Preparation method of slow light effect enhanced photo-thermal catalytic film and slow light effect enhanced photo-thermal catalytic film

Abstract

The invention provides a slow light effect enhanced photo-thermal catalytic film preparation method, which comprises: 1, taking silica microspheres and dopamine to prepare monodisperse polydopamine microspheres, 2, dispersing the monodisperse polydopamine microspheres in ethanol to obtain a dispersion liquid I, dropwise adding the dispersion liquid I to a glass substrate, and carrying out a reaction at a temperature of 80-120 DEG C to obtain a slow light effect enhanced photo-thermal catalytic film; 3, taking cadmium selenide (CdSe), dispersing the cadmium selenide (CdSe) in a perfluorosulfonic acid polymer (Nafion) ethanol solution to obtain a dispersion liquid II, dropwise adding the dispersion liquid II on the photonic crystal film in the step 2, and obtaining the slow light effect enhanced photo-thermal catalytic film after the solvent is volatilized. The invention also provides the slow light effect enhanced photo-thermal catalytic film prepared by the preparation method. According to the prepared slow light effect enhanced photo-thermal catalytic film, polydopamine has photo-thermal conversion performance, and the efficiency of converting carbon dioxide into carbon monoxide can be improved through the synergistic effect of polydopamine and cadmium selenide.

Description

Technical Field

[0001] The present invention relates to the technical field of functional materials, and in particular to a preparation method of a photothermal catalytic film with enhanced slow-light effect and a photothermal catalytic film with enhanced slow-light effect. Background Art

[0002] Photocatalytic materials play an important role in energy and environmental issues such as water pollution control, photolysis of water to produce hydrogen, and carbon dioxide reduction. General photocatalytic materials have certain requirements for the wavelength and intensity of light. Long-wavelength light (such as infrared light) is often difficult to participate in photocatalytic reactions efficiently. Photothermal catalytic materials can utilize both light energy and heat energy generated by photothermal conversion, and can participate in photocatalytic reactions more efficiently.

[0003] The traditional method of preparing photothermal catalytic materials is often to compound the photocatalyst with the photothermal material to achieve overall heating. This heating speed is relatively slow and the heat is easily dissipated.

[0004] In order to solve the above problems, the present invention provides a method for preparing a photothermal catalytic film with enhanced slow-light effect and a photothermal catalytic film with enhanced slow-light effect. Summary of the invention

[0005] In view of the shortcomings of the prior art, the purpose of the present invention is to provide a method for preparing a photothermal catalytic film with enhanced slow-light effect. Dopamine and silica microspheres are used to prepare monodisperse polydopamine microspheres, which are then self-assembled to obtain a photonic crystal film. The photonic crystal film having a polydopamine layer is attached to a photocatalytic material to prepare a photothermal catalytic film with enhanced slow-light effect.

[0006] To achieve the above technical problems, the present invention provides the following technical solutions:

[0007] A method for preparing a photothermal catalytic film with enhanced slow light effect, the preparation steps comprising:

[0008] Step 1: preparing monodisperse polydopamine microspheres by reacting silica microspheres with dopamine.

[0009] Step 2, dispersing the monodisperse polydopamine microspheres in ethanol to obtain a dispersion solution 1, dropping the dispersion solution 1 on a glass substrate, and self-assembling to obtain a photonic crystal film after the solvent evaporates;

[0010] Step three, dispersing cadmium selenide (CdSe) in a perfluorosulfonic acid polymer (Naf ion) ethanol solution to obtain dispersion liquid 2, and dropping dispersion liquid 2 onto the photonic crystal film in step two, and obtaining a photothermal catalytic film with enhanced slow light effect after the solvent evaporates.

[0011] Specifically, the step of preparing the monodisperse polydopamine microspheres in step 1 includes:

[0012] S1.1: Add Tris-HCl into deionized water and stir;

[0013] S1.2: Continue to add sodium hydroxide solution until the pH reaches 8.5;

[0014] S1.3: Add monodisperse silica microspheres and stir;

[0015] S1.4: Add dopamine and stir;

[0016] S1.5: Use common solvents such as ethanol and water as cleaning agents to perform centrifugal cleaning, repeat 3 to 5 times to obtain the monodisperse polydopamine microspheres.

[0017] Specifically, the conditions for preparing the monodisperse polydopamine microspheres in step 1 specifically include:

[0018] The concentration of Tris-HCl in S1.1 is 0.5 mmol / L, and the stirring time is 30 min;

[0019] The concentration of sodium hydroxide solution in S1.2 is 1.0 mol / L;

[0020] The mass of monodisperse silica microspheres added in S1.3 was 100 mg, and the stirring time was 30 min;

[0021] The amount of dopamine added in S1.4 was 20 mg, and the stirring time was 22 h;

[0022] The centrifugal speed in S1.5 is 10000r / min.

[0023] Specifically, the conditions for preparing the photonic crystal film in step 2 specifically include:

[0024] Take 1g of monodisperse polydopamine microspheres, dissolve in 5mL of anhydrous ethanol, stir for 30min, and the size of the glass substrate is 25*20mm 2 , thickness 1mm, and the amount of dispersion added per drop is 90μL.

[0025] Specifically, the conditions for preparing the slow-light effect enhanced photothermal catalytic film 1 in step 3 specifically include:

[0026] The amount of cadmium selenide (CdSe) is 0.2 g, the concentration of the perfluorosulfonic acid polymer (Nafion) ethanol solution is 1% 10 ml, and the amount of the second drop of the dispersion is 100 μL.

[0027] Another object of the present invention is to prepare a photothermal catalytic film with enhanced slow-light effect by using the above-mentioned method for preparing a photothermal catalytic film with enhanced slow-light effect.

[0028] The monodisperse polydopamine microspheres in the photonic crystal film obtained by the preparation method of the slow light effect enhanced photothermal catalytic film provided by the present invention are coated with a layer of polydopamine on the surface of the silicon dioxide microspheres. Since polydopamine has a strong adhesion ability, the monodisperse polydopamine microspheres can be adhered to each other, which is convenient for the photonic crystal film to adhere to cadmium selenide, and also convenient for the photothermal catalytic film of the present invention to adhere to other carriers. In addition, since polydopamine has photothermal conversion performance, its synergistic effect with cadmium selenide can improve the efficiency of converting carbon dioxide into carbon monoxide. BRIEF DESCRIPTION OF THE DRAWINGS

[0029] The present invention will be further described below in conjunction with the accompanying drawings and embodiments.

[0030] In the figure: Figure 1 Schematic diagram of the structure of monodisperse polydopamine microspheres;

[0031] Figure 2 Schematic diagram of the structure of the photothermal catalytic film enhanced by the slow light effect.

[0032] Figure 3 It is a bar graph of the photocatalytic performance of Example 1, Comparative Example 1 and Comparative Example 2.

[0033] 1. Slow light effect enhanced photothermal catalytic film; 10. Photonic crystal film; 11. Monodisperse polydopamine microspheres; 111. Monodisperse inner core microspheres; 112. Polydopamine layer; 20. Photocatalytic material layer. DETAILED DESCRIPTION

[0034] In order to make the above-mentioned objects, features and advantages of the present invention more obvious and easy to understand, the specific implementation methods of the present invention are described in detail below in conjunction with the embodiments of the specification. The methods described are all conventional methods unless otherwise specified, and the raw materials described can be obtained from public commercial channels unless otherwise specified.

[0035] The term "one embodiment" or "embodiment" as used herein refers to a specific feature, structure, or characteristic that may be included in at least one implementation of the present invention. The term "in one embodiment" that appears in different places in this specification does not necessarily refer to the same embodiment, nor is it a separate or selective embodiment that is mutually exclusive with other embodiments.

[0036] The present invention is further described below with reference to the embodiments.

[0037] Reference Figure 1-2A slow-light-effect enhanced photothermal catalytic film 1 of the present invention comprises a photonic crystal film 10 and a photocatalytic material layer 20 covering the surface of the photonic crystal film 10. The photonic crystal film 10 is self-assembled by a plurality of monodisperse polydopamine microspheres 11. The monodisperse polydopamine microspheres 11 comprise monodisperse core microspheres 111 and a polydopamine layer 112 wrapped on the surface of the monodisperse microspheres 111.

[0038] The present invention provides a method for preparing a photothermal catalytic film with enhanced slow light effect, and the preparation steps include:

[0039] Step 1: Prepare monodisperse polydopamine microspheres 11 by taking silica microspheres and dopamine.

[0040] S1.1: Take Tris-HCl, add it into deionized water, stir,

[0041] S1.2: Continue to add sodium hydroxide solution until the pH reaches 8.5.

[0042] S1.3: Add monodisperse silica microspheres and stir.

[0043] S1.4: Add dopamine, stir,

[0044] S1.5: Use ethanol, water and other common solvents as cleaning agents, perform centrifugal cleaning, repeat 3 to 5 times, and obtain monodisperse polydopamine microspheres 11.

[0045] Step 2: Monodisperse polydopamine microspheres 11 are dispersed in ethanol to obtain dispersion 1, and dispersion 1 is added dropwise onto a glass substrate. After the solvent evaporates, the dispersion 1 is self-assembled to obtain a photonic crystal film 10.

[0046] The polydopamine microspheres prepared in step 2 have uniform particle size and can be controlled by experimental parameters.

[0047] Step 3: Disperse cadmium selenide (CdSe) in a perfluorosulfonic acid polymer (Nafion) ethanol solution to obtain a dispersion solution 2, and dropwise add the dispersion solution 2 onto the photonic crystal film 10 in step 2, and after the solvent evaporates, obtain a photothermal catalytic film 1 with enhanced slow light effect.

[0048] S3.1: Disperse cadmium selenide (CdSe) in a 1% perfluorosulfonic acid polymer (Nafion) ethanol solution, referred to as dispersion solution 2.

[0049] S3.2: Take the above-mentioned photonic crystal film 10, drop the dispersion 2 onto the photonic crystal film 10, and after the solvent evaporates, obtain the photothermal catalytic film 1 with enhanced slow light effect.

[0050] Embodiment 1:

[0051] (1) Take 78.8 mg of tris-HCl, add it to 50 mL of deionized water, and stir for 30 min.

[0052] (2) Continue to add 1 mol / L sodium hydroxide until the pH reaches 8.5.

[0053] (3) Add 100 mg of monodisperse silica microspheres and stir for 30 min.

[0054] (4) Add 20 mg of dopamine and stir for 22 h.

[0055] (5) Using ethanol as a cleaning agent, centrifugal cleaning was performed three times at a speed of 10,000 r / min to obtain monodisperse polydopamine microspheres 11.

[0056] (6) Disperse 1 g of monodisperse polydopamine microspheres 11 in 5 mL of ethanol and stir for 30 min. This is referred to as dispersion 1.

[0057] (7) Take a glass substrate with a size of 25*20 mm and a thickness of 1 mm, add 90 μL of dispersion 1, and after the solvent evaporates, self-assemble to obtain the photonic crystal film 10.

[0058] (8) Disperse 0.2 g of cadmium selenide (CdSe) in 10 mL of 1% perfluorosulfonic acid polymer (Nafion) ethanol solution, which is referred to as dispersion solution 2.

[0059] (9) Take the above-mentioned photonic crystal film 10, drop 100 μL of dispersion liquid 2 onto the photonic crystal film 10, and after the solvent evaporates, obtain a photothermal catalytic film 1 with enhanced slow light effect.

[0060] Comparative Example 1:

[0061] (1) 0.2 g of cadmium selenide (CdSe) was dispersed in 10 mL of 1% perfluorosulfonic acid polymer (Nafion) ethanol solution, which was recorded as dispersion 1.

[0062] (2) Take a glass substrate with a size of 25*20 mm and a thickness of 1 mm, drop 100 μL of dispersion liquid 1 on the glass substrate, and after the solvent evaporates, a photocatalytic film is obtained.

[0063] Comparative Example 2:

[0064] (1) Disperse 1 g of monodisperse silica microspheres in 5 mL of ethanol and stir for 30 min. This is referred to as dispersion 1.

[0065] (2) Take a glass substrate with a size of 25*20 mm and a thickness of 1 mm, add 90 μL of dispersion 1, and after the solvent evaporates, self-assemble to obtain the photonic crystal film 10.

[0066] (3) 0.2 g of cadmium selenide (CdSe) was dispersed in 10 mL of 1% perfluorosulfonic acid polymer (Nafion) ethanol solution, which was recorded as dispersion solution 2.

[0067] (4) Take the above-mentioned photonic crystal film 10 (without the polydopamine layer 112), drip 100 μL of dispersion 2 onto the photonic crystal film 10 (without the polydopamine layer 112), and obtain a photothermal catalytic film after the solvent evaporates.

[0068] Experimental Example 1:

[0069] Take a piece of photothermal catalytic film of Example 1 and mix it with 100 μL H2O, and place the mixture at the bottom of a quartz glass vessel. Seal the reaction vessel, introduce carbon dioxide, and exhaust the air. After the air in the reaction vessel is exhausted, use a 300W xenon lamp as the light source, react for 10 hours, and after the reaction is completed, use a gas chromatograph to detect the concentration of carbon monoxide in the gas at the outlet of the reaction vessel, and take the average as the performance.

[0070]

[0071] η represents the carbon monoxide yield.

[0072] C co Represents the carbon monoxide concentration measured by the gas chromatograph;

[0073] T represents the reaction time;

[0074] Experimental Example 2:

[0075] Take a piece of photothermal catalytic film of comparative example 1 and mix it with 100 μL H2O, and place the mixture at the bottom of a quartz glass vessel. Seal the reaction vessel, introduce carbon dioxide, and exhaust the air. After the air in the reaction vessel is evacuated, use a 300W xenon lamp as the light source, react for 10 hours, and after the reaction is completed, use a gas chromatograph to detect the concentration of carbon monoxide in the gas at the outlet of the reaction vessel, and take the average as the performance.

[0076]

[0077] η represents the carbon monoxide yield.

[0078] C co Represents the carbon monoxide concentration measured by the gas chromatograph;

[0079] T represents the reaction time;

[0080] Experimental Example 3:

[0081] Take a piece of photothermal catalytic film of comparative example 2 and mix it with 100 μL H2O, and place the mixture at the bottom of a quartz glass vessel. Seal the reaction vessel, introduce carbon dioxide, and exhaust the air. After the air in the reaction vessel is evacuated, use a 300W xenon lamp as the light source, react for 10 hours, and use a gas chromatograph to detect the concentration of carbon monoxide in the gas at the outlet of the reaction vessel after the reaction is completed, and take the average as the performance.

[0082]

[0083] η represents the carbon monoxide yield.

[0084] C co Represents the carbon monoxide concentration measured by the gas chromatograph;

[0085] T represents the reaction time;

[0086] Table 1:

[0087] Carbon monoxide yields in Experimental Example 1, Experimental Example 2, and Experimental Example 3

[0088] project Example 1 Comparative Example 1 Comparative Example 2 <![CDATA[Yield (μmol g -1 h -1 )]]> 48 10 32

[0089] As shown in Table 1, compared with Comparative Example 1, Example 1 adds a photonic crystal film 10 prepared by monodisperse polydopamine microspheres 11, and the photon bandgap position of the photonic crystal film 10 is close to the absorption band edge of the photocatalytic material, thereby achieving photothermal catalysis enhanced by the slow light effect, and improving the photothermal catalytic performance by 4.8 times.

[0090] Compared with Comparative Example 2, Example 1 adds a polydopamine layer 112 on the surface of the silica microsphere microcore, and the photon bandgap position of the film is close to the absorption band edge of the photocatalytic material, achieving photothermal catalysis enhanced by the slow light effect, and improving the photothermal catalytic performance by 1.5 times.

[0091] Compared with Comparative Example 1, Comparative Example 2 adds a photonic crystal film 10 prepared from silica microspheres (without polydopamine layer 112 wrapping), and the photon bandgap position of the photonic crystal film 10 is close to the absorption band edge of the photocatalytic material, so that the photothermal catalytic performance is improved by 3.2 times.

[0092] Therefore, the photothermal catalytic film 1 with enhanced slow light effect and the preparation method provided by the present invention have at least the following beneficial effects:

[0093] The monodisperse polydopamine microspheres in the photonic crystal film obtained by the preparation method of the slow light effect enhanced photothermal catalytic film provided by the present invention are coated with a layer of polydopamine on the surface of the silicon dioxide microspheres. Since polydopamine has a strong adhesion ability, the monodisperse polydopamine microspheres can be adhered to each other, which is convenient for the photonic crystal film to adhere to cadmium selenide, and also convenient for the photothermal catalytic film of the present invention to adhere to other carriers. In addition, since polydopamine has photothermal conversion performance, its synergistic effect with cadmium selenide can improve the efficiency of converting carbon dioxide into carbon monoxide.

[0094] Photonic crystals have a special periodic structure, and their optical properties form a photonic bandgap. When the wavelength of light falls near the edge of the photonic bandgap, a slow light effect occurs, slowing down the group velocity of light. By constructing a photonic crystal film, the energy conversion from long-wavelength light to heat can be achieved through the oscillation of the lattice, which means that the propagation speed of light in the photonic crystal is reduced and the interaction time between light and matter is prolonged. In photothermal catalysis, this enables the catalyst to absorb the energy of photons more fully and improve the utilization rate of light, thereby providing more energy for the catalytic reaction, thereby increasing the temperature of the photocatalytic reaction, promoting the migration of carriers, and improving the photocatalytic activity.

[0095] The embodiments of the present invention have been described above, and the above description is exemplary, not exhaustive, and is not limited to the disclosed embodiments. Without departing from the scope and technical principles of the described embodiments, many modifications and changes are obvious to those of ordinary skill in the art, and these modifications and changes should also be regarded as the scope of protection of the present invention.

Claims

1. A method for preparing a photothermal catalytic film with enhanced slow light effect, comprising: Step 1: preparing monodisperse polydopamine microspheres by reacting silica microspheres with dopamine. Step 2, dispersing the monodisperse polydopamine microspheres in ethanol to obtain a dispersion solution 1, dropping the dispersion solution 1 on a glass substrate, and self-assembling to obtain a photonic crystal film after the solvent evaporates; Step three, dispersing cadmium selenide (CdSe) in a perfluorosulfonic acid polymer (Nafion) ethanol solution to obtain dispersion liquid 2, and dropping dispersion liquid 2 onto the photonic crystal film in step two, and obtaining a photothermal catalytic film with enhanced slow light effect after the solvent evaporates.

2. The method for preparing a photothermal catalytic film with enhanced slow light effect according to claim 1, characterized in that: The method for preparing the monodisperse polydopamine microspheres in step 1 is: S1.1: Add Tris-HCl into deionized water and stir; S1.2: Continue to add sodium hydroxide solution until the pH reaches 8.5; S1.3: Add monodisperse silica microspheres and stir; S1.4: Add dopamine and stir; S1.5: Use common solvents such as ethanol and water as cleaning agents to perform centrifugal cleaning, repeat 3 to 5 times to obtain the monodisperse polydopamine microspheres.

3. The method for preparing a photothermal catalytic film with enhanced slow light effect according to claim 2, characterized in that: The conditions for preparing the monodisperse polydopamine microspheres in step 1 specifically include: The concentration of Tris-HCl in S1.1 is 0.5 mmol / L, and the stirring time is 30 min; The concentration of sodium hydroxide solution in S1.2 is 1.0 mol / L; The mass of monodisperse silica microspheres added in S1.3 was 100 mg, and the stirring time was 30 min; The amount of dopamine added in S1.4 was 20 mg, and the stirring time was 22 h; The centrifugal speed in S1.5 is 10000r / min.

4. The method for preparing a photothermal catalytic film with enhanced slow light effect according to claim 1, characterized in that: The conditions for preparing the photonic crystal film in step 2 specifically include: Take 1g of monodisperse polydopamine microspheres, dissolve in 5mL of anhydrous ethanol, stir for 30min, and the size of the glass substrate is 25*20mm 2 , thickness 1mm, and the amount of dispersion added per drop is 90μL.

5. The method for preparing a photothermal catalytic film with enhanced slow light effect according to claim 6, characterized in that: The conditions for preparing the photothermal catalytic film with enhanced slow light effect in step 3 specifically include: The amount of cadmium selenide (CdSe) is 0.2 g, the concentration of the perfluorosulfonic acid polymer (Nafion) ethanol solution is 2.5% 10 ml, and the amount of the second drop of dispersion is 100 μL.

6. A photothermal catalytic film with enhanced slow light effect, characterized in that: The photothermal catalytic film is prepared by the method for preparing a photothermal catalytic film with enhanced slow light effect as described in any one of claims 1 to 5.

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