatalysis material comprises the following steps of (3): the electrochemical deposition time is 40 to 160 min.
The flexible TiO 2 An electrochemical preparation method of the @ AC @ CTs photoelectrocatalysis material comprises the following steps of (4): the freeze drying time is 12 to 24h; the baking temperature is 600 to 800 ℃, the baking time is 2 to 4 hours, the baking atmosphere is argon atmosphere, and the argon flow rate is 40 to 60SCCM.
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention.
Example 1
Flexible TiO 2 The electrochemical preparation method of the @ AC @ CTs photoelectrocatalysis material comprises the following steps:
1) Under the protection of 180 SCCM argon gas, firstly heating the carbon fiber fabric to 900 ℃, then introducing 60SCCM methane gas, depositing an amorphous carbon coating on the surface of the carbon fiber fabric for 40 min, and naturally cooling to room temperature to obtain a flexible AC @ CTs carbon/carbon composite material;
2) Dissolving titanium sulfate and sodium nitrate in deionized water to obtain a solution A, wherein the mass concentration of the titanium sulfate in the solution A is 20 g/L, and the mass concentration of the sodium nitrate is 6 g/L;
3) Immersing flexible AC @ CTs carbon/carbon composite material serving as a working electrode into the solution A, and depositing TiO on the surface of the flexible AC @ CTs carbon/carbon composite material by adopting a constant potential method 2 Carrying out electrochemical deposition on the nano rods for 40 min;
4) The electrochemical deposition product is firstly frozen and dried for 12 hours and then roasted for 2 hours at the temperature of 600 ℃ under the protection of 40 SCCM argon gas to prepare the flexible TiO 2 @ AC @ CTs.
5) Flexible TiO 2 The @ AC @ CTs photoelectrocatalysis material has excellent photoelectrocatalysis performance, the degradation rate of the photoelectrocatalysis to rhodamine B is 95.2 percent within 60 min, the photoelectrocatalysis efficiency is more than the sum of the photocatalysis efficiency and the electrocatalysis efficiency, and the flexible TiO 2 @ AC @ CTs lightIn the process of photoelectrocatalysis, the electrocatalysis and the photocatalysis have synergistic effect.
Example 2
The flexible TiO 2 The electrochemical preparation method of the @ AC @ CTs photoelectrocatalysis material comprises the following steps:
1) Under the protection of 210 SCCM argon, firstly heating the carbon fiber fabric to 1000 ℃, then introducing 120 SCCM methane gas, depositing an amorphous carbon coating on the surface of the carbon fiber fabric, wherein the deposition time is 30 min, and naturally cooling to room temperature to obtain a flexible AC @ CTs carbon/carbon composite material;
2) Dissolving titanium sulfate and sodium nitrate in deionized water to obtain a solution A, wherein the mass concentration of the titanium sulfate in the solution A is 25 g/L, and the mass concentration of the sodium nitrate is 8 g/L;
3) Immersing flexible AC @ CTs carbon/carbon composite material serving as a working electrode into the solution A, and depositing TiO on the surface of the flexible AC @ CTs carbon/carbon composite material by adopting a potentiostatic method 2 Carrying out electrochemical deposition on the nano rods for 80 min;
4) The electrochemical deposition product is firstly frozen and dried for 18 hours and then roasted for 3 hours at 700 ℃ under the protection of 50 SCCM argon gas to prepare the flexible TiO 2 @ AC @ CTs photocatalytic material.
5) Flexible TiO 2 The @ AC @ CTs photoelectrocatalysis material has excellent photoelectrocatalysis performance, the degradation rate of the photoelectrocatalysis to rhodamine B is 99.8 percent within 60 min, the photoelectrocatalysis efficiency is more than the sum of the photocatalysis efficiency and the electrocatalysis efficiency, and the flexible TiO is 2 In the photoelectrocatalysis process of the @ AC @ CTs photoelectrocatalysis material, the electrocatalysis and the photocatalysis have synergistic effect.
Example 3
The flexible TiO 2 The electrochemical preparation method of the @ AC @ CTs photoelectrocatalysis material comprises the following steps:
1) Under the protection of argon gas of 180-240 SCCM, firstly heating the carbon fiber fabric to 1100 ℃, then introducing 180 SCCM methane gas, depositing an amorphous carbon coating on the surface of the carbon fiber fabric for 20 min, and naturally cooling to room temperature to obtain a flexible AC @ CTs carbon/carbon composite material;
2) Dissolving titanium sulfate and sodium nitrate in deionized water to obtain a solution A, wherein the mass concentration of the titanium sulfate in the solution A is 30 g/L, and the mass concentration of the sodium nitrate is 10 g/L;
3) Immersing flexible AC @ CTs carbon/carbon composite material serving as a working electrode into the solution A, and depositing TiO on the surface of the flexible AC @ CTs carbon/carbon composite material by adopting a potentiostatic method 2 Carrying out electrochemical deposition on the nano-rods for 160 min;
4) The electrochemical deposition product is firstly frozen and dried for 24 hours and then roasted for 4 hours at 800 ℃ under the protection of 60SCCM argon gas to prepare the flexible TiO 2 @ AC @ CTs.
5) Flexible TiO 2 The @ AC @ CTs photoelectrocatalysis material has excellent photoelectrocatalysis performance, the degradation rate of the photoelectrocatalysis to rhodamine B is 99.9 percent within 60 min, the photoelectrocatalysis efficiency is greater than the sum of the photocatalysis efficiency and the electrocatalysis efficiency, and the flexible TiO 2 In the process of photoelectrocatalysis of the @ AC @ CTs photoelectrocatalysis material, the electrocatalysis and the photocatalysis have synergistic effect.
Flexible TiO prepared in examples 1 to 3 2 The results of evaluation of the @ AC @ CTs photoelectrocatalytic material are shown in FIGS. 1 to 11.
FIG. 1 example 1, the amorphous carbon coating is useful for increasing the TiO content of the surface of the carbon fiber fabric 2 And (3) the stability of the nano rod. As can be seen from FIG. 1 (a), tiO is directly deposited on the surface of the carbon fiber fabric in an electrochemical way 2 Nanorod, carbon fiber fabric surface TiO 2 The nano rod is easy to fall off. As shown in FIG. 1 (b), an amorphous carbon coating is deposited on the surface of the carbon fiber fabric by CVD method, and then TiO is electrochemically deposited 2 Nano-rod, carbon fiber fabric and TiO 2 The nano-rods are tightly combined without shedding phenomenon. Indicating that the amorphous carbon coating not only can promote TiO 2 The chemical epitaxial growth of the nano-rod on the surface of the carbon fiber fabric improves the carbon fiber fabric and TiO 2 The bonding strength of the nanorods.
FIG. 2 in examples 1, 2 and 3, anatase TiO can be deposited on the surface of the carbon fiber fabric by a constant potential deposition method 2 Nano rod photocatalytic material for powdered TiO 2 The separation and recovery of the nano-rod in the water treatment process are difficult, and the design of a photoelectrocatalysis device is facilitated.
FIG. 3 in example 1, flexible TiO 2 SEM photograph of @ AC @ CTs photoelectrocatalytic material, tiO is seen in FIG. 3 2 The nano rods are firmly and uniformly distributed on the surface of the carbon fiber.
FIG. 4 in example 2, a flexible TiO 2 SEM photograph of @ AC @ CTs photoelectrocatalytic material, as can be seen from FIG. 4, tiO 2 The nano rods are firmly and uniformly distributed on the surface of the carbon fiber, and compared with the embodiment 1, the TiO on the surface of the carbon fiber fabric can be increased by increasing the electrochemical deposition time 2 The number of nano rods.
FIG. 5 in example 3, a flexible TiO 2 SEM photograph of @ AC @ CTs photoelectrocatalytic material, tiO is seen in FIG. 5 2 The nano rods are firmly and uniformly distributed on the surface of the carbon fiber, and TiO is on the surface of the carbon fiber fabric 2 The quantity of the nano rods is large.
FIG. 6 in examples 1, 2 and 3, tiO 2 Nanorods and flexible TiO 2 Ultraviolet-visible diffuse reflection spectrum contrast of @ AC @ CTs photoelectrocatalysis material, flexible TiO 2 The spectral intensity of the @ AC @ CTs photoelectrocatalysis material is obviously higher than that of TiO in a visible light region 2 Nanorod, indicating flexible TiO 2 The @ AC @ CTs photoelectrocatalysis material has higher light absorption performance and visible light utilization efficiency, thereby having higher photocatalysis and photoelectrocatalysis performance.
FIG. 7 examples 1, 2 and 3, different deposition times of Flexible TiO 2 Comparison of photocurrent of the @ AC @ CTs photoelectrocatalytic material, it can be seen from FIG. 7 that extension of the electrochemical deposition time can enhance the flexible TiO 2 @ AC @ CTs photocatalytic material photoproduces electron/hole separation efficiency.
FIG. 8 in examples 1, 2 and 3, the TiO is flexible at different deposition times 2 Comparison of electrochemical impedance spectra of the @ AC @ CTs photoelectrocatalysis material. As can be seen from FIG. 8, extending the electrochemical deposition time can improve the flexibility of TiO 2 The photoproduction electron/hole separation efficiency of @ AC @ CTs photocatalytic materials.
FIG. 9 example 1, flexible TiO 2 In the process of degrading rhodamine B through electro-photocatalysis of @ AC @ CTs, the rhodamine B has ultraviolet-visible absorption spectrum with different degradation time. As can be seen in FIG. 9, the flexible TiO 2 The @ AC @ CTs photoelectric catalytic material has advantagesGood photoelectrocatalysis performance, and the degradation rate of the photoelectrocatalysis to rhodamine B is 95.2% within 60 min.
FIG. 10 example 2, a Flexible TiO 2 In the process of degrading rhodamine B through the photoelectrocatalysis of @ AC @ CTs, the rhodamine B has ultraviolet-visible absorption spectrum in different degradation time. As can be seen from FIG. 10, the flexible TiO 2 The @ AC @ CTs photoelectrocatalysis material has excellent photoelectrocatalysis performance, and the degradation rate of the photoelectrocatalysis to rhodamine B within 60 min is 99.8%. In addition, extending the electrochemical deposition time can improve the flexibility of the TiO 2 The photoelectrocatalytic efficiency of the @ AC @ CTs photoelectrocatalytic material.
FIG. 11 example 3, a Flexible TiO 2 In the process of degrading rhodamine B through the photoelectrocatalysis of @ AC @ CTs, the rhodamine B has ultraviolet-visible absorption spectrum in different degradation time. As can be seen from FIG. 11, the flexible TiO 2 The @ AC @ CTs photoelectrocatalysis material has excellent photoelectrocatalysis performance, and the degradation rate of the photoelectrocatalysis to rhodamine B is 99.9% within 60 min.
It should be noted that the above-mentioned embodiments illustrate rather than limit the scope of the invention, which is defined by the appended claims. It will be apparent to those skilled in the art that certain insubstantial modifications and adaptations of the present invention can be made without departing from the spirit and scope of the invention.

Claims (7)

1. The electrochemical preparation method of the photoelectrocatalysis material is characterized in that the photoelectrocatalysis material is flexible TiO 2 An @ AC @ CTs photocatalytic material, the method comprising the steps of:
(1) The method comprises the following steps of (1) depositing amorphous carbon on the surface of a carbon fiber fabric by using methane as a carbon source and adopting a chemical vapor deposition method to prepare a flexible AC @ CTs carbon/carbon composite material;
(2) Dissolving titanium sulfate and sodium nitrate in deionized water to obtain a solution A;
(3) Immersing flexible AC @ CTs carbon/carbon composite material serving as a working electrode into the solution A, and depositing TiO on the surface of the flexible AC @ CTs carbon/carbon composite material by adopting a constant potential method 2 A nanorod;
(4) Freeze drying and roasting the electrochemical deposition product to prepare flexible TiO 2 @ AC @ CTs photocatalytic material.
2. The electrochemical preparation method of a photoelectrocatalytic material as set forth in claim 1, wherein: in the step (1), the chemical vapor deposition is carried out under the protection of 180-240 SCCM argon, the carbon fiber fabric is heated to 900-1100 ℃, then 60-180 SCCM methane gas is introduced, the deposition time is 20-40 min, and the carbon fiber fabric is naturally cooled to the room temperature, so that the flexible AC @ CTs carbon/carbon composite material is obtained.
3. The electrochemical preparation method of a photoelectrocatalytic material according to claim 1, wherein: in the step (2), the mass concentration of the titanium sulfate in the solution A is 20 to 30 g/L, and the mass concentration of the sodium nitrate is 6 to 10 g/L.
4. The electrochemical preparation method of a photoelectrocatalytic material as set forth in claim 1, wherein: in the step (3), the electrochemical deposition time is 40-160 min.
5. The electrochemical preparation method of a photoelectrocatalytic material according to claim 1, wherein: in the step (4), the freeze drying time is 12 to 24h; the roasting temperature is 600 to 800 ℃, the time is 2 to 4h, the roasting atmosphere is argon atmosphere, and the argon flow speed is 40 to 60SCCM.
6. Flexible TiO produced by the electrochemical production method according to any one of claims 1 to 5 2 @ AC @ CTs.
7. The flexible TiO of claim 6 2 The application of the @ AC @ CTs photoelectrocatalysis material in the aspect of organic wastewater treatment.
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