CN111939937A - Zinc stannate/indium sulfide barbed nanoflower piezoelectric/photocatalyst and preparation method thereof - Google Patents
Zinc stannate/indium sulfide barbed nanoflower piezoelectric/photocatalyst and preparation method thereof Download PDFInfo
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- 239000002057 nanoflower Substances 0.000 title claims abstract description 62
- 239000011941 photocatalyst Substances 0.000 title claims abstract description 18
- BNEMLSQAJOPTGK-UHFFFAOYSA-N zinc;dioxido(oxo)tin Chemical compound [Zn+2].[O-][Sn]([O-])=O BNEMLSQAJOPTGK-UHFFFAOYSA-N 0.000 title claims abstract description 17
- UCKMPCXJQFINFW-UHFFFAOYSA-N Sulphide Chemical compound [S-2] UCKMPCXJQFINFW-UHFFFAOYSA-N 0.000 title claims abstract description 14
- 229910052738 indium Inorganic materials 0.000 title claims abstract description 14
- APFVFJFRJDLVQX-UHFFFAOYSA-N indium atom Chemical compound [In] APFVFJFRJDLVQX-UHFFFAOYSA-N 0.000 title claims abstract description 14
- 238000002360 preparation method Methods 0.000 title abstract description 15
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims abstract description 99
- PSCMQHVBLHHWTO-UHFFFAOYSA-K indium(iii) chloride Chemical compound Cl[In](Cl)Cl PSCMQHVBLHHWTO-UHFFFAOYSA-K 0.000 claims abstract description 52
- 229910007694 ZnSnO3 Inorganic materials 0.000 claims abstract description 44
- YUKQRDCYNOVPGJ-UHFFFAOYSA-N thioacetamide Chemical compound CC(N)=S YUKQRDCYNOVPGJ-UHFFFAOYSA-N 0.000 claims abstract description 26
- DLFVBJFMPXGRIB-UHFFFAOYSA-N thioacetamide Natural products CC(N)=O DLFVBJFMPXGRIB-UHFFFAOYSA-N 0.000 claims abstract description 26
- 238000003756 stirring Methods 0.000 claims abstract description 24
- 239000000243 solution Substances 0.000 claims abstract description 20
- 238000006243 chemical reaction Methods 0.000 claims abstract description 19
- 238000001035 drying Methods 0.000 claims abstract description 19
- 238000004140 cleaning Methods 0.000 claims abstract description 17
- 239000011259 mixed solution Substances 0.000 claims abstract description 17
- 238000000227 grinding Methods 0.000 claims abstract description 11
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 11
- 239000007788 liquid Substances 0.000 claims abstract description 11
- 238000000034 method Methods 0.000 claims abstract description 9
- 238000002156 mixing Methods 0.000 claims abstract description 9
- ZOIORXHNWRGPMV-UHFFFAOYSA-N acetic acid;zinc Chemical compound [Zn].CC(O)=O.CC(O)=O ZOIORXHNWRGPMV-UHFFFAOYSA-N 0.000 claims description 18
- TVQLLNFANZSCGY-UHFFFAOYSA-N disodium;dioxido(oxo)tin Chemical compound [Na+].[Na+].[O-][Sn]([O-])=O TVQLLNFANZSCGY-UHFFFAOYSA-N 0.000 claims description 18
- 229940079864 sodium stannate Drugs 0.000 claims description 18
- 239000004246 zinc acetate Substances 0.000 claims description 18
- 229910007717 ZnSnO Inorganic materials 0.000 claims description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 9
- 239000004570 mortar (masonry) Substances 0.000 claims description 8
- 238000005303 weighing Methods 0.000 claims description 8
- 238000009210 therapy by ultrasound Methods 0.000 claims description 4
- 239000002105 nanoparticle Substances 0.000 claims description 3
- 230000035484 reaction time Effects 0.000 claims description 2
- 238000013033 photocatalytic degradation reaction Methods 0.000 abstract description 2
- 239000003054 catalyst Substances 0.000 abstract 1
- 239000000203 mixture Substances 0.000 description 7
- 230000001699 photocatalysis Effects 0.000 description 7
- 239000002131 composite material Substances 0.000 description 6
- 239000008367 deionised water Substances 0.000 description 6
- 229910021641 deionized water Inorganic materials 0.000 description 6
- 230000015556 catabolic process Effects 0.000 description 3
- 238000006731 degradation reaction Methods 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 230000007613 environmental effect Effects 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 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 3
- 229940012189 methyl orange Drugs 0.000 description 3
- GKCNVZWZCYIBPR-UHFFFAOYSA-N sulfanylideneindium Chemical compound [In]=S GKCNVZWZCYIBPR-UHFFFAOYSA-N 0.000 description 3
- 230000003197 catalytic effect Effects 0.000 description 2
- 239000000975 dye Substances 0.000 description 2
- 239000002086 nanomaterial Substances 0.000 description 2
- 238000007146 photocatalysis Methods 0.000 description 2
- 238000002604 ultrasonography Methods 0.000 description 2
- 238000002441 X-ray diffraction Methods 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- 230000005284 excitation Effects 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 125000004435 hydrogen atom Chemical class [H]* 0.000 description 1
- 239000001048 orange dye Substances 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- 238000005215 recombination Methods 0.000 description 1
- 230000006798 recombination Effects 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
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- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/02—Sulfur, selenium or tellurium; Compounds thereof
- B01J27/04—Sulfides
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Abstract
The invention discloses a zinc stannate/indium sulfide barbed nanoflower piezoelectric/photocatalyst and a preparation method thereof, wherein the catalyst comprises ZnSNO3/In2S 3. The method specifically comprises the following steps: (1) preparing ZnSnO3 nanoflower by a hydrothermal method; (2) uniformly grinding the nanoflower obtained in the step (1); (3) dispersing the nanoflower obtained in the step (2) in an ethylene glycol solution, and putting the solution into an ultrasonic groove to uniformly disperse the nanoflower in the ethylene glycol; (4) adding indium trichloride and thioacetamide into ethylene glycol to completely dissolve the indium trichloride and the thioacetamide to prepare an indium trichloride/thioacetamide mixed solution; (5) mixing the liquid in the step (3) and the liquid in the step (4), and uniformly stirring; (6) and (3) putting the liquid in the step (5) into an ultrasonic groove, carrying out ultrasonic reaction, centrifuging, cleaning and drying the obtained product to obtain the zinc stannate/indium sulfide barbed nanoflower. The novel barbed nanoflower piezoelectric/photocatalyst can obviously enhance the photocatalytic degradation performance under the ultrasonic action.
Description
Technical Field
The invention relates to the technical field of preparation of photocatalysts, in particular to a zinc stannate/indium sulfide barbed nanoflower piezoelectric/photocatalyst and a preparation method thereof.
Background
Energy crisis and environmental problems are two major problems facing humans at present. The use of sustainable, renewable clean energy to replace and produce non-renewable energy is very important to alleviate energy and environmental problems. The photocatalysis technology can utilize solar energy to degrade pollutants in the environment and decompose water to produce hydrogen, oxygen and the like, and the solar energy is clean, environment-friendly and renewable energy and is ubiquitous and inexhaustible, so the photocatalysis technology has a very application prospect.
Because the content of visible light in sunlight is nearly half, the visible light is utilized to complete the catalysis process, and the utilization rate of the sunlight can be improved. Because the photocatalytic material has higher electron-hole recombination rate, the photocatalytic performance is often limited, and in order to solve the problem, the invention proposes to adopt a piezoelectric material to enhance the photocatalytic performance.
Indium sulfide is a narrow bandgap semiconductor whose excitation wavelength is well in the visible range. The zinc stannate is a piezoelectric material, and has the advantages of simple preparation, environmental protection, low price and the like. The zinc stannate and the indium sulfide are compounded together, and the separation of photo-generated electron-hole pairs of the indium sulfide can be improved by utilizing the piezoelectric potential generated by the piezoelectric effect of the zinc stannate, so that the photocatalytic performance is improved.
Disclosure of Invention
The invention provides a zinc stannate/indium sulfide piezoelectric/photocatalyst with an thorn nanoflower structure and a preparation method thereof, aiming at the defects of the prior art.
The component of the nanostructured flower piezoelectric/photocatalyst with thorns is ZnSnO3/In2S3Comprising ZnSnO3Nanoflower, and In coated on surface thereof2S3And (4) nano needles.
A preparation method of zinc stannate/indium sulfide barbed nanoflower piezoelectric/photocatalyst is characterized by comprising the following steps:
(1) according to a molar ratio of 1: 1 weighing zinc acetate and sodium stannate, and respectively dissolving in water;
(2) dropwise adding the prepared sodium stannate solution in the step (1) into the zinc acetate solution, and stirring continuously;
(3) transferring the mixed solution obtained in the step (2) to a reaction kettle, and placing the reaction kettle in a drying box for hydrothermal reaction to obtain ZnSnO3A nanoflower;
(4) ZnSnO obtained in (2)3Cleaning the nanoflower, drying and fully grinding by using a mortar;
(5) grinding ZnSnO3Dispersing the nanoflower in ethylene glycol, and putting the nanoflower into an ultrasonic groove for ultrasonic treatment to uniformly disperse the nanoflower in the ethylene glycol;
(6) adding indium trichloride and thioacetamide into ethylene glycol, and stirring to completely dissolve the indium trichloride and the thioacetamide to prepare an indium trichloride/thioacetamide mixed solution;
(7) mixing the liquids of (5) and (6), stirring thoroughly, placing in an ultrasonic tank for ultrasonic treatment for 5min-1h, centrifuging, cleaning, and drying to obtain ZnSnO3/In2S3The flower is a flower with thorns.
Preferably, the concentration of the zinc acetate and sodium stannate solution in the step (1) is 0.1-80 mmol/L;
preferably, the temperature of the hydrothermal reaction in the step (3) is 150-.
Preferably, ZnSnO in step (5)3The addition amount of the nanoflower is 0.001-1mol per liter of ethylene glycol.
Preferably, the amount of indium trichloride added in step (6) is 0.01 to 1mol per one liter of ethylene glycol, and the amount of thioacetamide added is 0.02 to 2mol per one liter of ethylene glycol.
Preferably, the power of the ultrasonic reaction in the step (7) is 50-300W, and the frequency is 20kHz-200 kHz.
The invention has the following effects: this is a ZnSnO3/In2S3The spiny nanoflower piezoelectric/photocatalyst utilizes the piezoelectric potential generated by the piezoelectric effect of ZnSnO3 to enhance the photocatalytic performance of In2S 3; the preparation process is simple and finishedThe cost is low, the efficiency is high, and the performance is good.
Drawings
FIG. 1 shows ZnSnO in the invention3XRD pattern of nanoflower;
FIG. 2 shows ZnSnO in the invention3/In2S3SEM picture of the nano flower with thorns;
FIG. 3 shows ZnSnO in the invention3/In2S3The catalytic degradation efficiency of the nano flower with the thorns on methyl orange organic dye is realized under the conditions of ultrasound and stirring.
Detailed Description
Example 1
ZnSnO3/In2S3The preparation method of the barbed nanometer flower comprises the following steps:
(1) weighing 1.1g of zinc acetate and 1.33g of sodium stannate, and respectively dissolving in 50ml of deionized water;
(2) dropwise adding the prepared sodium stannate solution in the step (1) into the zinc acetate solution, and stirring continuously;
(3) transferring the mixed solution obtained in the step (2) to a reaction kettle, and carrying out hydrothermal reaction at 260 ℃ for 12 hours;
(4) centrifuging, cleaning and drying the product, and grinding the product by using a mortar to obtain ZnSnO3A nanoflower;
(5) dispersing 10mg of ground ZnSnO3 nanoflower in 10ml of ethylene glycol, and putting the ZnSnO3 nanoflower into an ultrasonic groove to uniformly disperse the nanoflower in the ethylene glycol;
(6) adding 1.106g of indium trichloride and 0.752g of thioacetamide into 40ml of ethylene glycol, and stirring to completely dissolve the indium trichloride and the thioacetamide to prepare an indium trichloride/thioacetamide mixed solution;
(7) mixing the liquids of (5) and (6), stirring thoroughly, placing in an ultrasonic tank, performing ultrasonic reaction for 1h with ultrasonic power of 200W and frequency of 20kH, centrifuging, cleaning, and drying to obtain ZnSnO3/In2S3A composite material.
In the embodiment, the concentrations of indium trichloride and thioacetamide are higher, and the adding amount of ZnSnO3 nanoflower is less, so that a large amount of In2S3 nanoparticles and only a small amount of ZnSnO nanoparticles exist In the obtained product3/In2S3Composite material and needle-like structure is not obvious.
Example 2
ZnSnO3/In2S3The preparation method of the barbed nanometer flower comprises the following steps:
(1) weighing 1.1g of zinc acetate and 1.33g of sodium stannate, and respectively dissolving in 50ml of deionized water;
(2) dropwise adding the prepared sodium stannate solution in the step (1) into the zinc acetate solution, and stirring continuously;
(3) transferring the mixed solution obtained in the step (2) to a reaction kettle, and carrying out hydrothermal reaction at 260 ℃ for 12 hours;
(4) centrifuging, cleaning and drying the product, and grinding the product by using a mortar to obtain ZnSnO3A nanoflower;
(5) dispersing 100mg of ground ZnSnO3 nanoflower in 10ml of ethylene glycol, and putting the mixture into an ultrasonic groove to uniformly disperse the nanoflower in the ethylene glycol;
(6) 0.553g of indium trichloride and 0.376g of thioacetamide are added into 40ml of ethylene glycol, and the mixture is stirred to be completely dissolved to prepare an indium trichloride/thioacetamide mixed solution;
(7) mixing the liquids of (5) and (6), stirring thoroughly, placing in an ultrasonic tank, performing ultrasonic reaction for 15min with ultrasonic power of 300W and frequency of 80kHz, centrifuging, cleaning, and drying to obtain ZnSnO3/In2S3Nano flower with thorns;
the product obtained in this example can be seen as a distinct barbed nanoflower structure, and fig. 1 is ZnSnO in this example3XRD of nanoflower, it can be seen that it has a pure phase structure, and FIG. 2 is ZnSnO in this example3/In2S3SEM picture of the spiny nanoflower, ZnSnO can be seen3Spiny In2S3 grows on the surface of the nanoflower. FIG. 3 is ZnSnO3/In2S3The photocatalytic degradation efficiency of the methyl orange dye of the spiny nanoflower can be seen as ZnSnO3/In2S3The degradation performance of the nano flower with the thorns under the ultrasonic condition is obviously superior to that of the nano flower with the thorns under the stirring condition.
Example 3
ZnSnO3/In2S3The preparation method of the barbed nanometer flower comprises the following steps:
(1) weighing 5.49g of zinc acetate and 3.99g of sodium stannate, and respectively dissolving in 50ml of deionized water;
(2) dropwise adding the prepared sodium stannate solution in the step (1) into the zinc acetate solution, and stirring continuously;
(3) transferring the mixed solution obtained in the step (2) to a reaction kettle, and carrying out hydrothermal reaction at 300 ℃ for 1 h;
(4) centrifuging, cleaning and drying the product, and grinding the product by using a mortar to obtain ZnSnO3A nanoflower;
(5) dispersing 20mg of ground ZnSnO3 nanoflower in 10ml of ethylene glycol, and putting the ZnSnO3 nanoflower into an ultrasonic groove to uniformly disperse the nanoflower in the ethylene glycol;
(6) 3.318g of indium trichloride and 2.8g of thioacetamide are added into 40ml of ethylene glycol, and the mixture is stirred to be completely dissolved to prepare an indium trichloride/thioacetamide mixed solution;
(7) mixing the liquids of (5) and (6), stirring thoroughly, placing in an ultrasonic tank, performing ultrasonic reaction for 1h with ultrasonic power of 200W and frequency of 200kHz, centrifuging, cleaning, and drying to obtain ZnSnO3/In2S3A composite material.
Example 4
ZnSnO3/In2S3The preparation method of the barbed nanometer flower comprises the following steps:
(1) weighing 1.83g of zinc acetate and 1.33g of sodium stannate, and respectively dissolving in 50ml of deionized water;
(2) dropwise adding the prepared sodium stannate solution in the step (1) into the zinc acetate solution, and stirring continuously;
(3) transferring the mixed solution obtained in the step (2) to a reaction kettle, and carrying out hydrothermal reaction at 220 ℃ for 12 hours;
(4) centrifuging, cleaning and drying the product, and grinding the product by using a mortar to obtain ZnSnO3A nanoflower;
(5) 80mg of ground ZnSnO3 nanoflower is dispersed in 10ml of ethylene glycol and placed in an ultrasonic groove, so that the nanoflower is uniformly dispersed in the ethylene glycol;
(6) adding 1.106g of indium trichloride and 0.3g of thioacetamide into 40ml of ethylene glycol, and stirring to completely dissolve the indium trichloride and the thioacetamide to prepare an indium trichloride/thioacetamide mixed solution;
(7) mixing the liquids of (5) and (6), stirring thoroughly, placing in an ultrasonic tank, performing ultrasonic reaction for 1h with ultrasonic power of 50W and frequency of 30kHz, centrifuging, cleaning, and drying to obtain ZnSnO3/In2S3A composite material.
Example 5
A preparation method of ZnSnO3/In2S3 barbed nanoflower comprises the following steps:
(1) weighing 1.1g of zinc acetate and 1.33g of sodium stannate, and respectively dissolving in 50ml of deionized water;
(2) dropwise adding the prepared sodium stannate solution in the step (1) into the zinc acetate solution, and stirring continuously;
(3) transferring the mixed solution obtained in the step (2) to a reaction kettle, and carrying out hydrothermal reaction at 200 ℃ for 24 hours;
(4) centrifuging, cleaning and drying the product, and grinding the product by using a mortar to obtain ZnSnO3A nanomaterial;
(5) dispersing 100mg of ground ZnSnO3 in 10ml of ethylene glycol, and putting the mixture into an ultrasonic groove to uniformly disperse ZnSnO3 in the ethylene glycol;
(6) 0.553g of indium trichloride and 0.376g of thioacetamide are added into 40ml of ethylene glycol, and the mixture is stirred to be completely dissolved to prepare an indium trichloride/thioacetamide mixed solution;
(7) mixing the liquids of (5) and (6), stirring thoroughly, placing in an ultrasonic tank, performing ultrasonic reaction for 15min with ultrasonic power of 300W and frequency of 80kHz, centrifuging, cleaning, and drying to obtain ZnSnO3/In2S3A composite material;
example 6
A preparation method of ZnSnO3/In2S3 barbed nanoflower comprises the following steps:
(1) weighing 1.1g of zinc acetate and 1.33g of sodium stannate, and respectively dissolving in 50ml of deionized water;
(2) dropwise adding the prepared sodium stannate solution in the step (1) into the zinc acetate solution, and stirring continuously;
(3) transferring the mixed solution obtained in the step (2) to a reaction kettle, and carrying out hydrothermal reaction at 260 ℃ for 2 h;
(4) centrifuging, cleaning and drying the product, and grinding the product by using a mortar to obtain ZnSnO3A nanomaterial;
(5) dispersing 100mg of ground ZnSnO3 in 10ml of ethylene glycol, and putting the mixture into an ultrasonic groove to uniformly disperse ZnSnO3 in the ethylene glycol;
(6) 0.553g of indium trichloride and 0.376g of thioacetamide are added into 40ml of ethylene glycol, and the mixture is stirred to be completely dissolved to prepare an indium trichloride/thioacetamide mixed solution;
(7) mixing the liquids of (5) and (6), stirring thoroughly, placing in an ultrasonic tank, performing ultrasonic reaction for 2min with ultrasonic power of 100W and frequency of 50kHz, centrifuging, cleaning, and drying to obtain ZnSnO3/In2S3A composite material;
in this example, the ultrasonic reaction time In the step (7) was short, and thus needle-like In was formed2S3And has not yet been formed.
As shown in FIG. 3, is ZnSnO in the invention3/In2S3The catalytic degradation efficiency of the nano flower with the thorns on methyl orange organic dye is realized under the conditions of ultrasound and stirring.
Claims (7)
1. Zinc stannate/indium sulfide spiny nanoflower piezoelectric/photocatalyst, wherein the piezoelectric/photocatalyst comprises ZnSnO3/In2S3Comprising ZnSnO3Nanoflower, and In coated on surface thereof2S3And (4) nano needles.
2. The method for preparing zinc stannate/indium sulfide barbed nanoflower piezoelectric/photocatalyst according to claim 1, wherein the method specifically comprises the following steps:
(1) according to a molar ratio of 1: 1 weighing zinc acetate and sodium stannate, and respectively dissolving in water;
(2) dropwise adding the prepared sodium stannate solution in the step (1) into the zinc acetate solution, and stirring continuously;
(3) transferring the mixed solution obtained in the step (2) to a reaction kettle, and placing the reaction kettle in a drying box for hydrothermal reaction to obtain ZnSnO3A nanoflower;
(4) ZnSnO obtained in (2)3Cleaning the nanoflower, drying and fully grinding by using a mortar;
(5) grinding ZnSnO3Dispersing the nanoflower in ethylene glycol, and putting the nanoflower into an ultrasonic groove for ultrasonic treatment to uniformly disperse the nanoflower in the ethylene glycol;
(6) adding indium trichloride and thioacetamide into ethylene glycol, and stirring to completely dissolve the indium trichloride and the thioacetamide to prepare an indium trichloride/thioacetamide mixed solution;
(7) mixing the liquids of (5) and (6), stirring thoroughly, placing in an ultrasonic tank for ultrasonic treatment for 5min-1h, centrifuging, cleaning, and drying to obtain ZnSnO3/In2S3The flower is a flower with thorns.
3. The method for preparing zinc stannate/indium sulfide barbed nanoflower piezoelectric/photocatalyst according to claim 2, wherein the concentration of the zinc acetate and sodium stannate solution in step (1) is 0.1-80 mmol/L.
4. The method for preparing zinc stannate/indium sulfide barbed nanoflower piezoelectric/photocatalyst according to claim 2, wherein the hydrothermal reaction temperature in step (3) is 150-300 ℃ and the reaction time is 10min-24 h.
5. The method for preparing zinc stannate/indium sulfide barbed nanoflower piezoelectric/photocatalyst according to claim 2, wherein ZnSnO in step (5)3The amount of nanoparticles added is 0.001-1mol per liter of ethylene glycol.
6. The method for preparing zinc stannate/indium sulfide barbed nanoflower piezoelectric/photocatalyst according to claim 2, wherein the amount of indium trichloride added in step (6) is 0.01-1mol per liter of ethylene glycol, and the amount of thioacetamide added is 0.02-2mol per liter of ethylene glycol.
7. The method for preparing zinc stannate/indium sulfide barbed nanoflower piezoelectric/photocatalyst according to claim 2, wherein the power of the ultrasonic reaction in step (7) is 50-300W, and the frequency is 20kHz-200 kHz.
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