CN114308132A - Protonated CdS-COF-366-M composite photocatalyst and preparation method thereof - Google Patents

Protonated CdS-COF-366-M composite photocatalyst and preparation method thereof Download PDF

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CN114308132A
CN114308132A CN202111496223.8A CN202111496223A CN114308132A CN 114308132 A CN114308132 A CN 114308132A CN 202111496223 A CN202111496223 A CN 202111496223A CN 114308132 A CN114308132 A CN 114308132A
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composite photocatalyst
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CN114308132B (en
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段芳
盛家亮
张景琛
朱罕
陆双龙
杜明亮
陈明清
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Jiangnan University
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Abstract

The invention discloses a protonated CdS-COF-366-M composite photocatalyst and a preparation method thereof. Adding pre-prepared COF-366-M with different contents into Diethylenetriamine (DETA) precursor solution containing CdS seeds, synthesizing the CdS-COF-366-M composite photocatalyst in situ by a solvothermal method, and finally protonating the CdS-COF-366-M composite photocatalyst by adopting ascorbic acid. The problems that the visible light response range of CdS is narrow, photoproduction electrons and holes are easy to recombine and the like can be solved by coupling COF-366-M with CdS, and in addition, the transfer and separation efficiency of photoproduction charges can be further improved by protonation, so that the photocatalytic activity is improved. The synthesis method has simple process and easy operation. The prepared CdS-COF-366-M composite photocatalyst has excellent hydrogen production performance under the catalysis of visible light.

Description

Protonated CdS-COF-366-M composite photocatalyst and preparation method thereof
Technical Field
The invention belongs to the field of photocatalysis, and particularly relates to a protonated CdS-COF-366-M composite photocatalyst and a preparation method thereof.
Background
With the rapid development of industrialization and urbanization, there is an increasing concern about the sustainable supply of fossil fuels (such as oil, coal, and natural gas) and the serious environmental problems caused by the use of these fossil fuels. Therefore, there is a pressing need to solve environmental and energy problems through an operable and scalable technology to achieve an alternative, sustainable clean energy. The solar-driven photocatalytic process is a method capable of effectively utilizing solar energy to obtain clean energy, and is mainly applied to multiple aspects of organic pollutant degradation, photocatalytic hydrogen production, water oxidation, photocatalytic carbon dioxide reduction, photocatalytic organic conversion and the like. Among many renewable energy projects, hydrogen energy is considered as an alternative to fossil energy due to its advantages of environmental protection and high energy density, and the photocatalytic water cracking reaction is considered as one of the most promising ways to obtain hydrogen energy. Therefore, research on a semiconductor-based photocatalyst to efficiently decompose water by collecting inexhaustible and clean solar energy is a key technology for photocatalytic hydrogen evolution.
Solar photocatalytic hydrogen production by water splitting has become a potential and effective technology for obtaining alternative energy sources in the last decade. In order to improve the photocatalytic hydrogen evolution activity of semiconductor-based photocatalysts, researchers design and construct photocatalysts with high activity, strong visible light absorption and low cost. Of these developed photocatalysts, cadmium sulfide (CdS) semiconductor is considered a good candidate for photocatalytic hydrogen production due to the narrow band gap, visible light response, and appropriate conduction and valence band positions. However, its application is limited due to its fast electron-hole recombination rate and easy agglomeration of nano-sized cadmium sulfide.
Disclosure of Invention
Aiming at the problems, the CdS-COF-366-M photocatalyst is prepared by a solvothermal method, and the prepared CdS-COF-366-M photocatalyst is subjected to protonation treatment by using ascorbic acid, so that the protonized photocatalyst well solves the problem of strong combination of photo-generated electron-hole pairs of the CdS photocatalyst, effectively improves the photocatalytic activity of the CdS photocatalyst, has excellent photocatalytic hydrogen production performance, and also has good light absorption performance and stability, and the method is simple in process and easy to operate. The invention provides a protonated CdS-COF-366-M composite photocatalyst which is used for photocatalytic hydrogen production and has good photocatalytic stability and a preparation method thereof.
The invention is realized by the following technical scheme:
the first purpose of the invention is to provide a preparation method of a protonated CdS-COF-366-M composite photocatalyst, which comprises the following steps:
(1) preparation of COF-366-M: mixing 5,10,15, 20-tetra (4-aminophenyl) porphyrin metal, terephthalaldehyde, mesitylene and absolute ethyl alcohol, performing ultrasonic treatment to obtain a uniform suspension, adding an acetic acid aqueous solution, uniformly mixing, performing quick freezing in liquid nitrogen, performing multiple freezing-pump-unfreezing circulation degassing, sealing under vacuum, reacting at 110-130 ℃ for 3 days, and washing, centrifuging and freeze-drying a product obtained by the reaction to obtain COF-366-M; the central metal ion M of COF-366-M is Ni2+、Zn2+、Co2+And Fe2+Any one of the above;
(2) preparing a CdS-COF-366-M composite photocatalyst: adding Cd into the solution2+Dispersing a source and sublimed sulfur in diethylenetriamine, adding COF-366-M obtained in the step (1), stirring to form a uniform suspension, transferring the suspension into a high-pressure reaction kettle, reacting at 80-100 ℃ for 36-48 h, and washing, centrifuging and drying a product obtained by the reaction to obtain the CdS-COF-366-M composite photocatalyst;
(3) protonation of the CdS-COF-366-M composite photocatalyst: and (3) uniformly mixing the CdS-COF-366-M composite photocatalyst obtained in the step (2) with an ascorbic acid aqueous solution, continuously stirring for reaction, centrifuging a product obtained by the reaction, and freeze-drying to obtain the protonated CdS-COF-366-M composite photocatalyst.
As a preferred embodiment of the present invention, in the step (1), the molar ratio of 5,10,15, 20-tetrakis (4-aminophenyl) porphyrin metal to terephthalaldehyde is 1: 2; the volume ratio of the mesitylene to the absolute ethyl alcohol is 1: 1; the amount of the aqueous acetic acid solution added was 0.2mL, the reaction temperature was 120 ℃ and the reaction time was 3 days.
In a preferred embodiment of the invention, in the step (2), the addition amount of the Cd2+ source is 0.8mmol, the addition amount of the sublimed sulfur is 4-8 mmol, and the addition amount of the diethylenetriamine is 20-35 mL.
In a preferred embodiment of the invention, in the step (2), the addition amount of the COF-366-M is 2-30% of the theoretical mass of the CdS.
In a preferred embodiment of the invention, in the step (2), the addition amount of the COF-366-M is 10-30% of the theoretical mass of the CdS.
As a preferred embodiment of the invention, in the step (2), the addition amount of COF-366-M is 20% of the theoretical mass of CdS.
In the step (2), which is a preferred embodiment of the present invention, the Cd2+The source is one of cadmium chloride and cadmium nitrate.
In step (1), as a preferred embodiment of the present invention, the washing is specifically performed using N, N-dimethylformamide and acetone.
In a preferred embodiment of the present invention, the freeze-drying time in step (1) is 24 hours.
In a preferred embodiment of the present invention, in the step (1), the concentration of the aqueous acetic acid solution is 6M.
In a preferred embodiment of the present invention, the number of times of degassing in the freeze-pump-thaw cycle in step (1) is 3.
In step (2), as a preferred embodiment of the present invention, the washing is specifically deionized water and ethanol.
As a preferred embodiment of the invention, in the step (2), the drying is drying for 6-12 hours at constant temperature in an oven.
In a preferred embodiment of the present invention, in the step (3), the stirring time is 30 to 60 min.
In a preferred embodiment of the invention, in the step (3), the molar concentration of the ascorbic acid is 0.1M, and the ratio of the CdS-COF-366-M composite photocatalyst obtained in the step (2) to the ascorbic acid aqueous solution is 1 mg: 2 mL.
The second purpose of the invention is to provide the protonated CdS-COF-366-M composite photocatalyst prepared by the method.
The third purpose of the invention is to provide the application of the protonated CdS-COF-366-M composite photocatalyst in photocatalytic hydrogen production.
Compared with the prior art, the invention has the following remarkable advantages:
(1) according to the invention, COF-366-M is prepared by a solvothermal method, a heterojunction is constructed by coupling COF-366-M and CdS, the CdS-COF-366-M composite photocatalyst is prepared, and the protonated CdS-COF-366-M composite photocatalyst is obtained by protonating the CdS-COF-366-M composite photocatalyst by ascorbic acid.
(2) Compared with other traditional photocatalysts, the CdS-COF-366-M composite photocatalyst prepared by the invention has a 2D lamellar structure, and COF-366-M is effectively dispersed on the surface of CdS and is in close contact with the CdS to form a heterostructure, so that photo-generated electron-hole pairs are more effectively separated and transferred, and the photocatalytic hydrogen production activity is improved.
(3) The prepared CdS-COF-366-M composite photocatalyst is subjected to protonation treatment in an ascorbic acid aqueous solution, so that the visible light response range of the catalyst is effectively widened; the second aspect improves the hydrophilicity of the photocatalyst; the third aspect can also promote the separation and transfer of photo-generated electron-hole pairs, and further improve the photocatalytic activity.
(4) The protonized CdS-COF-366-M composite photocatalyst prepared by the invention can be applied to photocatalytic hydrogen production, has high hydrogen yield (when the mass fraction of the added COF-366-Ni reaches 20%, the hydrogen yield reaches 18.23mmol/g/h based on the method for testing the photocatalytic hydrogen production performance), and has potential application value.
Drawings
FIG. 1 shows X-ray diffraction patterns of CdS-xCOF-366-Ni (X is the mass fraction of COF-366-Ni) composite photocatalysts with different COF-366-Ni contents;
FIG. 2 shows ultraviolet-visible absorption spectra of CdS-xCOF-366-Ni (x is the mass fraction of COF-366-Ni) composite photocatalysts with different COF-366-Ni contents;
FIG. 3 shows the photocatalytic hydrogen production performance of CdS-xCOF-366-Ni (x is the mass fraction of COF-366-Ni) composite photocatalysts with different COF-366-Ni contents.
Detailed Description
The present invention is further described below with reference to examples, but the embodiments of the present invention are not limited thereto.
Example 1
A preparation method of a protonated CdS-10% COF-366-Ni photocatalyst (COF-366-Ni mass fraction is 10%) comprises the following steps:
(1) preparation of COF-366-Ni: adding 0.02mmol of 5,10,15, 20-tetra (4-aminophenyl) nickel porphyrin and 0.04mmol of terephthalaldehyde into a Pyrex tube, adding 2mL of mixed solution of mesitylene and absolute ethyl alcohol (the volume ratio of the mesitylene to the absolute ethyl alcohol is 1:1), and performing ultrasonic treatment for 30min to form uniform suspension; then adding 0.2mL of 6M acetic acid aqueous solution, quickly freezing a Pyrex tube in liquid nitrogen, carrying out three times of freezing-pump-unfreezing cycle degassing, sealing under vacuum, reacting at 120 ℃ for 3 days, washing a product obtained after the reaction by DMF (dimethyl formamide) and acetone, centrifuging, and carrying out freeze drying for 24 hours to obtain COF-366-Ni;
(2) preparation of CdS-COF-366-Ni photocatalyst: 0.8mmol of cadmium chloride (CdCl) was weighed2·2.5H2O) and 5mmol of sublimed sulfur (S) are dispersed in 30mL of Diethylenetriamine (DETA) solvent to form uniform suspension liquid, so that cadmium sulfide precursor liquid is obtained; adding the COF-366-Ni (the mass ratio of the COF-366-Ni to the CdS is controlled to be 1:10) obtained in the step (1) with the mass fraction of 10%, and stirring for 30min to form a uniform suspension; and transferring the suspension into a 50mL stainless steel high-pressure reaction kettle with a polytetrafluoroethylene liner, reacting for 48h at 80 ℃, respectively washing solid products obtained after the reaction with deionized water and ethanol, and then transferring to an oven for constant-temperature drying for 12h to obtain the CdS-10% COF-366-Ni composite photocatalyst.
(3) Protonation of CdS-COF-366-Ni photocatalyst: uniformly mixing the CdS-10% COF-366-Ni photocatalyst obtained in the step (2) with 0.1M ascorbic acid aqueous solution, and stirring to react for 30 min; and then centrifuging the obtained product to obtain a solid, and freeze-drying for 24h to obtain the protonated CdS-10% COF-366-Ni composite photocatalyst. Wherein the dosage ratio of the CdS-10% COF-366-Ni photocatalyst to 0.1M ascorbic acid aqueous solution is 10 mg: 20 mL.
Example 2
The preparation method in the embodiment refers to the embodiment 1, the difference is only that the COF-366-Ni obtained in the step (1) with the mass fraction of the added COF-366-Ni being 20% in the step (2) of the embodiment (the mass ratio of the COF-366-Ni to the CdS is controlled to be 2:10), and the rest conditions are not changed.
Example 3
The preparation method in the embodiment refers to the embodiment 1, the difference is only that the COF-366-Ni obtained in the step (1) with the mass fraction of the added COF-366-Ni being 30% in the step (2) of the embodiment (the mass ratio of the COF-366-Ni to the CdS is controlled to be 3:10), and the rest conditions are not changed.
Example 4
A protonated CdS-20% COF-366-Co photocatalyst (COF-366-Co mass fraction of 20%), the preparation method in this example refers to example 2, except that in step (1) of this example, 5,10,15, 20-tetrakis (4-aminophenyl) porphyrin cobalt is substituted for 5,10,15, 20-tetrakis (4-aminophenyl) porphyrin nickel to prepare COF-366-Co; and (3) adding the COF-366-Co with the mass fraction of 20% in the step (2) to the COF-366-Co obtained in the step (1) (controlling the mass ratio of the COF-366-Co to the CdS to be 2:10), and keeping the rest conditions unchanged to finally obtain the CdS-20% COF-366-Co photocatalyst.
Comparative example 1
The production method in this example refers to example 2 except that the step of adding COF-366-Ni is omitted in step (2) of this example and the remaining conditions are unchanged.
Comparative example 2
The preparation method in this example refers to example 2, except that the step of mixing the CdS-10% COF-366-Ni photocatalyst obtained in step (2) with 0.1M ascorbic acid aqueous solution is omitted in step (3) of this example, and the rest conditions are unchanged.
Comparative example 3
The preparation method in this example refers to example 2, except that the addition of cadmium chloride (CdCl) is omitted in step (2) of this example2·2.5H2O) and sublimating sulphur (S), the rest conditions being unchanged.
X-ray diffraction characterization is carried out on CdS-xCOF-366-Ni photocatalysts with different COF-366-Ni contents, and as shown in figure 1, the phase and crystallinity of CdS are not changed by the change of the content of COF-366-Ni.
The light absorption range of the photocatalyst was tested by uv-vis absorption spectroscopy, as shown in fig. 2. The spectral absorption range of the protonated CdS-COF-366-Ni photocatalyst is found to be obviously widened, which shows that the method greatly improves the absorption and utilization of the photocatalyst to visible light.
Example 5
In order to research the photocatalytic performance of the photocatalyst, the prepared photocatalyst is used for photocatalytic hydrogen production, and the specific experimental process is as follows:
weighing 10mg of photocatalyst, adding the photocatalyst into 40mL of deionized water, and adding 5mL of lactic acid solution (the volume ratio of lactic acid to water is 1:10) as a cavity sacrificial agent; and uniformly mixing the prepared solution, transferring the mixed solution into a hydrogen production reactor, sealing, introducing nitrogen for 30min to remove oxygen, then illuminating by using a 300W xenon lamp (adding a filter to filter light with the wavelength of less than 420 nm), and testing the hydrogen yield after reacting for 3 h.
The photocatalytic hydrogen production performance of CdS-xCOF-366-Ni (x is mass fraction) photocatalysts with different COF-366-Ni contents is shown in a figure 3, wherein (1) the photocatalyst is compared with that of a comparative example 1; (2) comparative example 3; (3) example 1; (4) example 2; (5) example 3, (6) comparative example 2, (7) example 4. It can be seen that hydrogen yield is significantly increased by the method of the present invention compared to comparative examples 1 and 2 after (3-7) CdS is complexed with COF-366-Ni; when the mass fraction of the added COF-366-Ni reached 20%, the hydrogen production reached a maximum (18.23 mmol/g/h). When the mass fraction of the added COF-366-Ni is more than 20 percent, the yield of hydrogen is reduced on the contrary because a large amount of COF-366-Ni can shield the catalytic active sites on the CdS surface, and meanwhile, the mass fraction of the added COF-366-Ni is larger than 20 percentDivalent nickel in COF-366-Ni can accelerate the transfer of photogenerated charges. In addition, the performance of the CdS-COF-366-Ni photocatalyst which is not protonated by ascorbic acid is found to be reduced, probably because the hydrophilicity of the material is increased after protonation, and the separation and transfer of photogenerated carriers are further improved, so that the photocatalytic activity of the photocatalyst can be improved. Protonation of the photocatalyst may also prevent the photocatalyst from being oxidized to some extent by its own holes. Under the same conditions, when the central metal of COF-366-M is changed into Co2+、Zn2+And Fe2+In the process, the prepared CdS-20% COF-366-Co composite photocatalyst has excellent photocatalytic hydrogen production performance after protonation.

Claims (10)

1. A preparation method of a protonated CdS-COF-366-M composite photocatalyst is characterized by comprising the following steps:
(1) preparation of COF-366-M: mixing 5,10,15, 20-tetra (4-aminophenyl) porphyrin metal, terephthalaldehyde, mesitylene and absolute ethyl alcohol, performing ultrasonic treatment to obtain a uniform suspension, adding an acetic acid aqueous solution, uniformly mixing, performing quick freezing in liquid nitrogen, performing multiple freezing-pump-unfreezing circulation degassing, sealing under vacuum, reacting at 110-130 ℃ for 3 days, and washing, centrifuging and freeze-drying a product obtained by the reaction to obtain COF-366-M; the central metal ion M of COF-366-M is Ni2+、Zn2+、Co2 +And Fe2+Any one of the above;
(2) preparing a CdS-COF-366-M composite photocatalyst: adding Cd into the solution2+Dispersing a source and sublimed sulfur in diethylenetriamine, adding COF-366-M obtained in the step (1), stirring to form a uniform suspension, transferring the suspension into a high-pressure reaction kettle, reacting at 80-100 ℃ for 36-48 h, and washing, centrifuging and drying a product obtained by the reaction to obtain the CdS-COF-366-M composite photocatalyst;
(3) protonation of the CdS-COF-366-M composite photocatalyst: and (3) uniformly mixing the CdS-COF-366-M composite photocatalyst obtained in the step (2) with an ascorbic acid aqueous solution, continuously stirring for reaction, centrifuging a product obtained by the reaction, and freeze-drying to obtain the protonated CdS-COF-366-M composite photocatalyst.
2. The method according to claim 1, wherein in step (1), the molar ratio of 5,10,15, 20-tetrakis (4-aminophenyl) porphyrin metal to terephthalaldehyde is 1: 2; the volume ratio of the mesitylene to the absolute ethyl alcohol is 1: 1; the amount of the aqueous acetic acid solution added was 0.2mL, the reaction temperature was 120 ℃ and the reaction time was 3 days.
3. The method of claim 1, wherein in step (2), Cd2+The adding amount of the source is 0.8mmol, the adding amount of the sublimed sulfur is 4-8 mmol, and the adding amount of the diethylenetriamine is 20-35 mL.
4. The method according to claim 1, wherein in the step (2), the addition amount of COF-366-M is 2-30% of the theoretical mass of CdS.
5. The method according to claim 4, wherein in the step (2), the addition amount of COF-366-M is 10-30% of the theoretical mass of CdS.
6. The process according to claim 5, wherein in step (2), the amount of COF-366-M added is 20% of the theoretical mass of CdS.
7. The method according to claim 1, wherein in the step (3), the stirring time is 30-60 min.
8. The method as claimed in claim 1, wherein in the step (3), the molar concentration of the ascorbic acid is 0.1M, and the ratio of the CdS-COF-366-M composite photocatalyst obtained in the step (2) to the ascorbic acid aqueous solution is 1 mg: 2 mL.
9. A protonated CdS-COF-366-M composite photocatalyst made according to the method of any one of claims 1 to 8.
10. The use of the protonated CdS-COF-366-M composite photocatalyst as defined in claim 9 in photocatalytic hydrogen production.
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