CN115028234B - Mixed phase 1T/2H MoSe 2 Application of nanosheets in piezoelectric catalysis - Google Patents

Mixed phase 1T/2H MoSe 2 Application of nanosheets in piezoelectric catalysis Download PDF

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CN115028234B
CN115028234B CN202210695894.5A CN202210695894A CN115028234B CN 115028234 B CN115028234 B CN 115028234B CN 202210695894 A CN202210695894 A CN 202210695894A CN 115028234 B CN115028234 B CN 115028234B
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马江权
吴棉棉
李楠
李庆飞
沈文静
史明豪
孙桂芳
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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
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Abstract

The application relates to the technical field of piezocatalysis, and in particular discloses a mixed phase 1T/2H MoSe 2 Use of nanoplatelets in piezocatalysis, by simply adjusting the hydrothermal temperature, successfully constructed with adjustable 1T/2H MoSe 2 A catalyst. Increasing MoSe 2 The 1T phase content of the polymer can enhance the piezoelectric effect and improve the transmission capacity of carriers, thereby improving MoSe 2 Is used for the piezoelectric catalysis of the fuel cell. In particular, moSe with the highest proportion of 1T phase (80%) prepared at 220 ℃ 2 (MoSe 2 220) rhodamine B is completely decomposed within 15 seconds, hexavalent chromium is reduced within 20 minutes, and an effective strategy is provided for constructing the high-activity piezoelectric catalyst.

Description

Mixed phase 1T/2H MoSe 2 Application of nanosheets in piezoelectric catalysis
Technical Field
The application belongs to the technical field of piezocatalysis, and in particular relates to a mixed phase 1T/2H MoSe 2 Use of nanoplatelets in piezoelectric catalysis.
Background
In recent decades, with the rapid development of modern industry, environmental pollution has become a major problem. Recently, piezoelectric catalysis based on piezoelectric materials is becoming a progressive strategy to solve environmental problems. When a mechanical force is applied, the piezoelectric material generates polarized positive and negative charges on both sides of the catalyst surface, and then forms a built-in electric field to separate electrons and holes, thereby inhibiting the recombination of carriers. Although many efforts have been made in the innovation of piezoelectric catalysts, most piezoelectric catalysts still have problems of weak piezoelectric polarization and insufficient catalytic active sites, which severely restrict the performance of piezoelectric catalysis. Therefore, developing a new strategy to improve the efficiency of piezocatalysis is critical to achieving breakthrough of piezocatalysis.
Transition Metal Dihalides (TMDs) have been extensively studied in the fields of photocatalysis, energy storage, nano-generators and electronic devices, and electrocatalysis. Notably, 2D TMD exhibits strong piezoelectricity due to the non-centrosymmetric structure. Wherein MoSe 2 Due to its excellent physical and electrical propertiesAnd electrochemical performance, have been attracting attention in recent years. MoSe is based on the arrangement of Se atoms 2 There are two phases: a semiconductor 2H phase with triangular prisms and a metal 1T phase with octahedral coordination. Both experimental and theoretical results indicate that the MoSe of the 1T phase 2 MoSe exhibiting a phase ratio of 2H due to relatively high electron conductivity 2 Better catalytic activity. However, it should be noted that pure 1T phase MoSe 2 Is metastable and can be transferred to stable 2H MoSe in natural environment 2 . Thus, 1T/2H hybrid phase MoSe 2 (1T/2H MoSe 2 ) It is expected to combine the rich active sites of the 1T phase with good conductivity with the environmental stability of the 2H phase.
Here, by adjusting the reaction temperature, the MoSe with adjustable 1T content is successfully synthesized 2 The nano-sheet is applied to piezoelectric catalysis for the first time to remove rhodamine B and hexavalent chromium in water. The results show that 1T/2H MoSe 2 The piezoelectric ceramic has ultrahigh piezoelectric catalytic degradation efficiency on rhodamine B and hexavalent chromium. The ultra-high redox activity is attributed to the establishment of an internal electric field at the 1T and 2H phase boundaries that drives the separation of electron-hole pairs, allowing the redox reaction to proceed efficiently. The results confirm MoSe 2 The nano-sheet has good application prospect in removing pollutants.
Disclosure of Invention
The application aims to provide a mixed phase 1T/2H MoSe 2 Application of nanosheets in piezoelectric catalysis and mixed phase 1T/2H MoSe under specific 1T content 2 The nano-sheets (1T and 2H are two crystal structures of molybdenum selenide) can realize the efficient degradation of rhodamine B and the efficient reduction of hexavalent chromium, thereby achieving the purpose of removing organic pollutants and heavy metal ions in industrial wastewater. The catalyst has good stability, and the preparation method is simple and efficient, low in cost, economical and environment-friendly.
In order to achieve the aim of the application, the adopted specific technical scheme is as follows:
mixed phase 1T/2H MoSe 2 Application of nanosheets in piezocatalysis for piezocatalysis degradation of rhodamine B or piezoreduction of hexavalent chromium, and mixed phase 1T/2H MoSe 2 The 1T content in the nano-sheet is 70% -80%, and the application method comprisesThe method comprises the following steps: mixing the mixed phase 1T/2H MoSe 2 The nano-sheet is added into rhodamine B or hexavalent chromium salt solution to carry out piezoelectric catalytic reaction under the dark state condition.
Further, mixed phase 1T/2H MoSe 2 The preparation method of the nano-sheet comprises the following steps:
the molar ratio was set to 4:2: naBH of 1 4 Se powder and Na 2 MoO 4 Mixing together, then dissolving in deionized water, and carrying out hydrothermal reaction after full dispersion, wherein the reaction temperature is 200-225 ℃.
As preferable: the reaction time is 18-22 h. The synthesis conditions are simple, the operation is easy, the method is rapid and efficient, energy-saving and environment-friendly, the stability is good, and the like.
More preferably: the hydrothermal temperature is 220 ℃, and the hydrothermal time is 20h.
Mixed phase 1T/2H MoSe 2 The preparation of the nanoplatelets further comprises a purification step: after natural cooling, the black precipitate was collected by centrifugation, washed several times with deionized water and absolute ethanol, and then dried overnight under vacuum at 60 ℃ to give a black powder.
Further, the drying temperature is 45-65 ℃ and the drying time is 12-16 h.
Further, the piezocatalysis reaction is carried out under the ultrasonic condition, the ultrasonic power is 240W, and the reaction time is 60s.
Compared with the prior art, the application has the following beneficial effects: the application firstly mixes the mixed phase 1T/2H MoSe with specific 1T content 2 Nanosheets as piezo-electric catalysts, mixed phase 1T/2HMoSe at specific 1T content 2 The nano-sheet has better conductivity, higher polarizability, more active centers and better piezoelectric catalysis performance, and the catalysis performance reaches or even exceeds that of the existing piezoelectric catalyst, and the nano-sheet has ultrahigh piezoelectric catalysis activity in piezoelectric catalysis degradation of rhodamine B and reduction of hexavalent chromium.
Drawings
FIG. 1 is MoSe of example 1, example 2, example 7 and comparative example 4 2 XRD pattern of the catalyst.
FIG. 2 is MoSe of example 1 2 Is transmitted through (a)And (5) an electron microscope.
FIG. 3 shows MoSe having different 1T phase contents in examples 1, 2 and 7 and comparative example 4 2 XPS profile of Se 3 d.
FIG. 4 shows the MoSe differences in examples 1, 2, and 7 and comparative example 4 2 Bar graph of 1T concentration of samples.
FIG. 5 shows MoSe having different 1T phase contents in examples 1, 2 and 7 and comparative example 4 2 Performance profile of degradation rhodamine B.
FIG. 6 shows MoSe having different 1T phase contents in examples 1, 2 and 7 and comparative example 4 2 Performance diagram of hexavalent chromium reduction.
Fig. 7 is a graph of the equilibrium of the addition of the different capture agents to the catalyst degradation rhodamine B in examples 8, 9 and 10.
Fig. 8 is a graph of the balance of the addition of the different capture agents versus the reduction of hexavalent chromium by the catalyst in examples 8, 9 and 10.
FIG. 9 is a graph of the stability performance of the catalyst of example 1 for degradation of rhodamine B.
FIG. 10 is a graph of the stability of the catalyst in example 1 to reduce hexavalent chromium.
Detailed Description
The present application is not limited to the following embodiments, and those skilled in the art can implement the present application in various other embodiments according to the present application, or simply change or modify the design structure and thought of the present application, which fall within the protection scope of the present application. It should be noted that, without conflict, the embodiments of the present application and features of the embodiments may be combined with each other.
The application is further described in detail below in connection with the examples:
the present application will be described in detail with reference to specific examples.
The degradation efficiency is calculated according to the following formula:
R＝(C-C 0 )/C 0 *100％
r, degradation efficiency
C 0 Initial concentration
And C, the concentration after degradation reaction.
Example 1
0.304g of NaBH 4 0.316g Se powder and 0.484g Na 2 MoO 4 Mix together and then dissolve in 75mL deionized water and stir for 20min. The solution was then transferred to a 100mL teflon lined stainless steel autoclave and heated to 220 ℃ for 20 hours. And (5) cooling to room temperature, centrifuging, washing, drying and grinding to obtain black powder.
The obtained catalyst is analyzed by XPS test, and MoSe is calculated according to the peak area ratio of deconvolution peaks in Se 3d XPS spectrum 2 The 1T phase content of the catalyst was 80.0%.
Weighing 10mg of catalyst and 30mL of rhodamine B with the concentration of 10mg/L, stirring for 120s under the dark state condition to reach adsorption-desorption balance, taking a sample every 15s after ultrasonic degradation for 60s, calculating degradation efficiency by measuring absorbance, and obtaining the degradation efficiency of 99.6% through analysis and calculation.
Weighing 10mg of catalyst and 30mL of hexavalent chromium solution with the concentration of 10mg/L, stirring for 30min under dark condition to reach adsorption-desorption balance, reducing for 20min under ultrasound, sampling every 5min, measuring absorbance, calculating degradation efficiency, and analyzing to obtain the degradation efficiency of 95.0%.
Example 2
Compared with example 1, the difference is that: in the preparation process, the hydrothermal temperature is changed to 180 ℃, and other preparation methods are the same as in example 1. The catalyst obtained in example 2 gave a 1T content of 67.0% by XPS analysis.
Application method the same as in example 1, moSe prepared in example 2 2 The degradation efficiency of the catalyst for 30mL of rhodamine B with the concentration of 10mg/L is 62.4 percent, and the reduction efficiency for hexavalent chromium with the concentration of 30mL of 10mg/L is 51.6 percent.
Example 3
Compared with example 1, the difference is that: in the preparation process, the hydrothermal temperature is changed to 200 ℃, and other preparation methods are the same as in example 1. The catalyst obtained in example 3 gave a 1T content of 72.0% by XPS analysis.
The method of application is the same as that of example 1, example 3MoSe 2 The degradation efficiency of the catalyst for 30mL of rhodamine B with the concentration of 10mg/L is 70.0%, and the reduction efficiency for 30mL of hexavalent chromium with the concentration of 10mg/L is 65.5%.
Example 4
Compared with example 1, the difference is that: the hydrothermal temperature was changed to 215℃during the preparation, and the other preparation methods were the same as in example 1. The catalyst obtained in example 4 gave a 1T content of 75.0% by XPS analysis.
Application method the same as in example 1, moSe prepared in example 4 2 The degradation efficiency of the catalyst for 30mL of rhodamine B with the concentration of 10mg/L is 80.2%, and the reduction efficiency for hexavalent chromium with the concentration of 30mL of 10mg/L is 78.9%.
Example 5
Compared with example 1, the difference is that: the hydrothermal temperature was changed to 225℃during the preparation process, and the other preparation methods were the same as in example 1. The catalyst obtained in example 5 gave a 1T content of 72.0% by XPS analysis.
Application method the same as in example 1, moSe prepared in example 5 2 The degradation efficiency of the catalyst for 30mL of rhodamine B with the concentration of 10mg/L is 71.3 percent, and the reduction efficiency for hexavalent chromium with the concentration of 30mL of 10mg/L is 71.0 percent.
Example 6
Compared with example 1, the difference is that: the hydrothermal temperature was changed to 230℃during the preparation, and the other preparation methods were the same as in example 1. The catalyst obtained in example 6 gave a 1T content of 52.0% by XPS analysis.
Application method the same as in example 1, moSe prepared in example 6 2 The degradation efficiency of the catalyst for 30mL of rhodamine B with the concentration of 10mg/L is 50.2%, and the reduction efficiency for hexavalent chromium with the concentration of 30mL of 10mg/L is 55.5%.
Example 7
Compared with example 1, the difference is that: the hydrothermal temperature was changed to 240℃during the preparation, and the other preparation methods were the same as in example 1. The catalyst obtained in example 7 gave a 1T content of 30.0% by XPS analysis.
Application method the same as in example 1, moSe prepared in example 7 2 The degradation efficiency of the catalyst for 30mL of rhodamine B with the concentration of 10mg/L is 18.7 percent, and the reduction efficiency for hexavalent chromium with the concentration of 10mg/L is 28.0 percent。
Example 8
Active groups in the piezoelectric degradation and reduction process are tested, and a capturing experiment is carried out, wherein the specific steps are as follows:
10mg of the catalyst of example 1 and 0.372g of disodium ethylenediamine tetraacetate were weighed, dispersed in 30mL of a 10mg/L rhodamine B solution, stirred for 120s under dark conditions to reach adsorption-desorption equilibrium, subjected to ultrasonic degradation for 60s, sampled every 15s, and the degradation efficiency was calculated by measuring absorbance, and was calculated to be 99.6% by analysis.
The catalyst obtained in example 1 was analyzed by XPS to obtain a 1T content of 80.0%.
10mg of the catalyst of example 1 and 0.270g of potassium persulfate are weighed, dispersed in 30mL of a hexavalent chromium solution of 10mg/L, stirred for 20min under dark condition to reach adsorption-desorption equilibrium, reduced for 20min under ultrasonic conditions, sampled every 5min, absorbance is measured, degradation efficiency is calculated, and the degradation efficiency is calculated to be 57% through analysis.
Example 9
Compared with example 8, the difference is that: 100. Mu.L of isopropanol was added during the reaction, and the other preparation was the same as in example 8. MoSe prepared in example 1 2 The degradation efficiency of the catalyst for 30mL of rhodamine B with the concentration of 10mg/L is 88.2%, and the reduction efficiency for hexavalent chromium with the concentration of 30mL of 10mg/L is 95.0%.
Example 10
Compared with example 8, the difference is that: during the reaction, 0.18g of p-benzoquinone was added, and the other preparation methods were the same as in example 8. MoSe prepared in example 1 2 The degradation efficiency of the catalyst for 30mL of rhodamine B with the concentration of 10mg/L is 74.0%, and the reduction efficiency for 30mL of hexavalent chromium with the concentration of 10mg/L is 76.0%.
Comparative example 1
MoSe in example 1 2 The nanosheets are calcined for 2 hours in a nitrogen atmosphere at 300 ℃, and the obtained catalyst can obtain the 1T content of 15.0% through XPS analysis.
Weighing 10mg of catalyst and 30mL of rhodamine B with the concentration of 10mg/L, stirring for 120s under the dark state condition to reach adsorption-desorption balance, taking a sample every 15s after ultrasonic degradation for 60s, calculating degradation efficiency by measuring absorbance, and obtaining the degradation efficiency of 17.6% through analysis and calculation.
Weighing 10mg of catalyst and 30mL of hexavalent chromium solution with the concentration of 10mg/L, stirring for 30min under the dark state condition to reach adsorption-desorption balance, performing ultrasonic degradation for 20min, taking a sample every 5min, measuring absorbance, calculating degradation efficiency, and analyzing to obtain the degradation efficiency of 25.2%.
Comparative example 2
Compared with comparative example 1, the difference is that: the calcination temperature was changed to 400℃and the other preparation methods were the same as in comparative example 1. The catalyst obtained in comparative example 2 was found to have a 1T content of 8.0% by XPS analysis.
The application method is the same as that of comparative example 1 and MoSe prepared in comparative example 2 2 The degradation efficiency of the catalyst for 30mL of rhodamine B with the concentration of 10mg/L is 16.4 percent, and the reduction efficiency for hexavalent chromium with the concentration of 30mL of 10mg/L is 22.1 percent.
Comparative example 3
Compared with comparative example 1, the difference is that: the calcination temperature was changed to 500℃and the other preparation methods were the same as in comparative example 1. The catalyst obtained in comparative example 3 was found to have a 1T content of 5.0% by XPS analysis.
The application method is the same as that of comparative example 1 and MoSe prepared in comparative example 3 2 The degradation efficiency of the catalyst for 30mL of rhodamine B with the concentration of 10mg/L is 15.0%, and the reduction efficiency for 30mL of hexavalent chromium with the concentration of 10mg/L is 19.0%.
Comparative example 4
Compared with comparative example 1, the difference is that: the calcination temperature was changed to 600℃and the other preparation methods were the same as in comparative example 1. The catalyst obtained in comparative example 4 was analyzed by XPS to obtain a 1T content of 0%.
The application method is the same as that of comparative example 1 and MoSe prepared in comparative example 4 2 The degradation efficiency of the catalyst for 30mL of rhodamine B with the concentration of 10mg/L is 13.0%, and the reduction efficiency for 30mL of hexavalent chromium with the concentration of 10mg/L is 16.6%.
To further demonstrate MoSe 2 Stability of 220 nanosheets XRD and XPS of the fresh and used catalyst of example 1 were tested and compared. There was no significant difference in the crystal structure between the recycled and fresh catalyst. XPS spectrum shows cyclic MoSe 2 The surface chemistry of the 220 nanosheets is unchanged and MoSe 2 The 1T phase content of-220 remains around 80% (RhB-79.2%, cr (VI) -78.9%), which proves that MoSe 2 The 220 nanometer sheet has good stability.
The foregoing is only a preferred embodiment of the present application, but the scope of the present application is not limited thereto, and any person skilled in the art, who is within the scope of the present application, should make equivalent substitutions or modifications according to the technical scheme and the concept of the present application, and should be covered by the scope of the present application.

Claims (3)

1. Mixed phase 1T/2H MoSe 2 The application of the nano-sheet in piezoelectric catalysis is characterized in that: used for piezocatalysis degradation of rhodamine B or piezoreduction of hexavalent chromium, and mixed phase 1T/2H MoSe 2 The 1T content in the nano-sheet is 80%, and the application method comprises the following steps: mixing the mixed phase 1T/2H MoSe 2 Adding the nano-sheet into rhodamine B or hexavalent chromium salt solution, and performing piezoelectric catalytic reaction under dark state conditions;
1T/2H MoSe 2 the preparation method of the nano-sheet comprises the following steps: 0.304g of NaBH 4 0.316g Se powder and 0.484g Na 2 MoO 4 Mix together and then dissolve in 75mL deionized water and stir for 20min, then transfer the solution to a 100mL teflon lined stainless steel autoclave and heat to 220 ℃ for 20 hours.
2. The mixed phase 1T/2H MoSe of claim 1 2 The application of the nano-sheet in piezoelectric catalysis is characterized in that: mixed phase 1T/2H MoSe 2 The preparation of the nanoplatelets further comprises a purification step: after natural cooling, the black precipitate was collected by centrifugation, washed several times with deionized water and absolute ethanol, and then dried overnight under vacuum at 60 ℃ to give a black powder.
3. The mixed phase 1T/2H MoSe of claim 1 2 The application of the nano-sheet in piezoelectric catalysis is characterized in that: the saidThe piezoelectric catalytic reaction is carried out under the ultrasonic condition, the ultrasonic power is 240W, and the reaction time is 60s.
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Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109970153A (en) * 2019-04-24 2019-07-05 夸克能源工程实验室(深圳)有限公司 A kind of WSe2The method of nanometer sheet piezoelectricity catalyst efficient degradation organic pollutant
CN113955823A (en) * 2021-11-19 2022-01-21 常州大学 1T/2H MoSe2/Bi2WO6Application of piezoelectric-optical composite catalyst

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109970153A (en) * 2019-04-24 2019-07-05 夸克能源工程实验室(深圳)有限公司 A kind of WSe2The method of nanometer sheet piezoelectricity catalyst efficient degradation organic pollutant
CN113955823A (en) * 2021-11-19 2022-01-21 常州大学 1T/2H MoSe2/Bi2WO6Application of piezoelectric-optical composite catalyst

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