CN116920903B - MoS (MoS)2Preparation method and application of/h-BN composite piezoelectric catalyst - Google Patents
MoS (MoS)2Preparation method and application of/h-BN composite piezoelectric catalystInfo
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- CN116920903B CN116920903B CN202310790575.7A CN202310790575A CN116920903B CN 116920903 B CN116920903 B CN 116920903B CN 202310790575 A CN202310790575 A CN 202310790575A CN 116920903 B CN116920903 B CN 116920903B
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/46—Treatment of water, waste water, or sewage by electrochemical methods
- C02F1/461—Treatment of water, waste water, or sewage by electrochemical methods by electrolysis
- C02F1/467—Treatment of water, waste water, or sewage by electrochemical methods by electrolysis by electrochemical disinfection; by electrooxydation or by electroreduction
- C02F1/4672—Treatment of water, waste water, or sewage by electrochemical methods by electrolysis by electrochemical disinfection; by electrooxydation or by electroreduction by electrooxydation
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- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/24—Nitrogen compounds
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- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
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- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
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Abstract
本发明公开了一种MoS2/h‑BN复合压电催化剂的制备方法和应用，该复合压电催化剂的制备以硫脲、二水合钼酸钠、尿素、硼酸为原料，采用水热合成法和高温煅烧法分别得到MoS2NFs(纳米花)和h‑BN，通过加水搅拌得到MoS2/h‑BN复合压电催化剂，其中，搅拌时间为8～12h。本发明制备得到的MoS2/h‑BN复合压电催化剂制备工艺简单、产量大，具有催化活性高和反应位点多的特点，该材料能够在超声条件下活化过硫酸盐，对水中双酚F进行高效催化降解。
The invention discloses a preparation method and application of a MoS2 /h-BN composite piezoelectric catalyst. The composite piezoelectric catalyst is prepared by using thiourea, sodium molybdate dihydrate, urea and boric acid as raw materials, adopting a hydrothermal synthesis method and a high-temperature calcination method to obtain MoS2NFs (nanoflowers) and h-BN respectively, and adding water and stirring to obtain the MoS2 /h-BN composite piezoelectric catalyst, wherein the stirring time is 8 to 12 hours. The MoS2 /h-BN composite piezoelectric catalyst prepared by the invention has a simple preparation process, a large output, and has the characteristics of high catalytic activity and multiple reaction sites. The material can activate persulfate under ultrasonic conditions and efficiently catalyze the degradation of bisphenol F in water.
Description
Technical Field
The invention belongs to the field of preparation of electrocatalysts, and particularly relates to a preparation method and application of a MoS 2/h-BN composite piezoelectric catalyst.
Background
Bisphenol a (BPA) is widely used as a representative of Endocrine Disruptors (EDCs) for producing various chemical materials such as polycarbonate plastics and epoxy resins. Due to the potential adverse effects of BPA on human health, there is an increasing concern that many countries have banned the use of BPA in certain products, such as canada, china, and the european union. Thus, manufacturers must use BPA substitutes to comply with new regulations.
Bisphenol-f (4, 4-dihydroxydiphenylmethane, BPF) is widely used in a variety of industrial applications due to its excellent thermal and photostability, and is considered as a "safer" alternative to BPA. Despite this stability, BPF is often detected in environmental matrices in the course of many years of research. The potential adverse effects of BPF on the human body have been found by many researchers to pose a direct threat to human health, including cytotoxicity, neurotoxicity, reproductive toxicity, genotoxicity, and carcinogenicity. Therefore, the research on the BPF removal method has important practical significance.
Molybdenum disulfide (MoS 2) is a typical two-dimensional piezoelectric material with a large specific surface area, multiple active sites, strong adsorption properties, and high piezoelectric response. In recent years, moS 2 materials have received extensive attention as piezoelectric catalysts for the removal of organic contaminants. Hexagonal boron nitride (h-BN) is also widely used in the research of environmental functional materials as a class of graphite-like two-dimensional materials with piezoelectric nanostructures, because the polarity of B-N bonds and a wide band gap of the hexagonal boron nitride (h-BN) show higher organic pollutant adsorption characteristics and photocatalytic properties.
At present, a plurality of researches are carried out on respective composite materials of MoS 2 and BN, but the composite piezoelectric materials of MoS 2 and BN heterostructure are not reported yet, and the piezoelectric catalysis mechanism is still unclear.
Disclosure of Invention
This section is intended to outline some aspects of embodiments of the application and to briefly introduce some preferred embodiments. Some simplifications or omissions may be made in this section as well as in the description of the application and in the title of the application, which may not be used to limit the scope of the application.
The present invention has been made in view of the above and/or problems occurring in the prior art.
Therefore, the invention aims to overcome the defects in the prior art and provide a preparation method of the MoS 2/h-BN composite piezoelectric catalyst.
In order to solve the technical problems, the invention provides a preparation method of a MoS 2/h-BN composite piezoelectric catalyst, which comprises the following steps of,
Mixing thiourea and sodium molybdate dihydrate, dissolving in water, adding hydrochloric acid to adjust pH, and heating to obtain a hydrothermal product;
filtering, washing to neutrality, and drying to obtain MoS 2 NFs powder;
dissolving urea and boric acid in ultrapure water, heating to generate white solid, calcining at high temperature, and grinding to obtain h-BN powder;
Adding MoS 2 NFs and h-BN into ultrapure water, mixing, centrifuging, washing and drying to obtain the product MoS 2/h-BN composite piezoelectric catalyst.
As a preferable scheme of the preparation method, the mass ratio of the thiourea to the sodium molybdate dihydrate is 3:4-10.
The preparation method is characterized by comprising the steps of adding hydrochloric acid to adjust pH, heating to obtain a hydrothermal product, wherein the pH value is 1, the heating temperature is 180-200 ℃, and the reaction time is 20-24 hours.
As a preferable scheme of the preparation method, the pore diameter of a filter membrane adopted in the filtering is 0.22-0.45 mu m, moS 2 NFs powder is prepared by drying, the drying temperature is 50-70 ℃, and the drying type is vacuum drying.
As a preferable scheme of the preparation method, the molar ratio of the urea to the boric acid is 1:40-50.
The preparation method is characterized by comprising the steps of heating to generate white solid, calcining at a high temperature of 60-70 ℃, wherein the high temperature calcining is performed in a nitrogen atmosphere at 800-1000 ℃ for 4-6 hours.
As a preferable scheme of the preparation method, moS 2 NFs and h-BN are added into ultrapure water to be mixed, wherein the mass ratio of MoS 2 to h-BN is 1:1-98:2, and the mixing time is 8-12 h.
As a preferable scheme of the preparation method, the centrifugal rotating speed is 8000-9000 r/min, and the centrifugal time is 4-6 min.
It is yet another object of the present invention to overcome the deficiencies of the prior art and to provide a MoS 2/h-BN composite piezoelectric catalyst product.
It is another object of the present invention to overcome the deficiencies of the prior art by providing a composite piezoelectric catalyst for the degradation of bisphenol F in water comprising,
Adding MoS 2/h-BN composite piezoelectric catalyst into bisphenol F solution;
adding peroxymonosulfate to perform piezoelectric catalytic reaction;
The mass ratio of the piezoelectric catalyst to bisphenol F is 20-100:1, and the mass ratio of the piezoelectric catalyst to the peroxymonosulfate is 25:10-60.78.
The invention has the beneficial effects that:
(1) According to the preparation method, moS 2 NFs is obtained through organic synthesis, and MoS 2/h-BN composite piezoelectric catalyst is obtained through mixing, so that the cost is low, the process is simple, and the yield is high;
(2) The catalyst prepared by the preparation method can be applied to degradation of bisphenol F in water, and can be used for carrying out high-efficiency catalytic degradation on the bisphenol F in water, and the removal rate of the bisphenol F can reach 84.2% at most after 30 min;
(3) The piezoelectric catalyst can activate persulfate under ultrasound, and has low energy consumption and low cost compared with the traditional ultraviolet light activated persulfate.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings that are needed in the description of the embodiments will be briefly described below, it being obvious that the drawings in the following description are only some embodiments of the present invention, and that other drawings may be obtained according to these drawings without inventive effort for a person skilled in the art. Wherein:
FIG. 1 is a scanning electron microscope image of MoS 2 NFs in an embodiment of the present invention;
FIG. 2 is a scanning electron microscope image of h-BN in an embodiment of the invention;
FIG. 3 is a transmission electron microscope image of h-BN in an embodiment of the invention;
FIG. 4 is a scanning electron microscope image of the MoS 2/0.20 BN composite piezoelectric catalyst of example 1 of the invention;
FIG. 5 is a graph showing the comparison of the effect of activating PMS to degrade 10mg/L bisphenol F under ultrasound for different materials prepared in the present invention;
FIG. 6 is a graph showing the comparison of the reaction kinetic constants of various materials prepared according to the present invention for degradation of 10mg/L bisphenol F by PMS activated under ultrasound.
Detailed Description
In order that the above-recited objects, features and advantages of the present invention will become more apparent, a more particular description of the invention will be rendered by reference to specific embodiments thereof which are illustrated in the appended drawings.
In the following description, numerous specific details are set forth in order to provide a thorough understanding of the present invention, but the present invention may be practiced in other ways other than those described herein, and persons skilled in the art will readily appreciate that the present invention is not limited to the specific embodiments disclosed below.
Further, reference herein to "one embodiment" or "an embodiment" means that a particular feature, structure, or characteristic can be included in at least one implementation of the invention. The appearances of the phrase "in one embodiment" in various places in the specification are not necessarily all referring to the same embodiment, nor are separate or alternative embodiments mutually exclusive of other embodiments.
Example 1
The preparation method of the MoS 2/h-BN composite piezoelectric catalyst comprises the following steps:
(1) Thiourea and sodium molybdate dihydrate are dissolved in 90mL of ultrapure water according to the mass ratio of 3:4 (0.9 g,1.2 g), the pH value is regulated to be 1 by hydrochloric acid, and the temperature is 180 ℃ and the mixture is placed in a polytetrafluoroethylene lining for organic synthesis for 24 hours;
(2) Filtering, washing to neutrality and drying the hydrothermal product to obtain MoS 2 NFs powder, wherein the pore size of the filtering membrane is 0.22 μm, and the drying temperature is 60 ℃;
(3) Dissolving urea and boric acid in a molar ratio of 1:40 (1 mol,40 mol) in 40mL of ultrapure water, heating the mixed solution at 65 ℃ to carry out organic synthesis to generate white solid, calcining at high temperature in nitrogen atmosphere, heating to 900 ℃ at 4 ℃ per min, calcining for 5 hours, and grinding to obtain h-BN powder;
(4) MoS 2 and h-BN with the mass ratio of 4:1 (80 mg,20 mg) are put into 30mL of ultrapure water to be stirred for 8 hours, and the obtained uniform suspension is centrifuged, washed and dried to obtain a product MoS 2/h-BN composite piezoelectric catalyst which is marked as MoS 2/0.20 BN;
The MoS 2/h-BN composite piezoelectric catalyst obtained by the preparation method can be applied to degradation of bisphenol F in water, and comprises the following steps:
10mg of MoS 2/h-BN composite piezoelectric catalyst is taken and placed in 50mL of bisphenol F solution (10 mg/L), the solution is firstly kept stand for 30min under the dark condition, an ultrasonic reactor (US=120W) is opened after the adsorption balance is achieved, at the moment, peroxymonosulfate is added, and the MoS 2/h-BN composite piezoelectric catalyst is uniformly mixed to obtain an activated persulfate system under the ultrasonic condition, wherein the mass ratio of MoS 2/h-BN to bisphenol F is 20:1, and the mass ratio of MoS 2/h-BN to peroxymonosulfate is 10:46.11.
Fig. 1 is a scanning electron microscope image of MoS 2 NFs, showing a nanoflower shape.
FIG. 2 is a scanning electron microscope image of h-BN, FIG. 3 is a transmission electron microscope image of h-BN, the morphology of h-BN is complete and is in a round cake shape, and FIG. 4 is a scanning electron microscope image of MoS 2/0.20 BN composite piezoelectric catalyst, and the successful embedding of h-BN into MoS 2 can be seen, which indicates that the two are successfully composited.
Example 2
The preparation method of the MoS 2/h-BN composite piezoelectric catalyst comprises the following steps:
(1) Thiourea and sodium molybdate dihydrate are dissolved in 90mL of ultrapure water according to the mass ratio of 3:4 (0.9 g,1.2 g), the pH value is regulated to be 1 by hydrochloric acid, and the temperature is 180 ℃ and the mixture is placed in a polytetrafluoroethylene lining for organic synthesis for 24 hours;
(2) Filtering, washing to neutrality and drying the hydrothermal product to obtain MoS 2 NFs powder, wherein the pore size of the filtering membrane is 0.22 μm, and the drying temperature is 60 ℃;
(3) Dissolving urea and boric acid in a molar ratio of 1:40 (1 mol,40 mol) in 40mL of ultrapure water, heating the mixed solution at 65 ℃ to carry out organic synthesis to generate white solid, calcining at high temperature in nitrogen atmosphere, heating to 900 ℃ at 4 ℃ per min, calcining for 5 hours, and grinding to obtain h-BN powder;
(4) MoS 2 and h-BN with the mass ratio of 98:2 (98 mg,2 mg) are put into 30mL of ultrapure water to be stirred for 8 hours, and the obtained uniform suspension is centrifuged, washed and dried to obtain a product MoS 2/h-BN composite piezoelectric catalyst which is marked as MoS 2/0.02 BN;
The MoS 2/h-BN composite piezoelectric catalyst obtained by the preparation method can be applied to degradation of bisphenol F in water, and comprises the following steps:
10mg of MoS 2/h-BN composite piezoelectric catalyst is taken and placed in 50mL of bisphenol F solution (10 mg/L), the solution is firstly kept stand for 30min under the dark condition, an ultrasonic reactor (US=120W) is opened after the adsorption balance is achieved, at the moment, peroxymonosulfate is added, and the MoS 2/h-BN composite piezoelectric catalyst is uniformly mixed to obtain an activated persulfate system under the ultrasonic condition, wherein the mass ratio of MoS 2/h-BN to bisphenol F is 20:1, and the mass ratio of MoS 2/h-BN to peroxymonosulfate is 10:46.11.
Example 3
The preparation method of the MoS 2/h-BN composite piezoelectric catalyst comprises the following steps:
(1) Thiourea and sodium molybdate dihydrate are dissolved in 90mL of ultrapure water according to the mass ratio of 3:4 (0.9 g,1.2 g), the pH value is regulated to be 1 by hydrochloric acid, and the temperature is 160 ℃ and the mixture is placed in a polytetrafluoroethylene lining for organic synthesis for 24 hours;
(2) Filtering, washing to neutrality and drying the hydrothermal product to obtain MoS 2 NFs powder, wherein the pore size of the filtering membrane is 0.22 μm, and the drying temperature is 60 ℃;
(3) Dissolving urea and boric acid in a molar ratio of 1:40 (1 mol,40 mol) in 40mL of ultrapure water, heating the mixed solution at 65 ℃ to carry out organic synthesis to generate white solid, calcining at high temperature in nitrogen atmosphere, heating to 900 ℃ at 4 ℃ per min, calcining for 5 hours, and grinding to obtain h-BN powder;
(4) MoS 2 and h-BN with the mass ratio of 95:5 (95 mg,5 mg) are put into 30mL of ultrapure water to be stirred for 8 hours, and the obtained uniform suspension is centrifuged, washed and dried to obtain a product MoS 2/h-BN composite piezoelectric catalyst which is marked as MoS 2/0.05 BN;
The MoS 2/h-BN composite piezoelectric catalyst obtained by the preparation method can be applied to degradation of bisphenol F in water, and comprises the following steps:
10mg of MoS 2/h-BN composite piezoelectric catalyst is taken and placed in 50mL of bisphenol F solution (10 mg/L), the solution is firstly kept stand for 30min under the dark condition, an ultrasonic reactor (US=120W) is opened after the adsorption balance is achieved, at the moment, peroxymonosulfate is added, and the MoS 2/h-BN composite piezoelectric catalyst is uniformly mixed to obtain an activated persulfate system under the ultrasonic condition, wherein the mass ratio of MoS 2/h-BN to bisphenol F is 20:1, and the mass ratio of MoS 2/h-BN to peroxymonosulfate is 10:46.11.
Example 4
The preparation method of the MoS 2/h-BN composite piezoelectric catalyst comprises the following steps:
(1) Thiourea and sodium molybdate dihydrate are dissolved in 90mL of ultrapure water according to the mass ratio of 3:4 (0.9 g,1.2 g), the pH value is regulated to be 1 by hydrochloric acid, and the temperature is 160 ℃ and the mixture is placed in a polytetrafluoroethylene lining for organic synthesis for 24 hours;
(2) Filtering, washing to neutrality and drying the hydrothermal product to obtain MoS 2 NFs powder, wherein the pore size of the filtering membrane is 0.22 μm, and the drying temperature is 60 ℃;
(3) Dissolving urea and boric acid in a molar ratio of 1:40 (1 mol,40 mol) in 40mL of ultrapure water, heating the mixed solution at 65 ℃ to carry out organic synthesis to generate white solid, calcining at high temperature in nitrogen atmosphere, heating to 900 ℃ at 4 ℃ per min, calcining for 5 hours, and grinding to obtain h-BN powder;
(4) MoS 2 and h-BN with the mass ratio of 9:1 (90 mg,10 mg) are put into 30mL of ultrapure water to be stirred for 8 hours, and the obtained uniform suspension is centrifuged, washed and dried to obtain a product MoS 2/h-BN composite piezoelectric catalyst which is marked as MoS 2/0.10 BN;
The MoS 2/h-BN composite piezoelectric catalyst obtained by the preparation method can be applied to degradation of bisphenol F in water, and comprises the following steps:
10mg of MoS 2/h-BN composite piezoelectric catalyst is taken and placed in 50mL of bisphenol F solution (10 mg/L), the solution is firstly kept stand for 30min under the dark condition, an ultrasonic reactor (US=120W) is opened after the adsorption balance is achieved, at the moment, peroxymonosulfate is added, and the MoS 2/h-BN composite piezoelectric catalyst is obtained after uniform mixing, wherein the mass ratio of MoS 2/h-BN to bisphenol F is 20:1, and the mass ratio of MoS 2/h-BN to peroxymonosulfate is 10:46.11.
Example 5
The preparation method of the MoS 2/h-BN composite piezoelectric catalyst comprises the following steps:
(1) Thiourea and sodium molybdate dihydrate are dissolved in 90mL of ultrapure water according to the mass ratio of 3:4 (0.9 g,1.2 g), the pH value is regulated to be 1 by hydrochloric acid, and the temperature is 180 ℃ and the mixture is placed in a polytetrafluoroethylene lining for organic synthesis for 24 hours;
(2) Filtering, washing to neutrality and drying the hydrothermal product to obtain MoS 2 NFs powder, wherein the pore size of the filtering membrane is 0.22 μm, and the drying temperature is 60 ℃;
(3) Dissolving urea and boric acid in a molar ratio of 1:40 (1 mol,40 mol) in 40mL of ultrapure water, heating the mixed solution at 65 ℃ to carry out organic synthesis to generate white solid, calcining at high temperature in nitrogen atmosphere, heating to 900 ℃ at 4 ℃ per min, calcining for 5 hours, and grinding to obtain h-BN powder;
(4) MoS 2 and h-BN with the mass ratio of 1:1 (50 mg ) are put into 30mL of ultrapure water to be stirred for 8 hours, and the obtained uniform suspension is centrifuged, washed and dried to obtain a product MoS 2/h-BN composite piezoelectric catalyst which is marked as MoS 2/0.50 BN;
The MoS 2/h-BN composite piezoelectric catalyst obtained by the preparation method can be applied to degradation of bisphenol F in water, and comprises the following steps:
placing MoS 2/h-BN composite piezoelectric catalyst in 50mL bisphenol F solution (10 mg/L), standing for 30min under dark condition, opening an ultrasonic reactor (US=120W) after adsorption balance is achieved, adding persulfate at the moment, and uniformly mixing to obtain the MoS 2/h-BN composite piezoelectric catalyst activated persulfate system under ultrasonic condition, wherein the mass ratio of MoS 2/h-BN to bisphenol F is 20:1, and the mass ratio of MoS 2/h-BN to persulfate is 10:46.11.
Comparative example 1
In this comparative example, moS 2 NFs was used as a piezoelectric catalyst, and other raw materials, ratios, preparation methods and detection methods were the same as those of example 1, and the bisphenol F removal rate reached 59.2% at 30 min.
FIG. 5 is a graph showing the effect of different materials prepared according to the invention on PMS activation to degrade 10mg/L bisphenol F under ultrasound, wherein MoS 2/0.02BN、MoS2/0.05BN、MoS2/0.10BN、MoS2/0.20 BN and MoS 2/0.50 BN represent the mass ratios of MoS 2 to h-BN of 98:2, 95:5, 9:1, 4:1 and 1:1, respectively;
As can be seen from the graph, the removal rates of bisphenol F after 30min of piezoelectric degradation of MoS 2、MoS2/0.02BN、MoS2/0.05BN、MoS2/0.10BN、MoS2/0.20 BN and MoS 2/0.50 BN were 59.2%, 68.7%, 63.6%, 68.0%, 84.2% and 56.8%, respectively.
It can be seen that the degradation effect of MoS 2/0.20 BN is optimal.
FIG. 6 is a graph showing the comparison of the reaction kinetic constants of the different materials prepared by the invention for degrading 10mg/L bisphenol F by activating PMS under ultrasound, wherein the reaction kinetic constants of MoS 2、MoS2/0.02BN、MoS2/0.05BN、MoS2/0.10BN、MoS2/0.20 BN and MoS 2/0.50 BN after 30min of piezoelectric degradation for removing bisphenol F are respectively 0.027, 0.039, 0.032, 0.038, 0.055 and 0.028.
It can be seen that the degradation rate of MoS 2/0.20 BN is the fastest.
By comparison of comparative example 1 with example 1, the removal rate of MoS 2 for the ultrasonic degradation of bisphenol F was lower than the range of the present invention.
In conclusion, the preparation method of the MoS 2/h-BN composite piezoelectric catalyst provided by the invention can be used for efficiently catalyzing and degrading bisphenol F in water, can be used for efficiently degrading bisphenol F which is a new pollutant difficult to degrade, and has high degradation efficiency. The piezoelectric catalyst can activate persulfate under ultrasound, and has low energy consumption and low cost compared with the traditional ultraviolet light activated persulfate.
It should be noted that the above embodiments are only for illustrating the technical solution of the present invention and not for limiting the same, and although the present invention has been described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that the technical solution of the present invention may be modified or substituted without departing from the spirit and scope of the technical solution of the present invention, and it should be covered in the scope of the present invention.
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| Limin Song et al..Performance and mechanism on hydrogen evolution of two-dimensional boron nitride under mechanical vibration.《Fuel》.2022,第331卷第1页摘要、右栏. * |
| Performance and mechanism on hydrogen evolution of two-dimensional boron nitride under mechanical vibration;Limin Song et al.;《Fuel》;20220827;第331卷;第1页摘要、右栏 * |
| Piezocatalytic enhanced peroxymonosulfate activation for bisphenol F degradation with amorphous MoSx/h-BN: The pivotal role of sulfur vacancies;Jiandong Zhu et al.;《Separation and Purification Technology》;20231206;第333卷;第1-13页 * |
| Piezoelectric activation of peroxymonosulfate by MoS2 nanoflowers for the enhanced degradation of aqueous organic pollutants;Shuhui Liu et al.;《Environ. Sci.: Nano》;20210209;第8卷;Supporting Information第3页 * |
| Shuhui Liu et al..Piezoelectric activation of peroxymonosulfate by MoS2 nanoflowers for the enhanced degradation of aqueous organic pollutants.《Environ. Sci.: Nano》.2021,第8卷第784-794页. * |
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