CN115893523A - Preparation method and application of transition metal phosphide - Google Patents
Preparation method and application of transition metal phosphide Download PDFInfo
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- CN115893523A CN115893523A CN202211533073.8A CN202211533073A CN115893523A CN 115893523 A CN115893523 A CN 115893523A CN 202211533073 A CN202211533073 A CN 202211533073A CN 115893523 A CN115893523 A CN 115893523A
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- 150000003624 transition metals Chemical class 0.000 title claims abstract description 33
- 238000002360 preparation method Methods 0.000 title claims abstract description 22
- 239000003054 catalyst Substances 0.000 claims abstract description 30
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 claims abstract description 26
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- 238000006243 chemical reaction Methods 0.000 claims abstract description 20
- 239000002131 composite material Substances 0.000 claims abstract description 19
- 239000011941 photocatalyst Substances 0.000 claims abstract description 16
- 238000003756 stirring Methods 0.000 claims abstract description 8
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- KBJMLQFLOWQJNF-UHFFFAOYSA-N nickel(ii) nitrate Chemical compound [Ni+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O KBJMLQFLOWQJNF-UHFFFAOYSA-N 0.000 claims description 22
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- STZCRXQWRGQSJD-GEEYTBSJSA-M methyl orange Chemical compound [Na+].C1=CC(N(C)C)=CC=C1\N=N\C1=CC=C(S([O-])(=O)=O)C=C1 STZCRXQWRGQSJD-GEEYTBSJSA-M 0.000 description 4
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- JQMFQLVAJGZSQS-UHFFFAOYSA-N 2-[4-[2-(2,3-dihydro-1H-inden-2-ylamino)pyrimidin-5-yl]piperazin-1-yl]-N-(2-oxo-3H-1,3-benzoxazol-6-yl)acetamide Chemical compound C1C(CC2=CC=CC=C12)NC1=NC=C(C=N1)N1CCN(CC1)CC(=O)NC1=CC2=C(NC(O2)=O)C=C1 JQMFQLVAJGZSQS-UHFFFAOYSA-N 0.000 description 2
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 2
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- FBMUYWXYWIZLNE-UHFFFAOYSA-N nickel phosphide Chemical compound [Ni]=P#[Ni] FBMUYWXYWIZLNE-UHFFFAOYSA-N 0.000 description 2
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- LDXJRKWFNNFDSA-UHFFFAOYSA-N 2-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)-1-[4-[2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidin-5-yl]piperazin-1-yl]ethanone Chemical compound C1CN(CC2=NNN=C21)CC(=O)N3CCN(CC3)C4=CN=C(N=C4)NCC5=CC(=CC=C5)OC(F)(F)F LDXJRKWFNNFDSA-UHFFFAOYSA-N 0.000 description 1
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- RMZAYIKUYWXQPB-UHFFFAOYSA-N trioctylphosphane Chemical compound CCCCCCCCP(CCCCCCCC)CCCCCCCC RMZAYIKUYWXQPB-UHFFFAOYSA-N 0.000 description 1
Images
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/30—Hydrogen technology
- Y02E60/36—Hydrogen production from non-carbon containing sources, e.g. by water electrolysis
Abstract
The invention discloses a preparation method and application of transition metal phosphide, the transition metal phosphide is prepared by a simple one-step hydrothermal method, a non-toxic and low-cost phosphorus source is used, common metal salt is used as a metal source, the phosphorus source and the metal source are added into a solvent according to a certain proportion, and a hydrothermal reaction is carried out in a reaction kettle after stirring and mixing, the synthesis method has simple steps, mild conditions and environmental friendliness, reactants are non-toxic and non-corrosive, and a target product is easily prepared. In addition, the prepared transition metal phosphide, cadmium sulfide, carbon nitride and the like are prepared into the composite photocatalyst by a one-step hydrothermal method, and the photocatalyst performance of the composite transition metal phosphide catalyst is obviously improved and the composite transition metal phosphide catalyst has higher practical value compared with the single cadmium sulfide, carbon nitride and the like under the same test condition.
Description
Technical Field
The invention belongs to the technical field of material chemistry and photocatalysis, and particularly relates to a preparation method and application of transition metal phosphide.
Background
Semiconductor photocatalytic technology has been used as the most promising strategy to address the energy and environmental crisis for the generation of hydrogen energy and the removal of environmental pollutants.
For the last decades, titania-based semiconductor photocatalysts have been considered as the best photocatalysts for decomposing water. However, the wide band gap of titanium dioxide makes it only excitable by ultraviolet light, and more solar radiation energy is not available. Therefore, the development of visible light-responsive photocatalysts is a current trend. Of the various semiconductor materials, cadmium sulfide and carbon nitride are typical materials that can exhibit both of the above properties. Cadmium sulfide has a narrow band gap, a proper conduction band position and a unique photoelectrochemical effect, and carbon nitride has a large specific surface area, good adsorption performance and a stable molecular structure, and attracts great attention in the field of visible light catalysis. Unfortunately, their further practical application is limited by the high rate of charge recombination, low charge transfer capability and the inherent photo-corrosive properties of cadmium sulfide. Therefore, the important task at present is to improve the separation efficiency of photo-generated charges, and the basic strategy is to design a composite photocatalyst capable of assisting electron transport.
As is well known, the most commonly used electron transfer media in the heterojunction catalyst are noble metals such as Au and Pt, but the practical popularization and application are limited due to high cost.
Disclosure of Invention
This section is for the purpose of summarizing some aspects of embodiments of the invention and to briefly introduce some preferred embodiments. In this section, as well as in the abstract and title of the application, simplifications or omissions may be made to avoid obscuring the purpose of the section, the abstract and the title, and such simplifications or omissions are not intended to limit the scope of the invention.
As one aspect of the present invention, there is provided a method for preparing a transition metal phosphide, comprising the steps of,
dispersing nickel nitrate in water to obtain a nickel nitrate solution, dispersing red phosphorus in the nickel nitrate solution, uniformly stirring, adding into a forced air drying oven, reacting at 100-160 ℃ for 8-24 h, cooling, washing and drying to obtain the transition metal phosphide.
As a preferred embodiment of the preparation method of the transition metal phosphide provided by the invention: the molar ratio of the nickel nitrate to the red phosphorus is 1: 5-20.
As a preferred embodiment of the preparation method of the transition metal phosphide provided by the invention: the molar ratio of the nickel nitrate to the red phosphorus is 1: 10, the reaction is carried out for 10 hours at 120 ℃, and the transition metal phosphide is Ni 2 P。
As a preferable scheme of the preparation method of the transition metal phosphide, the following steps are carried out: the molar ratio of the nickel nitrate to the red phosphorus is 1: 5, the reaction is carried out for 10 hours at 140 ℃, and the transition metal phosphide is Ni 12 P 5 。
As a preferable scheme of the preparation method of the transition metal phosphide, the following steps are carried out: and the washing is to carry out 3-5 times of centrifugal washing on the solid material by using deionized water and absolute ethyl alcohol respectively.
As a preferred embodiment of the preparation method of the transition metal phosphide provided by the invention: and drying at 60 ℃ for 10h.
The invention also provides an application of the transition metal phosphide in preparing the composite photocatalyst: compounding the transition metal phosphide and a matrix catalyst to obtain a photocatalyst; wherein, the matrix catalyst comprises one or more of graphite-like carbon nitride, cadmium sulfide and titanium dioxide.
Dispersing nickel nitrate in water to obtain a nickel nitrate solution, adding red phosphorus and a matrix catalyst, dispersing the nickel nitrate solution into the nickel nitrate solution, uniformly stirring, adding the nickel nitrate solution into an air-blast drying oven, reacting for 8-24 h at 100-160 ℃, cooling, washing and drying to obtain the composite photocatalyst.
Wherein the matrix catalyst is g-C 3 N 4 Red phosphorus with g-C 3 N 4 The mass ratio of (A) to (B) is 1: 9-11.
Wherein the matrix catalyst is CdS, and the mass ratio of red phosphorus to CdS is 1: 9-11.
The invention has the beneficial effects that:
1) The phosphorus source used in the synthesis of the transition metal phosphide is red phosphorus which is cheap, easy to obtain and nontoxic, but not white phosphorus, triphenylphosphine or trioctylphosphine which has strong toxicity or is expensive.
2) The invention realizes the preparation of different target products at lower temperature and in shorter time by hydrothermal reaction and by controlling the material proportion and the reaction temperature.
3) The solvent used in the hydrothermal reaction is water instead of organic solvents such as ethylenediamine, ethylene glycol, isopropanol, triethanolamine and the like, so that the operation and experiment process is safer to a certain extent, and secondary pollution to the environment is avoided.
4) The invention does not use surface active agent in the reaction process, the specific surface area of the product is high, and more reaction active sites can be provided.
5) In the preparation of the actual composite photocatalyst, the invention can use a direct one-step hydrothermal method for in-situ compounding, and is convenient to apply.
6) The method has the advantages of environmental friendliness, low cost, high safety, high practical value and the like in preparation.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings needed to be used in the description of the embodiments will be briefly introduced below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and it is obvious for those skilled in the art to obtain other drawings based on these drawings without inventive exercise. Wherein:
FIG. 1 is an X-ray diffraction (XRD) pattern of the product prepared in example 1;
FIG. 2 is an X-ray diffraction (XRD) pattern of the product prepared in example 2;
FIG. 3 is a UV-visible diffuse reflectance (UV-vis DRS) spectrum of the product prepared in example 2;
FIG. 4 shows N of the product obtained in example 2 2 Adsorption-desorption isotherm (BET) curves;
FIG. 5 is a graph of the photocatalytic activity of the product obtained in example 2 and the degradation rate constant k corresponding to the photocatalytic degradation of methyl orange app Drawing;
FIG. 6 is an X-ray diffraction (XRD) pattern of the product made in example 3;
FIG. 7 is a UV-visible diffuse reflectance (UV-vis DRS) spectrum of the product obtained in example 3;
FIG. 8 shows N for the product obtained in example 3 2 Adsorption-desorption isotherm (BET) curves;
FIG. 9 is a graph of the photocatalytic activity of the product obtained in example 3 and the degradation rate constant k corresponding to the photocatalytic degradation of methyl orange app Figure (a).
FIG. 10 is an X-ray diffraction pattern of each product of comparative example 1.
FIG. 11 is an X-ray diffraction pattern of each product of comparative example 2.
FIG. 12 is an X-ray diffraction pattern of each product of comparative example 3.
FIG. 13 shows Ni prepared in example 2 2 P/g-C 3 N 4 The photocatalytic hydrogen production activity diagram.
FIG. 14 shows Ni prepared in example 3 12 P 5 A photocatalytic hydrogen production activity diagram of CdS.
FIG. 15 is a graph showing the effect of temperature on photocatalytic hydrogen production activity of the product in comparative example 4.
FIG. 16 shows the effect of molar ratio of comparative example 4 on the photocatalytic hydrogen production activity of the product.
FIG. 17 shows Ni in comparative example 5 2 P/g-C 3 N 4 And Ni 12 P 5 /g-C 3 N 4 The photocatalytic hydrogen production activity of (2).
FIG. 18 is a comparisonNi in example 5 2 P/CdS and Ni 12 P 5 Photocatalytic hydrogen production activity of CdS.
Detailed Description
In order to make the aforementioned objects, features and advantages of the present invention more comprehensible, embodiments accompanying specific embodiments of the present invention are described in detail below.
The reagents used in the following examples were purchased from national reagents, inc. (China) and used for experiments without further purification; deionized water is used as experimental water.
Example 1:
pretreatment of commercial red phosphorus. After 4.0g of commercial Red Phosphorus (RP) was ground and refined in an agate mortar, it was transferred to a polytetrafluoroethylene liner having a volume of 100mL and placed in a stainless steel autoclave and heat-insulated at 200 ℃ for 10 hours. After the reaction is finished, cooling to room temperature, taking out, centrifugally washing the product by deionized water, drying at 70 ℃ and collecting a red powder product.
Ni 2 P is synthesized by a hydrothermal method. Weighing a certain amount of Ni (NO) 3 ) 2 ·6H 2 O is dispersed and dissolved in a reaction vessel liner containing 30mL of deionized water, and then 0.31g of treated red phosphorus (molar ratio Ni (NO)) 3 ) 2 ·6H 2 O: P = 1: 10) was dispersed into the above solution, stirred for 1h, and then the mixed mass was transferred to an air-blast drying oven, set at a temperature of 120 ℃, for a reaction time of 10h. After the substitution reaction is finished, cooling to room temperature, centrifugally washing the product for a plurality of times by using deionized water and absolute ethyl alcohol, drying at 60 ℃ and collecting to obtain black solid Ni 2 P。
Ni 12 P 5 The hydrothermal method. Weighing a certain amount of Ni (NO) 3 ) 2 ·6H 2 O is dispersed and dissolved in a reaction kettle lining containing 30mL of deionized water, and then the treated red phosphorus (the molar ratio of Ni (NO) is weighed 3 ) 2 ·6H 2 O: P = 1: 5) was dispersed into the above solution and stirred for 1h. The mixture was subsequently transferred to an air-drying oven, the temperature set at 140 ℃ and the reaction time 10h. After the reaction is finished, cooling to room temperature, centrifugally washing the product for a plurality of times by using deionized water and absolute ethyl alcohol,drying at 60 deg.C, collecting to obtain black solid Ni 12 P 5 。
FIG. 1 shows the X-ray diffraction pattern of the product obtained in example 1, from which Ni was obtained 2 There are significant diffraction spectrum peaks for P at 2 θ =29.1 °, 31.2 °, 44.8 °, 50.5 ° and 54.6 ° (JCPDS: 74-1385); produced Ni 12 P 5 The diffraction peaks (JCPDS: 74-1381) are obvious at 2 theta =33.0 degrees, 36.5 degrees, 38.5 degrees, 42.6 degrees, 45.0 degrees, 47.5 degrees and 49.5 degrees, the peak shapes are sharp, and other miscellaneous peaks are absent, which indicates that the prepared material has high crystallization degree and high purity of the product.
Comparative example 1:
investigation of Ni 2 In the hydrothermal synthesis process of P, the influence of the reaction temperature on the product morphology is reduced by Ni 2 The hydrothermal temperatures of P were set to 100 deg.C, 120 deg.C, 140 deg.C, and 160 deg.C, respectively, and other preparation conditions were the same as in example 1. The X-ray diffraction patterns of the products obtained at different temperatures are shown in FIG. 10. As can be seen from FIG. 10, the obtained nickel phosphide can form pure Ni at 100 ℃ and 120 ℃ 2 P, belonging to Ni, with increasing temperature 2 The characteristic peak of P is gradually weakened in relative intensity and belongs to Ni 12 P 5 The relative intensity of the characteristic peak of the Ni-based amorphous alloy is gradually enhanced, which shows that under certain other conditions, the crystal form of the prepared substance is made of Ni along with the increase of the temperature 2 P gradually goes to Ni 12 P 5 The transformation takes place. Furthermore, ni at 120 deg.C 2 The crystallinity of P is stronger.
Comparative example 2:
study of Ni 12 P 5 In the hydrothermal synthesis of (1), ni (NO) 3 ) 2 ·6H 2 Influence of O: P molar ratio on the morphology of the product, adding Ni (NO) 3 ) 2 ·6H 2 The molar ratio of O to P was adjusted to 1: 5,1: 10,1: 15,1: 20, respectively, and other preparation conditions were the same as in example 1. The X-ray diffraction patterns of the products obtained at different temperatures are shown in FIG. 11. As can be seen from FIG. 11, when Ni (NO) is added 3 ) 2 ·6H 2 The molar ratio of O to P is respectively as follows: the X-ray diffraction peak of the solid product obtained at 1: 5,1: 10,1: 15,1: 20 can be mixed with Ni without special impurity 12 P 5 The characteristic peaks of (a) substantially coincide. Under other conditions, the relative intensity of the partial diffraction peaks corresponding to the product changes with increasing molar ratio, corresponding to Ni at 54.2 ° 2 The characteristic peak relative intensities of the P (002) and (300) crystal planes gradually increase. Description of Ni 12 P 5 Is subjected to Ni (NO) formation 3 ) 2 ·6H 2 The effect of the change in the molar ratio of O to P, while the effect of the temperature plays a dominant role. When a reaction temperature of 140 ℃ was given, ni was confirmed to be substantially in the range of experimental ratio 12 P 5 Formation of Ni (NO) 3 ) 2 ·6H 2 The molar ratio of O to P is 1: 5, and the Ni can be used as Ni 12 P 5 Preferred preparation conditions of (2).
Comparative example 3:
investigation of Ni 2 In the hydrothermal synthesis process of P, the influence of the reaction time on the product morphology is reduced, and Ni is added 2 The hydrothermal reaction times of P were adjusted to 8h,10h,12h and 24h, respectively, and the preparation conditions were the same as in example 1. The X-ray diffraction patterns corresponding to the products obtained at different reaction times are shown in FIG. 12. As can be seen from FIG. 12, the reaction times were determined to be 8h,10h,12h and 24h under other conditions, respectively, which indicated pure Ni 2 And P. Namely, with the increase of the reaction time, the crystal form of the prepared substance can not be changed, the relative intensity of the characteristic diffraction peak can be increased, and the crystallinity is better.
Example 2:
Ni 2 P/g-C 3 N 4 synthesis, characterization and application of the composite catalyst.
Ni in this example and example 1 2 The only difference in the hydrothermal synthesis of P is that 0.30g of g-C are added simultaneously with the addition of red phosphorus 3 N 4 Stirring and mixing uniformly together. The other preparation methods were the same as in example 1.
FIG. 2 is the X-ray diffraction pattern of the product obtained in example 2, and it can be seen from FIG. 2 that at a lower loading, the composite also slightly shows Ni 2 P and g-C 3 N 4 Characteristic diffraction peak of (2), indicating Ni 2 P is successfully loaded on g-C 3 N 4 The above. FIG. 3 shows the product obtained in example 2Ultraviolet-visible diffuse reflectance (UV-vis DRS) spectra of the preparations. As can be seen, pure Ni 2 P has excellent absorption performance in the spectral region and g-C 3 N 4 Upper load of Ni 2 After P, the light absorption range of the catalyst is expanded, and the light utilization efficiency is improved. FIG. 4 shows N in the product obtained in example 2 2 Adsorption-desorption isotherms.
Ni with a mass of 0.02g 2 P/g-C 3 N 4 The composite catalyst was added to a beaker containing 30mL of methyl orange solution (10 mg/L), followed by slow stirring in the absence of light for 30min to allow thorough mixing to reach an equilibrium state of adsorption and desorption. And then placing the reaction kettle under a 300W xenon lamp with a cut-420nm filter for reaction, namely the reaction is carried out under visible light (lambda is more than or equal to 420 nm), and in addition, keeping the beaker at the constant temperature of 6 ℃ in the reaction process and stirring continuously. After the start of illumination, a certain amount of the mixture was extracted every 30min, centrifuged, filtered, and the absorbance at 464nm was measured. And evaluating the catalytic degradation performance of the catalyst according to the change of the liquid absorbance before and after illumination.
Another 0.05gNi is selected 2 P/g-C 3 N 4 Putting the composite catalyst into a reactor, adding 45mL of deionized water into the reactor, adding 5mL of triethanolamine as a sacrificial agent, dispersing and mixing uniformly under an ultrasonic condition, putting the reactor under a 300W xenon lamp with a cut-420nm optical filter for reaction, sampling once every 1h, and analyzing products through gas chromatography. Under the same conditions to Ni 2 P and g-C 3 N 4 Tests were performed for comparison.
FIG. 5 is a graph of the photocatalytic activity of the product prepared in example 2 and the degradation rate constant k corresponding to the photocatalytic degradation of methyl orange app FIG. 13 shows Ni 2 P/g-C 3 N 4 The photocatalytic hydrogen production activity diagram. Known as Ni complex 2 P/g-C 3 N 4 Compared with pure g-C 3 N 4 The method has remarkable improvement, and the original reason is that the photoproduction electrons on the conduction band of the photocatalyst substrate can be quickly transferred to the transition metal phosphide through the interface due to the participation of the transition metal phosphide, thereby promoting the photoproductionThe separation of the carriers further improves the catalytic activity of the photocatalyst.
Example 3:
Ni 12 P 5 and synthesizing, characterizing and applying the/CdS composite catalyst. Ni in this example and example 1 12 P 5 The hydrothermal synthesis method is only characterized in that 0.30g of CdS is added simultaneously when red phosphorus is added, and the mixture is stirred and mixed uniformly.
Example 3 the product characterization was the same as example 2, the photocatalytic degradation activity test conditions were the same as example 2, except that methyl orange solution was used at a concentration of 20mg/L, the adsorption and desorption equilibrium time in the absence of light was 20min, the sampling time interval during the reaction was 20min, and 0.35M Na was used in the photocatalytic hydrogen production activity test 2 SO 3 And 0.25M Na 2 S solution is used as a sacrificial agent, and figure 9 is a photo-catalytic activity diagram of the product prepared in example 3 and a degradation rate constant k corresponding to photo-catalytic degradation of methyl orange app Figure (a). FIG. 14 shows Ni 12 P 5 A photocatalytic hydrogen production activity diagram of CdS. Is known to be Ni 12 P 5 As a cocatalyst, it positively affects the catalytic performance of the catalyst on the rapid transfer of photo-generated electrons.
Comparative example 4:
ni obtained in comparative example 1 2 P Ni preparation according to example 2 2 P/g-C 3 N 4 Compounding the catalyst and testing the photocatalytic hydrogen generation performance of the product under the same condition. From the obtained photocatalytic hydrogen production rate chart 15, it can be known that Ni prepared under different temperature conditions 2 P has a different co-catalytic effect on the catalyst substrate. Among the data obtained by the experiment, the compound prepared at 120 ℃ and 140 ℃ has the best photocatalytic hydrogen production activity. The reason for this may be due to the influence of the preparation temperature on the phosphide size and crystal plane.
Ni obtained in comparative example 2 12 P 5 Ni production according to example 3 12 P 5 The catalyst is/CdS composite catalyst, and the photocatalytic hydrogen generation performance of the product is tested under the same condition. From the obtained photocatalytic hydrogen production rate chart 16, it can be seen that different Ni (NO) s 3 ) 2 ·6H 2 At a molar ratio of O to P to obtainNi of (2) 12 P 5 The catalyst has different promoting effects on the catalyst matrix, wherein the composite photocatalyst prepared when the ratio of Ni to P is 1: 5 is the best in the expression of catalytic activity. The reason for this may be due to the influence of the preparation parameters on the morphology and crystal planes of the phosphide.
Comparative example 5:
ni obtained in example 1 2 P and Ni 12 P 5 Ni was produced according to the methods of example 2 and example 3, respectively 2 P/g-C 3 N 4 ,Ni 12 P 5 /g-C 3 N 4 ,Ni 2 P/CdS and Ni 12 P 5 The catalyst is a CdS composite catalyst, and the photocatalytic hydrogen production performance of the product is tested under the same condition to discuss the promotion effect of different nickel phosphide on the catalytic activity of a substrate under the same substrate.
From FIGS. 17 and 18, ni can be seen 2 P/g-C 3 N 4 ,Ni 12 P 5 /g-C 3 N 4 ,Ni 2 P/CdS and Ni 12 P 5 The CdS composite catalyst obviously improves the photocatalytic hydrogen production activity of a matrix, and the catalytic effect of the CdS composite catalyst is superior to that of the load of a noble metal Pt. Furthermore, ni 2 P/g-C 3 N 4 And Ni 12 P 5 /g-C 3 N 4 In contrast, ni 2 P/g-C 3 N 4 Has a significantly higher catalytic activity of Ni 2 P/CdS and Ni 12 P 5 Relative to CdS, ni 12 P 5 The catalytic activity of the/CdS is obviously higher.
It should be noted that the above-mentioned embodiments are only for illustrating the technical solutions of the present invention and not for limiting, and although the present invention is described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that modifications or equivalent substitutions can be made to the technical solutions of the present invention without departing from the spirit and scope of the technical solutions of the present invention, which should be covered by the claims of the present invention.
Claims (10)
1. A method for preparing a transition metal phosphide is characterized by comprising the following steps: the method comprises the following steps of (1),
dispersing nickel nitrate in water to obtain a nickel nitrate solution, dispersing red phosphorus in the nickel nitrate solution, uniformly stirring, adding into a forced air drying oven, reacting at 100-160 ℃ for 8-24 h, cooling, washing and drying to obtain the transition metal phosphide.
2. The method for preparing a transition metal phosphide according to claim 1, wherein: the mol ratio of the nickel nitrate to the red phosphorus is 1: 5-20.
3. The method for preparing a transition metal phosphide according to claim 1, characterized in that: the molar ratio of the nickel nitrate to the red phosphorus is 1: 10, the reaction is carried out at 120 ℃ for 10h, and the transition metal phosphide is Ni 2 P。
4. The method for preparing a transition metal phosphide according to claim 1, characterized in that: the molar ratio of the nickel nitrate to the red phosphorus is 1: 5, the reaction is carried out at 140 ℃ for 10h, and the transition metal phosphide is Ni 12 P 5 。
5. The method for producing a transition metal phosphide as recited in any one of claims 1 to 4, characterized in that: and the washing is to carry out 3-5 times of centrifugal washing on the solid material by using deionized water and absolute ethyl alcohol respectively.
6. The method for producing a transition metal phosphide as recited in any one of claims 1 to 4, characterized in that: and drying at 60 ℃ for 10h.
7. The use of a transition metal phosphide as claimed in claim 1 in the preparation of a composite photocatalyst, wherein: compounding the transition metal phosphide and a matrix catalyst to obtain a photocatalyst; wherein, the matrix catalyst comprises one or more of graphite-like carbon nitride, cadmium sulfide and titanium dioxide.
8. Use according to claim 7, characterized in that: dispersing nickel nitrate in water to obtain a nickel nitrate solution, adding red phosphorus and a matrix catalyst, dispersing the nickel nitrate solution into the nickel nitrate solution, uniformly stirring, adding the nickel nitrate solution into an air-blast drying oven, reacting for 8-24 h at 100-160 ℃, cooling, washing and drying to obtain the composite photocatalyst.
9. Use according to claim 8, characterized in that: the matrix catalyst is g-C 3 N 4 Red phosphorus with g-C 3 N 4 The mass ratio of (A) to (B) is 1: 9-11.
10. Use according to claim 8, characterized in that: the matrix catalyst is CdS, and the mass ratio of red phosphorus to CdS is 1: 9-11.
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CN104944396A (en) * | 2015-06-09 | 2015-09-30 | 辽宁科技学院 | Controllable synthesis method of nickel phosphide micro-nano material |
GB202104470D0 (en) * | 2021-03-30 | 2021-05-12 | Zhuang wuyi | Titanium dioxide/nickel phosphide photocatalyst for hydrogen production by degrading plastics and a preparation method thereof |
CN114471639A (en) * | 2022-02-21 | 2022-05-13 | 内蒙古科技大学 | Transition metal element doped and cadmium sulfide loaded transition metal phosphide photocatalytic material with sulfur vacancy and preparation method thereof |
CN114588925A (en) * | 2022-03-21 | 2022-06-07 | 福州大学 | Noble-metal-free supported nickel phosphide/carbon nitride visible-light-driven photocatalyst and preparation method thereof |
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CN104944396A (en) * | 2015-06-09 | 2015-09-30 | 辽宁科技学院 | Controllable synthesis method of nickel phosphide micro-nano material |
GB202104470D0 (en) * | 2021-03-30 | 2021-05-12 | Zhuang wuyi | Titanium dioxide/nickel phosphide photocatalyst for hydrogen production by degrading plastics and a preparation method thereof |
CN114471639A (en) * | 2022-02-21 | 2022-05-13 | 内蒙古科技大学 | Transition metal element doped and cadmium sulfide loaded transition metal phosphide photocatalytic material with sulfur vacancy and preparation method thereof |
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