CN114849738A - Preparation method and application of manganese cadmium sulfide @ nickel oxide composite photocatalyst - Google Patents

Preparation method and application of manganese cadmium sulfide @ nickel oxide composite photocatalyst Download PDF

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CN114849738A
CN114849738A CN202210619720.0A CN202210619720A CN114849738A CN 114849738 A CN114849738 A CN 114849738A CN 202210619720 A CN202210619720 A CN 202210619720A CN 114849738 A CN114849738 A CN 114849738A
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manganese
cadmium
sulfide
nickel oxide
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李忠玉
马亭
徐松
梁倩
周满
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Changzhou University
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    • B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
    • B01J27/02—Sulfur, selenium or tellurium; Compounds thereof
    • B01J27/04—Sulfides
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    • B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
    • B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
    • B01J23/74—Iron group metals
    • B01J23/755—Nickel
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    • B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
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    • C01B3/02—Production of hydrogen or of gaseous mixtures containing a substantial proportion of hydrogen
    • C01B3/04—Production of hydrogen or of gaseous mixtures containing a substantial proportion of hydrogen by decomposition of inorganic compounds, e.g. ammonia
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Abstract

The invention relates to a preparation method and application of a manganese cadmium sulfide @ nickel oxide composite photocatalyst. Firstly, preparing spherical manganese cadmium Mn sulfide 0.5 Cd 0.5 S, adding cadmium manganese sulfide and an ascorbic acid chelating agent into deionized water, slowly adding nickel acetate into the deionized water, stirring, slowly adding an ammonia water solution, performing oil bath treatment, centrifuging to collect a product, washing and drying to obtain the cadmium manganese sulfide @ nickel oxide core-shell composite photocatalyst (Mn) containing nickel oxide and cadmium manganese sulfide in a certain molar ratio 0.5 Cd 0.5 S @ NiO). The invention has the beneficial effects that: the preparation method is simple and convenient to operate, the preparation conditions are well controlled, and the prepared manganese cadmium sulfide @ nickel oxide composite photocatalyst has good photocatalytic hydrogen production activity and stability and has a certain application prospect.

Description

Preparation method and application of manganese cadmium sulfide @ nickel oxide composite photocatalyst
Technical Field
The invention belongs to the technical field of photocatalytic nano materials, and relates to a preparation method and application of a manganese cadmium sulfide @ nickel oxide composite photocatalyst.
Background
The problems of environmental pollution and energy crisis are getting more severe while the modern economy and society are rapidly developing. The ever-increasing energy demand and environmental issues have accelerated active research into the development of new sustainable green energy technologies. Since Fujishima and Honda demonstrated the photocatalytic decomposition of water on a photoactive semiconductor catalyst in 1972, efforts have been directed to developing highly efficient photocatalysts that are capable of collecting solar energy and converting it into chemical energy. Over the past few decades, various photocatalysts have been developed, including metal oxides, metal sulfides, and organic polymers. Of these, cadmium sulfide has received much attention due to its narrow band gap (2.4eV) and relatively high catalytic performance. However, the hydrogen generating activity of cadmium sulfide is severely limited due to the rapid recombination of carriers and photo-corrosion problems. Various solid solutions composed of cadmium sulfide and other semiconductors have been developed to overcome the above problems due to their similar crystal structures.
Sulfide-based materials are considered to be a good choice for photocatalytic hydrogen production due to their appropriate conduction band edge and narrow band gap. Among them, sulfide solid solutions (e.g., ZnIn) 2 S 4 、CuInS 2 And Zn 1-x Cd x S) is favored for its adjustable bandgap width and superior visible-light hydrogen production performance. Novel ternary solid solution manganese cadmium sulfide (Mn) x Cd 1-x S) has been used for photocatalytic hydrogen production. For example CN 201910904088.2A containing Mn 0.5 Cd 0.5 Preparation method of S and Au supported photocatalyst, CN201910904090.X containing Mn 0.5 Cd 0.5 S and Cu 2 In the preparation method of O supported photocatalyst, Mn is involved 0.5 Cd 0.5 Preparation of S support, existing Mn 0.5 Cd 0.5 The S carrier has defects, and although the cadmium manganese sulfide has great potential in the aspect of photocatalytic hydrogen production, the S carrier still has great improvement space.
Nickel oxide itself has little activity and therefore has little application in photocatalytic hydrogen production. In the present invention byHydrothermal method for successfully synthesizing novel manganese cadmium sulfide (Mn) 0.5 Cd 0.5 S) and further coating nickel oxide on the cadmium manganese sulfide by an in-situ growth method, wherein the prepared photocatalyst shows remarkably enhanced hydrogen production efficiency under the irradiation of visible light, and can be applied to the field of visible light photocatalysis.
Disclosure of Invention
The invention provides a preparation method of a manganese cadmium sulfide and nickel oxide composite visible-light-driven photocatalyst, which aims to solve the technical problems in the background technology.
The technical scheme adopted by the invention for solving the technical problems is as follows: a preparation method of a manganese cadmium sulfide @ nickel oxide composite photocatalyst comprises the following steps:
(1) cadmium manganese sulfide (Mn) 0.5 Cd 0.5 S) preparation: manganese acetate (Mn (CH) 3 COO) 2 ·4H 2 O) and cadmium acetate (Cd (CH) 3 COO) 2 ·2H 2 O) was dissolved in deionized water containing sodium hydroxide and stirred for 0.5 hours. Then, thioacetamide was added to the above solution and stirred until the color became yellow. The resulting mixture was transferred to a stainless steel autoclave of polytetrafluoroethylene, sealed and heated at 180 ℃ for 18 hours. After natural cooling, the product was centrifuged, washed with deionized water and ethanol and dried at 60 ℃ for 12 hours to give a yellow powder product.
The invention is used for preparing Mn 0.5 Cd 0.5 When the S solid solution carrier is used, sodium hydroxide is added to adjust the acid-base environment, so that the hydrogen production performance is improved. Further, preferably, the molar ratio of the manganese acetate, the cadmium acetate, the sodium hydroxide and the thioacetamide used in the step (1) is 1: 1: 8: 4.
(2) preparing a manganese cadmium sulfide @ nickel oxide composite photocatalyst: adding the cadmium manganese sulfide and the ascorbic acid chelating agent prepared in the step (1) into deionized water, stirring for 0.5 hour, and adding a calculated amount of nickel acetate (Ni (CH) 3 COO) 2 ·4H 2 O) was slowly added to the mixed solution, and stirred for another 1 hour, and then, during the reaction, an aqueous ammonia solution was slowly added to the above solution, and then the mixture was subjected to 60 deg.CThe obtained product is centrifugally collected, washed by deionized water and ethanol and dried at a certain temperature to obtain the manganese cadmium sulfide @ nickel oxide core-shell composite photocatalyst (Mn) with a certain molar ratio of nickel oxide to manganese cadmium sulfide 0.5 Cd 0.5 S@NiO)。
Further, the mass ratio of the ascorbic acid to the manganese cadmium sulfide in the step (2) is 1: 1.8-2.0; the mass fraction of the ammonia water is 25%, and the dosage of nickel acetate ammonia water per 0.0625-0.1875 g is 5 mL.
Further, in the step (2), the molar ratio of the cadmium manganese sulfide to the nickel acetate is 1: 0.25 to 0.75. Further preferred molar ratios are 1: 0.25 to 0.50.
The invention adds ascorbic acid as a chelating agent, which can obviously improve the compounding efficiency, thereby improving the catalytic performance of the catalyst. The manganese cadmium sulfide @ nickel oxide prepared by the invention is of a core-shell structure, the core-shell structure has a remarkable improvement effect on the catalytic performance,
the prepared manganese cadmium sulfide @ nickel oxide composite photocatalyst has good photocatalytic hydrogen production activity, and can be used as a photocatalyst for catalytic hydrogen production under visible light.
The invention has the beneficial effects that: the preparation method is simple and easy to implement, the preparation conditions are easy to control, and the prepared manganese cadmium sulfide @ nickel oxide composite photocatalyst has good photocatalytic hydrogen production activity and a certain application prospect.
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The invention is further described below with reference to the accompanying drawings.
FIG. 1 is an X-ray diffraction diagram of a cadmium manganese sulfide, a nickel oxide and a cadmium manganese sulfide @ nickel oxide composite photocatalyst prepared in examples 1-3 of the present invention;
FIG. 2 is a scanning electron microscope image of the manganese cadmium sulfide @ nickel oxide composite photocatalyst prepared in example 2 of the present invention;
FIG. 3 is a transmission electron microscope image of the manganese cadmium sulfide @ nickel oxide composite catalyst prepared in example 2 of the present invention;
FIG. 4 is a graph showing the hydrogen production effect of the manganese cadmium sulfide @ nickel oxide composite catalyst prepared in examples 1-3 of the present invention.
Detailed Description
The invention will now be further illustrated by reference to specific examples, which are intended to be illustrative of the invention and are not intended to be a further limitation of the invention.
Example 1
(1) Cadmium manganese sulfide (Mn) 0.5 Cd 0.5 S) preparation: 0.2451g of manganese acetate (Mn (CH) 3 COO) 2 ·4H 2 O) and 0.2665g of cadmium acetate (Cd (CH) 3 COO) 2 ·2H 2 O) was dissolved in 60ml of deionized water containing 0.32g of sodium hydroxide and stirred for 0.5 hour. Then, 0.3005g of thioacetamide was added to the above solution and stirred until the color turned yellow. The resulting mixture was transferred to a stainless steel autoclave of polytetrafluoroethylene, sealed and heated at 180 ℃ for 18 hours. After natural cooling, the product was centrifuged, washed with deionized water and ethanol and dried at 60 ℃ for 12 hours to give the final product as a yellow powder: manganese cadmium sulfide Mn 0.5 Cd 0.5 S。
(2) Preparing a manganese cadmium sulfide @ nickel oxide composite photocatalyst: 0.116g of manganese cadmium sulfide Mn prepared in the step (1) 0.5 Cd 0.5 S and 0.06g ascorbic acid were added to 60ml deionized water, and after stirring for 0.5 hour, 0.0625g nickel acetate (Ni (CH) 3 COO) 2 ·4H 2 O) is slowly added into the mixed solution, and then stirred for 1 hour, then 5ml of ammonia water is slowly added into the solution in the reaction process, then the mixture is subjected to oil bath treatment for 12 hours at the temperature of 60 ℃, products are collected by centrifugation, washed by deionized water and ethanol, and dried, and the manganese cadmium sulfide @ nickel oxide core-shell composite photocatalyst (Mn) containing a certain molar ratio of nickel oxide to manganese cadmium sulfide is prepared 0.5 Cd 0.5 S@NiO0.25)。
Example 2
(1) Cadmium manganese sulfide (Mn) 0.5 Cd 0.5 S) preparation: 0.2451g of manganese acetate (Mn (CH) 3 COO) 2 ·4H 2 O) and 0.2665g of cadmium acetate (Cd (CH) 3 COO) 2 ·2H 2 O) was dissolved in 60ml of deionized water containing 0.32g of sodium hydroxideWater, and stirred for 0.5 hour. Then, 0.3005g of thioacetamide was added to the above solution and stirred until the color turned yellow. The resulting mixture was transferred to a stainless steel autoclave of polytetrafluoroethylene, sealed and heated at 180 ℃ for 18 hours. After natural cooling, the product was centrifuged, washed with deionized water and ethanol and dried at 60 ℃ for 12 hours to give the final product as a yellow powder: manganese cadmium sulfide Mn 0.5 Cd 0.5 S。
(2) Preparing a manganese cadmium sulfide @ nickel oxide composite photocatalyst: 0.116g of cadmium manganese sulfide prepared in the step (1) and 0.06g of ascorbic acid were added to 60ml of deionized water, and after stirring for 0.5 hour, 0.125g of nickel acetate (Ni (CH) 3 COO) 2 ·4H 2 O) is slowly added into the mixed solution, and then stirred for 1 hour, then in the reaction process, 5ml of ammonia water solution is slowly added into the solution, then the mixture is subjected to oil bath treatment for 12 hours at the temperature of 60 ℃, products are collected by centrifugation, washed by deionized water and ethanol, and dried at a certain temperature, and the manganese cadmium sulfide @ nickel oxide core-shell composite photocatalyst (Mn) containing a certain molar ratio of nickel oxide to manganese cadmium sulfide is prepared 0.5 Cd 0.5 S@NiO 0.5)。
Example 3
(1) Cadmium manganese sulfide (Mn) 0.5 Cd 0.5 S) preparation: 0.2451g of manganese acetate (Mn (CH) 3 COO) 2 ·4H 2 O) and 0.2665g of cadmium acetate (Cd (CH) 3 COO) 2 ·2H 2 O) was dissolved in 60ml of deionized water containing 0.32g of sodium hydroxide and stirred for 0.5 hour. Then, 0.3005g of thioacetamide was added to the above solution and stirred until the color turned yellow. The resulting mixture was transferred to a stainless steel autoclave of polytetrafluoroethylene, sealed and heated at 180 ℃ for 18 hours. After natural cooling, the product was centrifuged, washed with deionized water and ethanol and dried at 60 ℃ for 12 hours to give a yellow powder product.
(2) Preparing a manganese cadmium sulfide @ nickel oxide composite photocatalyst: 0.116g of cadmium manganese sulfide prepared in the step (1) and 0.06g of ascorbic acid are added into 60ml of deionized water, stirred for 0.5 hour, and then 0.1875g of acetic acid is addedNickel (Ni (CH) 3 COO) 2 ·4H 2 O) is slowly added into the mixed solution, and then stirred for 1 hour, then in the reaction process, 5ml of ammonia water solution is slowly added into the solution, then the mixture is subjected to oil bath treatment for 12 hours at the temperature of 60 ℃, products are collected by centrifugation, washed by deionized water and ethanol, and dried at a certain temperature, and the manganese cadmium sulfide @ nickel oxide core-shell composite photocatalyst (Mn) containing a certain molar ratio of nickel oxide to manganese cadmium sulfide is prepared 0.5 Cd 0.5 S@NiO 0.75)。
Preparation of nickel oxide: compared with the step (2) of the example 1, the nickel oxide can be prepared without adding cadmium manganese sulfide and changing other conditions. The nickel oxide alone is used as a photocatalyst, has almost no catalytic activity, and the hydrogen production is only 0.08 mmol/g/h.
Mn 0.5 Cd 0.5 S preparation: in comparison with example 1, only cadmium manganese sulfide (Mn) was prepared 0.5 Cd 0.5 S), the Mn 0.5 Cd 0.5 S is spherical in structure, Mn alone 0.5 Cd 0.5 The hydrogen production activity of S is 10.36 mmol/g/h.
Comparative example 1
Rod-like Mn 0.5 Cd 0.5 The preparation method of S comprises the following steps: 0.2451g of manganese acetate (Mn (CH) 3 COO) 2 ·4H 2 O) and 0.2665g of cadmium acetate (Cd (CH) 3 COO) 2 ·2H 2 O) were dissolved in deionized water and ethylenediamine (volume ratio 1: 1) to the solution and mixed after 0.5 hour of stirring. 0.3005g of thioacetamide were then added to the above solution and stirred until the color turned yellow; the resulting mixture was transferred to a stainless steel autoclave of polytetrafluoroethylene, sealed and heated at 200 ℃ for 24 hours. After natural cooling, the product was centrifuged, washed with deionized water and ethanol and dried at 60 ℃ for 24 hours to give a yellow powder product.
Mn prepared in comparative example 1 0.5 Cd 0.5 S is a rod-shaped structure, the hydrogen production activity of the S is 8.06mmol/g/h, which is not the same as Mn in the structure of the application 0.5 Cd 0.5 S。
Comparative example 2
Mn prepared in step (1) of comparative example 2 and example 1 0.5 Cd 0.5 Compared with the S method, the method has the following differences: mn was prepared in the same manner as in example 1 except that sodium hydroxide was not added 0.5 Cd 0.5 S。
Mn prepared in comparative example 2 0.5 Cd 0.5 S (acid-base environment is not adjusted) hydrogen production activity is 2.51 mmol/g/h; mn prepared in example 1 0.5 Cd 0.5 And the hydrogen production activity of S is 10.36 mmol/g/h. Therefore, the sodium hydroxide is added to adjust the acid-base environment, and the hydrogen production performance is obviously improved.
The crystal phase structures of the manganese cadmium sulfide, nickel oxide and manganese cadmium sulfide @ nickel oxide visible-light-induced photocatalyst prepared in examples 1-3 are analyzed by a Japanese-science D/max2500PC autorotation X-ray diffractometer, wherein X-rays are Cu target Ka
Figure BDA0003674269030000081
The voltage is 40kV, the current is 100mA, the step length is 0.02 degrees, and the scanning range is 10-80 degrees. The X-ray diffraction pattern is shown in figure 1, the peak shapes of all the positions are consistent with the CdS standard card, and along with Mn 2+ The addition of ions gradually shifts the diffraction peak of pure CdS to a higher angle, indicating the formation of Mn 0.5 Cd 0.5 The solid solution of S, rather than the simple mixture of CdS and MnS, fully demonstrates the successful synthesis of cadmium manganese sulfide materials, while all cadmium manganese sulfide @ nickel oxide composite materials do not find an obvious nickel oxide diffraction peak, probably due to the small amount of nickel oxide shells deposited on cadmium manganese sulfide nuclei and the low crystallinity.
The morphology of the manganese cadmium sulfide @ nickel oxide photocatalyst prepared in example 2 in a ratio of 1:0.5 is observed by using a Japanese JSM-6360A scanning electron microscope and a Japanese JEOL 2100 transmission electron microscope, and as can be seen from a scanning electron microscope in FIG. 2 and a transmission electron microscope in FIG. 3, the composite visible light photocatalyst nickel oxide prepared in the embodiment wraps the manganese cadmium sulfide to form a shell-core structure.
The manganese cadmium sulfide @ nickel oxide composite material prepared in examples 1-3 was used as a photocatalyst to produce hydrogen. 10mg of the synthesized photocatalyst was added to 50ml of deionized water to achieve uniform suspension, then certain amounts of sodium sulfide (0.35M) and sodium sulfite (0.25M) were added to the suspension as sacrificial agents, the reactor was sealed, and the reactor was bubbled with high-purity argon for half an hour to remove air from the reactor. And continuously measuring for 3h under the irradiation of a 300W xenon lamp with a 420nm optical filter serving as a light source for each measurement, and carrying out photocatalytic hydrogen production reaction. After illumination, samples are taken for 6 times in sequence of 30min, 60min, 90min, 120min, 150min and 180min, and the samples are injected into a gas chromatograph to analyze the content, the experimental result is shown in figure 4, the hydrogen production rate of pure cadmium manganese sulfide is 10.36mmol/g/h, the hydrogen production rate of the composite photocatalyst with the optimal proportion of cadmium manganese sulfide and nickel oxide of 0.5 is 50.53mmol/g/h which is about 4.88 times of that of the pure cadmium manganese sulfide, the visible load nickel oxide can effectively improve the photocatalytic hydrogen production activity of the composite photocatalyst, and the prepared composite photocatalyst with the cadmium manganese sulfide and the nickel oxide has higher photocatalytic activity.
In light of the foregoing description of the preferred embodiment of the present invention, many modifications and variations will be apparent to those skilled in the art without departing from the spirit and scope of the invention. The technical scope of the present invention is not limited to the content of the specification, and must be determined according to the scope of the claims.

Claims (6)

1. A preparation method of a manganese sulfide cadmium @ nickel oxide composite photocatalyst is characterized by comprising the following steps: the preparation method comprises the following steps:
(1) manganese cadmium sulfide Mn 0.5 Cd 0.5 S preparation: dissolving manganese acetate and cadmium acetate in deionized water containing sodium hydroxide, stirring, adding thioacetamide into the solution, stirring until the color becomes yellow, transferring the obtained mixture into a high-pressure kettle, sealing, heating for reaction, naturally cooling after the reaction, centrifuging the product, washing, and drying to obtain the manganese cadmium sulfide Mn 0.5 Cd 0.5 S；
(2) Preparing a manganese cadmium sulfide @ nickel oxide composite photocatalyst: manganese sulfide, cadmium sulfide and Mn prepared in the step (1) 0.5 Cd 0.5 S and ascorbic acid are added into deionized water, and after stirring, nickel acetate is slowly added into the mixed solution; cadmium manganese sulfideMn 0.5 Cd 0.5 The molar ratio of S to nickel acetate is 1: 0.25-0.75, stirring, slowly adding an ammonia water solution into the solution to obtain a mixture, heating the mixture for a period of time, collecting a product after reaction, washing and drying to obtain the manganese cadmium sulfide @ nickel oxide core-shell composite photocatalyst (Mn) 0.5 Cd 0.5 S@NiO)。
2. The preparation method of the manganese cadmium sulfide @ nickel oxide composite photocatalyst as claimed in claim 1, wherein: the molar ratio of the manganese acetate, the cadmium acetate, the sodium hydroxide and the thioacetamide in the step (1) is 1: 1: 8: 4.
3. the preparation method of the manganese cadmium sulfide @ nickel oxide composite photocatalyst as claimed in claim 1, wherein: the heating reaction in the step (1) means heating at 180 ℃ for 18 hours.
4. The preparation method of the manganese cadmium sulfide @ nickel oxide composite photocatalyst as claimed in claim 1, wherein: in the step (2), the molar ratio of the cadmium manganese sulfide to the nickel acetate is 1: 0.25 to 0.5.
5. The preparation method of the manganese cadmium sulfide @ nickel oxide composite photocatalyst as claimed in claim 1, wherein: the heating reaction in the step (1) means that the reaction is carried out in an oil bath at 60 ℃ for 12 hours.
6. The application of the cadmium manganese sulfide @ nickel oxide composite photocatalyst prepared by the method according to any one of claims 1 to 5 in catalytic hydrogen production under visible light.
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CN115672354A (en) * 2022-10-17 2023-02-03 常州大学 Preparation method and application of ZIF-67 derived hollow cobalt sulfide/cadmium manganese sulfide composite photocatalyst
CN115672354B (en) * 2022-10-17 2024-05-28 常州大学 Preparation method and application of ZIF-67-derived hollow cobalt sulfide/manganese cadmium sulfide composite photocatalyst
CN115672374A (en) * 2022-10-31 2023-02-03 中国科学技术大学 Metal monoatomic/metal nanoparticle nanocomposite with cascaded catalytic activity and preparation and application thereof
CN115672374B (en) * 2022-10-31 2024-02-23 中国科学技术大学 Nanocomposite of metal monoatoms/metal nanoparticles with cascade catalytic activity, preparation and application thereof
CN116651467A (en) * 2023-06-02 2023-08-29 常州大学 Hollow Cu 2-x S@ cadmium manganese sulfide composite photocatalyst and preparation method and application thereof
CN116713009A (en) * 2023-06-06 2023-09-08 常州大学 Preparation method and application of ZnCdS/NiO composite photocatalyst

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