JP2022086721A - Magnetic nanoparticle cleaning separation method and cleaning separation system - Google Patents

Abstract

To provide a magnetic nanoparticle cleaning separation method that shortens a time for required for manufacture of magnetic nanoparticles.SOLUTION: A magnetic nanoparticle cleaning separation method includes: a process in which magnetic nanoparticles are cleaned in a processor 47, and a cleaning liquid is introduced into the processor in which the magnetic nanoparticles are accommodated; a process in which a mixture of the introduced cleaning liquid and the magnetic nanoparticles is stirred; a process in which sedimentation treatment is performed for the mixture located in a magnetic field; and a process in which a supernatant liquid obtained by the sedimentation treatment is poured out of the processor. The cleaning liquid introduction process and stirring process are performed multiple times, and after performance of final stirring process, the process for sedimentation treatment and the process for pouring out the cleaning liquid are not performed. The method further includes an accumulation process in which the mixture derived from the processor is flown into a part of a flow channel of a separator 20, and the magnetic nanoparticles contained in the mixture are accumulated in the flow channel located in the magnetic field.SELECTED DRAWING: Figure 1

Description

The present invention relates to a method for cleaning and separating magnetic nanoparticles and a system for cleaning and separating magnetic nanoparticles.

At the time of producing nanoparticles, nanoparticles are generally settled and separated. In the method for producing metal oxide particles described in Patent Document 1, constant voltage pulse electrolysis is performed on the electrolyte solution provided between the electrodes, and the metal oxide particles are subjected to the first electrode or the second electrode of the electrode. It causes formation and separates the metal oxide particles from the electrolyte solution. In this separation step, the particles are settled in the electrolyte solution over time by gravity to remove the electrolyte solution.

Special Table 2016-531832 Gazette

The precipitation treatment described in Patent Document 1 requires a long time to precipitate the metal oxide particles, and there is a problem that it takes time to produce nanoparticles.

The present invention has been made in view of the above problems, and an object of the present invention is to shorten the time required for producing magnetic nanoparticles.

The method for cleaning and separating magnetic nanoparticles according to the present invention is a step of cleaning magnetic nanoparticles in a processing apparatus, which is a step of introducing a cleaning liquid into the processing apparatus containing the magnetic nanoparticles and a step of introducing the cleaning liquid. It includes a step of stirring the mixture of the magnetic nanoparticles and the magnetic nanoparticles, a step of performing a sedimentation treatment on the mixture arranged in a magnetic field, and a step of pouring out the supernatant liquid obtained by the sedimentation treatment from the processing apparatus. The step of introducing the cleaning liquid and the step of stirring are performed a plurality of times, and after the step of finally stirring, the step of performing the sedimentation treatment and the step of pouring out the supernatant liquid are not performed, and the processing apparatus. Further comprising a separation step of flowing the mixture derived from the above into a flow path of a separation device, depositing magnetic nanoparticles contained in the mixture in a part of the flow path arranged in a magnetic field, and separating the mixture.

In a preferred embodiment, the step of returning the mixture that has passed through the flow path to the processing apparatus is further included.

Another aspect of the present invention is a method for producing magnetic nanoparticles, which comprises a step of transporting magnetic nanoparticles deposited on a part of the flow path to a predetermined place together with a part of the flow path by the above-mentioned washing and separating method. be.

In a preferred embodiment, in the transporting step, the magnetic nanoparticles are transported to a drying device, and further includes a step of drying the magnetic nanoparticles by the drying device.

Another aspect of the present invention includes a processing device for cleaning magnetic nanoparticles and a separating device for separating magnetic nanoparticles, and the processing device contains a mixture of a cleaning liquid and magnetic nanoparticles. The separation device includes a processing container and a magnet arranged below the processing container to generate a magnetic field acting on the mixture, and the separation device is included in the mixture through which the mixture introduced from the processing container flows. It comprises a device body that constitutes a part of the flow path in which magnetic nanoparticles are deposited, and a magnet that is arranged below the device body and generates a magnetic field that acts on the mixture flowing through the part of the flow path. It is a cleaning and separation system for magnetic nanoparticles.

In a preferred embodiment, the apparatus main body of the separation device has an introduction port connected to the processing container to introduce the mixture, a flow path through which the mixture introduced from the introduction port is flowed, and the processing container. It is provided with an outlet from which the mixture connected to and flowing through the flow path is led out toward the processing container.

In a preferred embodiment, the device body is freely removable from the support means.

Another aspect of the present invention is the production of magnetic nanoparticles comprising the cleaning and separating system for magnetic nanoparticles and a drying device in which the main body of the separating device is housed and the nanoparticles deposited in the flow path are dried. It is a system.

According to one aspect of the present invention, the time required for producing magnetic nanoparticles can be shortened.

It is explanatory drawing which shows the schematic structure of the manufacturing system including the cleaning separation system of magnetic nanoparticles which concerns on one Embodiment of this invention. It is a side view which shows the schematic structure of the processing container. It is a side view of the separation device. It is a perspective view of the lid portion of the main body of the separating device, (A) is a perspective view of the lid portion viewed from the plane, side surface, and front, and (B) is a perspective view of the lid portion viewed from the bottom surface, side surface, and front surface. be. It is a top view from the plane, the side surface, and the front of the main body of the main body of the separation device. It is a top view of the separation device. It is a side view which shows the state which the apparatus main body of a separation apparatus is placed on the shelf board of a drying apparatus. It is a flowchart explaining the cleaning separation method and the manufacturing method of magnetic nanoparticles. It is a flowchart for demonstrating the process of separating magnetic nanoparticles from a mixture of a reaction solvent and magnetic nanoparticles. It is a flowchart for demonstrating the process of cleaning magnetic nanoparticles. It is a flowchart for demonstrating the process of cleaning magnetic nanoparticles. It is a flowchart for demonstrating the process of cleaning magnetic nanoparticles. It is a flowchart for demonstrating the process of cleaning magnetic nanoparticles. It is a flowchart for demonstrating the process of separating magnetic nanoparticles from a mixture of a cleaning liquid and magnetic nanoparticles, and the process of transporting them to a drying apparatus. It is a flowchart for demonstrating the process of separating magnetic nanoparticles from a mixture of a cleaning liquid and magnetic nanoparticles, and the process of transporting them to a drying apparatus.

Embodiments of the present invention will be described with reference to the drawings. The magnetic nanoparticles cleaning / separation system 10 according to the embodiment of the present invention is for separating and cleaning magnetic nanoparticles from a liquid containing magnetic nanoparticles to produce magnetic nanoparticles, and is a separation device 20 and a processing device 47. And have. The cleaning separation system 10 is connected to a first cleaning liquid recovery tank 60A, a second cleaning liquid recovery tank 60B, a solvent recovery tank 61, a waste liquid tank 62, a solvent disposal tank 63, and a cleaning liquid supply tank 64 that constitute a recovery tank. Has been done. The production shown in FIG. 1 is carried out by the cleaning separation system 10, each tank connected to the cleaning separation system 10, the reactor 12, the controller 53, the drying device 50 for drying the magnetic nanoparticles produced by the cleaning separation system 10, and the like. The system 11 is configured.

The processing device 47 has a processing container 40 and a processing container magnet 45. The processing container 40 is connected to the reactor 12 via a conduit 125, and the magnetic nanoparticles mixed liquid produced by the reactor 12 is introduced into the processing container 40. The magnetic nanoparticles mixed solution introduced from the reactor 12 is a mixture of the reaction solvent and the magnetic nanoparticles (reaction solution containing the magnetic nanoparticles). The magnetic nanoparticles are magnetic metal nanoparticles such as nickel nanoparticles, iron nanoparticles, cobalt nanoparticles, etc., and are liquid phase synthesized in the reactor 12 using reaction solvents such as primary amines and fatty acids. It is manufactured by the method. The reaction solvent is not limited to this, and may be a known reaction solvent used for producing magnetic nanoparticles. The average particle size of the magnetic nanoparticles produced is preferably 10 nm to 500 nm.

In the treatment container 40, a sedimentation treatment is performed on a mixture of the reaction solvent and the magnetic nanoparticles. The settling treatment is a treatment in which the mixture is allowed to stand and the magnetic nanoparticles are settled on the upper surface of the bottom wall 41 of the treatment container 40. The supernatant liquid by the sedimentation treatment is discharged from the treatment container 40 to obtain magnetic nanoparticles which are sediments, and then a washing liquid is added to the sediment to be stirred, settled, and the supernatant liquid is poured out to perform magnetic nanoparticles. To clean. As the cleaning liquid, for example, isopropyl alcohol (IPA) is used, but it may be a known cleaning liquid used when cleaning nanoparticles. The mixture of the cleaning liquid and the magnetic nanoparticles is subjected to a sedimentation treatment, and the supernatant liquid is taken out from the treatment container 40. The introduction of the cleaning liquid, stirring, sedimentation treatment, and derivation of the supernatant liquid may be performed multiple times. After the last round of stirring, the mixture of the washing liquid and the magnetic nanoparticles is drawn out from the processing container 40 without performing the sedimentation treatment. That is, from the processing container 40, the supernatant liquid of the mixture of the reaction solvent and the magnetic nanoparticles, the supernatant liquid of the mixture of the cleaning liquid and the magnetic nanoparticles, and the mixture of the cleaning liquid and the magnetic nanoparticles (when not distinguished, "magnetic nano". "Particle mixture") is led out toward the separation device 20.

As shown in FIG. 2, the processing container 40 has a cylindrical shape and has a bottom wall 41, a peripheral wall 42 erected from the peripheral edge of the bottom wall 41, and an upper wall 43. The bottom wall 41 is inclined diagonally with respect to the horizontal plane. The processing container 40 of this embodiment has a capacity of 1100 L. An electric motor type stirrer 44 is provided in the processing container 40, and the mixture of the cleaning liquid and the magnetic nanoparticles contained in the processing container 40 is stirred to clean the magnetic nanoparticles.

A magnet 45 for the processing container is provided below the bottom wall 41 of the processing container 40. The processing container magnet 45 has a size corresponding to the bottom surface of the bottom wall 41, and is free to approach and separate from the bottom wall 41 by the moving mechanism 46. The moving mechanism 46 is composed of, for example, a hydraulic or electric jack or an actuator, so that the upper surface of the processing container magnet 45 is aligned with the bottom wall 41 when the processing container magnet 45 is in close proximity to the bottom wall 41. The processing container magnet 45 is tilted and raised in the horizontal direction. As the processing container magnet 45, for example, an electromagnet or a permanent magnet is used, but any magnet can be used as long as it can generate a magnetic field and generate an attractive force with the magnetic nanoparticles. When the magnet 45 for the processing container is close to the bottom wall 41, the magnetic nanoparticles mixed liquid contained in the processing container 40 is arranged in the magnetic field. The strength of the magnetic field generated by the magnet 45 for the magnetic field processing container is the strength at which the magnetic nanoparticles can be attracted when the magnetic nanoparticles mixed liquid is placed in the magnetic field. When the processing container magnet 45 is not used by bringing the processing container magnet 45 close to the bottom wall 41 of the processing container 40 and applying the attractive force of the processing container magnet 45 to the magnetic nanoparticles when performing the settling treatment. The time required for the sedimentation process is significantly reduced compared to the above.

A cleaning liquid supply tank 64 for supplying the cleaning liquid to the processing container 40 is connected to the upper wall of the processing container 40 via a conduit 120. The conduit 120 is provided with an on-off valve 101. As the on-off valve 101, a known automatic valve such as an electromagnetic type or a hydraulic type is used, and its operation is controlled by the controller 53. The on-off valves 102 and 106 to 108, which will be described later, have the same configuration as the on-off valve 101. In the present embodiment, the cleaning liquid supply tank 64 has a capacity of about 10 L, but it is sufficient if a required amount of cleaning liquid can be accommodated.

The separation device 20 includes a device main body 21, although details will be described later. In the present embodiment, two device main bodies 21A and 21B (referred to as "device main body 21" when it is not necessary to distinguish them) are provided, and the device main bodies 21A and 21B are connected to the processing container 40 by a conduit 121. The number of device main bodies 21 is not limited to this embodiment, and may be one or three or more.

One end of the conduit 121 is connected to the lower part of the peripheral wall 42 of the processing container 40 at a position corresponding to the lowermost side of the diagonally inclined bottom wall 41. The other end of the conduit 121 is a bifurcated branch pipe 121a, 121b, and the branch pipes 121a, 121b are connected to the introduction ports 24 of the device main body 21A, 21B, respectively. A switching valve 100 constituting the switching means is provided at the branching point of the conduit 121, and the flow is switched so that the magnetic nanoparticles mixed liquid led out from the processing container 40 flows to either of the device main bodies 21A and 21B. As the switching valve 100, a known switching valve is used, for example, a ball-type three-way valve. In this embodiment, a manual switching valve is used, and the operator operates the switching valve to switch the flow of the magnetic nanoparticles mixed liquid, but even if an automatic switching valve that can be controlled by the controller 53 is used. good. A pump 110 and an on-off valve 102 are provided at predetermined positions between the switching valve 100 and the processing container 40 of the conduit 121. As the pump 110, a known pump such as an air-driven pump is used, and its operation is controlled by the controller 53. The pump 110 is set to, for example, a discharge rate of 50 L / min.

Each of the device main bodies 21A and 21B of the separation device 20 is connected to the first cleaning liquid recovery tank 60A, the second cleaning liquid recovery tank 60B, the solvent recovery tank 61, the waste liquid tank 62, and the processing container 40 via the conduit 122. .. The end on one end side of the conduit 122 is a bifurcated branch pipe 122a, 122b, and each branch pipe 122a, 122b is connected to an outlet 31 of each device main body 21A, 21B. Further, the conduit 122 has a first cleaning liquid recovery tank 60A, a second cleaning liquid recovery tank 60B, a solvent recovery tank 61, and branch pipes 122c to 122f connected to the waste liquid tank 62. Three-way valves 103 to 105 are provided at the branch points of the conduit 122 to the tanks 60A, 60B, 61, and 62, respectively, and magnetic nanoparticles are mixed through the apparatus main body 21 by controlling the three-way valves 103 to 105. The liquid can be flowed toward each of the tanks 60A, 60B, 61, 62. Further, the conduit 122 has a conduit 126 connected to the processing container 40, and a three-way valve 109 is provided at the branching point. The three-way valve 109 is provided on the upstream side of the three-way valve 103. The processing container 40, the separating device 20, the conduit 121 connecting each of them, a part of the conduit 122, and the conduit 126 form a circulation path for circulating a mixture of the cleaning liquid and the magnetic nanoparticles. The conduit 126 is connected to the reactor 126 to form a circulation path by the reactor 126, the conduit 125, the processing container 40, the separating device 20, the conduit 121 connecting each of them, a part of the conduit 122, and the conduit 126. You may. The three-way valves 103 to 105 and 109 are electromagnetic type, and their operation is controlled by the controller 53. Between the waste liquid tank 62 and the three-way valve 103, a pump 112 for sucking the magnetic nanoparticles mixed liquid that has passed through the apparatus main body 21 is provided in the waste liquid tank 62.

The first cleaning liquid recovery tank 60A and the second cleaning liquid recovery tank 60B are connected to the processing container 40 via a conduit 123, and the cleaning liquid contained in each of the tanks 60A and 60B is returned to the processing container 40. The conduit 123 is formed in branch pipes 123a and 123b whose one end is bifurcated, and the branch pipes 123a and 123b are connected to the first cleaning liquid recovery tank 60A and the second cleaning liquid recovery tank 60B, and each branch is formed. The pipes 123a and 123b are provided with on-off valves 106 and 107. Further, the other end side of the conduit 123 is connected to the upper wall of the processing container 40, and a pump 111 is provided between the processing container 40 of the conduit 123 and the branch portion. Further, the solvent recovery tank 61 is connected to the solvent disposal tank 63 by a conduit 124, and the reaction solvent contained in the solvent recovery tank 61 is sent toward the solvent disposal tank 63. The conduit 124 is provided with an on-off valve 108 and a pump 113. In the present embodiment, the first cleaning liquid recovery tank 60A and the second cleaning liquid recovery tank 60B have a capacity of about 600 L, and the solvent recovery tank 61 has a capacity of about 1100 L, but the present invention is not limited thereto. In the present embodiment, the first cleaning liquid recovery tank 60A and the second cleaning liquid recovery tank 60B are connected to the processing container 40 by the conduit 123, but may be connected to the reactor 12. In this case, the cleaning liquid contained in the first cleaning liquid recovery tank 60A and the second cleaning liquid recovery tank 60B is introduced into the processing container 40 via the reactor 12 and the conduit 125. As the pumps 111 to 113, known pumps such as an air-driven pump are used.

The separation device 20 will be described. As shown in FIGS. 3 to 6, the separation device 20 is for separating magnetic nanoparticles from the magnetic nanoparticles mixed liquid, and is a plate that is a support means for supporting the device main body 21 and the device main body 21. A shape support member 33, a magnet 35 arranged below the device main body 21 and freely provided close to and detached from the device main body 21, and a moving mechanism 36 for moving the magnet 35 close to and detached from the device main body 21. ..

As shown in FIG. 6, the apparatus main body 21 has a substantially rectangular shape when viewed from a plane as an example, and has a tapered outer shape of a substantially triangular shape with two corners cut off on one end side in the longitudinal direction. is doing. An introduction port 24 for introducing the magnetic nanoparticles mixed liquid is formed on the other side of the device main body 21 in the longitudinal direction, and an outlet 31 (FIG. 5) for leading out the magnetic nanoparticles mixed liquid is formed on one side. In the following description, the side where the introduction port 24 is provided is referred to as an upstream side, and the side where the outlet port 31 is provided is also referred to as a downstream side. In FIG. 3, the right side is the upstream side, the left side is the downstream side, and the direction from the upstream side to the downstream side is the direction in which the magnetic nanoparticles mixed liquid flows.

The device main body 21 includes a lid portion 22 and a main body portion 30. As shown in FIGS. 4A and 4B, the lid portion 22 includes an upper wall 22a and an edge portion 22b protruding downward from the peripheral edge of the upper wall 22a. An introduction port 24 is formed on the upstream side of the upper wall 22a, an introduction pipe 25 is inserted through the introduction port 24, and one end of the introduction pipe 25 is located in the main body portion 30. One end of the introduction pipe 25 may be attached to the upper surface of the upper wall 22a by welding or the like so as to communicate with the introduction port 24. The other end of the introduction pipe 25 is detachably connected to the branch pipes 121a and 121b of the conduit 121 connected to the processing container 40 via the connector 25a. Further, the upper wall 22a is formed with a through hole 26 for removing the gas generated from the magnetic nanoparticles mixed liquid, and a handle 27 is provided on the upper surface for the operator to attach / detach the lid portion 22 to the main body portion 30. ing.

As shown in FIG. 4B, a ridge portion 22c is provided on the lower surface of the upper wall 22a of the lid portion 22 in an annular shape along the edge portion 22b, and the ridge portion 22b and the ridge portion 22c are provided. The peripheral wall 30b and the rib plate 30d of the main body portion 30, which will be described later, are fitted in between. Cylindrical members 23 extending in the width direction of the lid 22 are arranged between the protrusions 22c on both sides of the lid 22 in the width direction. A through hole (not shown) provided in the peripheral wall of the cylindrical member 23 is connected to one end of the introduction pipe 25, and the hollow portion of the cylindrical member 23 and the inside of the introduction pipe 25 communicate with each other. The peripheral wall 30b of the cylindrical member 23 is formed with a slit 23a that communicates with the hollow portion over the entire length of the cylindrical member 23 in the length direction. The slit 23a is provided on the downstream side of the peripheral wall of the cylindrical member 23 in the cross section of the cylindrical member 23, and the magnetic nanoparticles mixed liquid introduced from the introduction port 24 via the introduction pipe 25 is in the width direction of the apparatus main body 21. It spreads out and falls on the main body 30.

As shown in FIG. 5, the main body portion 30 has a shape seen from a plane corresponding to the lid portion 22, and includes a bottom wall 30a and a peripheral wall 30b erected upward from the edge of the bottom wall 30a. There is. An outlet 31 is formed at the tip of the peripheral wall 30b on the downstream side, and the magnetic nanoparticles mixed liquid flowing out from the cylindrical member 23 passes through the bottom wall 30a of the main body 30 and heads toward the outlet 31. That is, the inside of the main body 30 constitutes a flow path of the magnetic nanoparticles mixed liquid. The inside of the main body 30, that is, the flow path is large enough to allow the magnetic nanoparticles mixed liquid to flow at a flow rate of, for example, 50 L / min, and for example, the length of the main body 30 in the longitudinal direction is long. The width is set to 50 cm, the width is set to 20 cm, and the height of the main body 30 is set to 30 cm. When the magnet 35, which will be described later, is located below the bottom wall 30a, the magnetic nanoparticles contained in the magnetic nanoparticles mixed liquid are deposited on a part of the bottom wall 30a which is a flow path due to the attractive force between the magnet 35 and the magnet 35. .. A pair of plate-shaped locking members 30c for locking the device main body 21 to the plate-shaped support member 33 are provided below the peripheral walls 30b on both sides in the width direction along the longitudinal direction of the device main body 21. Reinforcing rib plates 30d are provided at the corners of the upper end edge on the downstream side and the upper end edge on the upstream side of the peripheral wall 30b.

As shown in FIG. 3, one end 32b of a substantially L-shaped outlet pipe 32 is connected to the outside of the outlet 31 by an attachment means such as welding. The other end 32a of the lead-out pipe 32 is provided so that the flow path is located below the bottom wall 30a in a posture along the horizontal direction, and is open downward. A wide-diameter portion 122g having an open upper surface is provided at the tip of the branch pipe 122a (or 122b) of the conduit 122, and the other end 32a of the lead-out pipe 32 is a wide-diameter portion of the branch pipe 122a (or 122b) of the conduit 122. It is inserted in 122 g. The magnetic nanoparticles mixed liquid flows from the outlet 31 through the outlet pipe 32 to the wide diameter portion 122 g of the branch pipe 122a (or 122b) and flows through the branch pipe 122a (or 122b).

The support means is a pair (two) rod-shaped plate-shaped support members 33 provided in parallel at a predetermined interval, and as shown in FIG. 3, a posture tilted by a predetermined angle θ with respect to the horizontal direction. It is supported by the base 37. By placing the locking member 30c of the device main body 21 on the upper surface of the plate-shaped support member 33 so that the outlet 31 is on the lower side and the introduction port 24 is on the upper side, the device main body 21 is attached to and detached from the plate-shaped support member 33. Freely supported. The apparatus main body 21 is supported by the plate-shaped support member 33, the introduction port 24 is located above the outlet port 31, and the flow path has an inclination of a predetermined angle θ with respect to the horizontal direction. The particle mixture is easy to flow from the inlet to the outlet. The tilt angle θ of the plate-shaped support member 33 with respect to the horizontal direction is set to an angle at which the device main bodies 21A and 21B do not slip off due to the frictional force between the locking member 30c and the plate-shaped support member 33, and is set to an angle of 1 degree or more. , 20 degrees or less. The support means is not limited to the plate-shaped support member 33 of the present embodiment, and may be any form as long as the device main body 21 can be supported.

As shown in FIG. 6, a magnet 35 provided on the magnet support plate 34 is arranged between the two plate-shaped support members 33 and below the device main body 21. The magnet support plate 34 is a substantially rectangular plate member, and its downstream end is pivotally supported by a shaft 37a provided on the base 37 and is freely rotatable around the shaft 37a. Two rod-shaped magnets 35 are attached to the upper surface of the magnet support plate 34 at two locations on the upstream side and the downstream side of the bottom wall 30a of the main body portion 30 with an adhesive or the like. As the magnet 35, for example, an electromagnet or a permanent magnet is used, but any magnet 35 may be used as long as it can generate a magnetic field and generate an attractive force with the magnetic nanoparticles. When the magnet 35 is close to the device main body 21, the magnetic nanoparticle mixed liquid flowing through the device main body 21 is arranged in the magnetic field. The strength of the magnetic field generated by the magnet 35 is the strength at which an attractive force can be applied to the magnetic nanoparticles. In FIG. 6, the description of the moving mechanism 36 is omitted for the sake of explanation.

The moving mechanism 36 causes the magnet support plate 34 to which the magnet 35 is attached to approach and separate from the device main body 21, and as shown in FIG. 3, the bolt 36a and the bolt 36a are provided integrally with the bolt 36a. It is provided with a handle 36b for rotating the magnet. The bolt 36a and the handle 36b are freely rotatably supported by the base 37. A protruding piece 34a is connected to the upstream end edge of the magnet support plate 34, and a screw hole 34b into which the bolt 36a of the moving mechanism 36 is inserted is formed in the protruding piece 34a. The magnet support plate 34 rotates upward around the shaft 37a due to the rotation of the handle 36b in one direction, the magnet 35 approaches the bottom wall 30a of the device main body 21, and the magnet 35 rotates in the opposite direction of the handle 36b. The support plate 34 rotates downward around the shaft 37a, and the magnet 35 separates from the bottom wall 30a of the apparatus main body 21. The operator operates the handle 36b to bring the magnet 35 close to the device main body 21 when the magnetic nanoparticles mixed liquid flows into the flow path of the device main body 21.

In the present embodiment, the separation device 20 includes two sets (set A and set B) having one device main body 21, one plate-shaped support member 33, one magnet 35, and one moving mechanism 36. The device main body 21A, the plate-shaped support member 33A, the magnet 35A, and the moving mechanism 36A belong to the set A, and the device main body 21B, the plate-shaped support member 33B, the magnet 35B, and the moving mechanism 36B belong to the set B. Belongs to. The separation device 20 may further include a replacement device body 21. In this embodiment, three replacement device main bodies 21A ′, 21A ″, and 21B ′ are provided. The device main body 21A ′ and 21A ″ are attached to the plate-shaped support member 33A of the set A, and the device main body 21B ′ is attached to the plate-shaped support member 33B of the set B. The number of sets included in the separating device 20 is not limited to two, and may be one set or three or more sets.

When the magnetic nanoparticles mixed liquid is a mixture of a cleaning liquid and magnetic nanoparticles, the magnetic nanoparticles mixed liquid is poured only into one of the two device main bodies 21A and 21B of each set A and B (for example, the device main body 21A). When a predetermined amount of magnetic nanoparticles are deposited on the device main body 21A, the switching valve 100 is switched and the magnetic nanoparticles mixed liquid is flowed to the other device main body 21B. The device main body 21A on which magnetic nanoparticles are deposited is removed from the plate-shaped support member 33A and conveyed to the drying device 50, and a replacement device main body 21A'is attached to the plate-shaped support member 33A. When a predetermined amount of magnetic nanoparticles are deposited on the other device main body 21B, the switching valve 100 is switched and the magnetic nanoparticles mixed liquid is flowed to one device main body 21A'attached to the plate-shaped support member 33A. The device main body 21B on which magnetic nanoparticles are deposited is removed from the plate-shaped support member 33B and conveyed to the drying device 50, and a replacement device main body 21B'is attached to the plate-shaped support member 33B. This operation is repeated to separate the magnetic nanoparticles, and the removed device main body 21 is sequentially conveyed to the drying device 50. When the number of sets included in the separating device 20 is one, the switching valve 100 may not be provided, and when a predetermined amount of magnetic nanoparticles are deposited on the device main body 21A, the flow of the mixture is stopped by the pump 110. Then, the device main body 21A is removed and the replacement device main body 21A'is attached. When the number of sets included in the separation device 20 is 3 or more, the sets through which the mixture flows are sequentially switched by the switching valve 100, and the device main body 21 is replaced in the same manner as in the case of the two sets.

It should be noted that only the main body 30 of the device main bodies 21A and 21B may be provided for replacement. In this case, only two sets of lid portions 22 are provided, and the device main bodies 21A and 21B attached to the plate-shaped support members 33A and 33B respectively at the start of operation of the cleaning separation system 10 and the replacement device main bodies 21A'and 21A. The lid 22 is shared with'' and 21B'. Further, three or more sets of the above may be provided, or these sets may be divided into two or more groups, and the magnetic nanoparticles mixed liquid may be flowed to any of the groups by the switching valve 100.

The drying device 50 is a known hot air drying device 50 used for drying in the process of manufacturing magnetic nanoparticles, and has a structure in which air is taken in from an air inlet (not shown) provided in the lower part of the hot air drying device 50. It has become. As shown in FIG. 7, a shelf board 51 is provided in the hot air drying device 50, and heated hot air is generated by passing steam through a coil (not shown) attached to the lower surface of the shelf board 51. .. A spacer 52 is attached to the upper surface of the shelf board 51. The spacer 52 is made of a material such as synthetic resin. Of the main body 21 of the separating device 20, only the main body 30 is placed on the shelf board 51 of the drying device 50, and the lid 22 is removed. In the main body 30, the entire bottom wall 30a is above the spacer 52 in a posture in which the upstream side edge of the bottom wall 30a is in contact with the spacer 52 and the other end 32a of the lead-out pipe 32 is in contact with the shelf plate 51. It is placed on the shelf board 51 so as to be located. FIG. 7 shows the deposited magnetic nanoparticles m.

Since the lead-out pipe 32 of the main body portion 30 is located below the bottom wall 30a, a space S is formed between the shelf plate 51 and the main body portion 30, and the shelf plate heated by air is formed by this space S. It prevents the heat of 51 from being directly transmitted to the bottom wall 30a. Further, the spacer 52 prevents the shelf plate 51 and the bottom wall 30a from coming into direct contact with each other, and prevents heat from being transferred from the contact portion to the bottom wall 30a. When the shelf board 51 comes into direct contact with the bottom wall 30a of the main body 30, the temperature becomes non-uniform between the side near the shelf board 51 and the side far from the shelf board 51 of the magnetic nanoparticles deposited on the bottom wall 30a, which causes aggregation of the magnetic nanoparticles. However, in the present embodiment, the space S and the spacer 52 prevent the heat of the shelf board 51 from being directly transferred to the bottom wall 30a to prevent the aggregation of magnetic nanoparticles.

The controller 53 is connected to each part of the on-off valves 101, 102, 106 to 108, the three-way valves 103 to 105, 109, the moving mechanisms 36, 46 of the magnets 35, 45, the stirrer 44, etc. by a communication line (not shown). It controls the operation, and is realized by a computer having a control unit and a storage unit, and having a CPU, a memory, and the like. The storage unit stores programs for controlling operation operations and operation timings of each unit, and parameters for control. The parameters are, for example, a predetermined time required for the settling treatment, confirmation of installation of the main body of the apparatus, start / stop of stirring, charging of cleaning liquid, dispensing, and the like. Further, the controller 53 includes a touch panel, an alarm, and a buzzer (not shown) as a notification means for notifying the operator of the above contents and an input means for inputting an operation continuation instruction from the operator.

Next, a method for cleaning and separating magnetic nanoparticles and a method for producing magnetic nanoparticles using the manufacturing system 11 including the cleaning and separating system 10 shown in FIG. 1 will be described with reference to the flowcharts shown in FIGS. 8 to 15. These operations (each operation is indicated by "ST" in the figure) are repeatedly executed every time magnetic nanoparticles are manufactured. In the initial state, the cleaning liquids used in the third and fourth cleanings in the previous production of the magnetic nanoparticles are collected and stored in the first cleaning liquid recovery tank 60A and the second cleaning liquid recovery tank 60B, and the cleaning liquids are stored. The supply tank 64 contains an unused cleaning liquid, and the on-off valves 101, 102, 106 to 108 are all closed.

As shown in FIG. 8, the operation of the cleaning separation system 10 is a step of separating the magnetic nanoparticles from the mixture of the reaction solvent and the magnetic nanoparticles (ST1) and a step of cleaning the magnetic nanoparticles separated from the reaction solvent (ST1). ST2), a step of separating the magnetic nanoparticles from the mixture of the cleaning liquid and the magnetic nanoparticles, a step of transporting the magnetic nanoparticles to the drying apparatus 50 (ST3), and a drying step (ST4) are performed in this order.

First, the step (ST1) of separating the magnetic nanoparticles from the mixture of the reaction solvent and the magnetic nanoparticles will be described with reference to the flowchart of FIG. When the mixture of the reaction solvent and the magnetic nanoparticles is introduced from the reactor 12 into the processing container 40 (ST11), the controller 53 controls the moving mechanism 46 of the processing container magnet 45 to control the bottom wall of the processing container 40. The magnet 45 is brought close to 41 from below (ST12) and allowed to stand for a predetermined time to perform sedimentation treatment (ST13). As a result, the magnetic nanoparticles and the supernatant liquid to be deposited on the bottom wall 41 of the processing container 40 are obtained. The obtained supernatant is a reaction solvent containing magnetic nanoparticles that did not settle by the settling treatment.

When the controller 53 detects that a predetermined time required for the settling process has elapsed, the controller 53 notifies the operator by a notification means such as a touch panel that the settling process is completed and the apparatus main body 21 is installed (ST14). Upon confirming the notification, the operator installs the device main body 21A and 21B, and operates the switching valve 100 so that the supernatant liquid flows through the device main body 21A. Further, the handle 36b of the moving mechanism 36A is operated to bring the magnet 35 closer to the device main body 21 (ST15). The operator issues an operation continuation instruction to the controller 53 by an input means such as a touch panel.

The controller 53 switches the three-way valves 103, 104, 105, and 109 so that the supernatant liquid flows from the separation device 20 to the solvent recovery tank 61. Then, when the controller 53 opens the on-off valve 102 and drives the pump 110 (ST16), the supernatant liquid flows from the processing container 40 to the conduit 121 and is introduced into the device main body 21A of the separation device 20. The magnetic nanoparticles contained in the supernatant liquid are deposited on a part of the bottom wall 30a which is a flow path by the attractive force between the magnet 35 and the bottom wall 30a of the apparatus main body 21A (ST17). As a result, the magnetic nanoparticles contained in the supernatant liquid are separated. The supernatant liquid that has passed through the apparatus main body 21A is stored in the solvent recovery tank 61 through the conduit 122. When the controller 53 detects that all the supernatant liquid in the processing container 40 has been derived by the sensor provided in the processing container 40 (ST18), the on-off valve 102 is closed and the pump 110 is stopped (ST19). , Proceed to the next step. If it is not detected that all the supernatant liquid has been derived from the processing container 40, the process waits in ST17 until it is detected.

The suction speed of the pump is appropriately set according to the reaction solvent, the capacity of the processing container, and the like. The reaction solvent contained in the solvent recovery tank 61 is transferred to the solvent disposal tank 63 by the on-off valve 108 and the pump 113 and then discarded, but may be reused after being stored in the solvent recovery tank 61.

Next, the step (ST2) of washing the magnetic nanoparticles separated from the reaction solvent will be described with reference to the flowcharts of FIGS. 10 to 13. This step includes a step of stirring and washing the first to third times and a step of separating the magnetic nanoparticles from the supernatant liquid (FIGS. 10 to 12) and a step of performing a fourth stirring and washing (FIG. 13). In the present embodiment, the magnetic nanoparticles deposited in the processing container 40 are stirred four times to wash the magnetic nanoparticles, but the number of stirrings is appropriately set in advance depending on the type of the magnetic nanoparticles to be produced and the reaction solvent. It is stored in the storage unit.

The first stirring cleaning and the step of separating the magnetic nanoparticles from the supernatant liquid will be described with reference to the flowchart of FIG. The controller 53 opens the on-off valve 106 to operate the pump 111, and introduces the cleaning liquid contained in the first cleaning liquid recovery tank 60A into the processing container 40 via the conduit 123 (ST21). The controller 53 uses a sensor (not shown) to detect that all the cleaning liquid has been taken out from the first cleaning liquid recovery tank 60A, and closes the on-off valve 106. Next, the moving mechanism 46 of the processing container magnet 45 is controlled to separate the processing container magnet 45 from the bottom wall 41 of the processing container 40 (ST22). Then, the stirrer 44 is operated to stir and clean the magnetic nanoparticles and the cleaning liquid (ST23). The controller 53 controls the moving mechanism 46 of the magnet 45 for the processing container to bring the magnet 45 close to the bottom wall 41 of the processing container 40 (ST24), and allows the obtained mixture of the cleaning liquid and the magnetic nanoparticles to stand for a predetermined time. Then, the sedimentation treatment is performed (ST25). As a result, magnetic nanoparticles and a supernatant liquid deposited on the bottom wall 41 of the processing container 40 can be obtained. The obtained supernatant liquid is a cleaning liquid containing magnetic nanoparticles that did not settle by the settling treatment.

The controller 53 switches the three-way valves 103, 104, 105, and 109 so that the supernatant liquid flows from the separation device 20 to the waste liquid tank 62. When the controller 53 opens the on-off valve 102 and drives the pump 110 (ST26), the supernatant liquid is taken out from the processing container 40, flows through the conduit 121 to the device main body 21A of the separation device 20, and is contained in the supernatant liquid. The magnetic nanoparticles are deposited on a part of the bottom wall 30a, which is a flow path, by the attractive force between the magnet 35 and the bottom wall 30a of the apparatus main body 21A. As a result, the magnetic nanoparticles contained in the supernatant liquid are separated and recovered. The supernatant liquid that has passed through the apparatus main body 21A is stored in the waste liquid tank 62 through the conduit 122 (ST27). When the controller 53 detects that all the supernatant liquid in the processing container 40 has been derived by the sensor provided in the processing container 40 (ST28), the on-off valve 102 is closed and the pump 110 is stopped (ST29). , Proceed to the next step ST31. If it is not detected that all the supernatant liquid has been derived from the processing container 40, the ST28 waits until it is detected.

Next, the second step of stirring and washing and the step of separating the magnetic nanoparticles from the supernatant liquid will be described with reference to the flowchart of FIG. The controller 53 opens the on-off valve 107 to operate the pump 111, and introduces the cleaning liquid contained in the second cleaning liquid recovery tank 60B into the processing container 40 via the conduit 123 (ST31). The controller 53 uses a sensor (not shown) to detect that all the cleaning liquid has been taken out from the second cleaning liquid recovery tank 60B, and closes the on-off valve 107. Then, the operations of ST32 to ST39 are performed, but since the operations of ST32 to ST39 are the same as those of ST22 to ST29, the description thereof will be omitted.

Next, the third step of stirring and washing and separating the magnetic nanoparticles from the supernatant liquid will be described with reference to the flowchart of FIG. The controller 53 opens the on-off valve 101 and introduces the cleaning liquid contained in the cleaning liquid supply tank 64 into the processing container 40 via the conduit 120 (ST41). The controller 53 uses a sensor (not shown) to detect that a required amount of cleaning liquid has been taken out from the cleaning liquid supply tank 64, and closes the on-off valve 101. Next, the operations of ST42 to ST49 are performed, but since the operations of ST42 to ST45 and ST48 to ST49 are the same as the operations of ST22 to ST25 and ST27 to ST29, the description thereof will be omitted and the operations of ST46 and ST47 will be described below. do.

The controller 53 switches the three-way valves 103, 104, 105, and 109 so that the supernatant liquid flows from the separation device 20 to the first cleaning liquid recovery tank 60A. When the controller 53 opens the on-off valve 102 and drives the pump 110 (ST46), the supernatant liquid is taken out from the processing container 40. The supernatant liquid at this time flows through the conduit 121 to the device main body 21A of the separation device 20, and the magnetic nanoparticles contained in the supernatant liquid are attracted by the attractive force between the magnet 35 and the bottom wall 30a of the device main body 21A. It is separated and recovered by accumulating on a part of the bottom wall 30a which is a flow path. The supernatant liquid that has passed through the apparatus main body 21A is stored in the first cleaning liquid recovery tank 60A through the conduit 122 (ST47). The cleaning liquid contained in the first cleaning liquid recovery tank 60A is used in the first stirring cleaning during the production of the next magnetic nanoparticles.

By the steps shown in FIGS. 10 to 12, magnetic nanoparticles are deposited on the bottom wall 30a of the main body 30 of the main body 21A. The operator confirms the amount of magnetic nanoparticles recovered in the apparatus main body 21A after the steps of FIGS. 10 to 12 are completed or each step of FIGS. 10 to 12 is completed. If the amount exceeds a predetermined amount, the apparatus main body 21A is removed from the plate-shaped support member 33A, and the magnetic nanoparticles are conveyed together with the apparatus main body 21A. The magnetic nanoparticles are taken out from the apparatus main body 21A and conveyed to the drying apparatus 50. In the following description, it is assumed that the device main body 21A is removed from the plate-shaped support member 33A and the replacement device main body 21A'is attached to the plate-shaped support member 33A.

Next, as shown in FIG. 13, the step of the fourth stirring cleaning is performed, but since ST51 to ST53 are the same as ST41 to ST43 of the third cleaning, the description thereof will be omitted. That is, when the cleaning liquid is introduced and stirring is performed by the stirrer 44, the fourth stirring cleaning step is completed.

Next, a step of separating the magnetic nanoparticles from the mixture of the cleaning liquid and the magnetic nanoparticles and a step of transporting the magnetic nanoparticles to the drying device 50 (ST3) will be described with reference to the flowcharts of FIGS. 14 and 15. At the end of ST43, the processing container 40 contains a mixture of the cleaning liquid after stirring and the magnetic nanoparticles.

The controller 53 switches the three-way valve 109 so that the mixture flows from the separation device 20 to the processing container 40. Then, when the controller 53 opens the on-off valve 102 and drives the pump 110 (ST61), the mixture is taken out from the processing container 40. At this time, the mixture flows through the conduit 121 to the device main body 21A'of the separation device 20, and the magnetic nanoparticles contained in the mixture flow due to the attractive force between the magnet 35 and the bottom wall 30a of the device main body 21A'. It is deposited on a part of the bottom wall 30a which is a road. This separates the magnetic nanoparticles contained in the mixture. The mixture that has passed through the device body 21A'is flowed through the conduit 126 to the processing vessel 40. That is, the mixture circulates in the processing vessel 40, the separating device 20, and the circulation path formed by the conduit 121 connecting each, a part of the conduit 122, and the conduit 126 (ST62).

The controller 53 notifies the operator to confirm whether or not it is necessary to switch the device main body 21 by a notification means such as a touch panel (ST63). The operator confirms the amount of magnetic nanoparticles deposited on the device main body 21 and determines whether or not the device main body 21 needs to be switched (ST64). The switching valve 100 is operated so that the mixture flows. Further, the handle 36b of the moving mechanism 36B is operated to bring the magnet 35 closer to the device main body 21B (ST65). Then, the mixture flows through the conduit 121 to the device main body 21B of the separation device 20, and the magnetic nanoparticles contained in the mixture flow in the flow path due to the attractive force between the magnet 35 and the magnet 35 close to the bottom wall 30a of the device main body 21B. It is deposited on a part of a certain bottom wall 30a, and magnetic nanoparticles are separated. The mixture that has passed through the device body 21B is returned to the processing vessel 40 through the conduit 126 (ST66).

Further, when a predetermined amount of magnetic nanoparticles are not deposited in ST64, the operator determines whether the separation of the magnetic nanoparticles needs to be continued or whether the separation is completed (ST72). When the separation is continued, the ST64 waits until a predetermined amount of magnetic nanoparticles are deposited on the apparatus main body 21A'. If the worker determines that the separation has been sufficiently performed and the separation process has been completed, the process proceeds to ST81.

While the mixture is flowing through the device body 21B, the operator rotates the handle 36b of the moving mechanism 36 of the magnet 35 of the separating device 20 to separate the magnet 35 from the device body 21A', and causes the magnetic nanoparticles to be separated from the device body 21A'. 21A'is removed from the plate-shaped support member 33A and conveyed to the drying device 50 (ST67). Further, a replacement device main body 21A ″ is attached to the plate-shaped support member 33. The lid 22 of the device main body 21A'may be removed and the magnetic nanoparticles may be conveyed to the drying device 50 together with the main body 30 of the device main body 21A'.

The operator confirms the amount of magnetic nanoparticles deposited on the device main body 21B to determine whether or not the device main body 21 needs to be switched (ST68), and if switching is necessary, the device main body 21A''. The switching valve 100 is operated so that the mixture flows. Further, the handle 36b of the moving mechanism 36A is operated to bring the magnet 35 closer to the device main body 21A ″ (ST69). The mixture flows through the conduit 121 to the device body 21A'' of the separation device 20, and the magnetic nanoparticles contained in the mixture flow due to the attractive force between the magnet 35 and the magnet 35 close to the bottom wall 30a of the device body 21A''. It is deposited on a part of the bottom wall 30a which is a road (the part of the bottom wall 30a corresponding to the magnet 35 and the peripheral part thereof), and the magnetic nanoparticles are separated. The mixture that has passed through the device body 21A ″ is returned to the processing vessel 40 via the conduit 126 (ST70).

Further, when a predetermined amount of magnetic nanoparticles are not deposited in ST68, the operator determines whether the separation of the magnetic nanoparticles needs to be continued or whether the separation is completed (ST73). When the separation is continued, the ST68 waits until a predetermined amount of magnetic nanoparticles are deposited on the apparatus main body 21B. If the worker determines that the separation has been sufficiently performed and the separation process has been completed, the process proceeds to ST81.

While the mixture is flowing through the device main body 21A'', the operator rotates the handle 36b of the moving mechanism 36 of the magnet 35 of the separating device 20 to separate the magnet 35 from the device main body 21B, and makes the device main body 21B a plate. It is removed from the shape support member 33B and conveyed to the drying device 50 (ST71). Further, a replacement device main body 21B'is attached to the plate-shaped support member 33B. Then, the operation after ST64 is repeated.

In ST64 and ST68, when the operator determines that the separation process of the magnetic nanoparticles has been completed, the operator issues a command to the controller 53 to end the operation. The controller 53 switches the three-way valves 103, 104, 109, drives the pump 110, and stores the cleaning liquid in the second cleaning liquid recovery tank 60B via the conduit 121, the apparatus main body 21, and the conduit 122 (ST81). The cleaning liquid contained in the second cleaning liquid recovery tank 60B is used in the second stirring cleaning during the production of the next magnetic nanoparticles.

In the drying step (ST4), as shown in FIG. 7, the device main body 21 is arranged on the shelf board 51 of the drying device 50. The drying device 50 dries the magnetic nanoparticles based on the set temperature, time, and the like in the device. When the operation of the drying device 50 is completed, the operator takes out the magnetic nanoparticles from each device main body 21 to obtain dried magnetic nanoparticles. In this way, dried magnetic nanoparticles are produced.

In the above description of the method for cleaning and separating the magnetic nanoparticles and the method for producing the magnetic nanoparticles, an example is described in which the separation device 20 has two sets including the device main body 21, the magnet 35, the moving mechanism 36, and the like. However, when the number of sets is one, the operator confirms the amount of magnetic nanoparticles deposited on the device main body 21 and determines whether or not the device main body 21 needs to be switched (ST64), and the switching is performed. If necessary, the operation of the pump 111 is stopped to prevent the mixture from flowing out of the processing container 40 before operating the switching valve 100 in ST65. After switching the apparatus main body 21, the operation of the pump 111 is restarted, and the process returns to ST64. When the number of sets is three or more, the flow of the mixture is switched by the switching valve 100 so that the mixture flows in each set in order.

Further, the manufacturing system 11 of the present embodiment includes a drying device 50, and the magnetic nanoparticles separated by the separating device 20 are transported to the drying device 50, but the transport location is not limited to the drying device 50 and is magnetic. The nanoparticles may be transported to any place, such as a processing container for performing the next processing on the nanoparticles.

According to the cleaning separation system 10 of the present embodiment, the time required for producing the magnetic nanoparticles can be shortened.

According to the present embodiment, by applying an attractive force to the magnetic nanoparticles mixed liquid by the magnet 45 for the processing container during the sedimentation treatment in the processing container 40, the sedimentation treatment is required as compared with the case where the magnet 45 for the processing container is not provided. The time can be shortened. In addition, since the separated magnetic nanoparticles can be removed and transported together with the main body 21 of the apparatus, there is no need to transfer the separated magnetic nanoparticles to the transport container as in the prior art, and the work efficiency is improved and the manufacturing time is shortened. Will be done. Further, a plurality of device main bodies 21 of the separation device 20 are provided, and the device main body 21 through which the magnetic nanoparticles mixed liquid flows is switched by the switching valve 100, and while the magnetic nanoparticles mixed liquid is flowing through the other device main bodies 21. Since the apparatus main body 21 in which a predetermined amount of magnetic nanoparticles has already been deposited can be removed and transported, the time required for separation can be shortened.

Further, since the magnetic nanoparticles are separated into a plurality of device main bodies 21 in small portions, it is easy to carry. Further, by providing the device main body 2 for replacement according to the amount of magnetic nanoparticles to be separated, a desired amount of magnetic nanoparticles can be separated.

When the magnetic nanoparticles are separated from the mixture of the cleaning liquid and the magnetic nanoparticles after the cleaning is completed, the mixture that has passed through the separating device returns to the processing container 40 through the three-way valve 109 and the conduit 126. That is, the mixture circulates in the processing vessel 40, the separator 20, and the conduit 121 connecting them, a part of the conduit 122, and the circulation path formed by the conduit 126, and the mixture circulates in the separator 20. Since it passes through many times, the magnetic nanoparticles can be reliably deposited on the separation device 20. Further, in the separation device 20, by using the magnet 35, it is possible to surely separate the magnetic nanoparticles contained in the mixture and the supernatant liquid while flowing the mixture and the supernatant liquid in the flow path.

Further, when the device main body 21 is placed on the shelf plate 51 in the drying device 50, one end of the conduit is located below the flow path, so that the flow path is lifted by one end of the conduit and the flow path is opened. Since it does not come into direct contact with the shelf board 51, temperature differences are less likely to occur in the deposited magnetic nanoparticles, and aggregation can be prevented. Further, by inclining the flow path of the device main body 21 of the separation device 20, the mixture can easily flow from the introduction port 24 toward the outlet port 31.

Since the cleaning separation system 10 of the present embodiment includes the drying device 50, the magnetic nanoparticles can be conveyed to the drying device 50 together with the device main body 21 to perform the drying step.

Further, according to the washing separation system 10 of the present embodiment, the supernatant obtained by the precipitation treatment of the mixture of the reaction solvent and the magnetic nanoparticles or the supernatant obtained by the precipitation treatment of the mixture of the washing liquid and the magnetic nanoparticles. Since the liquid is flowed through the separation device 20 to separate the magnetic nanoparticles contained in the supernatant liquid, the recovery efficiency of the magnetic nanoparticles can be improved as compared with the case where the magnetic nanoparticles are not separated from the supernatant liquid.

Although one embodiment of the present invention has been described above, the present invention is not limited to the above embodiment, and various modifications can be made without departing from the spirit of the present invention.

10 Cleaning separation system 11 Manufacturing system 20 Separation device 21 (21A, 21B, 21A', 21A'', 21B') Device main body 22 Lid 24 Introductory port 30 Main body 31 Outlet port 32 Outlet tube 33 (33A, 33B) Plate Shape support member (support means)
35 (35A, 35B) Magnet 36 (36A, 36B) Moving mechanism 40 Processing container 45 Processing container magnet 47 Processing device 100 Switching valve (switching means)
50 Drying device 51 Shelf board 53 Controller 60A First cleaning liquid recovery tank 60B Second cleaning liquid recovery tank 61 Solvent recovery tank 62 Waste liquid tank

Claims (8)

A step of cleaning magnetic nanoparticles in a processing device, a step of introducing a cleaning liquid into the processing device containing the magnetic nanoparticles, and a step of introducing the cleaning liquid.
The step of stirring the introduced mixture of the cleaning liquid and the magnetic nanoparticles, and
A step of performing sedimentation treatment on the mixture placed in a magnetic field, and
Including a step of pouring out the supernatant liquid obtained by the sedimentation treatment from the treatment apparatus.
The step of introducing the cleaning liquid and the step of stirring are performed a plurality of times.
After the final stirring step, the step of performing the sedimentation treatment and the step of pouring out the supernatant liquid are not performed.
Further, a separation step of flowing the mixture derived from the processing device into the flow path of the separation device, depositing magnetic nanoparticles contained in the mixture in a part of the flow path arranged in a magnetic field, and separating the mixture. A method for cleaning and separating magnetic nanoparticles containing particles. The method for cleaning and separating magnetic nanoparticles according to claim 1, further comprising a step of returning the mixture that has passed through the flow path to the processing apparatus. A method for producing magnetic nanoparticles, which comprises a step of transporting the magnetic nanoparticles deposited on a part of the flow path to a predetermined place together with the part by the washing separation method according to claim 1 or 2. In the transporting step, the magnetic nanoparticles are transported to the drying device.
The method for producing magnetic nanoparticles according to claim 3, further comprising a step of drying the magnetic nanoparticles with the drying device. A processing device for cleaning magnetic nanoparticles and
Equipped with a separator for separating magnetic nanoparticles,
The processing apparatus comprises a processing container containing a mixture of a cleaning liquid and magnetic nanoparticles, and a magnet arranged below the processing container and generating a magnetic field acting on the mixture.
The separation device is arranged below the device main body and a device main body that constitutes a part of a flow path through which the mixture introduced from the processing container flows and magnetic nanoparticles contained in the mixture are deposited. A cleaning and separation system for magnetic nanoparticles comprising a magnet that produces a magnetic field acting on the mixture flowing through the portion of the flow path. The device main body of the separation device is connected to the processing container and is connected to an introduction port for introducing the mixture, a flow path through which the mixture introduced from the introduction port is flowed, and the processing container. The cleaning and separation system for magnetic nanoparticles according to claim 5, further comprising an outlet from which the mixture flowing through the flow path is led out toward the processing container. The cleaning and separation system for magnetic nanoparticles according to claim 6, wherein the main body of the device is freely detachable from the supporting means. The cleaning and separation system for magnetic nanoparticles according to any one of claims 5 to 7.
A magnetic nanoparticles manufacturing system including a drying device in which the main body of the separation device is housed and the nanoparticles accumulated in the flow path are dried.

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