阅读说明：本技术 一种磁性四氧化三铁纳米粒子的绿色制备方法 (Green preparation method of magnetic ferroferric oxide nanoparticles ) 是由 董华平 徐嘉逸 于 2020-07-09 设计创作，主要内容包括：本发明公开了一种磁性四氧化三铁纳米粒子的绿色制备方法,属于材料制备技术领域,包括以下步骤,S1：先用无氧水配置20～50mmol/L的吗啉丙磺酸溶液,且溶液的pH=7～9；S2：通过抽气管将内反应罐抽成真空状态,然后通过抽气管向内反应罐内通入微氧气体,且同步挤压密封盖一侧上方设置的滴加试管向反应罐内加入FeSO4溶液；S3：通过密封盖另一侧设置的滴加试管向反应罐内加入Fe(II),且Fe(II)的浓度为1～3mmol/L；S4：振荡驱动装置的驱动电机会驱动反应罐转动,且驱动电机的转速为100～300rpm；同时振荡驱动装置会对反应罐进行振荡,振荡时间为12h；本发明具有环保、粒子均匀等优点。(The invention discloses a green preparation method of magnetic ferroferric oxide nanoparticles, which belongs to the technical field of material preparation and comprises the following steps of S1: firstly, preparing a 20-50 mmol/L morpholine propanesulfonic acid solution by using oxygen-free water, wherein the pH of the solution is = 7-9; s2: pumping the inner reaction tank into a vacuum state through an exhaust tube, introducing micro-oxygen gas into the inner reaction tank through the exhaust tube, and synchronously extruding a dropping test tube arranged above one side of a sealing cover to add FeSO4 solution into the reaction tank; s3: adding Fe (II) into the reaction tank through a dropping test tube arranged on the other side of the sealing cover, wherein the concentration of the Fe (II) is 1-3 mmol/L; s4: a driving motor of the oscillation driving device drives the reaction tank to rotate, and the rotating speed of the driving motor is 100-300 rpm; meanwhile, the oscillation driving device can oscillate the reaction tank for 12 h; the invention has the advantages of environmental protection, uniform particles and the like.)

1. A green preparation method of magnetic ferroferric oxide nanoparticles is characterized by comprising the following steps:

s1: firstly, preparing a 20-50 mmol/L morpholine propanesulfonic acid solution with pH = 7-9 by using oxygen-free water, then dropwise adding the prepared morpholine propanesulfonic acid solution into a reaction tank (2) through a dropper, and then sealing through a sealing cover (5);

s2: pumping the inner reaction tank (2) into a vacuum state by using a suction pump through a suction pipe (4), introducing micro-oxygen gas into the inner reaction tank (2) through the suction pipe (4), and synchronously extruding a dropping test tube (3) arranged above one side of a sealing cover (5) to add FeSO4 solution into the reaction tank (2);

s3: adding Fe (II) into the reaction tank (2) through a dropping test tube (3) arranged on the other side of the sealing cover (5), wherein the concentration of Fe (II) is 1-3 mmol/L, and synchronously sealing the dropping test tube (3);

s4: a driving motor (61) of the oscillation driving device (6) can drive the reaction tank (2) to rotate, and the rotating speed of the driving motor (61) is 100-300 rpm; meanwhile, the oscillation driving device (6) can oscillate the reaction tank (2), and the oscillation time is 12 h; obtaining the black magnetic ferroferric oxide nano particles.

2. The green preparation method of the magnetic ferroferric oxide nanoparticles according to claim 1, characterized by comprising the following steps: the micro-oxygen gas is prepared by 1-3% of oxygen and 97-99% of nitrogen in proportion.

3. The green preparation method of the magnetic ferroferric oxide nanoparticles according to claim 1, characterized by comprising the following steps: a fixed tank (1) is sleeved outside the reaction tank (2), and an oscillation driving device (6) is arranged in the fixed tank (1); the oscillation driving device (6) comprises a driving motor (61), a rotating magnetic disk (62), a fixed inner cylinder (63), a magnetic sliding rod (64), an elastic extrusion bag (65), a fixed sliding seat (66), a sliding rod (67) and an expansion bag (68); a driving motor (61) is fixed in the bottom end of the fixed tank (1), and the output end of the driving motor (61) is connected to the bottom end wall of the reaction tank (2); the outer circumferential wall of the reaction tank (2) is provided with an elastic film layer; the outer wall of the output end of the driving motor (61) is sleeved with a rotating magnetic disk (62), and the rotating magnetic disk (62) is positioned at the bottom end of the reaction tank (2); the rotating magnetic disk (62) is uniformly divided into a plurality of magnetic pole blocks (7), and the magnetism between two adjacent magnetic pole blocks (7) is opposite; a fixed inner cylinder (63) is fixedly arranged on the inner wall of the fixed tank (1), and an extrusion cavity (631) is formed in the fixed inner cylinder (63); a plurality of magnetic sliding rods (64) are uniformly inserted in the circumferential direction of the outer side wall of the bottom end of the extrusion cavity (631) in a sliding and inserting mode, and the outer end portions of the magnetic sliding rods (64) are aligned with the outer ring wall of the rotating magnetic disk (62); a plurality of elastic extrusion bags (65) are uniformly arranged in the extrusion cavity (631), and the outer walls of the elastic extrusion bags (65) are connected with the end parts of the magnetic sliding rods (64); a plurality of fixed sliding seats (66) are uniformly arranged in the vertical direction and the circumferential direction of the outer cavity wall of the extrusion cavity (631), and sliding rods (67) are arranged in the fixed sliding seats (66) in a sliding manner; the end part of the sliding rod (67) is in sliding and pressing contact with the outer wall of the reaction tank (2), and the inner end part of the sliding rod (67) is positioned in the pressing cavity (631); a plurality of expansion bags (68) are fixed in the extrusion cavity (631), and the expansion bags (68) are communicated with the elastic extrusion bag (65) through air ducts (69); the outer walls of the plurality of expansion bags (68) are connected with sliding rods (67).

4. The green preparation method of the magnetic ferroferric oxide nanoparticles according to claim 2, characterized in that; a magnetic pole block (7) is arranged at the end part of each magnetic slide bar (64), and the magnetic poles (7) of two adjacent magnetic slide bars (64) are opposite in magnetism; the distance between two adjacent magnetic sliding rods (64) is larger than the width of a magnetic pole block (7) arranged on the rotary magnetic disk (62), and the width of the magnetic pole block (7) on the rotary magnetic disk (62) is larger than the width of the magnetic sliding rods (64).

5. The green preparation method of the magnetic ferroferric oxide nanoparticles according to claim 4, characterized by comprising the following steps: the end parts of two adjacent sliding rods (67) in the vertical direction are connected with an adhesive layer (8), and the outer wall of the adhesive layer (8) is provided with a burr belt (81); the outer wall of the reaction tank (2) is provided with a convex wool layer (9), and the convex wool layer (9) is in mutual bonding contact with the burr belt (81).

6. The green preparation method of the magnetic ferroferric oxide nanoparticles according to claim 5, characterized by comprising the following steps: a plurality of L-shaped fixing rods (10) are fixedly arranged on the outer wall of the top end of the reaction tank (2) in the circumferential direction, and the L-shaped fixing rods (10) are in rotating contact with the bottom end of the sealing cover (5); the bottom end of the sealing cover (5) is evenly provided with a plurality of cavity elastic layers (11) at intervals, and the cavity elastic layers (11) are in rotating extrusion contact with the L-shaped fixing rod (10).

7. The green preparation method of the magnetic ferroferric oxide nanoparticles according to claim 6, characterized by comprising the following steps: the outer wall of the air suction pipe (4) is wrapped with an elastic expansion film (12), and a plurality of vibration bulges (13) are fixed on the outer wall of the elastic expansion film (12); a clearance cavity (14) is formed between the elastic expansion film (12) and the outer wall of the exhaust tube (4); the plurality of cavity elastic layers (11) are communicated with the clearance cavity (14) through air guide grooves (51).

Technical Field

The invention belongs to the technical field of functional material preparation, and particularly relates to a green preparation method of magnetic ferroferric oxide nanoparticles.

Background

The magnetic ferroferric oxide nano material is a special nano material, has the basic characteristics of a common nano material, such as size effect, surface effect, quantum effect, macroscopic quantum tunnel effect and the like, and simultaneously has special superparamagnetism and enzyme-like activity, and is widely applied to the aspects of high-density information storage, nuclear magnetic resonance imaging, tissue drug release and treatment, cell marking and classification, biological product separation, immunoassay and the like at present. Based on the superparamagnetism characteristic, the magnetic separation adsorbent can be used for magnetic separation to realize the purpose of rapid recovery and is used as an adsorption carrier in the magnetic separation.

The existing method for preparing the magnetic ferroferric oxide nano particles mainly comprises a chemical method, a physical method and a biological method, and the prepared magnetic ferroferric oxide nano material has the advantages of smaller particle size, good magnetism and large specific surface area.

Chinese patent discloses a preparation method of ferroferric oxide magnetic nanoparticles, wherein the application number is 2014107387316, the mol ratio calculation is carried out, namely the proportion of Fe2+ salt to Fe3+ salt is 1.2-1.4: 2, the Fe2+ salt and the Fe3+ salt are added into distilled water, polyethylene glycol is added, the temperature is controlled to be 30-50 ℃ under the ultrasonic condition for reaction for 5-10 min, the pH of the obtained reaction liquid is adjusted to be 9-10 by sodium hydroxide aqueous solution with the mass percentage concentration of 20%, the ultrasonic reaction is continued for 15-20 min, the obtained reaction liquid is subjected to magnetic separation by a magnet, and then the reaction liquid is washed by ethanol for 3-5 times, so that the ferroferric oxide magnetic nanoparticles are obtained.

The above patent can prepare ferroferric oxide magnetic nanoparticles; however, some methods need to add sodium hydroxide aqueous solution for pH adjustment and polyethylene glycol reducing agent, which leads to higher cost of the production method and easy environmental pollution caused by the generated waste liquid; meanwhile, the existing oscillating device is difficult to uniformly precipitate and prepare the produced magnetic ferroferric oxide nano particles, so that the efficient and uniform preparation and production of the magnetic ferroferric oxide nano particles are influenced.

Disclosure of Invention

In order to make up for the defects of the prior art, the invention provides the green preparation method of the magnetic ferroferric oxide nano particles, which is mainly used for solving the problems that the existing production method has higher cost and the generated waste liquid is easy to cause environmental pollution; meanwhile, the existing oscillating device is difficult to uniformly precipitate and prepare the produced magnetic ferroferric oxide nano particles, so that the efficient and uniform preparation and production of the magnetic ferroferric oxide nano particles are influenced.

The technical scheme adopted by the invention for solving the technical problems is as follows: the invention relates to a green preparation method of magnetic ferroferric oxide nanoparticles, which comprises the following steps:

s1: firstly, preparing a 20-50 mmol/L morpholine propanesulfonic acid solution with pH = 7-9 by using oxygen-free water, then dropwise adding the prepared morpholine propanesulfonic acid solution into a reaction tank through a dropper, and then sealing through a sealing cover;

s2: pumping the inner reaction tank into a vacuum state by using a suction pump through a suction pipe, introducing micro-oxygen gas into the inner reaction tank through the suction pipe, and synchronously extruding a dropwise adding test tube arranged above one side of a sealing cover to add FeSO4 solution into the reaction tank; the FeSO4 solution is added under the micro-oxygen gas environment, so that the micro-oxygen gas can play a role in protecting the FeSO4 solution;

s3: adding Fe (II) into the reaction tank through a dropping test tube arranged on the other side of the sealing cover, wherein the concentration of the Fe (II) is 1-3 mmol/L, and synchronously sealing the dropping test tube; by adding the coordination of Fe (II) and the morpholine propanesulfonic acid, the morpholine propanesulfonic acid can play a role in buffering and protecting Fe (II), and no additional reagent is needed to be added, so that the method has the advantages of green pollutants, low cost, uniform particles and easiness in amplification production;

s4: a driving motor of the oscillation driving device drives the reaction tank to rotate, and the rotating speed of the driving motor is 100-300 rpm; meanwhile, the oscillation driving device can oscillate the reaction tank for 12 h; obtaining the black magnetic ferroferric oxide nano particles.

Preferably, the micro-oxygen gas is prepared by 1-3% of oxygen and 97-99% of nitrogen in proportion; the method adopts low-content micro-oxygen gas, the gas in the reaction tank only contains 1-3% of oxygen and 97-99% of nitrogen, and the nitrogen content is high, so that the protection effect can be achieved, and the phenomenon that black magnetic ferroferric oxide nano particles are difficult to form efficiently due to the influence of other gases contained in the reaction tank is reduced.

Preferably, a fixed tank is sleeved outside the reaction tank, and an oscillation driving device is arranged in the fixed tank; the oscillation driving device comprises a driving motor, a rotating magnetic disk, a fixed inner cylinder, a magnetic sliding rod, an elastic extrusion bag, a fixed sliding seat, a sliding rod and an expansion bag; a driving motor is fixed in the bottom end of the fixed tank, and the output end of the driving motor is connected to the bottom end wall of the reaction tank; the circumferential outer wall of the reaction tank is provided with an elastic film layer; the outer wall of the output end of the driving motor is sleeved with a rotating magnetic disk, and the rotating magnetic disk is positioned at the bottom end of the reaction tank; the rotating magnetic disk is uniformly divided into a plurality of magnetic pole blocks, and the magnetism between two adjacent magnetic pole blocks is opposite; a fixed inner cylinder is fixedly arranged on the inner wall of the fixed tank, and an extrusion cavity is formed in the fixed inner cylinder; a plurality of magnetic slide bars are uniformly inserted in the circumferential direction of the outer side wall of the bottom end of the extrusion cavity in a sliding manner, and the outer end parts of the magnetic slide bars are aligned with the outer ring wall of the rotating magnetic disk; a plurality of elastic extrusion bags are uniformly arranged in the extrusion cavity, and the outer walls of the elastic extrusion bags are connected with the end parts of the magnetic sliding rods; a plurality of fixed sliding seats are uniformly arranged in the vertical direction and the circumferential direction of the outer cavity wall of the extrusion cavity, and sliding rods are arranged in the fixed sliding seats in a sliding manner; the end part of the sliding rod is in sliding and extruding contact with the outer wall of the reaction tank, and the inner end part of the sliding rod is positioned in the extruding cavity; a plurality of expansion bags are fixed in the extrusion cavity and are communicated with the elastic extrusion bag through air ducts; the outer walls of the expansion bags are connected with sliding rods;

when the device works, when the solution in the reaction tank needs to be subjected to rotary oscillation reaction, the control unit can control the driving motor to rotate, the driving motor can drive the reaction tank to rotate in the fixed tank, the sealing cover is in a fixed state at the same time, the rotation of the driving motor can drive the rotary magnetic disk to rotate, the magnetism of one magnetic pole block can play a role in repelling the magnetic slide rod when the rotary magnetic disk rotates, so that the magnetic slide rod can slide and extrude an elastic extrusion bag arranged in the fixed inner tank, the gas in the elastic extrusion bag can enter a plurality of expansion bags arranged in the vertical direction through the air duct to expand the expansion bags, the expansion bags can push the slide rods to slide out of the fixed slide seat, the extension of the plurality of slide rods arranged in the vertical direction can play a role in elastic rapping on the outer wall of the reaction tank, an elastic film layer arranged on the outer wall of the reaction tank can be transmitted to the solution in the reaction tank to generate, the internal solution can be accelerated to react quickly to generate magnetic ferroferric oxide nano particles which are deposited at the bottom end of the reaction tank, when the magnetism of the magnet block on the rotating magnetic disk is separated from the repulsion of the magnetic slide rod, the restoring force of the elastic extrusion bag can push out the magnetic slide rod, and simultaneously gas in the expansion bag is pumped out, so that the slide rod is separated from the extrusion vibration of the outer wall of the reaction tank; meanwhile, the magnetic adsorption force on the rotating magnetic disk can adsorb the precipitated magnetic ferroferric oxide nanoparticles to the bottom end of the reaction tank, so that the phenomenon that the magnetic ferroferric oxide nanoparticles are broken or crushed due to the fact that the magnetic ferroferric oxide nanoparticles generated by the precipitation reaction are fragile when the reaction tank is oscillated is effectively prevented, and the forming uniformity and stability of the magnetic ferroferric oxide nanoparticles are influenced; when the gas stored in the elastic extrusion bag is pressurized, the expansion of the plurality of expansion bags arranged in the vertical direction can be met; meanwhile, the expansion deformation of the expansion bag adjacent to the elastic extrusion bag is large, so that the solvent at the layered part of the precipitate and the solution can be fully oscillated and reversed.

Preferably, a magnetic pole block is arranged at the end part of each magnetic slide bar, and the magnetic poles of the magnetic pole blocks of two adjacent magnetic slide bars are opposite in magnetism; the distance between two adjacent magnetic slide bars is greater than the width of a magnetic pole block arranged on the rotating magnetic disk, and the width of the magnetic pole block on the rotating magnetic disk is greater than the width of the magnetic slide bars; when the magnetic disk rotates, the S pole of the magnetic pole block of the rotating magnetic disk corresponds to the S pole of one of the magnetic slide bars, repulsive force is generated to the magnetic pole slide bars, and the magnetic slide bars can extrude the elastic extrusion bag; the distance between two adjacent magnetic slide bars is larger than the width of a magnetic pole block arranged on the rotating magnetic disk, so that the phenomenon that the magnetic pole block on the rotating magnetic disk can not completely repel and extrude the magnetic slide bars due to the fact that the rotating speed of the rotating magnetic disk is too high is prevented; meanwhile, when the rotating magnetic disk rotates to the N pole corresponding to the S pole of the magnetic slide rod, the rotating magnetic disk can play a role in magnetic adsorption on the magnetic slide rod, so that the elastic extrusion bag can be quickly recovered; and then along with the continuous rotation of rotating the magnetic disc, the magnetic slide bar of different magnetism that adjacent interval set up can play the interval to shake the effect to the outer wall of retort, and then makes the solution of retort inside be in and disturb the oscillation phenomenon, further improves the abundant high-efficient reaction of solution in the retort.

Preferably, the end parts of two adjacent sliding rods in the vertical direction are connected with an adhesive layer, and the outer wall of the adhesive layer is provided with a burr belt; the outer wall of the reaction tank is provided with a convex hair layer, and the convex hair layer is mutually bonded and contacted with the burr belt; when the reaction tank works, when the sliding rod shakes the outer wall of the reaction tank under the expansion of the expansion bag, the sliding rod slides out to drive the adhesive layer to be provided with the burr belt to be attached to the convex burr layer; when the slide bar contracts under the drive of the expansion bag, the slide bar can drive the burr belt to separate from the convex hair layer, and the burr belt and the convex hair layer are in an adhesion state, so that the burr belt can play a dragging force on the convex hair layer. The elastic film layer of the outer wall of the reaction tank can be synchronously driven by the pulling of the convex hair layer to generate elastic vibration, and meanwhile, when the burr belt plays a role in pulling the convex hair layer, the adjacent sliding rods can play a role in extruding and rapping the outer wall of the reaction tank, so that the elastic vibration of the outer wall of the reaction tank and the matching of the adjacent sliding rods in extruding and rapping the outer wall of the reaction tank can further play an oscillating effect on solution.

Preferably, a plurality of L-shaped fixing rods are fixedly arranged on the outer wall of the top end of the reaction tank in the circumferential direction, and the L-shaped fixing rods are in rotating contact with the bottom end of the sealing cover; a plurality of cavity elastic layers are uniformly arranged at the bottom end of the sealing cover at intervals, and the cavity elastic layers are in rotating extrusion contact with the L-shaped fixed rod; when the reaction tank works, when the sealing cover covers between the reaction tank and the fixed tank, the L-shaped fixed rod arranged on the outer wall of the reaction tank can elastically support and limit the sealing cover, so that the phenomenon that the reaction tank is extruded and deformed due to overlarge elastic extrusion force of the sealing cover on the reaction tank is prevented; and meanwhile, the reaction tank drives the L-shaped fixed rod to rotate. The top end part of the L-shaped fixed rod can rotate to extrude the elastic cavity layer, so that the phenomenon that the sealing cover is abraded due to the fact that the L-shaped fixed rod and the bottom end face of the sealing cover are excessively large in relative rotation friction force can be effectively prevented.

Preferably, the outer wall of the exhaust tube is wrapped by an elastic expansion film, and a plurality of vibration bulges are fixed on the outer wall of the elastic expansion film; a clearance cavity is formed between the elastic expansion film and the outer wall of the exhaust tube; the plurality of cavity elastic layers are communicated with the gap cavity through air guide grooves; the during operation, when the cavity elastic layer received the extrusion of L type dead lever, gaseous can get into big intermittent type intracavity through the air guide groove in the cavity elastic layer, and the intermittent type intracavity gets into a large amount of gas and can make the elasticity inflation membrane produce the elasticity inflation, and the inflation of elasticity inflation membrane can drive a plurality of vibration archs and carry out the oscillation operation to the solution of the inside central point of retort and put, and then improves the quick high-efficient reaction of retort internal solvent, reduces black magnetism ferroferric oxide nano particle manufacturing cost simultaneously.

The invention has the following beneficial effects:

1. according to the invention, Fe (II) and morpholine propanesulfonic acid are added for matching, and morpholine propanesulfonic acid can play a role in buffer protection on Fe (II), and no additional reagent is required to be added, so that the method has the advantages of green pollutants, low cost, uniform particles and easiness in scale-up production.

2. The oscillation driving device is matched with the method, when the reaction tank rotates, the vibration generated by the vibration of the elastic film layer arranged on the outer wall of the reaction tank can be transmitted to the solution in the reaction tank to generate oscillation, and further the rapid reaction of the solution in the reaction tank can be accelerated to generate magnetic ferroferric oxide nano particles to be precipitated at the bottom end of the reaction tank;

3. according to the invention, the magnetic disk is matched with the reaction tank, and the magnetic adsorption force on the magnetic disk can adsorb the precipitated magnetic ferroferric oxide nanoparticles to the bottom end of the reaction tank, so that the phenomenon that the magnetic ferroferric oxide nanoparticles are broken or crushed due to the fact that the magnetic ferroferric oxide nanoparticles generated by the precipitation reaction are fragile when the reaction tank is oscillated is effectively prevented, and the forming uniformity and stability of the magnetic ferroferric oxide nanoparticles are further influenced.

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 an X-ray diffraction diagram of magnetic ferroferric oxide nanoparticles prepared by the method;

FIG. 3 is an assembly view of the holding tank and the reaction tank of the present invention;

FIG. 4 is a cross-sectional view of FIG. 3 of the present invention;

FIG. 5 is an enlarged view of a portion of the invention at A in FIG. 4;

in the figure: the device comprises a fixed tank 1, a reaction tank 2, a dripping test tube 3, an air exhaust tube 4, a sealing cover 5, an air guide groove 51, an oscillation driving device 6, a driving motor 61, a rotating magnetic disc 62, a fixed inner cylinder 63, an extrusion cavity 631, a magnetic slide rod 64, an elastic extrusion capsule 65, a fixed slide seat 66, a slide rod 67, an expansion capsule 68, an air guide tube 69, a magnetic pole block 7, an adhesive layer 8, a burr belt 81, a convex hair layer 9, an L-shaped fixed rod 10, a cavity elastic layer 11, an elastic expansion membrane 12, a vibration bulge 13 and a clearance cavity 14.

Detailed Description

A green production method of magnetic ferroferric oxide nanoparticles according to an embodiment of the present invention will be described below with reference to fig. 1 to 5.

As shown in fig. 1 to 5, the green preparation method of magnetic ferroferric oxide nanoparticles according to the present invention includes the following steps:

s1: firstly, preparing a 20-50 mmol/L morpholine propanesulfonic acid solution with pH = 7-9 by using oxygen-free water, then dropwise adding the prepared morpholine propanesulfonic acid solution into a reaction tank 2 through a dropper, and then sealing through a sealing cover 5;

s2: pumping the inner reaction tank 2 into a vacuum state by using a suction pump through a suction pipe 4, introducing micro-oxygen gas into the inner reaction tank 2 through the suction pipe 4, and synchronously extruding a dropping test tube 3 arranged above one side of a sealing cover 5 to add FeSO4 solution into the reaction tank 2; the FeSO4 solution is added under the micro-oxygen gas environment, so that the micro-oxygen gas can play a role in protecting the FeSO4 solution;

s3: adding Fe (II) into the reaction tank 2 through a dropping test tube 3 arranged on the other side of a sealing cover 5, wherein the concentration of Fe (II) is 1-3 mmol/L, and synchronously sealing the dropping test tube 3; by adding Fe (II) and morpholine propanesulfonic acid for matching, the morpholine propanesulfonic acid can play a role in buffering and protecting Fe (II), and no additional reagent is needed to be added, so that the method has the advantages of green pollutants, low cost, uniform particles and easiness in amplification production;

s4: the driving motor 61 of the oscillation driving device 6 drives the reaction tank 2 to rotate, and the rotating speed of the driving motor 61 is 100-300 rpm; meanwhile, the oscillation driving device 6 oscillates the reaction tank 2 for 12 hours; obtaining the black magnetic ferroferric oxide nano particles.

As an embodiment of the invention, the micro-oxygen gas is prepared by 1-3% of oxygen and 97-99% of nitrogen; the low-content micro-oxygen gas is adopted, the gas in the reaction tank 2 only contains 1-3% of oxygen and 97-99% of nitrogen, the nitrogen content is high, the protection effect can be achieved, and the phenomenon that black magnetic ferroferric oxide nano particles are difficult to form efficiently due to the fact that the reaction tank 2 contains other gases is further reduced.

As an embodiment of the present invention, a fixed tank 1 is sleeved outside the reaction tank 2, and an oscillation driving device 6 is arranged in the fixed tank 1; the oscillation driving device 6 comprises a driving motor 61, a rotating magnetic disc 62, a fixed inner cylinder 63, a magnetic slide rod 64, an elastic extrusion bag 65, a fixed sliding seat 66, a slide rod 67 and an expansion bag 68; a driving motor 61 is fixed in the bottom end of the fixed tank 1, and the output end of the driving motor 61 is connected to the bottom end wall of the reaction tank 2; the outer circumferential wall of the reaction tank 2 is provided with an elastic film layer; the outer wall of the output end of the driving motor 61 is sleeved with a rotating magnetic disc 62, and the rotating magnetic disc 62 is positioned at the bottom end of the reaction tank 2; the rotating magnetic disk 62 is uniformly divided into a plurality of magnetic pole blocks 7, and the magnetism between two adjacent magnetic pole blocks 7 is opposite; the inner wall of the fixed tank 1 is fixedly provided with a fixed inner cylinder 63, and an extrusion cavity 631 is formed in the fixed inner cylinder 63; a plurality of magnetic sliding rods 64 are uniformly inserted in the circumferential direction of the outer side wall of the bottom end of the extrusion cavity 631 in a sliding manner, and the outer end parts of the magnetic sliding rods 64 are aligned with the outer ring wall of the rotating disk 62; a plurality of elastic squeezing bags 65 are uniformly arranged in the squeezing cavity 631, and the outer walls of the elastic squeezing bags 65 are connected with the end parts of the magnetic sliding rods 64; a plurality of fixed sliding seats 66 are uniformly arranged in the vertical direction and the circumferential direction of the outer cavity wall of the extrusion cavity 631, and sliding rods 67 are arranged in the fixed sliding seats 66 in a sliding manner; the end of the sliding rod 67 is in sliding pressing contact with the outer wall of the reaction tank 2, and the inner end of the sliding rod 67 is positioned in the pressing cavity 631; a plurality of expansion bags 68 are fixed in the extrusion cavity 631, and the expansion bags 68 are communicated with the elastic extrusion bag 65 through air ducts 69; a sliding rod 67 is connected to the outer wall of each of the plurality of expansion bladders 68;

when the device works, when the solution in the reaction tank 2 needs to be rotated for oscillation reaction, the control unit can control the driving motor 61 to rotate, the driving motor 61 can drive the reaction tank 2 to rotate in the fixed tank 1, meanwhile, the sealing cover 5 is in a fixed state, the rotation of the driving motor 61 can drive the rotating magnetic disk 62 to rotate, the magnetic of one of the magnetic pole blocks 7 can repel the magnetic slide rod 64 when the rotating magnetic disk 62 rotates, the magnetic slide rod 64 can slide and extrude the elastic extrusion bag 65 arranged in the fixed inner cylinder 63, the gas in the elastic extrusion bag 65 can enter the plurality of expansion bags 68 arranged in the vertical direction through the gas guide pipe 69 to expand the expansion bag, the expansion of the expansion bag 68 can push the slide rod 67 to slide out of the fixed slide seat 66, the stretching out of the plurality of slide rods 67 arranged in the vertical direction can play a role of elastic rapping on the outer wall of the reaction tank 2, the vibration generated by rapping on the outer wall of the reaction tank 2 can be transmitted to the inner part of the reaction The solution generates oscillation, so that the rapid reaction of the internal solution can be accelerated to generate magnetic ferroferric oxide nano particles to be deposited at the bottom end of the reaction tank 2, when the magnetism of the magnet block on the rotating magnetic disc 62 is separated from the repulsion of the magnetic slide rod 64, the restoring force of the elastic extrusion bag 65 pushes out the magnetic slide rod 64, and simultaneously the gas in the expansion bag 68 is pumped out, so that the slide rod 67 is separated from the extrusion and rapping on the outer wall of the reaction tank 2; meanwhile, the magnetic adsorption force on the rotating magnetic disc 62 can adsorb the precipitated magnetic ferroferric oxide nanoparticles to the bottom end of the reaction tank 2, so that the phenomenon that the magnetic ferroferric oxide nanoparticles are broken or crushed due to the fact that the magnetic ferroferric oxide nanoparticles generated by the precipitation reaction are fragile when the reaction tank 2 is oscillated is effectively prevented, and the forming uniformity and stability of the magnetic ferroferric oxide nanoparticles are influenced; the gas stored in the elastic extrusion bag 65 is subjected to pressure, so that the expansion of a plurality of expansion bags 68 arranged in the vertical direction can be met; meanwhile, the expansion deformation amount of the expansion bladder 68 adjacent to the elastic pressing bladder 65 is large, so that the solvent at the layered part of the sediment and the solution can be fully oscillated and reversed.

As an embodiment of the present invention, a magnetic pole block 7 is disposed at an end of each of the magnetic slide bars 64, and the magnetic poles 7 of two adjacent magnetic slide bars 64 are opposite in magnetism; the distance between two adjacent magnetic sliding rods 64 is greater than the width of the magnetic pole block 7 arranged on the rotating magnetic disk 62, and the width of the magnetic pole block 7 on the rotating magnetic disk 62 is greater than the width of the magnetic sliding rod 64; when the magnetic disk 62 rotates, the magnetic poles of the magnetic pole blocks 7 of the magnetic disk 62 correspond to the magnetic poles of one of the magnetic slide bars 64, so that repulsive force is generated to the magnetic pole blocks 7, and the magnetic slide bars 64 can extrude the elastic extrusion bag 65; the distance between two adjacent magnetic sliding rods 64 is larger than the width of the magnetic pole block 7 arranged on the rotating magnetic disk 62, so that the phenomenon that the magnetic pole block 7 on the rotating magnetic disk 62 cannot completely repel and extrude the magnetic sliding rods 64 due to the fact that the rotating speed of the rotating magnetic disk 62 is too high is prevented; meanwhile, when the rotating magnetic disc 62 rotates to the N pole corresponding to the S pole of the magnetic slide bar 64, the rotating magnetic disc 62 can perform a magnetic adsorption effect on the magnetic slide bar 64, so that the elastic pressing bag 65 can be quickly recovered; further, along with the continuous rotation of the rotating magnetic disc 62, the magnetic slide bars 64 with different magnetism and arranged adjacently at intervals can play an interval rapping effect on the outer wall of the reaction tank 2, so that the solution in the reaction tank 2 is in a disturbing oscillation phenomenon, and the sufficient and efficient reaction of the solution in the reaction tank 2 is further improved.

As an embodiment of the present invention, the end portions of two vertically adjacent sliding rods 67 are connected with an adhesive layer 8, and a burr belt 81 is disposed on the outer wall of the adhesive layer 8; the outer wall of the reaction tank 2 is provided with a convex hair layer 9, and the convex hair layer 9 is in mutual bonding contact with the burr belt 81; when the device works, when the sliding rod 67 vibrates the outer wall of the reaction tank 2 under the expansion of the expansion bag 68, the sliding of the sliding rod 67 drives the burr belt 81 arranged on the viscose layer 8 to be attached to the convex burr layer 9; when the slide bar 67 is contracted under the drive of the expansion bag 68, the slide bar 67 drives the burr belt 81 to separate from the raised hair layer 9, and the burr belt 81 is in an adhesion state with the raised hair layer 9, so that the burr belt 81 can exert a pulling force on the raised hair layer 9. The elastic film layer that drags meeting synchronous drive retort 2 outer wall of protruding matte layer 9 produces elastic vibration, and when burr area 81 played the dragging to protruding matte layer 9 simultaneously, adjacent slide bar 67 can play the effect that the extrusion was beaten to the outer wall of retort 2, and then the elastic vibration of retort 2 outer wall and the cooperation of adjacent slide bar 67 to the extrusion of retort 2 outer wall are beaten can further play the oscillating effect to the solution.

As an embodiment of the present invention, a plurality of L-shaped fixing rods 10 are fixedly arranged on the circumferential direction of the outer wall of the top end of the reaction tank 2, and the L-shaped fixing rods 10 are in rotational contact with the bottom end of the sealing cover 5; a plurality of cavity elastic layers 11 are uniformly arranged at the bottom end of the sealing cover 5 at intervals, and the cavity elastic layers 11 are in rotating extrusion contact with the L-shaped fixed rod 10; when the reaction tank works, when the sealing cover 5 covers between the reaction tank 2 and the fixed tank 1, the L-shaped fixed rod 10 arranged on the outer wall of the reaction tank 2 can elastically support and limit the sealing cover 5, so that the phenomenon that the reaction tank 2 is extruded and deformed due to overlarge elastic extrusion force of the sealing cover 5 on the reaction tank 2 is avoided; meanwhile, the reaction tank 2 drives the L-shaped fixing rod 10 to rotate. The top end part of the L-shaped fixed rod 10 can rotate and extrude the elastic cavity layer, so that the phenomenon that the sealing cover 5 is abraded due to the fact that the relative rotating friction force between the L-shaped fixed rod 10 and the bottom end face of the sealing cover 5 is too large can be effectively prevented.

As an embodiment of the present invention, the outer wall of the extraction tube 4 is wrapped by an elastic expansion film 12, and a plurality of vibration protrusions 13 are fixed on the outer wall of the elastic expansion film 12; a clearance cavity 14 is formed between the elastic expansion membrane 12 and the outer wall of the exhaust tube 4; the plurality of cavity elastic layers 11 are communicated with the clearance cavity 14 through air guide grooves 51; the during operation, when cavity elastic layer 11 receives the extrusion of L type dead lever 10, gaseous can get into big intermittent type intracavity through air guide groove 51 in cavity elastic layer 11, it can make elasticity inflation membrane 12 produce the elasticity inflation to get into a large amount of gas in the intermittent type intracavity, the inflation of elasticity inflation membrane 12 can drive a plurality of vibration archs 13 and carry out the oscillation operation to the solution of retort 2 inside central point positions, and then improve the quick high-efficient reaction of 2 inside solvents of retort, reduce black magnetism ferroferric oxide nano particle manufacturing cost simultaneously.

The specific working process is as follows:

when the device works, when the solution in the reaction tank 2 needs to be rotated for oscillation reaction, the control unit can control the driving motor 61 to rotate, the driving motor 61 can drive the reaction tank 2 to rotate in the fixed tank 1, meanwhile, the sealing cover 5 is in a fixed state, the rotation of the driving motor 61 can drive the rotating magnetic disk 62 to rotate, the magnetic of one of the magnetic pole blocks 7 can repel the magnetic slide rod 64 when the rotating magnetic disk 62 rotates, the magnetic slide rod 64 can slide and extrude the elastic extrusion bag 65 arranged in the fixed inner cylinder 63, the gas in the elastic extrusion bag 65 can enter the plurality of expansion bags 68 arranged in the vertical direction through the gas guide pipe 69 to expand the expansion bag, the expansion of the expansion bag 68 can push the slide rod 67 to slide out of the fixed slide seat 66, the stretching out of the plurality of slide rods 67 arranged in the vertical direction can play a role of elastic rapping on the outer wall of the reaction tank 2, the vibration generated by rapping on the outer wall of the reaction tank 2 can be transmitted to the inner part of the reaction The solution of generate the oscillation, after the magnetism of magnet piece breaks away from repulsion with magnetic slide bar 64 on rotating magnetic disc 62, the resilience of elasticity extrusion bag 65 can be released magnetic slide bar 64, simultaneously take out the gas in expansion bag 68, and then rotate the continuous rotation of magnetic disc 62, can make magnetic slide bar 64 produce reciprocating motion, make the inside solution of retort 2 produce high-efficient quick oscillatory effect, after the inside solution reaction of retort 2 is accomplished, operating personnel opens sealed lid 5, take out the supernatant earlier, then take out the inside magnetic ferroferric oxide nano particle of retort 2 and wash, and then obtain magnetic ferroferric oxide nano particle.

In the description of the present invention, it is to be understood that the terms "center", "front", "rear", "vertical", "horizontal", "top", "bottom", "inner", "outer", etc., indicate orientations or positional relationships based on those shown in the drawings, and are used only for convenience in describing the present invention and for simplicity in description, and do not indicate or imply that the device or element being referred to must have a particular orientation, be constructed and operated in a particular orientation, and therefore, should not be taken as limiting the scope of the present invention.

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.