CN109364903B - High-specific-surface-area nano titanium dioxide photocatalytic coating and preparation method thereof - Google Patents
High-specific-surface-area nano titanium dioxide photocatalytic coating and preparation method thereof Download PDFInfo
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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
- B01J37/34—Irradiation by, or application of, electric, magnetic or wave energy, e.g. ultrasonic waves ; Ionic sputtering; Flame or plasma spraying; Particle radiation
- B01J37/349—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 flames, plasmas or lasers
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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
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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
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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
- B01J35/50—Catalysts, in general, characterised by their form or physical properties characterised by their shape or configuration
- B01J35/56—Foraminous structures having flow-through passages or channels, e.g. grids or three-dimensional monoliths
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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
- B01J37/02—Impregnation, coating or precipitation
- B01J37/0215—Coating
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Abstract
The invention relates to a high-specific surface area nano titanium dioxide photocatalytic coating and a preparation method thereof, belonging to the field of material preparation. The nano titanium dioxide powder is agglomerated into loose spherical particles, the loose spherical particles are conveyed into a high-power plasma spray gun (180kW-3000A, the air flow reaches 200slpm) in a low-pressure controlled environment (the pressure is less than 10mbar) through carrier gas, the loose spherical particles are completely gasified in expanded high-temperature high-speed jet flow, and then a nano titanium dioxide photocatalytic coating with a high specific surface area is formed at the tail end of the jet flow. The coating prepared by the invention has a feather-columnar micro-nano structure, high specific surface area, excellent adsorption performance and strong photocatalytic performance, and the preparation method is simple to operate, low in cost and suitable for industrial production.
Description
Technical Field
The invention relates to a high specific surface area nano titanium dioxide photocatalytic coating and a preparation method thereof.
Background
Environmental problems such as atmospheric environmental pollution and water resource pollution become key problems affecting human survival and development, and advanced environmental management technologies need to be developed. The photocatalytic technology is a technology for accelerating chemical reaction by means of a photocatalyst under the irradiation of light, can drive photocatalytic reaction by using continuous solar energy, and has potential application value in the fields of environment, energy and the like. Meanwhile, the catalyst has high catalytic efficiency, generates non-toxic byproducts, and is considered to be a feasible technology for solving the environmental problem.
TiO2The photocatalyst material has the advantages of stable chemical property, high durability, low price, no toxicity, strong oxidation capability and the like, and has the best application prospect. Wherein, the TiO is in the form of nano particles2The catalyst has small particle size, large specific surface area and high catalytic activity. However, in practice, in particular in the liquid phase, the granular catalyst requires subsequent centrifugation or filtration devices for its recycling, which undoubtedly increases the economic investment and the technical complexity. In addition, secondary environmental pollution may be caused. By sol-gel method, chemical vapor deposition method, thermal spray method, electrochemical methodAnd the like, can be used to prepare TiO2Preparation of TiO by fixing nanoparticles on a support2Coating to solve the recycling problem. However, in contrast to nano-particle TiO2Coating of TiO2The specific surface area of (A) is extremely low, so that the catalytic activity and the adsorption performance of the catalyst are greatly reduced.
The invention patent of 201610337956.X, a micro-nano structure composite coating and a preparation method thereof, adopts a liquid material thermal spraying mode to spray to prepare TiO with high corrosion resistance and bonding strength2And (4) coating. By adding polyurethane or absolute ethyl alcohol into the feed, the hydrophilic and hydrophobic properties of the surface of the coating are controllable, which is beneficial to the exertion of the photocatalysis function. Further, the invention patent with application number 201610336095.3 'a micro-nano structure photocatalytic coating and a preparation method thereof' uses hydroxyapatite to coat nano TiO2Forming a suspension of the composite material, and depositing the suspension on the surface of the substrate through a thermal spraying process to obtain the photocatalytic coating. The invention calls HA-TiO prepared by the method2The nano composite photocatalytic coating has the characteristics of porous micro-nano structure, excellent adsorption performance and strong photocatalytic performance, but the reported specific surface area is still lower and is only 104m2/g。
Disclosure of Invention
The invention aims to provide a high-specific surface area nano titanium dioxide photocatalytic coating aiming at the defects in the prior art.
The invention also aims to provide a preparation method of the nano titanium dioxide photocatalytic coating with high specific surface area.
A high-specific-surface-area nano titanium dioxide photocatalytic coating is characterized in that the coating material is composed of nano titanium dioxide, the thickness of the coating material is 100-200 mu m, the coating has a feather-column-shaped micro-nano structure, the porosity is not less than 25%, and the specific surface area is not less than 150m2/g。
The method for preparing the high specific surface area nano titanium dioxide photocatalytic coating according to claim 1, characterized in that the method comprises the following steps:
(1) adding TiO into the mixture2The powder is put into deionized water, and the binder and the dispersion are stableCarrying out high-speed ball milling and dispersing for 6-10 hours to prepare stable suspension slurry;
(2) carrying out high-speed centrifugal spray granulation on the suspension slurry obtained in the last step to obtain agglomerated powder;
(3) cleaning and decontaminating a substrate, installing the substrate on a sample support of a vacuum cavity, vacuumizing to 0.5mbar, backfilling argon to 40mbar, starting a high-power plasma spray gun, gradually vacuumizing to 1.5mbar, and enabling Ar-He plasma jet to expand;
(4) by using N2And (3) conveying the agglomerated powder in the step (2) into a high-power plasma spray gun by carrier gas, completely gasifying the agglomerated powder in a high-temperature and high-speed jet flow, and then forming a nano titanium dioxide coating with a feather-column micro-nano structure on a substrate.
The TiO is2The average particle diameter of the powder is 50nm, and the maximum particle diameter is not more than 100 nm.
The suspension slurry comprises the following components in percentage by mass: TiO 225-20% of powder, 0.1-10% of binder, 0.1-5% of dispersion stabilizer and the balance of deionized water.
The agglomerated powder has a loose structure and a particle size of 15-40 mu m.
The parameters for preparing the coating are as follows: the power of the high-power plasma spray gun is 100-180 kW, the argon gas flow is 60-100 slpm, the helium gas flow is 30-100 slpm, and the powder feeding carrier gas N is2The distance between the substrate and the spray gun is 950-2000 mm at 16L/min.
In order to analyze the microstructure and the performance of the coating prepared by the method and clarify the beneficial effects of the method, an X-ray diffractometer (XRD) is adopted to represent the phase of the coating, a Scanning Electron Microscope (SEM) is adopted to represent the section of the coating, a nitrogen adsorption method is adopted to detect the specific surface area of the coating, and the coating degrades methylene blue solution to represent the photocatalytic performance of the coating.
The invention has the beneficial effects that:
1) the coating prepared by the invention has a feather-columnar micro-nano structure, has excellent adsorption performance and is beneficial to TiO2The exertion of the photocatalytic function of (2);
2) the porosity of the coating prepared by the invention is not less than 25%, and the specific surface area is not more thanBelow 150m2(iv)/g, far exceeding prior art solutions;
3) the preparation method disclosed by the invention is simple to operate, low in cost and suitable for industrial production.
Drawings
FIG. 1 results of phase analysis of the coating of example 1: an alpha-anatase phase, a beta-rutile phase;
FIG. 2 SEM cross-section of the coating of example 2: 1) a substrate, 2) a coating;
figure 3 example 2 the coating degrades methylene blue.
Detailed Description
The preparation process of the present invention will be further described with reference to the following specific examples.
Example 1
(1) 100g of nano TiO2Putting the powder into 1000g of deionized water, sequentially adding 5g of polyethylene glycol and 1g of tannic acid, and carrying out high-speed ball milling and dispersion for 10 hours to prepare stable suspension slurry; (2) carrying out high-speed centrifugal spray granulation on the suspension slurry obtained in the last step to obtain agglomerated powder with the particle size of 15-40 microns;
(3) cleaning and decontaminating low-carbon steel, installing the low-carbon steel on a substrate support of a vacuum cavity, vacuumizing to 0.5mbar, backfilling argon to 40mbar, starting a high-power plasma spray gun, gradually vacuumizing to 1.5mbar, and enabling Ar-He plasma jet to expand;
(4) by using N2And (3) conveying the agglomerated powder in the step (2) into a high-power plasma spray gun by carrier gas, completely gasifying the agglomerated powder in a high-temperature and high-speed jet flow, and then forming a nano titanium dioxide coating on the substrate. The spraying parameters used were: the power of the high-power plasma spray gun is 125kW, the argon gas flow is 100slpm, the helium gas flow is 40slpm, and the powder feeding carrier gas N216L/min, the distance between the substrate and the spray gun was kept at 950 mm.
The coating phase was characterized using an X-ray diffractometer (XRD) and the corresponding test structure is shown in fig. 1. XRD spectrum analysis shows that the coating is mainly anatase phase and rutile phase, and mixed crystal of the two phases is favorable for improving the photocatalytic performance.
Example 2
(1) 100g of nano TiO2Putting the powder into 1000g of deionized water, sequentially adding 5g of polyethylene glycol and 2g of gum arabic, and carrying out high-speed ball milling and dispersion for 8 hours to prepare stable suspension slurry;
(2) carrying out high-speed centrifugal spray granulation on the suspension slurry obtained in the last step to obtain agglomerated powder with the particle size of 15-40 microns;
(3) cleaning and decontaminating a 316L stainless steel substrate, installing the substrate on a bracket of a vacuum cavity, vacuumizing to 0.5mbar, backfilling argon to 40mbar, starting a high-power plasma spray gun, gradually vacuumizing to 1.5mbar, and enabling Ar-He plasma jet to expand;
(4) by using N2And (3) conveying the agglomerated powder in the step (2) into a high-power plasma spray gun by carrier gas, completely gasifying the agglomerated powder in a high-temperature and high-speed jet flow, and then forming a nano titanium dioxide coating on the substrate. The spraying parameters used were: the power of the high-power plasma spray gun is 130kW, the argon flow is 90slpm, the helium flow is 35slpm, and the powder feeding carrier gas N216L/min, the distance between the substrate and the spray gun was kept at 950 mm.
The microstructure of the coating cross section was characterized using a Scanning Electron Microscope (SEM), and fig. 2 is a SEM photograph. According to analysis, the coating has a feather-column micro-nano structure, and a large number of pores exist among feather-column micro-structure units, so that the coating is different from a photocatalytic coating obtained by the existing preparation technology.
Example 3
(1) 100g of nano TiO2Putting the powder into 1000g of deionized water, sequentially adding 5g of polyvinylpyrrolidone and 1g of tannic acid, and carrying out high-speed ball milling and dispersion for 10 hours to prepare stable suspension slurry;
(2) carrying out high-speed centrifugal spray granulation on the suspension slurry obtained in the last step to obtain agglomerated powder with the particle size of 15-40 microns;
(3) cleaning and decontaminating low-carbon steel, installing the low-carbon steel on a substrate support of a vacuum cavity, vacuumizing to 0.5mbar, backfilling argon to 40mbar, starting a high-power plasma spray gun, gradually vacuumizing to 1.5mbar, and enabling Ar-He plasma jet to expand;
(4) by using N2And (3) conveying the agglomerated powder in the step (2) into a high-power plasma spray gun by carrier gas, completely gasifying the agglomerated powder in a high-temperature and high-speed jet flow, and then forming a nano titanium dioxide coating on the substrate. The spraying parameters used were: the power of the high-power plasma spray gun is 125kW, the argon gas flow is 100slpm, the helium gas flow is 40slpm, and the powder feeding carrier gas N216L/min, the distance between the substrate and the spray gun was kept at 950 mm. The porosity of the coating is 26 percent and the specific surface area is 167m through the test of a nitrogen adsorption method2The coating is much higher than the coating prepared by the prior art.
Example 4
The photocatalytic performance of the coating was characterized by the degradation of the methylene blue solution of the coating:
1) a methylene blue solution was prepared at a concentration of 5ppm, and 50ml of the solution was placed in a petri dish.
2) The coating prepared in example 2 was cut into 4X4cm size samples and placed in methylene blue solution.
3) And (4) placing the methylene blue solution containing the sample in a dark room, and turning on an ultraviolet lamp for degradation. The power of the ultraviolet lamp is 15W, the wavelength is 365nm, and the distance between the sample and the ultraviolet lamp tube is kept at 15 cm. And (3) taking 5ml of methylene blue solution at an interval of 0.5h after the ultraviolet lamp is started, carrying out an absorbance test, and calculating the concentration of the methylene blue in the solution according to the absorbance value of the methylene blue at the wavelength of 664 nm. Fig. 3 shows the corresponding test results, concentrations. As can be seen from the degradation curve in the figure, compared with the pure blank group, the prepared coating has good degradation performance, and about 75% of methylene blue solution is degraded after 3.5 h.
It should be noted that the above-mentioned embodiments can enable those skilled in the art to more fully understand the present invention, but do not limit the present invention in any way. Thus, while the invention has been described in detail in this specification, it will be understood by those skilled in the art that various changes may be made and equivalents may be substituted; all technical solutions and modifications that do not depart from the spirit of the invention are intended to be included within the scope of the invention.
Claims (5)
1. High-specific-surface-area nano titanium dioxide photocatalysisThe coating is characterized in that the coating material is composed of nano titanium dioxide, the thickness of the coating is 100-200 mu m, the coating has a feather-column micro-nano structure, the porosity is not less than 25%, and the specific surface area is not less than 150m2The preparation method of the high specific surface area nano titanium dioxide photocatalytic coating comprises the following steps:
(1) adding TiO into the mixture2Placing the powder into deionized water, sequentially adding a binder and a dispersion stabilizer, and performing high-speed ball milling and dispersion for 6-10 hours to prepare stable suspension slurry;
(2) carrying out high-speed centrifugal spray granulation on the suspension slurry obtained in the last step to obtain agglomerated powder;
(3) cleaning and decontaminating a substrate, installing the substrate on a sample support of a vacuum cavity, vacuumizing to 0.5mbar, backfilling argon to 40mbar, starting a high-power plasma spray gun, gradually vacuumizing to 1.5mbar, and enabling Ar-He plasma jet to expand;
(4) by using N2The carrier gas sends the agglomerated powder in the step (2) into a high-power plasma spray gun to enable the agglomerated powder to be completely gasified in high-temperature and high-speed jet flow, the power of the high-power plasma spray gun is 100-180 kW, the argon flow is 60-100 slpm, the helium flow is 30-100 slpm, and the powder-feeding carrier gas N2The thickness of the coating is 16L/min, the distance between a substrate and a spray gun is 950-2000 mm, and then a nano titanium dioxide coating with a feather-column micro-nano structure is formed on the substrate.
2. The coating of claim 1, wherein the TiO is selected from the group consisting of2The average particle diameter of the powder is 50nm, and the maximum particle diameter is not more than 100 nm.
3. The coating of claim 1, wherein the suspending slurry comprises, in component to mass ratio: TiO 225-20% of powder, 0.1-10% of binder, 0.1-5% of dispersion stabilizer and the balance of deionized water.
4. The coating of claim 1, wherein the agglomerated powder has a loose structure and a particle size of 15 to 40 μm.
5. Use of the coating of claim 1 in photocatalysis.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811233516.5A CN109364903B (en) | 2018-10-23 | 2018-10-23 | High-specific-surface-area nano titanium dioxide photocatalytic coating and preparation method thereof |
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| CN111167469A (en) * | 2020-01-10 | 2020-05-19 | 北京工业大学 | Wire mesh with selective catalytic denitration function and preparation method thereof |
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| CN113941372A (en) * | 2021-09-29 | 2022-01-18 | 凯龙蓝烽新材料科技有限公司 | Production system of wall-flow type carrier catalyst |
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