Preparation method of PDACN-Si photocatalytic hydrogen production catalyst

Abstract

The application discloses a preparation method of a PDACN-Si photocatalyst for photocatalytic hydrogen production, and belongs to the field of photocatalysts. The method adopts a template method and a microwave-assisted heating strategy, uses dicyandiamide as a carbon nitride synthesis precursor, uses SiO2 as a hard template, and makes dicyandiamide and 2-aminothiophene-3-carbonitrile rapidly polymerize on the SiO2 template under microwave-assisted heating, and then etches the SiO2 template through NaOH, so that a PDACN-Si photocatalyst with a honeycomb structure of macropores is successfully prepared. The prepared PDACN-Si catalyst shows excellent photocatalytic activity in a photocatalytic hydrogen production reaction process.

Description

Technical Field

[0001] This invention belongs to the field of photocatalytic hydrogen production catalysts, specifically relating to PDACN-Si photocatalytic hydrogen production catalysts. Background Technology

[0002] Currently, my country is accelerating the transformation of its energy utilization methods and vigorously improving energy efficiency. Oil, gas, and coal resources are stored underground, with high exploration and development costs, significant environmental pollution, and dwindling resources. In contrast, wind and solar resources are inexhaustible, located on the surface, with low exploration and development costs and positive ecological effects. Therefore, the utilization and production of clean energy have attracted much attention from researchers.

[0003] Graphite carbon nitride (g-C3N4) has attracted widespread attention as a stable, easily synthesized, and readily functionalized visible light photocatalyst with high activity and stability. To date, high-nitrogen-content molecules such as dicyandiamide, melamine, and urea have been routinely used as precursors for g-C3N4 production. These precursors are obtained by calcination in air or an inert atmosphere at high temperatures (400–600 °C). During the polycondensation of g-C3N4, these high-nitrogen-content molecules can form various intermediates through several different reaction pathways. However, the low visible light utilization rate and high photogenerated electron-hole recombination efficiency of g-C3N4 remain problems. Therefore, improving the visible light photocatalytic activity of g-C3N4 has become a hot research topic.

[0004] In the research of photocatalytic hydrogen production catalysts, the main research direction is to select appropriate precursors, find suitable synthesis methods, and then modify them to improve catalytic activity. Summary of the Invention

[0005] This invention, considering the practical value of g-C3N4 photocatalysts, the comprehensive catalytic effect, and overcoming the shortcomings of the prior art, provides a method for preparing a PDACN-Si photocatalytic hydrogen production catalyst and its application. It addresses the deficiencies in the catalytic activity and stability of existing g-C3N4 photocatalysts, as well as the complexity of the synthesis process. The invention also discloses the selection and adjustment of the obtained PDACN-Si catalyst, demonstrating its promising prospects for practical application.

[0006] The preparation method of the PDACN-Si photocatalytic hydrogen production catalyst and its application according to the present invention are as follows:

[0007] A method for preparing a PDACN-Si photocatalytic hydrogen production catalyst includes the following steps:

[0008] Step 1: Disperse dicyandiamide in deionized water and stir until homogeneous to obtain a mixed solution;

[0009] Step 2: Disperse the silica in the mixed solution from Step 1 and stir until homogeneous to obtain a mixed solution;

[0010] Step 3: Freeze-dry the mixed solution obtained in Step 2 to remove moisture, and obtain a white solid;

[0011] Step 4: Place the white solid obtained in Step 3 into a crucible, irradiate it with microwave to obtain a light yellow block, and grind it into a light yellow powder in a mortar.

[0012] Step 5: Soak the yellow powder from Step 4 in sodium hydroxide solution, stir to dissolve the silicon dioxide, and obtain a yellow mixed solution;

[0013] Step 6: Filter, wash, dry and collect the yellow mixed solution from Step 5 to obtain the PDACN-Si catalyst.

[0014] Furthermore, 2-aminothiophene-3-carboxynitrile is also added to the mixed solution in step 1.

[0015] More preferably, the mass ratio of dicyandiamide and 2-aminothiophene-3-carboxynitrile in step 1 is (1.2 ~ 4):0.02.

[0016] Furthermore, the microwave irradiation method in step 4 involves placing a white solid into a crucible, inverting it into another crucible, filling the space between the two crucibles with insulating material, placing the two sealed crucibles into an outer crucible containing copper oxide powder, filling and sealing it with CuO, covering the crucible with a lid, and placing it in the center of a microwave oven.

[0017] Furthermore, the parameters for microwave irradiation in step 4 are: power 500 ~ 600 W, time 20 ~ 30 min.

[0018] Furthermore, the concentration of NaOH in step 5 is 0 ~ 2 mol / L.

[0019] The PDACN-Si photocatalytic hydrogen production catalyst obtained by the preparation method described above.

[0020] The PDACN-Si photocatalytic hydrogen production catalyst described herein is used as a photocatalyst in the photocatalytic production of hydrogen.

[0021] Compared with the prior art, the beneficial effects of the present invention are as follows:

[0022] In this invention, (1) a self-doped sulfur source can be achieved by copolymerizing 2-aminothiophene-3-carboxynitrile with dicyandiamide. A strategy combining template method and microwave irradiation heating can be used to easily prepare macroporous photocatalytic materials. Using dicyandiamide and 2-aminothiophene-3-carboxynitrile as precursors, rapid polymerization of the precursors can be achieved using microwave irradiation heating, successfully incorporating sulfur into the catalyst and synthesizing a catalyst with a macroporous honeycomb structure. By copolymerizing 2-aminothiophene-3-carboxynitrile with dicyandiamide, sulfur-containing groups can be introduced into the g-C3N4 structural framework, forming sulfur-doped graphitic carbon nitride with a high specific surface area. The photocatalyst synthesized in this way, with its good sheet-like bulk and dispersibility, exhibits high photocatalytic activity.

[0023] (2) In this invention, a DACN-Si catalyst is prepared using SiO2 as a template, and then the SiO2 in the catalyst is etched away using NaOH, so that the obtained PDACN-Si catalyst forms a defect structure. The preparation method using SiO2 as a hard template makes the specific surface area of ​​the PDACN-Si material higher, which is conducive to the exposure of more active sites, enhances electron transport and mass transfer processes, and the surface pore size of the catalyst can be adjusted by adjusting the size of the SiO2 hard template. The catalyst synthesized by this method can not only enhance light absorption, but also inhibit the recombination of electrons and holes, and at the same time has a large specific surface area, which makes it have higher photocatalytic activity.

[0024] (3) The catalyst preparation scheme of this invention is a synthesis technique with adjustable catalyst morphology. In this invention, graphitic carbon nitride is synthesized by replacing the traditional high-temperature heating process of muffle furnace / tube furnace with microwave irradiation heating. CuO is used as a microwave absorber. CuO can strongly and effectively absorb microwaves and can raise the temperature to 1285 K within 7 min, which can realize the rapid polymerization of the precursor. Compared with the traditional muffle furnace / tube furnace heating method, the carbon nitride material synthesized by microwave irradiation heating has higher crystallinity and a more obvious and single lamellar structure. Moreover, the lamellar structure of graphitic carbon nitride does not show blocky aggregation, which effectively enhances the specific surface area of ​​graphitic carbon nitride. Furthermore, compared with muffle furnace / tube furnace heating, microwave irradiation heating requires less heating time, which greatly saves synthesis costs and improves catalyst preparation efficiency.

[0025] (4) The graphitic carbon nitride obtained by copolymerization of 2-aminothiophene-3-carboxynitrile and dicyandiamide involved in this invention is prepared by a one-pot method, without involving the cumbersome preparation process of secondary catalytic recombination. It is a simple and efficient method for preparing photocatalysts.

[0026] (5) The PDACN-Si prepared by the method described above is used as a photocatalyst material in the photocatalytic hydrogen production process. Under experimental conditions, it exhibits excellent photocatalytic activity, and the hydrogen evolution rate reaches 864.87 µmol / h under visible light irradiation (λ>420nm). -1 g -1 It is 4.37 times that of the unmodified carbon nitride (DCN) sample, which greatly improves the photocatalytic performance. Attached Figure Description

[0027] Figure 1 A scanning electron microscope (SEM) schematic diagram of the PDACN-Si-100 prepared for implementation of Case 1;

[0028] Figure 2 X-ray diffraction patterns for implementation cases 1, 4, 5, and 6 are shown;

[0029] Figure 3 The schematic diagram shows the photocatalytic hydrogen production performance of PDACN-Si prepared in Case 1, 2, and 3.

[0030] Figure 4 The schematic diagram shows the photocatalytic hydrogen production performance of Case 4, 5, and 6. Detailed Implementation

[0031] The technical solutions in the examples of this invention are clearly and completely described below. Obviously, the described examples are only a part of the examples of this invention, and not all of them. Based on the embodiments of this invention, all other embodiments obtained by those skilled in the art without creative effort are within the scope of protection of this invention.

[0032] Unless otherwise specified, the experimental and testing methods described below are conventional methods; unless otherwise specified, the reagents and raw materials described below are commercially available.

[0033] Example 1

[0034] Step 1: Disperse 2 g of dicyandiamide and 20 mg of 2-aminothiophene-3-carboxynitrile in 15 ml of deionized water and stir magnetically until homogeneous to obtain a mixed solution;

[0035] Step 2: Disperse 1 g of silicon dioxide (SiO2) in the mixed solution of Step 1, and stir magnetically until a uniform mixed solution is obtained;

[0036] Step 3: Freeze-dry the mixed solution obtained in Step 2 to remove moisture, and obtain a white solid;

[0037] Step 4: Place the white solid obtained in Step 3 into a crucible and microwave it at 600 W for 30 min to obtain a light yellow block, and grind it into a light yellow powder in a mortar.

[0038] Step 5: Soak the yellow powder from Step 4 in 100 ml of 2 mol / L sodium hydroxide (NaOH) solution and stir magnetically for 12 h to obtain a yellow mixed solution;

[0039] Step 6: Filter, wash, dry and collect the yellow mixed solution from Step 5 to obtain the PDACN-Si-100 catalyst.

[0040] Step 7: First, take 20 mg of PDACN-Si-100 photocatalyst and place it in a top-illuminated quartz reactor. Add 18 mL of deionized water, and then measure 2 mL of 10 vol% triethanolamine as a sacrificial agent. Next, add a certain amount of H2PtCl6 to the resulting suspension for in-situ photodeposition of Pt as a co-catalyst. The mass fraction of Pt is 3%. Sonicate for 3 min to ensure thorough dispersion and obtain a uniform suspension. Before using a xenon lamp for irradiation, purge with ultrapure N2 for 20 min to remove dissolved O2 from the water, achieving complete air purification within the reactor. A 300W xenon lamp and an ultraviolet cutoff filter (λ>420 nm) are used for the photocatalytic reaction. The xenon lamp model is Beijing PLS-SXE 300, with an output light intensity of 100 mW cm⁻¹. -2 The product was analyzed using a gas chromatograph (Shimadzu GC-2014, with high-purity nitrogen as the carrier gas) equipped with a thermal conductivity detector and a 5A molecular sieve column. Product samples were extracted from the sealed reactor every hour for analysis.

[0041] The photocatalytic performance of the PDACN-Si-100 catalyst prepared in this embodiment was tested, as follows: Figure 2 As shown, the photocatalytic hydrogen production rate under the experimental conditions was 864.87 µmol•h. -1 ·g -1 .

[0042] Example 2

[0043] Step 1: Disperse 1.2 g of dicyandiamide and 20 mg of 2-aminothiophene-3-carboxynitrile in 15 ml of deionized water and stir magnetically until homogeneous to obtain a mixed solution;

[0044] Step 2: Disperse 1 g of silicon dioxide (SiO2) in the mixed solution of Step 1, and stir magnetically until a uniform mixed solution is obtained;

[0045] Step 3: Freeze-dry the mixed solution obtained in Step 2 to remove moisture, and obtain a white solid;

[0046] Step 4: Place the white solid obtained in Step 3 into a crucible and microwave it at 600 W for 30 min to obtain a light yellow block, and grind it into a light yellow powder in a mortar.

[0047] Step 5: Soak the yellow powder from Step 4 in 100 ml of 2 mol / L sodium hydroxide (NaOH) solution and stir magnetically for 12 h to obtain a yellow mixed solution;

[0048] Step 6: Filter, wash, dry and collect the yellow mixed solution from Step 5 to obtain the PDACN-Si-60 catalyst.

[0049] Step 7: First, take 20 mg of PDACN-Si-60 photocatalyst and place it in a top-illuminated quartz reactor. Add 18 mL of deionized water, and then measure 2 mL of 10 vol% triethanolamine as a sacrificial agent. Next, add a certain amount of H2PtCl6 to the resulting suspension, and in-situ photodeposit Pt as a co-catalyst. The mass fraction of Pt is 3%. Sonicate for 3 min to ensure thorough dispersion and obtain a uniform suspension. Before using a xenon lamp for irradiation, purge with ultrapure N2 for 20 min to remove dissolved O2 from the water, achieving complete air purification within the reactor. A 300W xenon lamp and an ultraviolet cutoff filter (λ>420 nm) are used for the photocatalytic reaction. The xenon lamp model is Beijing PLS-SXE 300, with an output light intensity of 100 mW cm⁻¹. -2 The product was analyzed using a gas chromatograph (Shimadzu GC-2014, with high-purity nitrogen as the carrier gas) equipped with a thermal conductivity detector and a 5A molecular sieve column. Product samples were extracted from the sealed reactor every hour for analysis.

[0050] Example 3

[0051] Step 1: Disperse 4 g of dicyandiamide and 20 mg of 2-aminothiophene-3-carboxynitrile in 15 ml of deionized water and stir magnetically until homogeneous to obtain a mixed solution;

[0052] Step 2: Disperse 1 g of silicon dioxide (SiO2) in the mixed solution of Step 1, and stir magnetically until a uniform mixed solution is obtained;

[0053] Step 3: Freeze-dry the mixed solution obtained in Step 2 to remove moisture, and obtain a white solid;

[0054] Step 4: Place the white solid obtained in Step 3 into a crucible and microwave it at 600 W to obtain a light yellow block, and grind it into a light yellow powder in a mortar.

[0055] Step 5: Soak the yellow powder from Step 4 in 100 ml of 2 mol / L sodium hydroxide (NaOH) solution and stir magnetically for 12 h to obtain a yellow mixed solution;

[0056] Step 6: Filter, wash, dry and collect the yellow mixed solution from Step 5 to obtain the PDACN-Si-200 catalyst.

[0057] Step 7: First, take 20 mg of PDACN-Si-200 photocatalyst and place it in a top-illuminated quartz reactor. Add 18 mL of deionized water, and then measure 2 mL of 10 vol% triethanolamine as a sacrificial agent. Next, add a certain amount of H2PtCl6 to the resulting suspension, and in-situ photodeposit Pt as a co-catalyst. The mass fraction of Pt is 3%. Sonicate for 3 min to ensure thorough dispersion and obtain a uniform suspension. Before using a xenon lamp for irradiation, purge with ultrapure N2 for 20 min to remove dissolved O2 from the water, achieving complete air purification within the reactor. A 300W xenon lamp and an ultraviolet cutoff filter (λ>420 nm) are used for the photocatalytic reaction. The xenon lamp model is Beijing PLS-SXE 300, with an output light intensity of 100 mW cm⁻¹. -2 The product was analyzed using a gas chromatograph (Shimadzu GC-2014, with high-purity nitrogen as the carrier gas) equipped with a thermal conductivity detector and a 5A molecular sieve column. Product samples were extracted from the sealed reactor every hour for analysis.

[0058] Example 4

[0059] Step 1: Disperse 1.2 g of dicyandiamide in 15 ml of deionized water and stir magnetically until homogeneous to obtain a mixed solution;

[0060] Step 2: Freeze-dry the mixed solution obtained in Step 1 to remove moisture, and obtain a white solid;

[0061] Step 3: Place the white solid obtained in Step 2 into a crucible and microwave it at 600 W for 30 min to obtain a light yellow block. Grind the block into a light yellow powder in a mortar to obtain the DCN catalyst.

[0062] Step 4: First, take 20 mg of DCN photocatalyst and place it in a top-illuminated quartz reactor. Add 18 mL of deionized water, and then measure 2 mL of 10 vol% triethanolamine as a sacrificial agent. Next, add a certain amount of H2PtCl6 to the resulting suspension for in-situ photodeposition of Pt as a co-catalyst. The mass fraction of Pt is 3%. Sonicate for 3 min to ensure thorough dispersion and obtain a uniform suspension. Before using the xenon lamp for irradiation, purge with ultrapure N2 for 20 min to remove dissolved O2 from the water, achieving complete air purification within the reactor. A 300W xenon lamp and an ultraviolet cutoff filter (λ>420 nm) are used for the photocatalytic reaction. The xenon lamp model is Beijing PLS-SXE 300, with an output light intensity of 100 mW cm⁻¹. -2 The product was analyzed using a gas chromatograph (Shimadzu GC-2014, with high-purity nitrogen as the carrier gas) equipped with a thermal conductivity detector and a 5A molecular sieve column. Product samples were extracted from the sealed reactor every hour for analysis.

[0063] Example 5

[0064] Step 1: Disperse 1.2 g of dicyandiamide and 20 mg of 2-aminothiophene-3-carboxynitrile in 15 ml of deionized water and stir magnetically until homogeneous to obtain a mixed solution;

[0065] Step 2: Freeze-dry the mixed solution obtained in Step 1 to remove moisture, and obtain a white solid;

[0066] Step 3: Place the white solid obtained in Step 2 into a crucible and microwave it at 600 W for 30 min to obtain a light yellow block. Grind the block into a light yellow powder in a mortar to obtain the DACN catalyst.

[0067] Step 4: First, take 20 mg of DACN photocatalyst and place it in a top-illuminated quartz reactor. Add 18 mL of deionized water, and then measure 2 mL of 10 vol% triethanolamine as a sacrificial agent. Next, add a certain amount of H2PtCl6 to the resulting suspension for in-situ photodeposition of Pt as a co-catalyst. The mass fraction of Pt is 3%. Sonicate for 3 min to ensure thorough dispersion and obtain a uniform suspension. Before using the xenon lamp for irradiation, purge with ultrapure N2 for 20 min to remove dissolved O2 from the water, achieving complete air purification within the reactor. A 300W xenon lamp and an ultraviolet cutoff filter (λ>420 nm) are used for the photocatalytic reaction. The xenon lamp model is Beijing PLS-SXE 300, with an output light intensity of 100 mW cm⁻¹. -2The product was analyzed using a gas chromatograph (Shimadzu GC-2014, with high-purity nitrogen as the carrier gas) equipped with a thermal conductivity detector and a 5A molecular sieve column. Product samples were extracted from the sealed reactor every hour for analysis.

[0068] Example 6

[0069] Step 1: Disperse 4 g of dicyandiamide and 20 mg of 2-aminothiophene-3-carboxynitrile in 15 ml of deionized water and stir magnetically until homogeneous to obtain a mixed solution;

[0070] Step 2: Disperse 1 g of silicon dioxide (SiO2) in the mixed solution of Step 1, and stir magnetically until a uniform mixed solution is obtained;

[0071] Step 3: Freeze-dry the mixed solution obtained in Step 2 to remove moisture, and obtain a white solid;

[0072] Step 4: Place the white solid obtained in Step 3 into a crucible and irradiate it with microwave at 600 W to obtain a light yellow block. Grind it into a light yellow powder in a mortar to obtain the DACN-Si catalyst.

[0073] Step 7: First, take 20 mg of DACN-Si photocatalyst and place it in a top-illuminated quartz reactor. Add 18 mL of deionized water, and then measure 2 mL of 10 vol% triethanolamine as a sacrificial agent. Next, add a certain amount of H2PtCl6 to the resulting suspension, and in-situ photodeposit Pt as a co-catalyst. The mass fraction of Pt is 3%. Sonicate for 3 min to ensure thorough dispersion and obtain a uniform suspension. Before using a xenon lamp for irradiation, purge with ultrapure N2 for 20 min to remove dissolved O2 from the water, achieving complete air purification within the reactor. A 300W xenon lamp and an ultraviolet cutoff filter (λ>420 nm) are used for the photocatalytic reaction. The xenon lamp model is Beijing PLS-SXE 300, with an output light intensity of 100 mW cm⁻¹. -2 The product was analyzed using a gas chromatograph (Shimadzu GC-2014, with high-purity nitrogen as the carrier gas) equipped with a thermal conductivity detector and a 5A molecular sieve column. Product samples were extracted from the sealed reactor every hour for analysis.

[0074] Characterization tests were performed on the sample in Example 1, and the results showed that:

[0075] Please see Figure 1 , Figure 1 The image shows a scanning electron microscope (SEM) image of the PDACN-Si-100 sample prepared in Example 1. As can be seen from the image, the lamellar structure of the sample was not destroyed by etching the SiO2 hard template with NaOH. The lamellars became thinner and all had obvious honeycomb-like macroporous structures.

[0076] Please see Figure 2 , Figure 2 The X-ray diffraction patterns of the samples prepared in Examples 1, 4, 5, and 6 are shown in the figure. As can be seen from the figure, Examples 1, 4, 5, and 6 all exhibit typical g-C3N4 diffraction peaks, indicating that carbon nitride can be obtained by thermal polycondensation of dicyandiamide and 2-aminothiophene-3-carboxynitrile.

[0077] Please see Figure 3 , Figure 3 This is a schematic diagram of the photocatalytic performance of the catalysts prepared in Examples 1, 2, and 3 of this invention. It can be seen that the photocatalytic hydrogen production rates of the catalysts prepared in Examples 1, 2, and 3 are 864.87 µmol / h, respectively. -1 g -1 508.125 µmol h -1 g -1 and 261.25 µmol h -1 g -1 By etching the SiO2 hard template with NaOH to create macropores in the sample structure, and by copolymerizing 2-aminothiophene-3-carboxynitrile with dicyandiamide, sulfur was introduced into the sample structural framework, which significantly improved the photocatalytic performance of the sample.

[0078] Please see Figure 4 , Figure 4 These are schematic diagrams illustrating the photocatalytic performance of the catalysts prepared in Examples 4, 5, and 6 of this invention. It can be seen that the photocatalytic hydrogen production rates of the catalysts prepared in Examples 4, 5, and 6 are 198.03 µmol / h, respectively. -1 g -1 335.63 µmol h -1 g -1 and 345.78 µmol h -1 g -1 By comparing with Examples 1, 2, and 3, it is shown that creating macropores in the sample structure and copolymerizing 2-aminothiophene-3-carboxynitrile with dicyandiamide to introduce sulfur into the sample structural framework can significantly improve the photocatalytic performance of the sample.

[0079] The above results demonstrate that the PDACN-Si photocatalyst of this invention exhibits a considerably high level of photocatalytic activity under ambient temperature and pressure conditions, as tested in photocatalytic hydrogen production performance tests. The PDACN-Si catalyst prepared in Example 1 achieved a photocatalytic hydrogen production rate of 864.87 µmol / h. -1 g -1 It is 4.37 times that of unmodified carbon nitride (Example 4), which greatly improves the photocatalytic activity of PDACN-Si.

[0080] Although the embodiments of the present invention have been disclosed above, they are not limited to the applications listed in the specification and embodiments. They can be applied to various fields suitable for the present invention. For those skilled in the art, other modifications can be easily made. Therefore, without departing from the general concept defined by the claims and their equivalents, the present invention is not limited to the specific details.

Claims

1. A method for preparing a PDACN-Si photocatalytic hydrogen production catalyst, characterized in that, Includes the following steps: Step 1: Disperse dicyandiamide in deionized water and stir until homogeneous to obtain a mixed solution; Step 2: Disperse silica in the mixed solution from Step 1 and stir until homogeneous to obtain a mixed solution, wherein 2-aminothiophene-3-formonitrile is also added to the mixed solution; Step 3: Freeze-dry the mixed solution obtained in Step 2 to remove moisture, and obtain a white solid; Step 4: Place the white solid obtained in Step 3 into a crucible, irradiate it with microwave to obtain a light yellow block, and grind it into a light yellow powder in a mortar. Step 5: Soak the yellow powder from Step 4 in sodium hydroxide solution, stir to dissolve the silicon dioxide, and obtain a yellow mixed solution; Step 6: Filter, wash, dry and collect the yellow mixed solution from Step 5 to obtain the PDACN-Si catalyst.

2. The preparation method of the PDACN-Si photocatalytic hydrogen production catalyst according to claim 1, characterized in that, The mass ratio of dicyandiamide and 2-aminothiophene-3-carboxynitrile in step 1 is (1.2 ~ 4):0.

02.

3. The preparation method of the PDACN-Si photocatalytic hydrogen production catalyst according to claim 1, characterized in that, The microwave irradiation method in step 4 is as follows: a white solid is placed in a crucible, which is then inverted into another crucible. The space between the two crucibles is filled with insulating material. The two sealed crucibles are then placed into an outer crucible containing copper oxide powder, filled and sealed with CuO, and the crucible lid is placed on top. The crucible is then placed in the center of the microwave oven.

4. The preparation method of the PDACN-Si photocatalytic hydrogen production catalyst according to claim 1, characterized in that, The parameters for microwave irradiation in step 4 are: power 500 ~ 600 W, time 20 ~ 30 min.

5. The method for preparing the PDACN-Si photocatalytic hydrogen production catalyst according to claim 1, characterized in that, The concentration of NaOH in step 5 is 2 mol / L.

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