CN111495351B - Preparation and application method of long-life friction-sensitive graphite alkynyl piezoelectric material - Google Patents

Preparation and application method of long-life friction-sensitive graphite alkynyl piezoelectric material Download PDF

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CN111495351B
CN111495351B CN202010552676.7A CN202010552676A CN111495351B CN 111495351 B CN111495351 B CN 111495351B CN 202010552676 A CN202010552676 A CN 202010552676A CN 111495351 B CN111495351 B CN 111495351B
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powder
graphite
alkynyl
composite
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CN111495351A (en
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孟凡庆
王英龙
朱兆友
崔培哲
齐建光
李鑫
孙萌娅
孙瑞
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Qingdao University of Science and Technology
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J21/00Catalysts comprising the elements, oxides, or hydroxides of magnesium, boron, aluminium, carbon, silicon, titanium, zirconium, or hafnium
    • B01J21/18Carbon
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J23/00Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
    • B01J23/16Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
    • B01J23/18Arsenic, antimony or bismuth
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J27/00Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
    • B01J27/02Sulfur, selenium or tellurium; Compounds thereof
    • B01J27/04Sulfides
    • B01J27/047Sulfides with chromium, molybdenum, tungsten or polonium
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J27/00Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
    • B01J27/02Sulfur, selenium or tellurium; Compounds thereof
    • B01J27/04Sulfides
    • B01J27/047Sulfides with chromium, molybdenum, tungsten or polonium
    • B01J27/051Molybdenum
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J35/00Catalysts, in general, characterised by their form or physical properties
    • B01J35/30
    • B01J35/33
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00Treatment of water, waste water, or sewage
    • C02F1/46Treatment of water, waste water, or sewage by electrochemical methods
    • YGENERAL 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
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02WCLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
    • Y02W10/00Technologies for wastewater treatment
    • Y02W10/30Wastewater or sewage treatment systems using renewable energies
    • Y02W10/37Wastewater or sewage treatment systems using renewable energies using solar energy

Abstract

The invention relates to a preparation and application method of a long-life friction-sensitive graphite alkynyl piezoelectric material, in particular to application of the material in the fields of interface catalytic reaction and water purification, and belongs to the technical field of preparation and application of novel functional materials. The novel graphite alkyne material with high piezoelectric response is mainly used as a structure regulating agent, and the piezoelectric material is induced to grow in an oriented manner at the edge of the structure regulating agent in situ to form an active defect, so that the separation of electrons and holes is accelerated, and the piezoelectric catalytic performance of the composite material is obviously improved. Meanwhile, the material is synthesized by a mechanochemical method, the size and the layer thickness of the material are regulated and controlled, the friction sensitivity of the composite piezoelectric catalytic material is improved, the mechanical stability of the composite piezoelectric catalytic material is enhanced, and the dual purposes of high piezoelectric activity and long service life are achieved. Under the condition that the in-situ ball milling method provides mechanical force, organic pollutants in water can be efficiently and sustainably oxidized and degraded through piezoelectric catalytic reaction.

Description

Preparation and application method of long-life friction-sensitive graphite alkynyl piezoelectric material
Technical Field
The invention provides a preparation method and an application method of a long-life friction-sensitive graphite alkynyl piezoelectric material, relates to a preparation method of a long-life friction-sensitive graphite alkynyl piezoelectric material, particularly relates to application of the long-life friction-sensitive graphite alkynyl piezoelectric material in the fields of interface catalytic reaction and water purification, and belongs to the technical field of preparation and application of functional materials.
Background
The piezoelectric catalytic material is one of the excellent materials emerging in recent years, but at present, most of the materials are mainly applied to the energy field, and the application in the environmental field is yet to be further expanded and researched. Recently, CN109331882A discloses an organic piezoelectric-photocatalytic composite helical fiber, which can continuously generate a self-repairing piezoelectric potential under the action of water flow, effectively promote the separation of a photocatalyst photo-generated electron-hole pair, and greatly improve the efficiency of photocatalytic degradation of pollutants. CN108772063A discloses an Ag 2 O/Bi 4 Ti 3 O 12 The piezoelectric photocatalyst and the synthesis method thereof obviously improve the capacity of the catalytic material for degrading organic matters under the condition of ultrasonic-assisted illumination catalysis. CN109529807A obtains composite catalyst material through normal position photogeneration titanium oxide nanoparticle parcel lead zirconate titanate piezoelectricity powder, when through fluid mechanical energy induction, can produce the piezoelectric field, it is obvious to show promotion photocatalytic reaction effect. Salifen and the like of the university of the theory of the great continuity of technology invents a photocatalytic self-bias pollution control system (CN 110165243A) constructed by piezoelectric materials, pollutants can be degraded under the illumination condition through the action of photocatalysis and piezoelectric effect, electric energy output can be realized through the action of piezoelectric effect under the non-illumination condition, and the sewage treatment effect can be improved by coupling an advanced oxidation technology. Therefore, most of the current environmental applications of piezoelectric catalysis need to be coupled with other purification technologies, and the environmental applications of single piezoelectric catalysis are relatively few.
The existing water treatment process equipment in China is relatively simple and is not easy to improve, and most of the water treatment process equipment is carried out in a dark environment, so how to realize a dark ringThe degradation of pollutants in water by coupling with the original process is difficult to study in the environment. Liu Zhiyong et al of Nanchang aviation university is marked by K 2 CO 3 、Na 2 CO 3 、Nb 2 O 5 、Li 2 CO 3 The potassium-sodium niobate based piezoelectric ceramics are obtained by high-temperature treatment and the high-efficiency degradation of the dye wastewater is realized by using ultrasonic to initiate a piezoelectric catalytic reaction (CN 110092440A). The Ouchun et al of Zhongshan university disclose the application of piezoelectric material barium titanate in ultrasonic activation persulfate treatment wastewater (CN 109607739A), can generate various free radicals in a piezoelectric activation persulfate system, has a removal rate of ibuprofen and other drug wastewater of more than 98 percent, has no selectivity, and can be widely applied to various wastewater treatment systems.
The catalytic activity and mechanical stability of the piezoelectric catalytic material are major factors that restrict its engineering applications. How to improve the piezoelectric catalytic activity of the material is also a hot spot of current research. Toyufei et al (CN 108411406B) of the university of SiAnli's industries compounds a piezoelectric ceramic precursor with a spinnable polymer through an electrostatic spinning technology, and reduces the impedance between composite materials through high-temperature calcination, thereby improving the piezoelectric performance of the materials. In addition, they also found that a piezoelectric material having a multilevel structure can be constructed by a multilevel hydrothermal reaction, and that the multilevel structure is advantageous to electron hole separation and improves the piezoelectric catalytic activity by a piezoelectric performance test (CN 110540430A). However, the active sites of the piezoelectric catalytic material are gradually destroyed under the action of mechanical force, and the activity is gradually reduced, and researches show that the stability of the material can be improved by fixing the piezoelectric catalytic material on PVDF, but after 10 cycles, the catalytic activity is only maintained by 80%.
Therefore, aiming at the defects of the prior art, the invention aims to provide a preparation method and an application method of a friction-sensitive graphite alkynyl piezoelectric material with long service life. The graphite alkyne material is introduced as a structure regulating agent and an electron transmission rapid channel, and the generation of the piezoelectric material is induced in situ to obtain the graphite alkyne composite piezoelectric catalytic material. In the process of synthesizing the material, a ball milling method is utilized to initiate a mechanochemical reaction for synthesis, the mesoscopic size of the material is regulated and controlled, the friction sensitivity of the material is enhanced, meanwhile, ball milling is applied to provide mechanical force, a piezoelectric catalytic reaction is initiated in situ, the self-repairing of active sites is realized, the stability of the material is obviously improved, and the engineering application field of the material is expanded.
Disclosure of Invention
The invention aims to provide a preparation and application method of a long-life friction-sensitive graphite alkynyl piezoelectric material aiming at the defects of the existing piezoelectric catalytic material and application. The mesoscopic size and the mechanical flexibility of the composite material are regulated and controlled in the ball milling process, the piezoelectric catalytic reaction is initiated in situ by a ball milling method, the self-repairing of active sites is realized, the catalytic activity and the service life are greatly improved, and the applicability of the composite material is improved.
In order to achieve the purpose, the invention adopts the following technical scheme:
the invention relates to a preparation and application method of a long-life friction sensitive graphite alkynyl piezoelectric material, which adopts the technical scheme and comprises the following steps:
1) Taking hexahalobenzene and calcium carbide as raw materials, and mixing the raw materials according to the weight ratio of the hexahalobenzene: the molar ratio of calcium carbide is 1: (5-10) accurately weighing hexahalobenzene and calcium carbide, and placing the hexahalobenzene and calcium carbide in a ball-milling reaction kettle of vacuum polytetrafluoroethylene
2) According to the following materials: weighing zirconia balls according to the mass ratio of 1-500, placing the zirconia balls in a reaction kettle, vacuumizing, and performing ball milling for 6-20h under the condition that the rotating speed is 500-1000 r/min.
3) Collecting the powder after ball milling, washing with deionized water and ethanol for 2 times in sequence, filtering to obtain a filter cake, and drying at 50-100 ℃ for 2-10h to obtain the thin-layer graphite alkyne powder.
4) Weighing 0.1-1g of graphite alkyne powder, weighing a piezoelectric material precursor according to the mass ratio of the graphite alkyne to the piezoelectric catalysis fabric precursor of 1 (50-1000), adding the piezoelectric material precursor into the graphite alkyne powder, and uniformly mixing.
5) Adding the mixed powder obtained in the step 4) into a polytetrafluoroethylene ball milling kettle, and mixing the materials: adding the zirconia balls according to the mass ratio of 1-500, and ball-milling for 3-5h at the rotating speed of 500-1500 r/min to obtain the graphite alkynyl composite piezoelectric catalytic material precursor powder.
6) The precursor powder was placed in a tube furnace at N 2 Activating at 300-500 deg.C for 2-5h in atmosphere, and naturally cooling to room temperature.
7) And collecting the cooled powder, washing the powder to be neutral by using deionized water, and drying the powder at the temperature of 120 ℃ for 5-24 hours to obtain the graphite alkynyl composite piezoelectric catalyst product.
8) Weighing graphite alkynyl composite piezoelectric catalyst powder with the mass of 0.01-0.5g, placing the graphite alkynyl composite piezoelectric catalyst powder in a piezoelectric catalysis system, and testing the piezoelectric catalysis performance, wherein the specific operation is as follows: weighing graphite alkynyl composite piezoelectric catalyst powder with the mass of 0.01-0.5g, adding the graphite alkynyl composite piezoelectric catalyst powder into a pollutant water sample with the volume of 20-80mL, introducing mechanical force to excite piezoelectric catalytic reaction for 0.01-2h, and centrifuging to take supernatant liquid to determine the concentration of a target pollutant.
9) Washing the catalyst powder obtained by centrifugation with deionized water for 3-5 times, drying at 120 ℃ for 5-24h, adding into a piezoelectric catalytic reaction system, repeating the piezoelectric catalytic reaction process of the step 6-7, and determining the repeatability of the catalyst sample.
The hexahalobenzene can be one or two or more mixed iron salts of hexachlorobenzene, hexabromobenzene and hexaiodobenzene.
The piezoelectric material precursor can be used for preparing MoS 2 、WS 2 、MoSe 2 、WSe 2 、ZnO、BiTiO 3 、 CdS、BaTiO 3 、Pb(Zr 0.52 Ti 0.48 )O 3 And precursors corresponding to the piezoelectric fibers and the piezoelectric ceramics.
The mechanical force initiation method applied to the piezoelectric catalytic reaction system can provide a mechanical force for one or more of a ball milling method, an ultrasonic method, a stirring method, an air flow method, a water flow method and the like.
The graphdiyne is a new two-dimensional carbon material in recent years, has the advantages of fast electron transmission, multi-level pore channels, multiple ion channels and the like, is an excellent structure regulating agent, has obvious piezoelectric response, and has less research on the piezoelectric property. Compared with other technologies, the invention has the advantages that: (1) The graphite alkynyl composite piezoelectric catalyst provided by the invention is simple in operation process, low in cost and easy for batch production. (2) The synthesized graphite alkynyl piezoelectric catalytic material has obvious friction response, and can realize in-situ piezoelectric catalysis and active site repair by an in-situ ball milling method. (3) The piezoelectric catalytic material prepared by the invention has high service life and high catalytic activity, and can meet the requirements of environmental engineering application.
Drawings
FIG. 1 shows the preparation of graphite alkynyl WS 2 Transmission electron micrographs of the composite.
FIG. 2 shows different mechanical force activation modes for graphene WS 2 The effect of the piezoelectric performance of the composite material.
FIG. 3 shows that the graphite alkynyl MoS prepared by the invention 2 The repeatability experiment result of the material piezoelectric catalysis degradation phenol.
FIG. 4 shows that the graphite alkynyl Bi prepared by the invention 4 Ti 3 O 12 The material is a diagram of the effect of degrading rhodamine through rapid piezoelectric catalysis.
Detailed Description
The following further describes a specific embodiment of the present invention with reference to the drawings and technical solutions.
Example 1
1) Weighing hexabromobenzene and calcium carbide according to the molar ratio of 1.
2) And taking out a powder sample subjected to ball milling, sequentially washing the powder sample with deionized water and ethanol for 2 times, and drying the powder sample at 90 ℃ for 10 hours to obtain the thin-layer graphite alkyne powder.
3) According to the molar ratio of 1:10: tungsten dioxide, thiourea and sodium hydroxide were weighed in a mass ratio of 0.1 and placed in a polytetrafluoroethylene ball-milling reaction vessel of 100 mL.
4) Weighing 0.2g of graphite alkyne powder obtained in the step 2), adding the graphite alkyne powder into the reaction kettle in the step 3), and performing ball milling for 3 hours at the speed of 800 r/min to obtain graphite alkyne composite piezoelectric catalytic material precursor powder.
5) Putting the precursor powder obtained in the step 4) into a tube furnace, and performing N reaction on the precursor powder 2 Activating at 450 deg.C for 2h under atmosphere, and naturally cooling to room temperature.
6) And collecting the cooled powder, washing the powder to be neutral by using deionized water, and drying the powder at 120 ℃ for 10 hours to obtain the graphite alkynyl composite piezoelectric catalyst product, wherein the transmission electron microscope characterization result of the product is shown in the attached figure 1.
7) Respectively measuring 3 parts of 50mL water samples containing 100mg/L tetracycline, wherein the serial numbers are 1, 2 and 3, respectively adding 0.05g of graphite alkynyl composite piezoelectric catalyst powder into the three groups of samples, placing the No. 1 system in a polytetrafluoroethylene ball-milling reaction kettle, ball-milling for 60min under the condition that the rotating speed is 1000 revolutions per minute, and centrifuging to take supernatant to determine the concentration of the tetracycline; placing the system No. 2 in a beaker, performing ultrasonic treatment at 200HZ for 60min, centrifuging, and taking supernatant to determine the concentration of tetracycline; the No. 3 system is placed in a beaker, and is magnetically stirred for 60min under the condition of 1000 revolutions per minute, the supernatant is centrifuged to measure the concentration of the tetracycline, and the removal effect of three groups of samples is compared with that of the attached figure 2.
8) The transmission electron microscope image shown in the attached figure 1 can prove that the graphite alkynyl WS is successfully prepared 2 Composite material having a lamellar structure, WS 2 Is grown along the epitaxial orientation of the graphdiyne segments, and the number of layers is about 3-10. The graphyne alkynyl WS can be known from the attached figure 2 2 The piezoelectric catalytic activity is different under different activation modes, and the piezoelectric catalytic activity is most sensitive under the action of ball milling friction force, so that more than 98% of tetracycline can be removed within 60 min.
Example 2
1) Weighing hexahalobenzene and calcium carbide according to a molar ratio of 1.
2) And taking out the ball-milled powder sample, washing the ball-milled powder sample with deionized water and ethanol for 2 times in sequence, and drying the ball-milled powder sample at 80 ℃ for 6 hours to obtain the thin-layer graphite alkyne powder.
3) According to the molar ratio of 1:8: ammonium molybdate, thiourea and sodium hydroxide are weighed according to the mass ratio of 0.5 and placed in a polytetrafluoroethylene ball-milling reaction kettle of 100 mL.
4) Weighing 0.1g of graphite alkyne powder obtained in the step 2), adding the graphite alkyne powder into the reaction kettle in the step 3), and performing ball milling for 5 hours at the speed of 800 r/min to obtain graphite alkyne composite piezoelectric catalytic material precursor powder.
5) Putting the precursor powder obtained in the step 4) into a tube furnace, and performing N reaction on the precursor powder 2 Activating at 500 deg.C for 4h under atmosphere, and naturally cooling to room temperature.
6) And collecting the cooled powder, washing the powder to be neutral by using deionized water, and drying the powder at 120 ℃ for 8 hours to obtain the graphite alkynyl composite piezoelectric catalyst product.
7) Weighing 50mL of water sample containing 100mg/L of phenol, adding 0.05g of graphite alkynyl composite piezoelectric catalyst powder, placing the mixture into a polytetrafluoroethylene ball-milling reaction kettle, carrying out ball milling for 60min under the condition that the rotating speed is 1000 revolutions/min, and centrifuging to take supernatant liquid to determine the concentration of the phenol.
8) Washing the catalyst powder obtained by centrifugation with deionized water for 3 times, drying at 120 ℃ for 5h, and repeating the reaction process of the step 7) for degrading phenol by piezoelectric catalysis for 50 times to obtain the repeatability of the catalyst sample under 50 cycles (shown in figure 3).
9) From FIG. 3, it can be seen that the graphite alkynyl MoS has 50 cycles 2 The removal rate of phenol is maintained above 95%, which shows that the method has high repeatability and long service life.
Example 3:
1) Weighing hexahalobenzene and calcium carbide according to a molar ratio of 1.
2) Removing the ball-milled sample, washing with deionized water and ethanol for 2 times in sequence, and drying to obtain the thin-layer graphite alkyne powder.
3) According to a molar ratio of 4:3 molar ratio of Bi (OH) 3 And Ti (OH) 4 And (3) putting the powder into a 100mL polytetrafluoroethylene ball-milling reaction kettle.
4) Weighing 0.5g of graphite alkyne powder obtained in the step 2), adding the graphite alkyne powder into the reaction kettle in the step 3), and performing ball milling for 6 hours under the condition of 1000 revolutions per minute to obtain graphite alkyne composite piezoelectric catalytic material precursor powder.
5) Putting the precursor powder obtained in the step 4) into a tube furnace, and performing reaction in a reactor under N 2 Activating at 250 deg.C for 4h under atmosphere, and naturally cooling to room temperature.
6) Collecting the cooled powder, washing the powder to be neutral by deionized water, and drying the powder for 10 hours at 120 ℃ to obtain the graphite alkynyl Bi 4 Ti 3 O 12 A composite piezoelectric catalyst product.
7) Weighing 50mL of water sample containing 100mg/L of rhodamine B, adding 0.05g of graphite alkynyl composite piezoelectric catalyst powder, placing the water sample in a polytetrafluoroethylene ball-milling reaction kettle, carrying out ball milling for 5min under the condition that the rotating speed is 1000 r/min, centrifuging, taking supernatant to measure the concentration of the rhodamine B, and obtaining the removing effect shown in the attached figure 4.
8) As can be seen from FIG. 4, the prepared graphite alkynyl Bi 4 Ti 3 O 12 The material can rapidly degrade rhodamine B under the action of friction force, and when the reaction time is 2min, the removal rate of the rhodamine B is close to 100%.

Claims (3)

1. A preparation method of a long-life friction sensitive graphite alkynyl piezoelectric material is characterized by comprising the following specific steps:
1) Taking hexahalobenzene and calcium carbide as raw materials, and mixing the raw materials according to the weight ratio of the hexahalobenzene: the molar ratio of calcium carbide is 1: (5-10) accurately weighing the hexahalobenzene and the calcium carbide, and placing the hexahalobenzene and the calcium carbide in a ball-milling reaction kettle of vacuum polytetrafluoroethylene;
2) According to the materials: weighing zirconia balls according to the mass ratio of 1-500, placing the zirconia balls in a reaction kettle, vacuumizing, and performing ball milling for 6-20h at the rotating speed of 500-1000 r/min;
3) Collecting the ball-milled powder, washing with deionized water and ethanol for 2 times in sequence, filtering to obtain a filter cake, and drying at 50-100 ℃ for 2-10h to obtain thin-layer graphite alkyne powder;
4) Weighing 0.1-1g of graphite alkyne powder, weighing a piezoelectric material precursor according to the mass ratio of the graphite alkyne to the piezoelectric catalytic material precursor of 1 (50-1000), adding the piezoelectric material precursor into the graphite alkyne powder, and uniformly mixing; precursor of piezoelectric material for preparing MoS 2 、WS 2 、MoSe 2 、WSe 2 、ZnO、BiTiO 3 、CdS、BaTiO 3 、Pb(Zr 0.52 Ti 0.48 )O 3 The corresponding reactant;
5) Adding the mixed powder obtained in the step 4) into a polytetrafluoroethylene ball milling kettle, and mixing the materials: adding zirconia balls according to the mass ratio of 1-100-500, and ball-milling for 3-5h at the rotation speed of 500-1500 r/min to obtain graphite alkynyl composite piezoelectric catalytic material precursor powder;
6) Putting the precursor powder of the graphite alkynyl composite piezoelectric material into a tube furnace, and putting the precursor powder into a furnace at N 2 Activating at 300-500 deg.C for 2-5h under atmosphere, and naturally cooling to room temperature;
7) Collecting the cooled powder, washing the powder to be neutral by using deionized water, and drying the powder at 120 ℃ for 5 to 24 hours to obtain a graphite alkynyl composite piezoelectric catalyst product;
8) Weighing graphite alkynyl composite piezoelectric catalyst powder with the mass of 0.01-0.5g, placing the graphite alkynyl composite piezoelectric catalyst powder in a piezoelectric catalytic system, and testing the piezoelectric catalytic performance of the graphite alkynyl composite piezoelectric catalyst powder, wherein the specific operation is as follows: weighing graphite alkynyl composite piezoelectric catalyst powder with the mass of 0.01-0.5g, adding the graphite alkynyl composite piezoelectric catalyst powder into a pollutant water sample with the volume of 20-80mL, introducing mechanical force to excite piezoelectric catalytic reaction for 0.01-2h, and centrifuging to take supernatant liquid to determine the concentration of a target pollutant;
9) Washing the catalyst powder obtained by centrifugation with deionized water for 3-5 times, drying at 120 ℃ for 5-24h, adding into a piezoelectric catalytic reaction system, repeating the piezoelectric catalytic reaction process of the step 8), and determining the repeatability of the catalyst sample.
2. The method as claimed in claim 1, wherein the hexahalobenzene in step 1) is one or a mixture of two or more of hexachlorobenzene, hexabromobenzene and hexaiodobenzene.
3. The method as claimed in claim 1, wherein the mechanical force inducing method applied by the piezo-electric catalytic reaction system in step 8) is a method for providing mechanical force for one or more of ball milling method, ultrasonic method, stirring method, gas flow method and water flow method.
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