CN109292829B - Porous nano CoFe2O4Process for preparing nanoparticles - Google Patents
Porous nano CoFe2O4Process for preparing nanoparticles Download PDFInfo
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- CN109292829B CN109292829B CN201811230296.0A CN201811230296A CN109292829B CN 109292829 B CN109292829 B CN 109292829B CN 201811230296 A CN201811230296 A CN 201811230296A CN 109292829 B CN109292829 B CN 109292829B
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Abstract
The invention belongs to the technical field of photocatalytic materials, and particularly relates to porous nano CoFe2O4Method for preparing nanoparticles using a vacuum treatment tankThe inner wall of the middle part of the tank body is provided with an induction coil; the induction coil is arranged around the supporting disk, and the graphite crucible is arranged on the supporting disk; the center of the bottom of the support plate is hinged to the end of the output shaft of the motor; one side of the supporting disc is rotatably connected with a liquid storage tank, the other side of the supporting disc is hinged with the upper end of a first connecting rod, the lower end of the first connecting rod is connected with the upper end of a second connecting rod through a supporting spring, and the lower end of the second connecting rod is hinged in the middle of the output shaft of the motor. CoFe prepared by the method of the invention2O4Aluminum powder is mixed into the sol, the aluminum powder is melted by high-frequency heating, and the melted aluminum powder heats and volatilizes the organic solvent and the compound template, so that the problem of pore channel collapse caused by overhigh temperature when the compound template is removed by a roasting method is solved, the separation efficiency is high, and the porous nano CoFe is improved2O4The preparation efficiency of (1).
Description
Technical Field
The invention belongs to the technical field of photocatalytic materials, and particularly relates to porous nano CoFe2O4A method for preparing nanoparticles.
Background
With the acceleration of the industrialization process, the energy crisis and the environmental crisis are becoming more serious, and the development of renewable new energy is receiving much attention. Solar energy is used as a clean energy source, is inexhaustible, pollution-free and cheap, can be freely and smoothly utilized by various countries all over the world, and is also the basis of various renewable energy sources such as biomass energy, wind energy, ocean energy, water energy and other energy sources. Governments of various countries pay attention to the development of renewable energy, and the renewable energy is a hot research field for the intense investment of various countries.
The photocatalyst is a semiconductor material necessary for developing and utilizing solar energy. At present, many kinds of semiconductor photocatalysts have been studied by scientists, such as TiO2, CdS, SrTiO3, RuO2, ZnO, Fe2O3 and the like. CoFe2O4As a class of semiconductor photocatalysts, the photocatalyst has the characteristics of good stability, difficult dissolution, environmental friendliness, narrow band gap, rich resources, low application cost and the like, can effectively improve the photocatalytic activity when being compounded with other semiconductors, and is one of the photocatalysts with good application prospects.
CoFe2O4The nano-and porous-transformation is to increase CoFe2O4One of the effective methods for photocatalytic efficiency. Preparation of porous Nano CoFe2O4The template method can be adopted, and the template mainly comprises a micro-emulsion template, an ionic surfactant template, a non-ionic surfactant template, a block copolymer template, a composition template (polyoxyethylene dodecyl ether and polyethylene glycol) and a monodisperse polymer particle template. By sol-gel reaction, CoFe2O4The sol reacts with the template by a secondary valence bond to form a skeleton structure, and then the template is removed by adopting a solvent extraction method or a high-temperature roasting method, so that holes with the size equivalent to that of the template are obtained. However, the preparation of porous nano CoFe using the above conventional template2O4In the process, the template is removed by adopting a roasting method or an extraction method, which has serious defects. When the template is removed by the roasting method, the high temperature for removing the template can cause the collapse of the pore channel, so that the prepared porous nano CoFe2O4The semiconductor photocatalyst has too many surface defects to become electron-hole recombination centers, and the photocatalytic efficiency is reduced. The extraction method is difficult to completely remove the template, so that the porous nano CoFe2O4The purity of the semiconductor photocatalyst is reduced, resulting in a decrease in photocatalytic performance. Therefore, how to prepare the porous nano CoFe with no collapse of pore channels, no defect on the surface, no residue on the template and high specific surface area2O4Semiconductor photocatalysts are an important issue.
Disclosure of Invention
In order to make up the defects of the prior art, the invention provides porous nano CoFe2O4Method for producing nanoparticles of CoFe2O4The aluminum powder is mixed into the sol, the aluminum powder is melted through high-frequency heating, and the melted aluminum powder heats and volatilizes the organic solvent and the compound template, so that the problem of pore canal collapse caused by high temperature of the template to be removed completely when the template is removed by a roasting method is solved, and the separation efficiency is high.
The technical scheme adopted by the invention for solving the technical problems is as follows: the invention relates to a preparation method of porous nanometer CoFe2O4 nanoparticles, which comprises the following steps:
s1: preparing 3-6 parts of ferric bromide, 4-6 parts of aluminum powder, 4-7 parts of cobalt sulfate, 2-3 parts of sublimable compound template, 3-6 parts of organic solvent, 1-2 parts of potassium hydroxide and 2-3 parts of deionized water;
s2: fully mixing ferric bromide and cobalt sulfate, adding half of deionized water to prepare a mixed solution, and mixing potassium hydroxide and the other half of deionized water to prepare an alkaline solution; slowly adding the mixed solution of ferric bromide and cobalt sulfate into the alkaline solution, and stirring and mixing for 2-3 h;
s3: centrifuging the product of S2 to obtain CoFe2O4Sol;
s4: in CoFe2O4Adding an organic solvent, a compound template and aluminum powder into the sol in sequence, wherein the added compound template is any one of p-benzoquinone, melamine, iodine, hexamethylenetetramine, camphor, anthraquinone, naphthalene, anthracene, trioxymethylene and triethylamine hydrochloride, and stirring and mixing uniformly;
s5: the mixture of S4 was calcined and centrifuged.
Preferably, the organic solvent is any one of methanol, ethanol, isopropanol, diethyl ether, isopropyl ether, formic acid, acetic acid and dichloromethane.
Preferably, S5 is performed in a vacuum processing tank, the vacuum processing tank including a tank body, a suction pump, a sealing cover, an induction coil, a support plate, a graphite crucible, a motor, a liquid storage tank, a first connecting rod, a support spring, a second connecting rod, and a controller; the top of the tank body is provided with an air pump, the top of the tank body is provided with a sealing cover which can be opened in a rotating way, and the inner wall of the middle part of the tank body is provided with a plurality of circles of induction coils for eddy current heating; the induction coil is arranged around a supporting plate, the supporting plate is used for placing a graphite crucible, a group of through holes communicated with the inner cavity of the graphite crucible are formed in the bottom of the graphite crucible, the graphite crucible is arranged on the supporting plate, and the graphite crucible is overhead by the supporting plate; the center of the bottom of the supporting disk is hinged to the end head of an output shaft of the motor, and the motor is used for driving the supporting disk to rotate; one side of the supporting plate is rotatably connected with a liquid storage tank, the other side of the supporting plate is hinged with the upper end of a first connecting rod, the lower end of the first connecting rod is connected with the upper end of a second connecting rod through a supporting spring, and the lower end of the second connecting rod is hinged in the middle of the output shaft of the motor; the controller is arranged on the outer wall of the tank body; wherein the content of the first and second substances,
in S5, the mixture in S4 is placed in a graphite crucible, after a sealing cover is closed, a controller controls an air pump to pump the interior of a tank body into a vacuum state, a motor is started, and an induction coil is electrified; firstly, heating and liquefying aluminum powder dispersed in a mixture into aluminum liquid by an induction coil, heating and volatilizing an organic solution and a compound template by the aluminum liquid, and realizing the nano CoFe2O4Separating particles, namely after the organic solution and the compound template are volatilized, discharging the aluminum liquid through a through hole at the bottom of the graphite crucible under the action of centrifugal force and gathering the aluminum liquid into a liquid storage tank; along with the rotation of the supporting disc, the liquid storage tank swings and changes the gravity center of the supporting disc, so that the supporting disc shakes while rotating, the swing amplitude of the supporting disc is controlled through the rotation speed control of the motor, molten aluminum liquid impacts and rolls the mixture, the organic solution and the compound template are fully separated, and the separation efficiency is improved.
Preferably, the inner cavity of the graphite crucible is circular or oval, a group of cast iron balls are placed in the cavity, the bottom surface of the inner cavity of the supporting disc inclines towards one side of the liquid storage tank, molten aluminum liquid conveniently and intensively flows into the liquid storage tank, the deflection angle of the supporting disc is increased, the swinging amplitude of the supporting disc is increased, the molten aluminum liquid impacts and rolls the mixture, the organic solution and the compound template are fully separated, and the separation efficiency is improved.
Preferably, a sliding column is fixedly connected to the upper end of the second connecting rod, a supporting spring is sleeved on the outer ring of the sliding column and made of rubber, two elastic baffle plates are fixedly connected to the lower end of the first connecting rod, the supporting spring is clamped by the two elastic baffle plates, and a group of grooves used for clamping the supporting spring is uniformly formed in the inner side of each elastic baffle plate. The supporting disk is when the swing, when the supporting disk rocks toward one side, and first connecting rod stretches the supporting spring on to the second connecting rod, and the supporting spring of card in the elastic baffle inslot was pulled out originally, and when supporting spring slided to another recess by a recess, first connecting rod vibration and feedback supporting disk to make graphite crucible vibrate, fully separate out organic solution and compound template, improve separation efficiency.
Preferably, the outer ring of the sliding column is provided with a group of arc-shaped grooves corresponding to the grooves of the elastic baffle. Supporting spring is stretched and is slided into the arc wall along the slip post in receiving the extrusion of elasticity baffle, when certain hoop of supporting spring falls into the arc wall, it is built on stilts with the slip post to be equivalent to elasticity baffle, is drawn by supporting spring and becomes to take off the sky in the twinkling of an eye, realizes the vibration of first link, and first link vibration feeds back the supporting disk to make graphite crucible vibration, fully separate out organic solution and compound template, improve separation efficiency.
Preferably, the slip post upper end is equipped with the jack, the middle part of first connecting rod lower extreme is equipped with the bracing piece, bracing piece slidable mounting is in the jack of slip post, and the outside of bracing piece is crisscross to be set up a set of semicircle lug, be equipped with the fixture block that corresponds the semicircle lug setting on the slip post, the fixture block can be followed the slip post and outwards slided out, set up two dental plates relatively in the arc wall, the interval of two dental plate ends is less than supporting spring's line footpath. When a certain hoop of the supporting spring falls into the arc-shaped groove, the convex block of the corresponding supporting rod pushes the fixture block to slide outwards, the supporting spring is extruded into an oval shape, the contracted hoop is clamped into the dental lamina, the supporting spring and the elastic baffle are completely separated through the action of the supporting rod and the pressing plate, the supporting spring is clamped into the groove of the elastic baffle and falls into the arc-shaped groove in an alternative process, the friction force of the outer wall of the supporting spring is reduced, the loss of vibration energy is reduced, and the generated vibration is fully used for separating the nanometer CoFe2O4And (4) particles are formed, so that the separation efficiency is improved.
Preferably, the top of the interior of the tank body is provided with an ultrasonic generator. When the generated ultrasonic waves act on a plurality of aluminum liquids, the aluminum liquids vibrate, the circulation of the aluminum liquids in the mixture is increased, the aluminum liquids can fully heat the organic solutions and the compound templates, and the separation efficiency is improved.
The invention has the following beneficial effects:
1. the invention discloses a preparation method of porous nano CoFe2O4 nano particles, which is implemented by adding CoFe2O4The aluminum powder is mixed in the sol, the aluminum powder is melted by high-frequency heating, and the melted aluminum powder heats and volatilizes the organic solvent and the compound template, so that the problem of pore canal collapse caused by high temperature of the template to be removed completely when the template is removed by a roasting method is solved, and the separation efficiency is high.
2. According to the preparation method of the porous nano CoFe2O4 nano particles, a vacuum treatment tank is used, the swing amplitude of a support plate is controlled by controlling the rotating speed of a motor, so that molten aluminum liquid can impact and roll a mixture, the organic solution and a compound template are fully separated, and the separation efficiency is improved.
3. The invention relates to a preparation method of porous nanometer CoFe2O4 nanoparticles, which uses a vacuum treatment tank, wherein a support spring of the vacuum treatment tank is stretched along a sliding column and is extruded by an elastic baffle plate to slide into an arc-shaped groove, when a certain hoop of the support spring falls into the arc-shaped groove, the elastic baffle plate and the sliding column are overhead, the support spring is pulled to become instant void, vibration of a first connecting rod is realized, the first connecting rod vibrates and feeds back to a support plate, so that a graphite crucible vibrates, the flowing efficiency of aluminum liquid in a mixture is realized, an organic solution and a compound template are fully heated, and the separation efficiency is improved.
Drawings
The invention will be further explained with reference to the drawings.
FIG. 1 is a flow chart of a method of the present invention;
FIG. 2 is a front view of the vacuum processing tank of the present invention;
FIG. 3 is an enlarged view of a portion E of FIG. 2;
FIG. 4 is a cross-sectional view A-A of FIG. 3;
in the figure: the device comprises a tank body 1, an air suction pump 11, a sealing cover 12, an induction coil 2, a sliding column 21, an elastic baffle 22, an arc-shaped groove 23, a support rod 24, a fixture block 25, a dental plate 26, an ultrasonic generator 31, a support plate 3, a graphite crucible 4, a motor 5, a liquid storage tank 6, a first connecting rod 7, a support spring 8 and a second connecting rod 9.
Detailed Description
In order to make the technical means, the creation characteristics, the achievement purposes and the effects of the invention easy to understand, the invention is further described with the specific embodiments.
As shown in FIGS. 1 to 4, the preparation method of the porous nano CoFe2O4 nanoparticles comprises the following steps:
s1: preparing 3-6 parts of ferric bromide, 4-6 parts of aluminum powder, 4-7 parts of cobalt sulfate, 2-3 parts of sublimable compound template, 3-6 parts of organic solvent, 1-2 parts of potassium hydroxide and 2-3 parts of deionized water;
s2: fully mixing ferric bromide and cobalt sulfate, adding half of deionized water to prepare a mixed solution, and mixing potassium hydroxide and the other half of deionized water to prepare an alkaline solution; slowly adding the mixed solution of ferric bromide and cobalt sulfate into the alkaline solution, and stirring and mixing for 2-3 h;
s3: centrifuging the product of S2 to obtain CoFe2O4Sol;
s4: in CoFe2O4Adding an organic solvent, a compound template and aluminum powder into the sol in sequence, wherein the added compound template is any one of p-benzoquinone, melamine, iodine, hexamethylenetetramine, camphor, anthraquinone, naphthalene, anthracene, trioxymethylene and triethylamine hydrochloride, and stirring and mixing uniformly;
s5: the mixture of S4 was calcined and centrifuged.
In one embodiment of the present invention, the organic solvent is any one of methanol, ethanol, isopropanol, diethyl ether, isopropyl ether, formic acid, acetic acid, and dichloromethane.
As an embodiment of the present invention, S5 is performed in a vacuum processing tank including a tank body 1, a suction pump 11, a sealing cover 12, an induction coil 2, a support plate 3, a graphite crucible 4, a motor 5, a liquid storage tank 6, a first link 7, a support spring 8, a second link 9, and a controller; the top of the tank body 1 is provided with an air pump 11, the top of the tank body 1 is provided with a sealing cover 12 which can be opened in a rotating way, and the inner wall of the middle part of the tank body 1 is provided with a plurality of circles of induction coils 2 for eddy current heating; the induction coil 2 is arranged around a supporting plate 3, the supporting plate 3 is used for placing a graphite crucible 4, a group of through holes communicated with the inner cavity of the graphite crucible 4 are formed in the bottom of the graphite crucible 4, the graphite crucible 4 is installed on the supporting plate 3, and the graphite crucible 4 is overhead by the supporting plate 3; the center of the bottom of the supporting disk 3 is hinged to the end head of an output shaft of a motor 5, and the motor 5 is used for driving the supporting disk 3 to rotate; one side of the supporting plate 3 is rotatably connected with a liquid storage tank 6, the other side of the supporting plate 3 is hinged with the upper end of a first connecting rod 7, the lower end of the first connecting rod 7 is connected with the upper end of a second connecting rod 9 through a supporting spring 8, and the lower end of the second connecting rod 9 is hinged with the middle part of an output shaft of the motor 5; the controller is arranged on the outer wall of the tank body 1; wherein the content of the first and second substances,
in S5, the mixture of S4 is put into the graphite crucible 4, after the sealing cap 12 is closed, the controller controls the suction pump 11 to vacuumize the tank 1, the motor 5 is turned on and the induction coil 2 is energized; firstly, the induction coil 2 heats and liquefies the aluminum powder dispersed in the mixture into aluminum liquid, and the aluminum liquid heats and volatilizes the organic solution and the compound template to realize the nano CoFe2O4Separating particles, namely after the organic solution and the compound template are volatilized, discharging the aluminum liquid through a through hole at the bottom of the graphite crucible 4 under the action of centrifugal force and gathering the aluminum liquid into a liquid storage tank 6; along with the rotation of the supporting disc 3, the liquid storage tank 6 swings and changes the gravity center of the supporting disc 3, so that the supporting disc 3 swings while rotating, the swing amplitude of the supporting disc 3 is controlled through the rotation speed control of the motor 5, molten aluminum liquid is enabled to impact and roll the mixture, the organic solution and the compound template are fully separated, and the separation efficiency is improved.
As an embodiment of the invention, the inner cavity of the graphite crucible 4 is circular or oval, a group of cast iron balls are placed in the inner cavity, the bottom surface of the inner cavity of the support plate 3 inclines towards one side of the liquid storage tank 6, so that molten aluminum liquid can flow into the liquid storage tank 6 in a centralized manner, the inclination angle of the support plate 3 is increased, the swing amplitude of the support plate 3 is increased, the molten aluminum liquid can impact and roll the mixture, the organic solution and the compound template are fully separated, and the separation efficiency is improved.
As an embodiment of the present invention, the upper end of the second connecting rod 9 is fixedly connected with a sliding column 21, the outer ring of the sliding column 21 is sleeved with a supporting spring 8, the supporting spring 8 is made of rubber, the lower end of the first connecting rod 7 is fixedly connected with two elastic baffles 22, the supporting spring 8 is clamped by the two elastic baffles 22, and a group of grooves for clamping the supporting spring 8 is uniformly arranged on the inner side of each elastic baffle 22. Support disk 3 is when the swing, when support disk 3 rocks toward one side, first connecting rod 7 stretches the supporting spring 8 on the second connecting rod 9, and the supporting spring 8 of card at elastic baffle 22 inslot is pulled out originally, and when supporting spring 8 slided to another recess by a recess, supporting disk 3 was fed back in the vibration of first connecting rod 7 to make 4 vibrations of graphite crucible, fully separate out organic solution and compound template, improve separation efficiency.
In one embodiment of the present invention, a set of arc-shaped slots 23 is disposed on the outer ring of the sliding column 21 corresponding to the grooves of the elastic baffle 22. Supporting spring 8 is stretched and is slided into arc 23 by the extrusion of elastic baffle 22 along sliding column 21, when a certain hoop of supporting spring 8 falls into arc 23, it is built on stilts with sliding column 21 to be equivalent to elastic baffle 22, draw by supporting spring 8 and become to come to nothing in the twinkling of an eye, realize the vibration of first connecting rod 7, first connecting rod 7 vibrates and feeds back to supporting disk 3 to make graphite crucible 4 vibrate, fully separate out organic solution and compound template, improve separation efficiency.
As an embodiment of the present invention, the upper end of the sliding column 21 is provided with a jack, the middle part of the lower end of the first connecting rod 7 is provided with a supporting rod 24, the supporting rod 24 is slidably installed in the jack of the sliding column 21, a group of semicircular protrusions are staggered on the outer side of the supporting rod 24, the sliding column 21 is provided with a fixture block 25 corresponding to the semicircular protrusions, the fixture block 25 can slide out from the sliding column 21, two tooth plates 26 are oppositely arranged in the arc-shaped groove 23, and the distance between the ends of the two tooth plates 26 is smaller than the wire diameter of the supporting spring 8. When a certain hoop of the supporting spring 8 falls into the arc-shaped groove 23, the convex block of the corresponding supporting rod 24 pushes the fixture block 25 to slide outwards, the supporting spring 8 is extruded into an oval shape, the contracted hoop is clamped into the dental lamina 26, and the supporting is arrangedThe action of the rod 24 and the pressing plate 26 makes the supporting spring 8 and the elastic baffle 22 completely separated, so that the friction force of the outer wall of the supporting spring 8 is reduced and the loss of vibration energy is reduced in the alternative process that the supporting spring 8 is clamped into the groove of the elastic baffle 22 and falls into the arc-shaped groove 23, and the generated vibration is fully used for separating the nano CoFe2O4And (4) particles are formed, so that the separation efficiency is improved.
In one embodiment of the present invention, an ultrasonic generator 31 is disposed at the top of the inside of the tank 1. When the generated ultrasonic waves act on a plurality of aluminum liquids, the aluminum liquids vibrate, the circulation of the aluminum liquids in the mixture is increased, the aluminum liquids can fully heat the organic solutions and the compound templates, and the separation efficiency is improved.
When in use, the mixture of S4 is placed in the graphite crucible 4, after the sealing cover 12 is closed, the air pump 11 is controlled by the controller to pump the tank body 1 into a vacuum state, the motor 5 is started, and the induction coil 2 is electrified; firstly, the induction coil 2 heats and liquefies the aluminum powder dispersed in the mixture into aluminum liquid, and the aluminum liquid heats and volatilizes the organic solution and the compound template to realize the nano CoFe2O4Separating particles, namely after the organic solution and the compound template are volatilized, discharging the aluminum liquid through a through hole at the bottom of the graphite crucible 4 under the action of centrifugal force and gathering the aluminum liquid into a liquid storage tank 6; along with the rotation of the supporting disc 3, the liquid storage tank 6 swings and changes the gravity center of the supporting disc 3, so that the supporting disc 3 swings while rotating, and the swing amplitude of the supporting disc 3 is controlled by controlling the rotating speed of the motor 5, so that molten aluminum liquid impacts and rolls on a mixture, the organic solution and a compound template are fully separated, and the separation efficiency is improved;
when the supporting disk 3 rocks toward one side, first connecting rod 7 stretches supporting spring 8 on to second connecting rod 9, the supporting spring 8 that originally the card was in elastic baffle 22 inslot is pulled out, when supporting spring 8 slided to another recess by a recess, supporting spring 8 is stretched and is slided into arc wall 23 by elastic baffle 22's extrusion along slip post 21, when a certain hoop of supporting spring 8 falls into arc wall 23, it is built on stilts equivalent to elastic baffle 22 and slip post 21, it becomes empting in the twinkling of an eye to be drawn by supporting spring 8, realize the vibration of first connecting rod 7, first connecting rod 7 vibrates and feeds back to supporting disk 3, thereby make graphite crucible 4 vibrate, fully separate out organic solution and compound template, improve separation efficiency.
While the invention has been described with reference to specific embodiments, it will be understood by those skilled in the art that various changes may be made and equivalents may be substituted without departing from the scope of the invention. In addition, many modifications may be made to adapt a particular situation or material to the teachings of the invention without departing from its scope. Therefore, it is intended that the invention not be limited to the particular embodiment disclosed, but that the invention will include all embodiments falling within the scope of the appended claims.
Claims (3)
1. Porous nano CoFe2O4A method for preparing nanoparticles, characterized in that the method comprises the steps of:
s1: preparing 3-6 parts of ferric bromide, 4-6 parts of aluminum powder, 4-7 parts of cobalt sulfate, 2-3 parts of sublimable compound template, 3-6 parts of organic solvent, 1-2 parts of potassium hydroxide and 2-3 parts of deionized water;
s2: fully mixing ferric bromide and cobalt sulfate, adding half of deionized water to prepare a mixed solution, and mixing potassium hydroxide and the other half of deionized water to prepare an alkaline solution; slowly adding the mixed solution of ferric bromide and cobalt sulfate into the alkaline solution, and stirring and mixing for 2-3 h;
s3: centrifuging the product of S2 to obtain CoFe2O4Sol;
s4: in CoFe2O4Adding organic solvent, compound template and aluminium powder into sol in turn, and adding CoFe2O4Aluminum powder is mixed in the sol, the aluminum powder is melted by high-frequency heating, the melted aluminum powder heats and volatilizes the organic solvent and the compound template, the problem that the pore channel collapses because the temperature of the template to be removed is high when the template is removed by a roasting method is solved, and the added compound template is any one of p-benzoquinone, melamine, iodine, hexamethylenetetramine, camphor, anthraquinone, naphthalene, anthracene, trioxymethylene and triethylamine hydrochlorideSeed planting, stirring and mixing uniformly;
s5: roasting the mixture of S4, and centrifuging;
the centrifugal separation operation in the step S5 is performed in a vacuum treatment tank, wherein the vacuum treatment tank comprises a tank body (1), an air pump (11), a sealing cover (12), an induction coil (2), a supporting disk (3), a graphite crucible (4), a motor (5), a liquid storage tank (6), a first connecting rod (7), a supporting spring (8), a second connecting rod (9) and a controller; the top of the tank body (1) is provided with an air pump (11), the top of the tank body (1) is provided with a sealing cover (12) which can be opened in a rotating way, and the inner wall of the middle part of the tank body (1) is provided with a plurality of circles of induction coils (2) for eddy current heating; the induction coil (2) is arranged around the supporting disc (3), the supporting disc (3) is used for placing a graphite crucible (4), a group of through holes communicated with the inner cavity of the graphite crucible (4) are formed in the bottom of the graphite crucible (4), the graphite crucible (4) is installed on the supporting disc (3), and the graphite crucible (4) is overhead by the supporting disc (3); the center of the bottom of the supporting disk (3) is hinged to the end head of an output shaft of the motor (5), and the motor (5) is used for driving the supporting disk (3) to rotate; one side of the supporting plate (3) is rotatably connected with a liquid storage tank (6), the other side of the supporting plate (3) is hinged with the upper end of a first connecting rod (7), the lower end of the first connecting rod (7) is connected with the upper end of a second connecting rod (9) through a supporting spring (8), and the lower end of the second connecting rod (9) is hinged with the middle part of an output shaft of the motor (5); the controller is arranged on the outer wall of the tank body (1); in S5, the mixture of S4 is placed in a graphite crucible (4), after a sealing cover (12) is closed, an air pump (11) pumps the interior of a tank body (1) to be in a vacuum state, a motor (5) is started, and an induction coil (2) is electrified;
the upper end of the second connecting rod (9) is fixedly connected with a sliding column (21), the outer ring of the sliding column (21) is sleeved with a supporting spring (8), the supporting spring (8) is made of rubber, the lower end of the first connecting rod (7) is fixedly connected with two elastic baffles (22), the supporting spring (8) is clamped by the two elastic baffles (22), and a group of grooves used for clamping the supporting spring (8) are uniformly formed in the inner side of each elastic baffle (22); a group of arc-shaped grooves (23) are formed in the outer ring of the sliding column (21) corresponding to the grooves of the elastic baffle (22); the upper end of the sliding column (21) is provided with a jack, the middle part of the lower end of the first connecting rod (7) is provided with a supporting rod (24), the supporting rod (24) is slidably mounted in the jack of the sliding column (21), the outer side of the supporting rod (24) is provided with a group of semicircular lugs in a staggered manner, a clamping block (25) arranged corresponding to the semicircular lugs is arranged on the sliding column (21), the clamping block (25) can slide out from the inside of the sliding column (21), two tooth plates (26) are oppositely arranged in the arc-shaped groove (23), and the distance between the ends of the two tooth plates (26) is smaller than the wire diameter of the supporting spring (8); the top inside the tank body (1) is provided with an ultrasonic generator (31).
2. Porous nano CoFe according to claim 12O4The preparation method of the nano particles is characterized by comprising the following steps: the organic solvent is any one of methanol, ethanol, isopropanol, diethyl ether, isopropyl ether, formic acid, acetic acid and dichloromethane.
3. Porous nano CoFe according to claim 12O4The preparation method of the nano particles is characterized by comprising the following steps: the inner cavity of the graphite crucible (4) is circular or oval, a group of cast iron balls are placed in the cavity, and the bottom surface of the inner cavity of the supporting disc (3) inclines to one side of the liquid storage tank (6).
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| CN105521789B (en) * | 2016-01-04 | 2019-05-14 | 南京林业大学 | A kind of porous nano BiFeO3Preparation method |
| CN105502286B (en) * | 2016-01-04 | 2018-05-15 | 南京林业大学 | A kind of porous nano NiFe2O4Preparation method |
| CN105664950B (en) * | 2016-01-04 | 2018-05-15 | 南京林业大学 | A kind of porous nano ZnFe2O4Preparation method |
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