CN112919457A - Nano material and preparation method thereof - Google Patents
Nano material and preparation method thereof Download PDFInfo
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- CN112919457A CN112919457A CN202110215959.7A CN202110215959A CN112919457A CN 112919457 A CN112919457 A CN 112919457A CN 202110215959 A CN202110215959 A CN 202110215959A CN 112919457 A CN112919457 A CN 112919457A
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- C01B32/00—Carbon; Compounds thereof
- C01B32/15—Nano-sized carbon materials
- C01B32/182—Graphene
- C01B32/184—Preparation
- C01B32/19—Preparation by exfoliation
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/15—Nano-sized carbon materials
- C01B32/158—Carbon nanotubes
- C01B32/168—After-treatment
- C01B32/174—Derivatisation; Solubilisation; Dispersion in solvents
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- C01B33/02—Silicon
Abstract
The invention belongs to the technical field of nano materials, and particularly relates to a nano material and a preparation method thereof, wherein the preparation method comprises the following steps: uniformly mixing a certain amount of raw materials and a solvent, and introducing into a buffer tank; introducing the slurry in the buffer tank into an ultrasonic unit for ultrasonic treatment; introducing the slurry subjected to ultrasonic treatment into an iron removal device, and returning the slurry into the buffer tank after the slurry flows out of the iron removal device to form slurry circulation; and obtaining the nano-material slurry after at least one slurry circulation. In this embodiment, magnetic impurities can be introduced in the process of preparing the nano material, particularly, the ultrasonic unit itself can fall off in the vibration process to pollute the slurry, and the magnetic impurities in the slurry after the ultrasonic treatment are removed by the iron removal device, so that the performance of the nano material is not affected.
Description
Technical Field
The invention belongs to the technical field of nano materials, and particularly relates to a nano material and a preparation method thereof.
Background
The nano material is concerned by people due to the unique structure and performance, is known as the most promising material in the 21 st century, and has important application value in the fields of national defense, electronics, chemical engineering, metallurgy, light industry, aerospace, ceramics, nuclear technology, catalysts, medicine and the like.
Present patent CN210434500U provides a nanometer thick liquids preparation facilities, adopts nanometer sand mill to grind thick liquids, and the grinding ball can cause the wearing and tearing to drop after long-time work, can't get rid of, causes the pollution to thick liquids, when peeling off to two-dimentional nano-material, if graphite alkene preparation, just smash on two-dimentional size, can't play great effect to peeling off of thickness direction, finally leads to the product to produce the property ability to be restricted.
In the prior patent CN109761226A, a method for preparing two-dimensional graphite nanoplatelets by liquid phase ball milling is provided, in which a prepared expanded graphite solution is placed in an ultrasonic machine for ultrasonic treatment, and the expanded graphite solution after ultrasonic treatment is poured into a container of a sand mill to obtain a two-dimensional graphite nanoplatelet solution, although a two-dimensional nano solution is obtained by using ultrasonic treatment and the sand mill, magnetic impurities can be introduced during ultrasonic treatment and ball milling, which pollutes slurry and affects the realization of the self-functions of the nano material.
Disclosure of Invention
The technical problem to be solved by the invention is as follows: aiming at the problem that the magnetic impurities are introduced in the preparation process of the existing nano material preparation device to influence the performance of the nano material, the nano material and the preparation method thereof are provided.
In order to solve the above technical problems, an embodiment of the present invention provides a method for preparing a nanomaterial, including the following steps:
uniformly mixing a certain amount of raw materials and a solvent, and introducing into a buffer tank;
introducing the slurry in the buffer tank into an ultrasonic unit for ultrasonic treatment;
introducing the slurry subjected to ultrasonic treatment into an iron removal device, and returning the slurry into the buffer tank after the slurry flows out of the iron removal device to form slurry circulation;
and obtaining the nano-material slurry after at least one slurry circulation.
Optionally, a certain amount of raw materials and a solvent are put into a premixing tank, then a dispersing agent and a viscosity reducer are added for 10-240 min, and the raw materials and the solvent are uniformly mixed and then introduced into the buffer tank.
Optionally, discharging the air in the premixing tank, filling the premixing tank with inert gas, and then putting the raw materials and the solvent into the premixing tank;
and discharging the air in the buffer tank, filling inert gas, and introducing the uniformly mixed slurry into the buffer tank.
Optionally, the magnetic induction intensity of the iron removal device is 10000-50000 GS.
Optionally, before ultrasonic treatment, feeding the slurry in the buffer tank into a sand mill for grinding, wherein the sand mill is connected with the ultrasonic unit in parallel;
the diameter of a sanding medium of the sand mill is 0.1-3 mm, the filling rate is 20-80%, and the sanding time is 1-10 h.
Optionally, the ultrasonic unit comprises an ultrasonic power supply and an ultrasonic radiation end, the output power of the ultrasonic power supply is 1-10 KW, the frequency is 15-100 KHz, and the ultrasonic radiation end is in a round bar structure, a dumbbell structure, a thin rod focusing structure or a porous structure; the ultrasonic time is 1-10 h, and the temperature in the ultrasonic process is 20-80 ℃.
Optionally, the temperature of the slurry circulation is 0-100 ℃, the pressure is 0-1 MPa, and the flow is 0-10 m3/h。
Optionally, a cooling device is arranged between the ultrasonic unit and the iron removal device, and the slurry subjected to ultrasonic processing flows through the cooling device and then is introduced into the iron removal device; the temperature of the condensed water of the cooling device is 5-15 ℃, and the flow rate is 0-29L/min.
Optionally, the buffer tank is used for storing the slurry in a ratio of 20-80% in the slurry circulation process.
In another aspect, the embodiment of the present invention provides a nanomaterial obtained by the preparation method as described above.
In the embodiment of the invention, magnetic impurities are introduced in the process of preparing the nano material, particularly, metal falls off to pollute slurry in the vibration process of the ultrasonic unit, and the magnetic impurities in the slurry finished by ultrasonic are removed by the iron removal device so as to avoid influencing the performance of the nano material.
Drawings
FIG. 1 is a flow chart of a preparation method according to an embodiment of the present invention.
Detailed Description
In order to make the technical problems, technical solutions and advantageous effects solved by the present invention more apparent, the present invention is further described in detail below with reference to the embodiments and the accompanying drawings. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
As shown in fig. 1, an embodiment of the present invention provides a method for preparing a nanomaterial, including the following steps:
uniformly mixing a certain amount of raw materials and a solvent, and introducing into a buffer tank;
introducing the slurry in the buffer tank into an ultrasonic unit for ultrasonic treatment;
introducing the slurry subjected to ultrasonic treatment into an iron removal device, and returning the slurry into the buffer tank after the slurry flows out of the iron removal device to form slurry circulation;
and obtaining the nano-material slurry after at least one slurry circulation.
In this embodiment, magnetic impurities can be introduced in the process of preparing the nano material, particularly, the ultrasonic unit itself can fall off in the vibration process to pollute the slurry, and the magnetic impurities in the slurry after the ultrasonic treatment are removed by the iron removal device, so that the performance of the nano material is not affected.
The ultrasonic unit can use ultrasonic equipment with different powers, frequencies and ultrasonic radiation end structures according to the characteristics of the sizes and the structures of different powders to be treated, the viscosity of mixed slurry and the like, and utilizes the cavitation effect formed by ultrasonic waves in different forms in the slurry, namely impact waves and microjets with huge energy generated by instant explosion of a large amount of tiny bubbles generated in the slurry to strip, break and disperse the powders in the slurry, so that the preparation efficiency of the nano material is improved.
Be provided with the stirring rake that has the wall function of scraping in the buffer tank, can prevent that thick liquids from splashing can't drop on the inner wall of the jar body, cause thick liquids inhomogeneous and extravagant. The buffer tank is provided with the discharge valve, the slurry obtained after multiple slurry circulations is discharged from the discharge valve of the buffer tank, the nano material is prepared by adopting a physical preparation process, the pollution is avoided, the production process is simple and feasible, the practicability is high, the process is controllable, and the prepared nano material has the advantages of high quality, few defects, good consistency and the like, and can be used for batch and industrial continuous and stable production.
In one embodiment, a certain amount of raw materials and a certain amount of solvent are put into a premixing tank, then a dispersing agent and a viscosity reducer are added for 10-240 min, and the raw materials and the solvent are uniformly mixed and then introduced into a buffer tank.
And the slurry in the premixing tank is introduced into the buffer tank through a circulating pump, the circulating pump and the stirring paddle in the premixing tank act simultaneously in the premixing process, the raw materials, the dispersing agent, the auxiliary agent and the like which are prepared in proportion are uniformly mixed with the solvent, the gas in contact with the solvent in the mixing process is air or inert gas and the like, and the inert gas is preferably nitrogen.
The slurry meeting the conditions is prepared through a premixing process, and the contact gas in the mixing process is inert gas, so that the condition that the slurry is polluted or combustion and explosion are formed after external air enters is prevented.
The slurry flowing out of the premixing tank can be returned to the premixing tank again through another circulating pump to form the self-circulation of the premixing tank.
It should be noted that the raw material and the solvent are necessary, the dispersant and the auxiliary agent (such as the viscosity reducer) are unnecessary, and may be selected according to actual production conditions, for example, when preparing the graphene slurry and the nano-silicon slurry, the requirement for the agglomeration property in the circulation process is not high, the dispersant and the auxiliary agent may not be added, for example, when producing the carbon nanotube slurry, the carbon nanotubes in the slurry are easy to agglomerate, and the dispersant and the viscosity reducer are required to be added, so as to improve the dispersibility and reduce the viscosity.
The circulating pump provides power and can be but not limited to a self-priming pump, a centrifugal pump, a rotor pump, a diaphragm pump or a screw pump, and the flow is 0.5-5 m3H is used as the reference value. Preferably, the circulating pump for introducing the slurry into the buffer tank adopts a rotor pump with a frequency converter, so that stability can be providedConstant flow velocity, preferably 1m flow3H is used as the reference value. The circulating pump of the premixing tank self-circulation preferably adopts a diaphragm pump.
In an embodiment, the buffer tank is used for ensuring that a certain amount of slurry is always reserved in the buffer tank in the slurry circulation process, the percentage of the reserved slurry is 20-80%, the gas in the buffer tank is air or inert gas, preferably, the percentage of the reserved slurry is 50%, and the inert gas is nitrogen.
In one embodiment, before premixing, the air in the premixing tank and the slurry circulation is exhausted and filled with inert gas, after the premixing tank is filled with inert gas, the raw materials and the solvent are put into the premixing tank, and the raw materials and the solvent are stirred by a stirring paddle in the premixing tank to obtain uniform slurry. And introducing the slurry into the buffer tank through a circulating pump.
The inert gas is preferably nitrogen gas, and nitrogen gas provides through nitrogen seal device, and nitrogen seal device includes nitrogen gas steel bottle and nitrogen seal valve, the nitrogen gas steel bottle passes through nitrogen gas pipe connection the nitrogen seal valve, premix jar with the top of buffer tank all is connected with the nitrogen seal valve. Before premixing, a nitrogen sealing valve is opened to fill nitrogen into the premixing tank and the buffer tank.
In one embodiment, the iron removing device comprises a strong magnet, and the magnetic induction intensity of the magnet is 10000-50000 GS, preferably 12000 GS. The slurry absorbs the magnetic impurities in the slurry when flowing through the iron removal device, in addition, the number of the iron removal device can be one or more, the connection form can be a plurality of series connection or two-to-two parallel connection or three-to-three parallel connection, preferably two-to-two parallel connection or three-to-three parallel connection, and one opening and one closing can be carried out in the continuous working process so as to clean the magnetic impurities absorbed by the iron removal device in time.
In one embodiment, before ultrasonic treatment, the slurry in the buffer tank is fed into a sand mill for grinding, and the sand mill is connected with the ultrasonic unit in parallel. The diameter of a sanding medium of the sand mill is 0.1-3 mm, the filling rate is 20-80%, and the sanding time is 1-10 h.
The sand mill is connected with the ultrasonic unit in parallel, slurry in the buffer tank can be simultaneously introduced into the sand mill and the ultrasonic unit, or sequentially pass through the sand mill and the ultrasonic unit, or the slurry only flows through the ultrasonic unit to be subjected to ultrasonic treatment, and whether the sand mill is selected or not is judged according to actually produced nano materials.
The sanding medium of the sander may be, but is not limited to, glass beads, zirconia beads, or steel beads. Zirconia beads with a diameter of 0.3mm and a filling rate of 50% are preferably used.
In one embodiment, the ultrasonic unit comprises an ultrasonic power supply and an ultrasonic radiation end, the output power of the ultrasonic power supply is 1-10 KW, the frequency is 15-100 KHz, the ultrasonic radiation end is in a round bar structure, a dumbbell structure, a thin rod focusing structure or a porous structure, the ultrasonic time is 1-10 hours, and the temperature in the ultrasonic process is 20-80 ℃.
The ultrasonic radiation end is an insertion type ultrasonic radiation end and is directly contacted with the slurry, the material is TC4 or 304 or a magnetic material, the ultrasonic radiation end can be metal-fallen in the vibration process and can be removed through a deironing device at the rear end, and therefore slurry pollution is avoided. In addition, the ultrasonic time and the power supply frequency also influence the amount of metal falling off from the ultrasonic radiation end, the metal always falls off from the ultrasonic radiation end in the slurry circulation process, the frequency is higher, the ultrasonic time is longer, the number of the fallen metal is larger, and different iron contents are obtained according to the ultrasonic time and the power supply frequency.
According to the actual requirement, the ultrasonic waves participating in the slurry circulation process can work in one set or a plurality of sets at the same time, namely any combination of different working frequencies, different forms of radiation ends and different vibration modes (continuous vibration or intermittent vibration). Preferably, the power supply has an output power of 3KW and a frequency of 20KHz and 40KHz in combination.
In one embodiment, the temperature of the slurry circulation is 0-100 ℃, the pressure is 0-1 MPa, and the flow rate is 0-10 m3H is used as the reference value. The slurry circulation system is provided with a flowmeter, two temperature monitoring meters and two pressure meters, wherein the flowmeter, the two temperature monitoring meters and the two pressure meters are respectively used for monitoring the flow, the temperature and the pressure in the circulation process, and the two temperature monitoring meters are respectively arranged at the front end and the rear end of the ultrasonic unit and can know the flow passing through the ultrasonic unitThe temperature of the slurry after the ultrasonic treatment by the ultrasonic unit changes. The flow meter may be, but is not limited to, a rotameter or an electromagnetic flow meter.
In one embodiment, a cooling device is arranged between the ultrasonic unit and the iron removal device, the slurry subjected to ultrasonic processing flows through the cooling device and then is introduced into the iron removal device, the temperature of condensed water of the cooling device is 5-15 ℃, and the flow rate is 0-29L/min. When the slurry passes through the ultrasonic unit, the temperature of the slurry can rise, and the cooling device cools the slurry to control the temperature of the materials in the slurry circulation.
The cooling device can be but not limited to a plate radiator, a tubular radiator or a jacketed condenser pipe radiator, preferably adopts a jacketed condenser pipe radiator, the temperature of condensed water is set at 10 ℃, and the flow rate is 10L/min.
In one embodiment, a needle valve is arranged on a pipeline from the iron removing device to the buffer tank, and the pressure of the slurry circulation can be adjusted according to requirements.
Another embodiment of the present invention provides a nanomaterial obtained by the preparation method as described above. The existing preparation methods of the nano-materials comprise a physical ball milling method, a sol-gel method, a precipitation method, a hydrothermal method, a microemulsion method and the like, which have advantages and disadvantages, but most of the methods still stay in a laboratory stage, and the prepared nano-materials have a series of problems of easy impurity introduction, high production cost, large energy consumption, environmental pollution and the like, so that the method for really realizing large-scale industrial application is few. The preparation method of the nano material provided by the invention can solve the problems, has the advantages of simple operation, easy control, short period, high efficiency, environmental protection and the like, can realize large-scale production application, and the prepared nano material has the advantages of good consistency, high quality and few defects.
The present invention will be further illustrated by the following examples.
Example 1
The graphene slurry is prepared by the preparation method, and the specific operation process is as follows:
the raw materials included expanded graphite and NMP solvent.
And discharging air in the premixing tank and the slurry circulation through a nitrogen-sealed valve to enable the premixing tank and the slurry circulation to be filled with nitrogen, putting 30Kg of dried expanded graphite and NMP solvent into the premixing tank according to the proportion that the solid content of the expanded graphite is 2.5%, and starting a stirring paddle and a diaphragm pump to enable the slurry to be uniformly mixed, wherein the premixing time is 120 min.
After premixing is finished, the slurry is conveyed to the slurry circulation through the diaphragm pump, the diaphragm pump for conveying the slurry is closed, then the rotor pump for circulating the slurry is started, the slurry sequentially passes through the ultrasonic unit, the pressure gauge, the temperature monitor, the electromagnetic flow meter, the 12000GS iron remover and the jacketed condenser pipe, and finally returns to the buffer tank to form a closed circulation process, wherein the flow rate is controlled to be 0.5m in the circulation process3H, pressure 0 MPa.
And starting cooling circulating water of the cooling device, wherein the water inlet temperature is set at 10 ℃, and the flow rate is 10L/min.
And starting a first ultrasonic power supply to strip the expanded graphite in the slurry, wherein the output power of the first ultrasonic power supply is 3000W, the frequency is 20KHz, an ultrasonic radiation head of an inserted round bar structure is adopted at an ultrasonic radiation end, the material is a magnetic material, the working mode is continuous working, and the ultrasonic time is 240 min.
And after the first ultrasonic power supply is turned off, the second ultrasonic power supply is turned on, the output power of the second ultrasonic power supply is 2000W, the frequency is 40KHz, the radiation end adopts a plug-in ultrasonic bar form, the material is a magnetic material, the working mode is continuous working, the ultrasonic time is 120min, and the temperature of the whole ultrasonic circulation process is controlled to be 30-40 ℃.
The graphene prepared by the method has the two-dimensional size of 5-15 mu m, the thickness of 1-10 nm and the iron content of less than 3 ppm.
And (3) closing all ultrasonic power supplies after the process is finished, continuously crushing the two-dimensional size of the graphene in the slurry by using a sand mill according to the requirement, wherein the volume of the sand mill is 3L, a zirconium oxide medium with the diameter of 0.6mm is selected, the filling rate is 50%, continuously treating the slurry for 60min, and obtaining the graphene slurry with the two-dimensional size smaller than 1 mu m, the thickness of 1-10 nm and the iron content smaller than 3 ppm. The graphene slurry prepared by the preparation method of the nano material has good conductivity, and is not agglomerated or layered after being stored for a long time.
Example 2
The carbon nano tube slurry prepared by the preparation method provided by the invention has the specific operation process that:
the raw materials comprise: carbon nano tubes, NMP solvent, dispersant and viscosity reducer.
And discharging air in the premixing tank and the slurry circulation by using a nitrogen seal valve to fill the air with nitrogen, putting 30Kg of dried multi-walled carbon nanotubes and NMP solvent into the premixing tank according to the proportion that the solid content of the multi-walled carbon nanotubes is 5%, adding 1% by mass of dispersing agent and viscosity reducer, and starting a stirring paddle and a diaphragm pump to uniformly mix the slurry, wherein the premixing time is 120 min.
After premixing is finished, the slurry is conveyed into the slurry circulating system through the diaphragm pump, the rotor pump of the slurry circulating system is started after the diaphragm pump for conveying the slurry is closed, the slurry is enabled to sequentially pass through the sand mill, the pressure gauge, the temperature monitor, the electromagnetic flow meter, the 12000GS iron remover and the jacketed condenser pipe, and finally returns to the buffer tank to form a closed circulating process, the flow speed is controlled to be 0.5m in the circulating process3H, pressure 0 MPa.
And starting cooling circulating water of the cooling device, wherein the water inlet temperature is set at 15 ℃, and the flow rate is 10L/min.
The sand mill is started, the volume of the sand mill is 3L, 0.6mm of zirconia medium is needed, the filling rate is 50%, and the sand milling time is 120 min. And D50 values are reduced from initial 40 mu m to 1-2 mu m through a laser particle sizer test, the viscosity is reduced from 12000mpa s to 5000-6000 mpa s through a viscometer test, and the main purpose of the sanding step is to reduce the viscosity of the slurry.
And after the sand mill is closed, the slurry finally returns to the buffer tank to form a closed circulation process through the ultrasonic unit, the pressure gauge, the temperature monitoring meter, the electromagnetic flow meter, the 12000GS iron remover and the jacketed condenser pipe. The flow rate in the circulation process is controlled to be 1m3H, pressure 0 MPa.
An ultrasonic power supply is started to disperse carbon nano tubes in the slurry, the power of the ultrasonic power supply is 3000W, the frequency is 20KHz, an ultrasonic radiation head of an inserted round bar structure is adopted at a radiation end, the material is a magnetic material, the working mode is continuous working, the ultrasonic time is 240min, and the temperature of the slurry is controlled at 30-40 ℃.
Through high-power ultrasonic waves, cavitation effect is generated in the slurry by utilizing the ultrasonic waves, so that some small hole-like defects existing on the tube wall of the multi-walled carbon nanotube can be broken by vibration from the defects to form short fibers, and then the short fibers are dispersed in the medium; and the impact wave with large energy generated by instantaneous explosion of tiny bubbles generated by the cavitation effect acts on the surrounding carbon nanotube clusters, so that the clusters bonded together by Van der Waals force can be torn, and finally the carbon nanotube slurry which has good dispersibility, fluidity and no agglomeration and delamination after long-time storage can be prepared, and the iron content is less than 3 ppm.
Example 3
The preparation method of the invention is used for preparing the nano silicon slurry, and the specific operation process is as follows:
the raw materials comprise: silicon powder and deionized water.
And discharging air in the premixing tank and the slurry circulation through a nitrogen-sealed valve to enable the premixing tank and the slurry circulation to be filled with nitrogen, putting 30Kg of silicon powder and deionized water into the premixing tank according to the proportion that the solid content of the silicon powder is 10 percent, enabling the D50 value of the silicon powder to be 30 mu m, and starting a stirring paddle and a diaphragm pump to enable the slurry to be uniformly mixed, wherein the premixing time is 20 min.
After premixing is finished, the slurry is conveyed into the slurry circulating system through the diaphragm pump, the rotor pump of the slurry circulating system is started after the diaphragm pump for conveying the slurry is closed, the slurry sequentially passes through the sand mill, the ultrasonic unit, the pressure gauge, the temperature monitoring meter, the electromagnetic flow meter, the 12000GS iron remover and the jacketed condenser pipe, and finally returns to the buffer tank to form a closed circulating process, wherein the flow speed is controlled to be 0.5m in the circulating process3H, pressure 0 MPa.
The cooling circulating water of the cooling device is started, the water inlet temperature is set at 10 ℃, and the flow rate is 20L/min.
The sand mill is started, the volume of the sand mill is 3L, a zirconia medium with the thickness of 0.6mm is adopted, and the filling rate is 50%.
The first ultrasonic power supply is started, the power supply outputs 3000W, the frequency is 20KHz, the ultrasonic radiation end adopts an ultrasonic radiation head with a plug-in dumbbell-shaped structure, the material is a magnetic material, and the working mode is continuous working.
And a second ultrasonic power supply is started, the power supply outputs 2000W, the frequency is 40KHz, an ultrasonic radiation head of a plug-in round bar structure is adopted at an ultrasonic radiation end, the material is a magnetic material, and the working mode is continuous working.
And (3) continuously operating the sand mill by the first ultrasonic wave and the second ultrasonic wave for 240min at the same time, so that the nano silicon slurry with the D50 value of less than 100nm can be prepared, and the iron content is less than 3 ppm.
Comparative example 1
The same as example 1 except that: in comparative example 1, the slurry did not flow through a 12000GS iron remover, and the iron content was found to be in the range of 1000 to 3000 ppm.
Comparative example 2
Basically the same as in example 2, except that: in comparative example 2, the slurry did not flow through a 12000GS iron remover, and the iron content was found to be in the range of 1000 to 3000 ppm.
Comparative example 3
Basically the same as in example 3, except that: in comparative example 3, the slurry did not flow through a 12000GS iron remover, and the iron content was found to be in the range of 1000 to 3000 ppm.
The preparation method combines the sand mill with the high-power ultrasonic unit for use, and uses the iron removal device to remove magnetic impurities, so that the efficiency can be improved in the preparation process of the nano material, high-quality and pollution-free nano powder can be prepared, and particularly in the preparation of the two-dimensional material, the prepared two-dimensional material has the advantages of few layers, controllable two-dimensional size, few defects and the like.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents and improvements made within the spirit and principle of the present invention are intended to be included within the scope of the present invention.
Claims (10)
1. The preparation method of the nano material is characterized by comprising the following steps of:
uniformly mixing a certain amount of raw materials and a solvent, and introducing into a buffer tank;
introducing the slurry in the buffer tank into an ultrasonic unit for ultrasonic treatment;
introducing the slurry subjected to ultrasonic treatment into an iron removal device, and returning the slurry into the buffer tank after the slurry flows out of the iron removal device to form slurry circulation;
and obtaining the nano-material slurry after at least one slurry circulation.
2. The method for preparing the nano-material according to claim 1, wherein a certain amount of raw materials and a certain amount of solvent are put into a premixing tank, then a dispersing agent and a viscosity reducer are added for 10-240 min, and the mixture is introduced into the buffer tank after being uniformly mixed.
3. The method for producing nanomaterial according to claim 2, wherein the air in the premix tank is exhausted, and after filling the premix tank with the inert gas, the raw material and the solvent are put into the premix tank;
and discharging the air in the buffer tank, filling inert gas, and introducing the uniformly mixed slurry into the buffer tank.
4. The method for preparing the nano-material according to claim 1, wherein the magnetic induction intensity of the iron removing device is 10000-50000 GS.
5. The method for preparing nano-materials according to claim 1, wherein before ultrasonic treatment, the slurry in the buffer tank is passed into a sand mill for grinding, and the sand mill is connected with the ultrasonic unit in parallel;
the diameter of a sanding medium of the sand mill is 0.1-3 mm, the filling rate is 20-80%, and the sanding time is 1-10 h.
6. The method for preparing the nano-material according to claim 1, wherein the ultrasonic unit comprises an ultrasonic power supply and an ultrasonic radiation end, the output power of the ultrasonic power supply is 1-10 KW, the frequency is 15-100 KHz, and the shape of the ultrasonic radiation end is a round bar structure, a dumbbell structure, a thin rod focusing structure or a porous structure; the ultrasonic time is 1-10 h, and the temperature in the ultrasonic process is 20-80 ℃.
7. The method for preparing the nanomaterial according to claim 1, wherein the temperature of the slurry circulation is 0-100 ℃, the pressure is 0-1 MPa, and the flow rate is 0-10 m3/h。
8. The method for preparing the nano-materials according to claim 1, wherein a cooling device is arranged between the ultrasonic unit and the iron removal device, and the slurry after ultrasonic processing flows through the cooling device and then is introduced into the iron removal device; the temperature of the condensed water of the cooling device is 5-15 ℃, and the flow rate is 0-29L/min.
9. The method for preparing the nano-material according to claim 1, wherein the buffer tank retains 20-80% of the slurry in the slurry circulation process.
10. Nanomaterial obtained by the production method according to any one of claims 1 to 9.
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