CN113860381B - Magnetic heteroplasmon nanometer material and preparation method thereof - Google Patents

Magnetic heteroplasmon nanometer material and preparation method thereof Download PDF

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CN113860381B
CN113860381B CN202111175872.8A CN202111175872A CN113860381B CN 113860381 B CN113860381 B CN 113860381B CN 202111175872 A CN202111175872 A CN 202111175872A CN 113860381 B CN113860381 B CN 113860381B
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CN113860381A (en
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许月阳
薛建明
朱法华
刘瑞江
王宏亮
柏源
徐振
蔡彦吟
石丽娜
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Jiangsu University
CHN Energy Group Science and Technology Research Institute Co Ltd
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    • C01G49/00—Compounds of iron
    • C01G49/02—Oxides; Hydroxides
    • C01G49/08—Ferroso-ferric oxide [Fe3O4]
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
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    • B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
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    • C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer

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Abstract

The invention belongs to the technical field of inorganic nonmetallic nano composite material preparation, and particularly relates to a heterobody nano sheet and a preparation method thereof. The invention discloses a raw material composition, which comprises ferric salt and dihydric phosphate, wherein the mole ratio of ferric ion to phosphate ion (2-6) is 1, the raw material composition is prepared into solution, and Fe is obtained after hydrothermal reaction and calcination of reducing agent 3 O 4 /α‑Fe 2 O 3 The magnetic heterogeneous nano-sheet prepared by the hydrothermal calcination has the advantages of wide raw material sources, low cost, simple process flow, simple and convenient operation, low requirements on required equipment, regular morphology and high yield of the obtained product, suitability for industrial mass production, saturation magnetization of 31-51emu/g and wide application.

Description

Magnetic heteroplasmon nanometer material and preparation method thereof
Technical Field
The invention belongs to the technical field of inorganic nonmetallic nanocomposite preparation, and particularly relates to a magnetic heteroplasmon nanomaterial and a preparation method thereof.
Background
In recent years, research on nanoscience and nanotechnology has been greatly developed. The unique physical and chemical properties of the nano material, including surface effect, catalytic performance, dielectric confinement, quantum effect, etc. make the nano material widely applied in ecological environment, biomedicine, electronic information, engineering application, optoelectronics, etc. The crystal form, particle size and morphology of the material have great influence on the performance of the material. The specific surface area of the nano material with the lamellar structure is high, so that the nano material with the lamellar structure exposes more active sites, and the reactivity is improved.
Iron oxide is a transition metal oxide that is non-toxic and harmless and widely exists in natural environments. Wherein, alpha-Fe 2 O 3 Has low biotoxicity, high corrosion resistance and excellent thermodynamic stability, thus having potential research value. However, alpha-Fe 2 O 3 To a certain extent, which limits its wide range of research and applications. To overcome this limitation, fe 3 O 4 /α-Fe 2 O 3 Magnetic hetero-nanoplatelets are prepared. The nano-sheet has controllable magnetic size, difficult agglomeration, safety, environmental protection, high catalytic performance and good biocompatibility.
At present, the particle size and morphology of the nano ferric oxide can be regulated and controlled by different synthesis methods, including a hydrolysis method, a coprecipitation method, a hydrothermal method, a solvothermal method, an ionic liquid assisted synthesis method, a thermal decomposition method, a combustion oxidation method and a sol-gel method. However, the preparation of Fe is reported 3 O 4 /α-Fe 2 O 3 The magnetic heterogeneous nano-sheet has few documents, the preparation method is complex, the period is long, the cost is high, and a surfactant or a toxic solvent is required to be used, so that the industrial production is not facilitated.
The prior Chinese patent document CN111847524 discloses Fe 3 O 4 /Fe 2 O 3 Magnetic heterogeneous nanotubes and method for preparing the same by controlling reducing sugar and alpha-Fe 2 O 3 The ratio of the nanotubes, the calcination temperature and the calcination time are controlled; the product has strong magnetism, regular shape, good stability and difficult agglomeration, but the preparation of Fe by adopting metal salt and other materials compared with the original materials is rarely reported 3 O 4 /α-Fe 2 O 3 The report of magnetic heteroplast nanometer, the prior art CN105417517 discloses that soluble ferric salt and metal ion-free phosphorus source solution are adopted, polyvinylpyrrolidone is used as a surfactant to prepare an iron phosphate material, but the prepared iron phosphate material is tremella-shaped, and is difficult to achieve an ideal form.
Disclosure of Invention
Therefore, the invention aims to solve the technical problems of Fe in the prior art 3 O 4 /α-Fe 2 O 3 The preparation process of the magnetic heteroplasmon nanometer sheet is insufficient, and Fe is prepared by adopting a hydrothermal calcination method 3 O 4 /α-Fe 2 O 3 The magnetic heterogeneous nano-sheet overcomes the defects of long period, high cost and the like of the prior preparation method, and provides the Fe which has simple operation, low cost, environmental protection and large-scale industrialized production 3 O 4 /α-Fe 2 O 3 A magnetic heterogeneous nano-sheet and a preparation method thereof.
The specific steps are as follows:
the invention discloses a raw material composition for synthesizing a magnetic heterogeneous nano material, which comprises ferric salt and dihydrogen phosphate, wherein the molar ratio of ferric ion to phosphate ion is (2-6): 1.
Further, the ferric salt comprises ferric chloride or/and ferric nitrate, and the dihydrogen phosphate comprises one or more of ammonium dihydrogen phosphate, sodium dihydrogen phosphate or potassium dihydrogen phosphate.
The invention also discloses a method for preparing the magnetic heteroplastid nano material by using the raw material composition, which comprises the following steps:
s1, ferric salt and dihydrogen phosphate are dissolved in a solvent according to the mole ratio of ferric ion to phosphate ion of (2-6): 1, and precursor solution is prepared at room temperature;
s2, performing a hydrothermal reaction on the precursor solution, and separating out an initial product;
s3, adding a reducing agent into the initial product, and calcining for 2-8h after the temperature is programmed to 450-700 ℃.
Further, in step S1, the precursor solution uses water as a solvent.
Further, the hydrothermal reaction in the step S2 is carried out in a hydrothermal kettle, the temperature is maintained at 200-220 ℃, and the constant temperature time is 12-24 hours.
Further, in the step S2, absolute ethyl alcohol or ionized water is adopted for ultrasonic mixing, hydrothermal reaction is carried out to obtain solid, and centrifugation is carried out for 5-6 times at 5000-10000rad/min for 5-10min each time, thus obtaining the initial product.
Further, the reducing agent in step S3 includes polyvinylpyrrolidone (PVP).
Further, the mass ratio of the initial product to the reducing agent in the step S3 is 1 (2-8).
The invention also discloses a magnetic heteroplasmon nanosheet material which is nanosheet and has a molecular formula of Fe 3 O 4 /α-Fe 2 O 3 Is prepared from the raw material composition or the preparation method.
Further, the average diameter of the magnetic heterogeneous nano-sheet is 153-292nm, and the average thickness is 29-44nm.
The technical scheme of the invention has the following advantages:
1. the invention discloses a raw material composition, which comprises ferric salt and dihydric phosphate, wherein the molar ratio of ferric ion to phosphate ion is (2-6): 1, and the raw material composition has the advantages of wide source, low price and environmental protection.
2. The invention also discloses a preparation method for preparing the magnetic heteroplastid nano material, which adopts a hydrothermal calcination method to prepare Fe 3 O 4 /α-Fe 2 O 3 The magnetic heterogeneous nano-sheet is prepared from the first raw materials of ferric salt, dihydrogen phosphate and poly (ferric salt)Vinyl Pyrrolidone (PVP), the preparation method and the process steps are novel, and the operation is simple and convenient; the requirements on required equipment are not high, the efficiency is high, and the process is easy to control; the polyvinylpyrrolidone (PVP) is used as a reducing agent in the calcination process of the whole process flow, so that the process is safer; the reaction process can prepare nano-sheets with different sizes by controlling three parameters of the proportion of ferric salt and dihydric phosphate, the hydrothermal temperature and the hydrothermal time, and Fe with different performances can be prepared by controlling the dosage of polyvinylpyrrolidone (PVP) and the calcination temperature and the calcination time 3 O 4 /α-Fe 2 O 3 Magnetic heterobody nanoplatelets; the product is uniformly distributed, has regular shape and strong magnetism, and is not easy to agglomerate. In addition, fe prepared by the method 3 O 4 /α-Fe 2 O 3 The magnetic heterogeneous nano-sheet has larger specific surface area, and is favorable for better application in the research of ecological environment.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the following description will briefly explain the drawings needed in the embodiments or the prior art, and it is obvious that the drawings in the following description are some embodiments of the present invention and that other drawings can be obtained according to these drawings without inventive effort for a person skilled in the art.
FIG. 1 shows Fe prepared in example 1 3 O 4 /α-Fe 2 O 3 X-ray diffraction pattern of magnetic hetero-body nano-sheet and alpha-Fe 2 O 3 Standard PDF card (JCPDS No. 89-0596) and Fe 3 O 4 A standard PDF card (JCPDS No. 75-0449) comparison chart;
FIG. 2 is a diagram of Fe prepared in example 1 3 O 4 /α-Fe 2 O 3 Scanning electron microscope pictures of magnetic heterogeneous nano-sheets, wherein the size of a scale in the picture is 100nm;
FIG. 3 is a diagram of Fe prepared in example 2 3 O 4 /α-Fe 2 O 3 Transmission electron micrographs of magnetic heteroplasmic nanoplatelets, wherein the scale in the figure is 100nm in size.
Detailed Description
The following examples are provided for a better understanding of the present invention and are not limited to the preferred embodiments described herein, but are not intended to limit the scope of the invention, any product which is the same or similar to the present invention, whether in light of the present teachings or in combination with other prior art features, falls within the scope of the present invention.
The specific experimental procedures or conditions are not noted in the examples and may be followed by the operations or conditions of conventional experimental procedures described in the literature in this field. The reagents or apparatus used were conventional reagent products commercially available without the manufacturer's knowledge.
Example 1
0.541g (2.001 mmol) of ferric trichloride hexahydrate and 0.094g (0.602 mmol) of sodium dihydrogen phosphate dihydrate were weighed into 80mL of deionized water, and stirred until completely dissolved, to obtain a precursor solution. Placing the precursor solution into a hydrothermal kettle, heating to 220 ℃, keeping the temperature constant for 24 hours, cooling to room temperature, adding deionized water into the obtained product, uniformly mixing by ultrasonic, centrifuging for 6 times at the rotating speed of 10000rad/min, centrifuging for 5 minutes each time, removing supernatant, transferring the product into a vacuum drying oven to obtain an initial product, weighing 0.4g polyvinylpyrrolidone (PVP) and 0.2g of the dried initial product, adding the initial product into a crucible, uniformly mixing, placing the crucible into a program temperature control furnace for calcining for 4 hours at 600 ℃, taking out solids in the crucible after the temperature of the program temperature control furnace is reduced to room temperature, and obtaining Fe 3 O 4 /α-Fe 2 O 3 Magnetic heterobody nanoplatelets; prepared Fe 3 O 4 /α-Fe 2 O 3 The average diameter of the magnetic heterogeneous nano-sheet is 260nm, the average thickness is 36nm, and the saturation magnetization is 38emu/g.
Fe prepared under the conditions described in this example 3 O 4 /α-Fe 2 O 3 X-ray diffraction pattern of magnetic hetero-body nano-sheet and alpha-Fe 2 O 3 Standard PDF card (JCPDS No. 89-0596) and Fe 3 O 4 A comparison chart of a standard PDF card (JCPDS No. 75-0449) is shown in FIG. 1; from the figures, it can be seen thatMost of the diffraction peak positions of the product and alpha-Fe 2 O 3 The diffraction peak positions of the standard PDF card correspond to each other; meanwhile, fe 3 O 4 /α-Fe 2 O 3 The diffraction peak ratio of the magnetic composite nano rod at two diffraction angles of 33 degrees and 35.6 degrees is obviously higher than that of standard Fe 2 O 3 The diffraction intensity ratio of (C) is small, and also indicates that Fe at 35.7 DEG 3 O 4 The presence of diffraction peaks.
Fe prepared under the conditions described in this example 3 O 4 /α-Fe 2 O 3 A scanning electron microscope photograph of the magnetic heterogeneous nano-sheet is shown in fig. 2; through statistical analysis, fe 3 O 4 /α-Fe 2 O 3 The average diameter of the magnetic hetero-body nano-sheets is 260nm, and the average thickness is 36nm.
Example 2
0.541g (2.001 mmol) of ferric trichloride hexahydrate and 0.038g (0.330 mmol) of monoammonium phosphate were weighed into 80mL of deionized water, and stirred until completely dissolved, to obtain a precursor solution. Placing the precursor solution into a hydrothermal kettle, heating to 220 ℃, keeping the temperature constant for 24 hours, cooling to room temperature, adding alcohol into the obtained product, carrying out ultrasonic mixing, centrifuging for 6 times at the rotating speed of 10000rad/min in the centrifuging step, centrifuging for 5 minutes each time, removing supernatant, transferring the product into a vacuum drying oven, weighing 0.2g polyvinylpyrrolidone (PVP) and 0.1g solid after drying, adding the mixture into a crucible, mixing uniformly, placing the crucible into a program temperature-controlled furnace, calcining at 600 ℃ for 2 hours, taking out the solid in the crucible after the temperature of the program temperature-controlled furnace is reduced to room temperature, and obtaining Fe 3 O 4 /α-Fe 2 O 3 Magnetic heterogeneous nanoplatelets. Prepared Fe 3 O 4 /α-Fe 2 O 3 The average diameter of the magnetic heterogeneous nano-sheet is 153nm, the average thickness is 44nm, and the saturation magnetization is 51emu/g.
Fe prepared under the conditions described in this example 3 O 4 /α-Fe 2 O 3 A transmission electron microscope photograph of the magnetic heterogeneous nano-sheet is shown in fig. 3; through statistical analysis, fe 3 O 4 /α-Fe 2 O 3 The average diameter of the magnetic hetero-nano-sheets was 153nm and the average thickness was 44nm.
Example 3
0.541g (2.001 mmol) of ferric trichloride hexahydrate and 0.051g (0.443 mmol) of monoammonium phosphate were weighed into 80mL of deionized water, and stirred until completely dissolved, to obtain a precursor solution. Placing the precursor solution into a hydrothermal kettle, heating to 220 ℃, keeping the temperature constant for 24 hours, cooling to room temperature, adding deionized water or alcohol into the obtained product, uniformly mixing by ultrasonic, centrifuging for 5 times at the rotating speed of 10000rad/min in the centrifuging step, centrifuging for 10 minutes each time, removing supernatant, transferring the product into a vacuum drying oven, weighing 0.6g polyvinylpyrrolidone (PVP) and 0.1g solid after drying, uniformly mixing in a crucible, placing the crucible into a program temperature control furnace for calcining for 6 hours at 600 ℃, taking out the solid in the crucible after the temperature of the program temperature control furnace is reduced to room temperature, and obtaining Fe 3 O 4 /α-Fe 2 O 3 Magnetic heterogeneous nanoplatelets. Through statistical analysis, fe is prepared 3 O 4 /α-Fe 2 O 3 The average diameter of the magnetic heterogeneous nano-sheet is 198nm, the average thickness is 40nm, and the saturation magnetization is 41emu/g.
Example 4
0.541g (2.001 mmol) of ferric trichloride hexahydrate and 0.156g (0.999 mmol) of sodium dihydrogen phosphate dihydrate were weighed into 80mL of deionized water, and stirred until completely dissolved, to obtain a precursor solution. Placing the precursor solution into a hydrothermal kettle, heating to 220 ℃, keeping the temperature constant for 24 hours, cooling to room temperature, adding deionized water or alcohol into the obtained product, uniformly mixing by ultrasonic, centrifuging at the rotating speed of 10000rad/min for 6 times and 5 minutes each time, removing supernatant, transferring the product into a vacuum drying box, weighing 0.8g polyvinylpyrrolidone (PVP) and 0.1g solid after drying, uniformly mixing, placing the crucible into a program temperature-controlled furnace for calcining at 600 ℃ for 8 hours, taking out the solid in the crucible after the temperature of the program temperature-controlled furnace is reduced to room temperature, and obtaining Fe 3 O 4 /α-Fe 2 O 3 Magnetic heterogeneous nanoplatelets. Through statistical analysis, fe is prepared 3 O 4 /α-Fe 2 O 3 The average diameter of the magnetic hetero-body nano-sheet is 292nm, the average thickness is 29nm, and the saturation magnetization is 31emu/g.
Example 5
0.541g (2.001 mmol) of ferric trichloride hexahydrate and 0.082g (0.603 mmol) of potassium dihydrogen phosphate were weighed into 80mL of deionized water, and stirred until completely dissolved, to obtain a precursor solution. Placing the precursor solution into a hydrothermal kettle, heating to 200 ℃, keeping the temperature constant for 24 hours, cooling to room temperature, adding deionized water or alcohol into the obtained product, uniformly mixing by ultrasonic, centrifuging at the rotating speed of 10000rad/min for 6 times and 5 minutes each time, removing supernatant, transferring the product into a vacuum drying box, weighing 0.4g polyvinylpyrrolidone (PVP) and 0.1g solid after drying, uniformly mixing, placing the crucible into a program temperature-controlled furnace for calcining for 4 hours at 450 ℃, taking out the solid in the crucible after the temperature of the program temperature-controlled furnace is reduced to room temperature, and obtaining Fe 3 O 4 /α-Fe 2 O 3 Magnetic heterogeneous nanoplatelets. Through statistical analysis, fe is prepared 3 O 4 /α-Fe 2 O 3 The average diameter of the magnetic hetero-body nano-sheet is 257nm, the average thickness is 37nm, and the saturation magnetization is 33emu/g.
Example 6
0.541g (2.001 mmol) of ferric trichloride hexahydrate and 0.082g (0.603 mmol) of potassium dihydrogen phosphate were weighed into 80mL of deionized water, and stirred until completely dissolved, to obtain a precursor solution. Placing the precursor solution into a hydrothermal kettle, heating to 210 ℃, keeping the temperature constant for 24 hours, cooling to room temperature, adding deionized water or alcohol into the obtained product, uniformly mixing by ultrasonic, centrifuging at the rotating speed of 10000rad/min for 6 times and 5 minutes each time, removing supernatant, transferring the product into a vacuum drying oven, weighing 0.4g polyvinylpyrrolidone (PVP) and 0.2g solid after drying, uniformly mixing, placing the crucible into a program temperature-controlled furnace for calcining at 700 ℃ for 4 hours, taking out the solid in the crucible after the temperature of the program temperature-controlled furnace is reduced to room temperature, and obtaining Fe 3 O 4 /α-Fe 2 O 3 Magnetic heterogeneous nanoplatelets. Through statistical analysis, fe is prepared 3 O 4 /α-Fe 2 O 3 The average diameter of the magnetic heterogeneous nano-sheet is 262nm, the average thickness is 38nm, and the saturation magnetization is 39emu/g.
Example 7
Weigh 0.541g (2.001 mmol) of sixFerric trichloride hydrate and 0.104g (0.666 mmol) of sodium dihydrogen phosphate dihydrate were added to 80mL of deionized water, and stirred until completely dissolved, to obtain a precursor solution. Placing the precursor solution into a hydrothermal kettle, heating to 220 ℃, keeping the temperature constant for 12 hours, cooling to room temperature, adding deionized water or alcohol into the obtained product, uniformly mixing by ultrasonic, centrifuging at the rotating speed of 10000rad/min for 6 times and 5 minutes each time, removing supernatant, transferring the product into a vacuum drying oven, weighing 0.3g polyvinylpyrrolidone (PVP) and 0.05g solid after drying, uniformly mixing, placing the crucible into a program temperature-controlled furnace for calcining at 600 ℃ for 4 hours, taking out the solid in the crucible after the temperature of the program temperature-controlled furnace is reduced to room temperature, and obtaining Fe 3 O 4 /α-Fe 2 O 3 Magnetic heterogeneous nanoplatelets. Through statistical analysis, fe is prepared 3 O 4 /α-Fe 2 O 3 The average diameter of the magnetic hetero-body nano-sheet is 276nm, the average thickness is 33nm, and the saturation magnetization is 35emu/g.
Example 8
0.541g (2.001 mmol) of ferric trichloride hexahydrate and 0.104g (0.666 mmol) of sodium dihydrogen phosphate dihydrate were weighed into 80mL of deionized water, and stirred until completely dissolved, to obtain a precursor solution. Placing the precursor solution into a hydrothermal kettle, heating to 220 ℃, keeping the temperature constant for 18 hours, cooling to room temperature, adding deionized water or alcohol into the obtained product, uniformly mixing by ultrasonic, centrifuging at the rotating speed of 10000rad/min for 6 times and 5 minutes each time, removing supernatant, transferring the product into a vacuum drying box, weighing 0.5g polyvinylpyrrolidone (PVP) and 0.1g solid after drying, uniformly mixing, placing the crucible into a program temperature-controlled furnace for calcining for 4 hours at 600 ℃, taking out the solid in the crucible after the temperature of the program temperature-controlled furnace is reduced to room temperature, and obtaining Fe 3 O 4 /α-Fe 2 O 3 Magnetic heterogeneous nanoplatelets. Through statistical analysis, fe is prepared 3 O 4 /α-Fe 2 O 3 The average diameter of the magnetic heterogeneous nano-sheet is 283nm, the average thickness is 32nm, and the saturation magnetization is 40emu/g.
Example 9
Weighing 0.541g (2.001 mmol) of ferric trichloride hexahydrate and 0.104g (0.666)mmol) sodium dihydrogen phosphate dihydrate was added to 80mL deionized water and stirred until completely dissolved to obtain a precursor solution. Placing the precursor solution into a hydrothermal kettle, heating to 220 ℃, keeping the temperature constant for 24 hours, cooling to room temperature, adding deionized water or alcohol into the obtained product, uniformly mixing by ultrasonic, centrifuging at the rotating speed of 10000rad/min for 6 times and 5 minutes each time, removing supernatant, transferring the product into a vacuum drying box, weighing 0.7g polyvinylpyrrolidone (PVP) and 0.1g solid after drying, uniformly mixing, placing the crucible into a program temperature-controlled furnace for calcining at 600 ℃ for 4 hours, taking out the solid in the crucible after the temperature of the program temperature-controlled furnace is reduced to room temperature, and obtaining Fe 3 O 4 /α-Fe 2 O 3 Magnetic heterogeneous nanoplatelets. Through statistical analysis, fe is prepared 3 O 4 /α-Fe 2 O 3 The average diameter of the magnetic heterogeneous nano-sheet is 281nm, the average thickness is 32nm, and the saturation magnetization is 43emu/g.
It is apparent that the above examples are given by way of illustration only and are not limiting of the embodiments. Other variations or modifications of the above teachings will be apparent to those of ordinary skill in the art. It is not necessary here nor is it exhaustive of all embodiments. And obvious variations or modifications thereof are contemplated as falling within the scope of the present invention.

Claims (4)

1. A method for preparing a magnetic heteroplasmic nanoplatelet material, comprising the steps of:
s1, ferric salt and dihydrogen phosphate are dissolved in a solvent according to the mole ratio of ferric ion to phosphate ion of (2-6): 1, and precursor solution is prepared at room temperature;
s2, carrying out hydrothermal reaction on the precursor solution, and separating out an initial product;
s3, adding a reducing agent polyvinylpyrrolidone into the initial product, and calcining at the temperature of 450-700 ℃ for 2-8 h;
the mass ratio of the initial product to the reducing agent in the step S3 is 1 (2-8);
the saidThe molecular formula of the nano-sheet material is Fe 3 O 4 /α-Fe 2 O 3 The average diameter is 153-292nm, and the average thickness is 29-44nm.
2. The method of claim 1, wherein the precursor solution in step S1 is water.
3. The method for preparing a magnetic heterogeneous nano-sheet material according to claim 1 or 2, wherein the hydrothermal reaction in step S2 is performed in a hydrothermal kettle, the temperature is maintained at 200-220 ℃, and the constant temperature time is 12-24h.
4. The method for preparing the magnetic heteroplasmic nano-sheet material according to claim 3, wherein in the step S2, absolute ethyl alcohol or ionic water is adopted for ultrasonic mixing, and hydrothermal reaction is carried out to obtain a solid, and centrifugation is carried out for 5-6 times at 5000-10000rad/min for 5-10min each time, so as to obtain an initial product.
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Citations (8)

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