CN114289047A - Cobalt hydroxide/carbon nitride photocatalytic material and preparation method and application thereof - Google Patents
Cobalt hydroxide/carbon nitride photocatalytic material and preparation method and application thereof Download PDFInfo
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- CN114289047A CN114289047A CN202111467448.0A CN202111467448A CN114289047A CN 114289047 A CN114289047 A CN 114289047A CN 202111467448 A CN202111467448 A CN 202111467448A CN 114289047 A CN114289047 A CN 114289047A
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Abstract
The invention belongs to the technical field of energy catalytic conversion, and particularly relates to a cobalt hydroxide/carbon nitride photocatalytic material, a preparation method thereof and application thereof in photocatalytic aquatic oxygen and/or photocatalytic total hydrolysis. The preparation method comprises the following steps: (1) g to C3N4Ultrasonically dispersing in a cobalt (II) salt solution, and adding alkali under the stirring condition to obtain a suspension; (2) and (2) carrying out suction filtration on the suspension obtained in the step (1), and washing and drying the obtained solid to obtain the cobalt hydroxide/carbon nitride photocatalytic material. The g to C3N4The carbon nitride precursor is calcined in a muffle furnace at the temperature of 520-600 ℃ for 2-6h to obtain the carbon nitride precursor. In the cobalt hydroxide/carbon nitride prepared by the invention, the oxidation type cocatalyst cobalt hydroxide is highly dispersed in g-C in the form of nano particles3N4The surface is tightly combined with the surface to realize the rapid transfer of photogenerated holes between the surface and the surface, so that the obtained material has higher photocatalytic oxygen generation activity.
Description
Technical Field
The invention belongs to the technical field of energy catalytic conversion, and particularly relates to a cobalt hydroxide/carbon nitride photocatalytic material, a preparation method thereof and application thereof in photocatalytic aquatic oxygen and/or photocatalytic total hydrolysis.
Background
Under the double pressure of energy crisis and environmental pollution, hydrogen energy is one of the most promising clean energy sources to replace petrochemical energy due to its advantages of no pollution, high calorific value and the like. The photocatalytic technology for producing hydrogen by decomposing water with sunlight has become a hot point of research. The photocatalytic decomposition water contains 2 half reactions of hydrogen production and oxygen production. Photocatalytic total hydrolysis remains a challenging task to date (see acc. chem. res.,2013,46:1900), and most studies remain in the photocatalytic semi-hydrolysis hydrogen or oxygen production stage.
In recent years, graphite phase carbon nitride (g-C)3N4) The photocatalytic semi-hydrolytic hydrogen production catalyst has excellent performance in the aspect of photocatalytic semi-hydrolytic hydrogen production, stable chemical property, simple preparation and easily obtained raw materials. But with respect to g-C3N4The reports of full water splitting are still less, and when the water splitting is carried out, a sacrificial agent (such as triethanolamine) is generally added to produce hydrogen. The essence of photocatalytic half-hydrolysis hydrogen production is the conversion of chemical energy into chemical energy (equivalent to the conversion of chemical energy of a sacrificial agent into chemical energy in hydrogen), and full hydrolysis is the conversion of light energy into chemical energy. Thus, only g-C is achieved3N4The photocatalysis water decomposition can really convert solar energy into hydrogen energy, which has profound significance for environmental protection and sustainable development of energy.
For g-C3N4Platinum is the best recognized promoter for the semi-decomposition of water to produce hydrogen. In g-C3N4The method for semi-decomposing water to produce hydrogen by loading platinum on the surface through a photo-deposition method is also mature (see nat. mater.,2009,8: 76). And g-C3N4The semi-hydrolysis of water to produce oxygen is difficult, and the g-C can be generated at present3N4Promoters that effect the production of oxygen by the hemihydrolysis of water are based primarily on metal oxides and hydroxides (see ACS appl. mater. processes,201608:2287), but the corresponding oxygen generating activity has yet to be improved. It is considered that the semi-hydrolytic oxygen generation reaction is g-C3N4Realizing the bottleneck of full water splitting. Thus, by reaction at g-C3N4The surface is loaded with proper oxygen-producing cocatalyst, so that the oxygen-producing activity of the catalyst is improved, and the full water decomposition is realized, and the method is a feasible method.
In view of this, the invention is particularly proposed.
Disclosure of Invention
In order to solve the defect that the photocatalyst in the prior art is difficult to meet the photocatalytic full-hydrolytic condition, the invention provides a method for loading an efficient oxygen production promoter (cobalt hydroxide nano-particle) on the surface of carbon nitride, and the obtained cobalt hydroxide/carbon nitride (Co (OH))2/g-C3N4) The photocatalytic material is used for full-hydrolysis and has high full-hydrolysis activity.
The invention adopts a simple chemical deposition method to lead the cobalt hydroxide nano particles as the oxygen-producing cocatalyst to grow in g-C in situ3N4The surface is treated to obtain the cobalt hydroxide/carbon nitride photocatalytic material, wherein the cobalt hydroxide is highly dispersed in g-C3N4The surface and the two are tightly combined, so that the quick transfer of photogenerated holes between the two is realized, and the g-C is greatly improved3N4The oxygen generating performance of the reactor is improved, and the full water decomposition is realized. The method has the advantages of simple preparation method, convenient operation, low cost, controllable loading capacity and the like.
In order to achieve the purpose, the invention adopts the following technical scheme:
a preparation method of a cobalt hydroxide/carbon nitride photocatalytic material specifically comprises the following steps:
(1) at room temperature, adding g-C3N4Ultrasonically dispersing in a cobalt (II) salt solution, and adding alkali under the stirring condition to obtain a suspension;
(2) and (2) carrying out suction filtration on the suspension obtained in the step (1), and washing and drying the obtained solid to obtain the cobalt hydroxide/carbon nitride photocatalytic material.
The method is carried out in a greenhouse, cobalt ions adsorbed on the surface of carbon nitride meet alkali, and cobalt hydroxide precipitate is immediately generated in situ. Because the cobalt ions adsorbed on the surface of the carbon nitride are more uniform, the formed cobalt hydroxide is also more uniform and has smaller particles. However, if the temperature of the solution is higher when cobalt hydroxide is formed, the thermal motion of the solution molecules and the formed cobalt hydroxide particles is more violent, so that the formed cobalt hydroxide is more easily agglomerated, and larger cobalt hydroxide particles are easier to obtain, which is not favorable for the transmission of photo-generated holes between carbon nitride and cobalt hydroxide and influences the oxygen production performance.
Further, said g-C in step (1)3N4The preparation method comprises the following steps: placing the carbon nitride precursor into a muffle furnace for calcining, and naturally cooling to room temperature to obtain light yellow g-C3N4。
Preferably, the carbon nitride precursor is selected from one or more of urea (also called urea, carbamide or carbamide), melamine (also called melamine or protamine), dicyandiamide (also called dicyandiamide, cyanoguanidine or dicyandiamide) and cyanamide (simply referred to as cyanamide); the calcining temperature is 520-600 ℃, and the heat preservation time is 2-6 h.
As a preferable proposal, when urea is used as the carbon nitride precursor, g-C with larger specific surface area is prepared3N4Nanosheets; when melamine or dicyanodiamine is used as a carbon nitride precursor, bulk phase g-C with small specific surface area is prepared3N4。
Preferably, the cobalt (II) salt in step (1) is a soluble divalent cobalt salt, and may be one or more of cobalt chloride, cobalt nitrate and cobalt acetate.
Preferably, the solvent in the cobalt (II) salt solution in step (1) is water, ethanol or methanol, and water may be selected as the solvent in the cobalt (II) salt solution in view of cost and green environmental requirements.
The dosage of the cobalt (II) salt is g-C calculated by cobalt element3N40.1-10 wt% of the mass.
Preferably, the base in step (1) is ammonia, triethylamine or sodium hydroxide.
Too little alkali is added and dissolvedCobalt (II) in the liquid does not completely deposit on g-C3N4On the surface, too much alkali is added, and the particle size of cobalt hydroxide in the product becomes large, resulting in deterioration of photocatalytic performance.
The invention also aims to provide the cobalt hydroxide/carbon nitride photocatalytic material prepared by the method.
The invention also aims to provide application of the cobalt hydroxide/carbon nitride photocatalytic material in photocatalytic water production of oxygen and/or photocatalytic full-hydrolysis water.
Compared with the prior art, the invention has the following effects:
(1) compared with the problems that in the prior art, hydrogen production can be realized only by adding a sacrificial agent to photocatalyst in photolysis water, or the performance of semi-hydrolysis oxygen production realized by loading platinum is low and the like, the invention adopts a simple chemical deposition method to ensure that the oxygen production promoter cobalt hydroxide grows in the g-C in situ in the form of nano particles3N4The surface is treated to obtain the cobalt hydroxide/carbon nitride photocatalytic material, wherein the cobalt hydroxide is highly dispersed in g-C3N4The surface and the two are tightly combined to realize the rapid transfer of a photoproduction cavity between the two, so that the obtained cobalt hydroxide/carbon nitride photocatalytic material has higher photocatalytic oxygen production activity.
(2) When Pt is used as a hydrogen production promoter, the cobalt hydroxide/carbon nitride photocatalytic material provided by the invention can realize photocatalytic full hydrolysis, and has profound significance for environmental protection and sustainable development of energy.
(3) The method has the advantages of simple process, simple and convenient operation and low preparation cost.
Drawings
FIG. 1 shows cobalt hydroxide/carbon nitride (Co (OH))2/g-C3N4) Scanning Electron Microscope (SEM) spectra of photocatalytic materials.
FIG. 2 shows g-C in example 13N4And Co (OH)2/g-C3N4X-ray diffraction (XRD) spectrum of (a).
FIG. 3 shows Co (OH) in example 12/g-C3N4High resolution transmission electron displayMicromirror (HRTEM) spectrum.
FIG. 4 shows Co (OH) in example 12/g-C3N4Photocatalytic material and Co (OH) in example 62/g-C3N4And (3) a full water splitting performance graph of the photocatalyst.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. The following description of at least one exemplary embodiment is merely illustrative in nature and is in no way intended to limit the invention, its application, or uses. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Unless specifically stated otherwise, the numerical values set forth in these examples do not limit the scope of the invention. Techniques, methods known to those of ordinary skill in the relevant art may not be discussed in detail, but are intended to be part of the specification where appropriate. In all examples shown and discussed herein, any particular value should be construed as merely illustrative, and not limiting. Thus, other examples of the exemplary embodiments may have different values.
Example 1: preparation of cobalt hydroxide/carbon nitride photocatalytic material
Weighing 20g of urea, placing the urea in a 100mL crucible, calcining the crucible in a muffle furnace at 600 ℃ for 4h, and naturally cooling to room temperature to obtain light yellow carbon nitride (g-C)3N4). Weighing 0.50g g-C respectively3N4And 60mg CoCl2·6H2And O, adding 40mL of distilled water into a beaker, and performing ultrasonic treatment for 20 minutes to uniformly disperse the carbon nitride. At room temperature, 1.5mL of ammonia water is added under the condition that the stirring speed is more than or equal to 60rpm, and the stirring is continued to obtain a suspension. Filtering the obtained suspension, washing the solid with distilled water, and drying to obtain the target product cobalt hydroxide/carbon nitride (Co (OH)2/g-C3N4) A photocatalytic material.
FIG. 1 shows the target product Co (OH)2/g-C3N4SEM picture of the photocatalytic material, as known from FIG. 1, the morphology of the product presents a more regular lamellar structure, but no obvious Co (OH) is observed2Nanoparticles, probably due to Co (OH)2The nanoparticles are too small.
FIG. 2 shows g-C3N4And Co (OH) prepared in this example2/g-C3N4XRD pattern of photocatalytic material. From which g-C can be found3N4And Co (OH)2/g-C3N42 obvious diffraction peaks appear at 13.1 degrees and 27.4 degrees of the photocatalytic material and are respectively assigned to g-C3N4The (100) and (002) crystal planes of (a). And sample Co (OH)2/g-C3N4Three new diffraction peaks appear at 2 θ ═ 19.0 °, 37.9 ° and 51.4 °, corresponding to co (oh), respectively2The (001), (101) and (102) planes of (A) show that Co (OH) is successfully synthesized in this example2/g-C3N4A material.
Co (OH) prepared in this example2/g-C3N4The high-resolution transmission electron microscope (HRTEM) pattern of the material is shown in FIG. 3, from which Co (OH) can be clearly observed2Lattice fringes of nanoparticles with interplanar spacing of 0.24nm, ascribed to Co (OH)2The (101) crystal plane of (a).
Example 2: preparation of cobalt hydroxide/carbon nitride photocatalytic material
Weighing 20g of urea, placing the urea in a 100mL crucible, calcining the crucible in a muffle furnace at 600 ℃ for 4h, and naturally cooling to room temperature to obtain light yellow carbon nitride (g-C)3N4). Weighing 0.50g g-C respectively3N4And 100mg CoCl2·6H2And O, adding 40mL of distilled water into a beaker, and performing ultrasonic treatment for 20 minutes to uniformly disperse the carbon nitride. At room temperature, 1.5mL of ammonia water is added under the condition that the stirring speed is more than or equal to 60rpm, and the stirring is continued to obtain a suspension. The resulting suspension was filtered with suction and the solid was washed with distilled waterDrying to obtain the target product cobalt hydroxide/carbon nitride Co (OH)2/g-C3N4A photocatalytic material.
Example 3: preparation of cobalt hydroxide/carbon nitride photocatalytic material
Weighing 20g of urea, placing the urea in a 100mL crucible, calcining the crucible in a muffle furnace at 550 ℃ for 4h, and naturally cooling to room temperature to obtain light yellow carbon nitride (g-C)3N4). Weighing 0.50g g-C respectively3N4And 90mg Co (NO)3)2·6H2And O, adding 40mL of distilled water into a beaker, and performing ultrasonic treatment for 20 minutes to uniformly disperse the carbon nitride. At room temperature, 1.5mL of ammonia water is added under the condition that the stirring speed is more than or equal to 60rpm, and the stirring is continued to obtain a suspension. Carrying out suction filtration on the obtained suspension, washing the solid with distilled water, and drying to obtain a target product cobalt hydroxide/carbon nitride Co (OH)2/g-C3N4A photocatalytic material.
Example 4: preparation of cobalt hydroxide/carbon nitride photocatalytic material
Weighing 20g of urea, placing the urea in a 100mL crucible, calcining the crucible in a muffle furnace at 600 ℃ for 4h, and naturally cooling to room temperature to obtain light yellow carbon nitride (g-C)3N4). Weighing 0.50g g-C respectively3N4And 60mg CoCl2·6H2And O, adding 40mL of ethanol into a beaker, and performing ultrasonic treatment for 20 minutes to uniformly disperse the carbon nitride. At room temperature, 0.4mL of triethylamine is added under the condition that the stirring speed is more than or equal to 60rpm, and the stirring is continued to obtain suspension. Carrying out suction filtration on the obtained suspension, washing the solid with distilled water, and drying to obtain a target product cobalt hydroxide/carbon nitride Co (OH)2/g-C3N4A photocatalytic material.
Example 5: preparation of cobalt hydroxide/carbon nitride photocatalytic material
Weighing 2.0g dicyanodiamine, placing in a 50mL crucible, calcining the crucible in a muffle furnace at 550 ℃ for 4h, naturally cooling to room temperature, and grinding the obtained solid in a mortar to obtain yellow powdered carbon nitride (g-C)3N4). Weighing 0.50g g-C respectively3N4And 10mg CoCl2·6H2And O, adding 30mL of distilled water into a beaker, and performing ultrasonic treatment for 20 minutes to uniformly disperse the carbon nitride. At room temperature, 1.0mL of ammonia water is added under the condition that the stirring speed is more than or equal to 60rpm, and the stirring is continued to obtain a suspension. Carrying out suction filtration on the obtained suspension, washing the solid with distilled water, and drying to obtain a target product cobalt hydroxide/carbon nitride Co (OH)2/g-C3N4A photocatalytic material.
Example 6: preparation of cobalt hydroxide/carbon nitride photocatalytic material
Weighing 2.0g of melamine, placing the melamine in a 50mL crucible, calcining the crucible in a muffle furnace at 550 ℃ for 4h, naturally cooling to room temperature, and grinding the obtained solid in a mortar to obtain yellow powdered carbon nitride (g-C)3N4). Weighing 0.50g g-C respectively3N4And 60mg CoCl2·6H2And O, adding 40mL of distilled water into a beaker, and performing ultrasonic treatment for 20 minutes to uniformly disperse the carbon nitride. At room temperature, 1.5mL of ammonia water is added under the condition that the stirring speed is more than or equal to 60rpm, and the stirring is continued to obtain a suspension. Carrying out suction filtration on the obtained suspension, washing the solid with distilled water, and drying to obtain a target product cobalt hydroxide/carbon nitride Co (OH)2/g-C3N4A photocatalytic material.
Experimental example: photocatalytic water splitting experiment
The test was carried out using a photocatalytic decomposition water system. Weighing 50mg of cobalt hydroxide/carbon nitride photocatalytic material prepared in example 1 and example 6, adding 100mL of secondary water, transferring to a reactor after ultrasonic treatment for a while, and adding H2PtCl6(3 wt%). During the whole test, stirring was maintained and cooling water was switched on to keep the reaction system at room temperature. And vacuumizing to remove all gas in the system. The light source (300W xenon lamp, simulated sunlight) was turned on to perform the photocatalytic reaction. The gas (H) produced by the reaction was determined by an on-line gas chromatography technique2And O2) The results are shown in FIG. 4.
FIG. 4 shows Co (OH) obtained in examples 1 and 6, respectively2/g-C3N4The full hydrolysis hydrogen production and oxygen production rate of the photocatalytic material. From the figure canIt is seen that g-C prepared in example 13N4After the nano-sheet is loaded with the cobalt hydroxide nano-particles by the method provided by the invention, the nano-sheet can show higher photocatalytic full-hydrolytic activity. Bulk phase g-C prepared in example 63N4In the existing reports, the catalyst does not have full hydrolytic activity, but can realize photocatalytic full hydrolytic activity after the cobalt hydroxide nanoparticles are loaded by the method provided by the invention. Co (OH) illustrating the invention2/g-C3N4The photocatalytic material can realize full water splitting under the irradiation of sunlight, and the preparation method is simple and universal and has good application prospect.
The above-mentioned embodiments are intended to illustrate the objects, technical solutions and advantages of the present invention in further detail, and it should be understood that the above-mentioned embodiments are only exemplary embodiments of the present invention, and are not intended to limit the present invention, and any modifications, equivalents, improvements and the like made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (8)
1. A preparation method of a cobalt hydroxide/carbon nitride photocatalytic material is characterized by comprising the following steps:
(1) at room temperature, adding g-C3N4Ultrasonically dispersing in a cobalt (II) salt solution, and adding alkali under the stirring condition to obtain a suspension;
(2) and (2) carrying out suction filtration on the suspension obtained in the step (1), and washing and drying the obtained solid to obtain the cobalt hydroxide/carbon nitride photocatalytic material.
2. The method for preparing cobalt hydroxide/carbon nitride photocatalytic material according to claim 1, wherein the g-C in step (1)3N4The preparation method comprises the following steps: placing the carbon nitride precursor into a muffle furnace for calcining, and naturally cooling to room temperature to obtain light yellow g-C3N4。
3. The method for preparing a cobalt hydroxide/carbon nitride photocatalytic material according to claim 2, wherein the carbon nitride precursor is selected from one or more of urea, melamine, dicyandiamide and cyanamide; the calcining temperature is 520-600 ℃, and the heat preservation time is 2-6 h.
4. The method for preparing cobalt hydroxide/carbon nitride photocatalytic material according to claim 1, wherein the cobalt (II) salt in step (1) is one or more of cobalt chloride, cobalt nitrate and cobalt acetate.
5. The method according to claim 1, wherein the solvent in the cobalt (II) salt solution in step (1) is water, ethanol or methanol, and the amount of the cobalt (II) salt added is g-C calculated on cobalt element3N40.1-10 wt% of the mass.
6. The method for preparing a cobalt hydroxide/carbon nitride photocatalytic material according to claim 1, wherein the base in step (1) is ammonia, triethylamine or sodium hydroxide.
7. A cobalt hydroxide/carbon nitride photocatalytic material prepared by the method of any one of claims 1-6.
8. Use of the cobalt hydroxide/carbon nitride photocatalytic material of claim 7 in photocatalytic water production of oxygen and/or photocatalytic total hydrolysis water.
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Application publication date: 20220408 |