JP2006272132A - Method and apparatus for manufacture of chemical substance - Google Patents

Abstract

<P>PROBLEM TO BE SOLVED: To provide a method and an apparatus for manufacturing a chemical substance which enable manufacture of a high-quality chemical substance because, even for a reaction system producing a gas during the first mixing reaction, the mixing can be performed uniformly and efficiently without disturbance of bubbles of the gas, while the gas in the reaction solution can be degassed thoroughly before the second mixing reaction. <P>SOLUTION: The method of manufacturing a chemical substance through a reaction producing a gas has the first mixing process of carrying out the first mixing reaction of two or more solutions L1 and L2 in the first tightly closed mixer 12, a degassing process of degassing bubbles 98 of the gas produced in the reaction solution LM prepared in the first mixing process, in a degassing unit 14 equipped with a gas-liquid interface 84 and the second mixing process of adding an additional solution L3 to the reaction solution LM degassed in the degassing process to carry out the second mixing reaction in the second mixer 13. The reaction solution LM is fed rapidly from the first mixing process to the degassing process, while fed to the second mixing process after completion of the degassing in the degassing process. <P>COPYRIGHT: (C)2007,JPO&INPIT

Description

  The present invention relates to a method and apparatus for producing a chemical substance, and more particularly to a method and apparatus for producing a chemical substance suitable for producing a chemical substance in a reaction system in which gas bubbles are generated by a liquid-liquid reaction.

  When handling a reaction system in which gas bubbles are generated in a liquid-liquid reaction, in order to stabilize the reaction at the start of the reaction and in the course of the reaction, the bubbles are actively removed in both the batch process and the continuous flow process. Need to degas.

  An example of a reaction system that generates a gas is the production of magnetic particles contained in a magnetic layer of a magnetic recording medium. In order to produce magnetic particles having a small particle size and excellent monodispersity, the liquids that initiate the reaction for forming the metal fine particles must be mixed uniformly and efficiently, and the gas generated by the reaction It is necessary to remove it quickly so that (for example, hydrogen gas) does not interfere with the mixing.

  However, the reaction system with gas generation is difficult to continuously process, and there is almost no prior art. This is because, in the case of continuous processing, if bubbles are mixed, the flow of continuous processing becomes unstable, the mixing field and reaction field become non-uniform, and the reaction equilibrium does not easily advance to the reaction promoting side. This is because the liquid feeding to the subsequent process becomes unstable and the quality of the chemical substance to be produced is difficult to be uniform.

As a conventional manufacturing apparatus having a degassing function, there is Patent Document 1, in which a stirrer for mixing is provided in a lower part in a reaction tank for performing a chemical reaction, and a defoaming blade is provided in an upper part in the reaction tank. It is disclosed that the bubbles of gas floating in the liquid are mechanically defoamed by destroying the bubbles of the gas with the force of the defoaming blade.
JP-A-9-10507

  However, in the manufacturing apparatus of Patent Document 1, when a solution is fed from a tank to a reaction tank and stirred for a certain time in the reaction tank and then discharged, a mixing reaction operation and a degas operation with a stirrer are performed in the reaction tank. Will proceed simultaneously. As a result, bubbles are accumulated in the reaction tank, so that the bubbles interfere with the mixing of the reaction liquids by the stirrer and the stirring efficiency is lowered. Due to the decrease in the stirring efficiency, the mixing for starting the reaction is not uniformly performed, so that the reaction at the start of the reaction and the reaction progressing process becomes unstable.

  In addition, when the additive solution must be added to the reaction solution in the first mixing reaction and the second mixing reaction must be performed as in the production of magnetic particles, the gas generated in the first mixing reaction There is a problem that fine and monodispersed magnetic particles cannot be produced unless a second mixing reaction is performed after sufficiently degassing the bubbles.

  The present invention has been made in view of such circumstances, and even in a reaction system in which gas is generated during the first mixing reaction, mixing can be performed uniformly and efficiently without being obstructed by gas bubbles. An object of the present invention is to provide a method and an apparatus for producing a chemical substance capable of producing a high-quality chemical substance because the gas in the reaction solution can be sufficiently degassed before the second mixing reaction. And

  According to claim 1 of the present invention, in order to achieve the above object, in a method for producing a chemical substance that produces a chemical that generates gas along with the reaction, a plurality of solutions are mixed and reacted in a first mixing unit of a closed system. A first mixing step to be performed; a degassing step of degassing a gas bubble generated from the reaction solution mixed and reacted in the first mixing step in a degassing section having a gas-liquid interface; and the degassing step And a second mixing step in which an addition solution is added to the reaction solution degassed in step 2 and a mixing reaction is performed in the second mixing unit, and the reaction solution is sent from the first mixing step to the degassing step. In addition, the present invention provides a method for producing a chemical substance, characterized in that after the degassing in the degassing step is completed, the liquid is sent to the second mixing step.

  According to the first aspect of the present invention, the first mixing portion of the closed system in the first mixing step in which the first mixing reaction is performed, and the gas bubbles generated when the reaction is started by mixing are removed from the reaction solution. The degassing part having a liquid interface was separated. And since the reaction liquid mixed at the 1st mixing process was sent to the degassing process, mixing was performed uniformly and efficiently in the 1st mixing part without being disturbed by the gas bubble generated with reaction. It can be carried out. Thereby, the reaction at the start of the reaction can be stabilized.

  Further, gas bubbles generated as the reaction proceeds are efficiently degassed from the gas-liquid interface in the degassing section. Thereby, the reaction in the course of the reaction can be stabilized, and the flow of the reaction liquid in the degassing part is stabilized. Therefore, since the liquid feeding amount from the degassing step to the second mixing step can be stabilized, mixing can be performed at an accurate mixing ratio, and mixing can be performed uniformly and efficiently without being disturbed by bubbles.

  Here, although it is time to send the reaction liquid from the first mixing section to the degassing section, it is preferable to select the method according to the reaction rate to be handled. For example, when gas bubbles are generated immediately after completion of mixing at a high reaction rate, it is preferable to immediately send the reaction solution to the degassing unit within 0.1 to 5 seconds after mixing in the first mixing unit. More preferably, it is within 0.1 to 3 seconds.

  In addition, the method for producing a chemical substance of the present invention batch-mixes the liquid charged in the first mixing unit, and when the mixing is completed, all the reaction liquid mixed in the first mixing unit is charged in the degassing unit. In addition, it may be used for a batch system in which the degassed reaction liquid is charged into the second mixing unit, or a tank for storing liquid is prepared, and the first mixing unit, degassing unit, second tank are prepared from the tank. You may use for the continuous flow system which flows continuously in the order of a mixing part.

  A second aspect of the present invention is characterized in that, in the first aspect, a plurality of stages of mixing / degassing units including the first mixing step and the degassing step are provided in series.

  Depending on the reaction system, a plurality of stages of mixing and desulfurization processes in which the first mixing process and the degassing process are combined may be provided in series.

  A third aspect of the present invention provides the first solution according to the first or second aspect, wherein the first mixing step includes a first solution containing two or more metal ions selected from groups 8, 9 and 10 of the periodic table, and a reducing agent. In the second mixing step, the reaction solution mixed in the first mixing step is mixed with one or more selected from Group 11, 12, 13, 14 and 15 of the periodic table. A third solution containing metal ions is added and mixed to produce magnetic particles as the chemical substance.

  Claim 3 defines a preferable solution for producing magnetic particles as a chemical substance, and can effectively exhibit the effects of the present invention, so that magnetic particles excellent in monodispersity can be produced. it can.

  A fourth aspect of the present invention is characterized in that in any one of the first to third aspects, instantaneous mixing is performed in at least the first mixing step of the first mixing step and the second mixing step.

  This is because if the time from the start of mixing to the end of mixing is long in the first mixing step, there is a problem that the gas generated in the latter half of the mixing lowers the mixing efficiency, but there is no such problem if instantaneous mixing is performed.

  According to a fifth aspect of the present invention, in any one of the first to fourth aspects, the degassing part is a passage that forms the gas-liquid interface by a liquid part formed by the reaction liquid and a space part in which the gas removed from the reaction liquid is accumulated. And the bubble of the gas in the reaction liquid which flows through the said channel | path is removed to the said space part, It is characterized by the above-mentioned.

  Since the degassing part is configured as a passage having a gas-liquid interface between the liquid part by the reaction liquid and the space part in which the gas removed from the reaction liquid is accumulated, the gas generated as the reaction proceeds Bubbles can be removed continuously and efficiently from the gas-liquid interface. Moreover, since the passage length for degassing can be ensured long by using the passage, degassing can be reliably performed.

  A sixth aspect of the present invention according to the fifth aspect is characterized in that the pressure in the space portion is reduced.

  In this way, by reducing the pressure in the space, gas bubbles in the reaction solution will escape into the space.

A seventh aspect of the present invention is the method according to the fifth or sixth aspect, wherein the passage has an ascending passage and a descending passage through which the reaction solution continuously flows, and the air interface is provided at a portion where the flow is reversed from the ascending passage to the descending passage. It is characterized by forming.

  According to the seventh aspect, since the gas-liquid interface is formed in the portion where the flow of the reaction liquid is reversed from the ascending passage to the descending passage, the bubbles rising together with the reaction solution in the ascending passage stay at the gas-liquid interface, and the reaction Only descend the down passage. Bubbles staying at the gas-liquid interface are gradually broken and collected as gas in the space. In this way, by providing the reaction liquid ascending passage in the passage, both the buoyancy of the bubbles and the ascent of the reaction liquid can be used, so that the bubbles can be more effectively levitated and separated. .

  An eighth aspect is characterized in that, in any one of the fifth to seventh aspects, the reaction temperature is controlled by heating or cooling the reaction liquid flowing through the degassing section.

  By controlling the reaction temperature by heating or cooling the reaction liquid flowing through the degassing section, the reaction conditions can be kept constant regardless of the temperature and room temperature, so the amount of gas generated is not affected by the temperature. Can be kept constant. This makes it possible to perform degassing with high accuracy and accurately reproduce the degassing amount in the designed degassing device regardless of the season and room temperature. Can be fixed.

A ninth aspect is characterized in that in any one of the fifth to eighth aspects, ultrasonic waves are applied to the reaction liquid flowing through the degassing section.

  Bubbles attached to the wall of the passage are difficult to be degassed, but by attaching ultrasonic waves to the reaction liquid flowing through the degassing part and vibrating the reaction liquid, the bubbles attached to the wall surface are easily peeled off. Bubbles can be degassed.

A tenth aspect of the present invention is characterized in that, in any one of the fifth to ninth aspects, the flow rate of the reaction liquid flowing through the descending passage is slower than the rising speed of the bubbles.

  Gas bubbles are also generated in the reaction liquid flowing in the descending passage, but in the descending passage, the buoyancy of the bubbles and the flow of the reaction liquid are reversed, and the bubbles are less likely to float and separate at the gas-liquid interface. Therefore, if the flow rate of the reaction liquid flowing in the descending passage is made slower than the rising speed of the bubbles, the bubbles can be efficiently levitated and separated also in the descending passage.

An eleventh aspect is characterized in that, in any one of the first to tenth aspects, the inside of the degassing part can be seen through.

  Since the inside of the degassing part can be seen through, the degassing state can be accurately grasped.

  According to a twelfth aspect of the present invention, in order to achieve the above object, in a chemical substance production apparatus for producing a chemical substance that generates a gas in response to a reaction, a closed first mixing unit that performs a mixing reaction with a plurality of solutions. Between the reaction solution mixed in the first mixing unit and the second mixing unit in which the addition solution is added to the reaction solution mixed in the first mixing unit to perform a mixing reaction. There is provided a chemical substance production apparatus characterized in that a degassing part having a gas-liquid interface for removing bubbles from the reaction liquid is provided.

  The twelfth aspect of the present invention is configured as an apparatus, and in the first mixing section, the mixing can be performed uniformly without being obstructed by gas bubbles generated by the reaction. The reaction in the course of progress can be stabilized. In addition, since the gas bubbles generated as the reaction proceeds are efficiently degassed from the gas-liquid interface in the degassing part, the reaction in the reaction progressing process can be stabilized and the reaction liquid in the degassing part can be stabilized. Therefore, the liquid can be stably fed to the second mixing unit that performs the second mixing reaction. Thereby, even in the second mixing unit, mixing can be performed uniformly and efficiently without being disturbed by bubbles.

  In a thirteenth aspect of the present invention, in the twelfth aspect, at least one of the first mixing section and the second mixing section has at least one liquid of the plurality of liquids in a mixing chamber having a residence time of 5 seconds or less. A high-pressure mixing device that supplies a high-pressure jet flow of 1 MPa or more and instantaneously mixes with another liquid.

  At least the first mixing unit of the first mixing unit and the second mixing unit supplies at least one liquid of the plurality of liquids to a mixed chamber having a residence time of 5 seconds or less by a high-pressure jet flow of 1 MPa or more. Since the high-pressure mixing device instantaneously mixes with other liquids, instantaneous mixing can be performed in the first mixing unit.

  A fourteenth aspect of the present invention is the method according to the twelfth or thirteenth aspect, wherein the degassing part is a passage that forms the gas-liquid interface by a liquid part by the reaction liquid and a space part in which the gas removed from the reaction liquid is accumulated. A degassing vessel having an inlet and an outlet for the reaction solution, a plurality of dam plates standing from the bottom of the degassing vessel and having an upper end located below the gas-liquid interface, and between the dam plates The upper end is located above the gas-liquid interface and the lower end is a baffle plate spaced from the bottom of the degassing container, and the reaction solution continuously flows in the degassing container. An ascending passage and a descending passage are formed, and the gas-liquid interface is formed at a portion where the flow is reversed from the ascending passage to the descending passage.

  Claim 14 shows a preferred embodiment in which the degassing part is configured as a passage having a gas-liquid interface between the reaction liquid and the space part. As described above, the degassing container includes a dam plate and a baffle plate. It constitutes a passage.

  A fifteenth aspect is characterized in that in the fourteenth aspect, the space portion is not partitioned by the baffle plate.

  Thus, the pressure of the whole space part can be equalized by not partitioning a space part with a baffle plate. In this case, a baffle plate may not be provided in a portion corresponding to the space portion, or a communication hole may be formed in a portion corresponding to the space portion of the baffle plate.

A sixteenth aspect is characterized in that, in the fourteenth or fifteenth aspect, the height of the weir plate is lowered from the entrance to the exit of the degassing vessel.

  This is because, in the passage formed in the degassing vessel, the closer to the inlet side, the larger the amount of gas generated from the reaction solution, and the smaller the amount of gas generated toward the outlet side. For this reason, it is necessary to ensure a longer passage length to the gas-liquid interface on the inlet side of the passage. Therefore, if the height of the weir plate is lowered as it goes from the inlet to the outlet of the degassing vessel, the passage length to the gas-liquid interface can be formed according to the amount of gas generated, and it is necessary to unnecessarily increase the passage length. Absent.

A seventeenth aspect is characterized in that in any one of the fourteenth to sixteenth aspects, a pressure adjusting means for adjusting the pressure of the space portion is provided.

  By adjusting the pressure in the space by the pressure adjusting means, it is possible to form a space pressure in which bubbles can easily escape from the reaction solution flowing through the passage.

  According to an eighteenth aspect of the present invention, in the degassing section according to any one of the twelfth to seventeenth aspects, the degassing section is provided with a temperature adjusting means for controlling a reaction temperature by heating or cooling the reaction liquid. And

  By controlling the reaction temperature by heating or cooling the reaction liquid flowing through the degassing section, the reaction conditions can be kept constant regardless of the temperature and room temperature, so the amount of gas generated is not affected by the temperature. Can be kept constant. This makes it possible to perform degassing with high accuracy and accurately reproduce the degassing amount in the designed degassing device regardless of the season and room temperature. Can be fixed.

  According to a nineteenth aspect of the present invention, in any one of the twelfth to eighteenth aspects, the degassing unit is provided with an ultrasonic wave applying unit that applies an ultrasonic wave to the reaction solution.

  Degassing efficiency can be improved by irradiating the reaction liquid flowing through the passage with ultrasonic waves.

A twentieth aspect of the present invention is characterized in that, in any one of the fourteenth to nineteenth aspects, a stirrer that forms a flow that prevents stagnation is provided at the bottom of the ascending passage formed in the degassing vessel. To do.

  For example, when metal fine particles are generated by reaction as in the production of magnetic particles, the metal fine particles easily settle at the bottom of the degassing vessel, but a stirrer that forms a flow that prevents stagnation at the bottom of the ascending passage It is possible to make it difficult to settle.

  A twenty-first aspect is characterized in that, in any one of the fourteenth to twentieth aspects, a cross-sectional area of the descending passage with respect to the ascending passage is made different.

  For example, if the flow rate of the reaction liquid flowing through the passage is set to be slower in the descending passage than in the ascending passage, bubbles generated in the descending passage are also easily floated and separated at the gas-liquid interface.

  A twenty-second aspect of the present invention is the method according to any one of the fourteenth to twenty-first aspects, wherein the inner surface of the degassing vessel, the surface of the barrier plate, and the surface of the baffle plate are subjected to a surface treatment that prevents the gas bubbles from adhering. It is characterized by being.

  Since surface treatment that prevents gas bubbles from adhering to the inner surface of the degassing container, the surface of the weir plate, and the surface of the baffle plate has been performed, the bubbles are less likely to adhere and are easily degassed.

  A twenty-third aspect is characterized in that, in any one of the fourteenth to twenty-second aspects, a bottom shape of a degassing container in which the flow of the reaction solution is reversed from the downward flow to the upward passage is formed in an arc shape.

  Since the bottom shape of the degassing vessel that reverses from the descending passage to the ascending passage is formed in an arc shape, the reaction solution flows smoothly in the passage, and even when fine particles are generated by the reaction as described above, the bottom of the container Therefore, it is difficult to deposit fine particles.

  Claims 24 and 25 are magnetic particles produced by the method and apparatus for producing a chemical substance of the present invention, and claim 26 is a magnetic recording medium containing the magnetic particles in a magnetic layer.

  As described above, according to the method and apparatus for producing a chemical substance of the present invention, even in a reaction system in which gas is generated during the first mixing reaction, mixing is performed uniformly without being disturbed by gas bubbles. In addition, since the gas in the reaction solution can be sufficiently degassed by the second mixing reaction, a high-quality chemical substance can be produced. Therefore, the present invention is effective for the production of magnetic particles contained in the magnetic layer of a magnetic recording medium, for example.

  Hereinafter, preferred embodiments of a method and an apparatus for producing a chemical substance according to the present invention will be described with reference to the accompanying drawings.

  FIG. 1 is an overall configuration diagram of a chemical substance manufacturing apparatus 10 according to the present invention.

  The chemical substance production apparatus 10 of the present invention can be applied to both a batch method and a continuous flow method in a liquid phase reaction method (liquid-liquid reaction) as long as it is a reaction that continuously generates gas as the reaction proceeds. However, in the present embodiment, an example in which metal fine particles contained in a magnetic layer of a magnetic recording medium are manufactured by a continuous flow method will be described below.

  As shown in FIG. 1, the chemical substance manufacturing apparatus 10 mainly includes a first mixing device 12 in a closed system that starts a reaction by mixing a first solution L1 and a second solution L2, and a first mixing device. From the reaction solution LM mixed and reacted in the first mixing device 12 between the second mixing device 13 that performs the mixing reaction by adding the third solution L3 to the reaction solution LM mixed and reacted in the device 12 A degassing device 14 for removing generated gas bubbles from the reaction liquid LM is provided.

  As the first solution L1, a solution containing two or more kinds of metal ions selected from groups 8, 9, and 10 of the periodic table can be suitably used. Fe, Pt, Co, Ni, Pd The metal ions are preferred. As the second solution L2, a reducing agent solution can be suitably used. As the third solution L3, a solution containing one or more metal ions selected from the groups 11, 12, 13, 14, and 15 of the periodic rate table can be suitably used. Cu, Ag, Au , Al, Zn, and Sn are preferred.

Of the liquid phase reaction methods, the reverse micelle method that allows easy control of the particle size of the metal fine particles is preferable, and the first to third solutions L1, L2, and L3 are made of a water-insoluble organic solvent containing a surfactant. It is preferable to prepare a reverse micelle solution. An oil-soluble surfactant is used as the surfactant to be used. Specifically, sulfonate type (for example, aerosol OT (manufactured by Wako Pure Chemical Industries), quaternary ammonium salt type (for example, cetyltrimethylammonium bromide), ether type (for example, pentaethylene glycol dodecyl ether) and the like can be mentioned. Further, preferable examples of the water-insoluble organic solvent for dissolving the surfactant include alkanes, ethers, alcohols, etc. The alkanes are preferably alkanes having 7 to 12 carbon atoms. Is preferably heptane, octane, isooctane, nonane, decane, undecane, dodecane, etc. The ether is preferably diethyl ether, dipropyl ether, dibutyl ether, etc. The alcohol is preferably ethoxyethanol, ethoxypropanol, or the like. , Reducing agent solution The reducing agent, alcohols, _{polyalcohols; H 2; HCHO, S 2} O 6 2-, BH 4 -, + N 2 H 5, H 2 PO 3 - be used alone compounds containing such However, it is preferable to use two or more in combination.

  The first solution L1 and the second solution L2 are separately prepared in the first preparation tank 16 and the second preparation tank 18 disposed in the vicinity of the first mixing device 12. That is, in the first preparation tank 16, a water-insoluble organic solvent containing a surfactant and a metal salt aqueous solution containing two or more kinds of metal ions selected from Groups 8, 9, and 10 of the periodic table are stirred. A reverse micelle solution of the first solution L1 is prepared by mixing at 16a. In the second preparation tank 18, a water-insoluble organic solvent containing a surfactant and a reducing agent aqueous solution are mixed with a stirrer 18a to prepare a reverse micelle solution of the second solution L2. In addition, heating jackets 20 and 20 are provided on the outer peripheries of the first preparation tank 16 and the second preparation tank 18, respectively, and are heated to an appropriate temperature at which an initial reaction is performed.

  Further, the third solution is prepared in a third preparation tank 15 disposed in the vicinity of the second mixing device 13. That is, a water-insoluble organic solvent containing a surfactant and a metal aqueous solution containing one or more metal ions selected from Groups 11, 12, 13, 14, and 15 of the periodic table are mixed with a stirrer 15a. A reverse micelle solution of the third solution L3 is prepared. A heating jacket 20 is provided on the outer periphery of the third preparation tank 15 and heated to an appropriate temperature.

  The first and second solutions L1 and L2 prepared in the first and second preparation tanks 16 and 18 are supplied to the first mixing device 12 via the supply pipes 22 and 24 by the supply pumps 26 and 28, respectively. Supplied. In the first mixing device 12, the two solutions L 1 and L 2 are instantaneously mixed and quickly discharged from the first mixing device 12, flowing through the pipe 30, and sent to the degassing device 14. The reaction is started by the mixing in the first mixing device 12, and gas is continuously generated from the reaction liquid LM as the reaction proceeds. The reaction liquid LM that has started the reaction in the first mixing device 12 proceeds in the degassing device 14, and the generated gas is continuously degassed via the gas-liquid interface. After the degassing, the reaction solution LM flows through the pipe 32 and is sent to the second mixing device 13, and the third solution L 3 is added from the third preparation tank 15 to the second mixing device 13 by the supply pump 17. Is done. In the second mixing device 13, the reaction liquid LM degassed by the degassing device 14 and the third solution L3 are mixed, and different metal atoms are continuously introduced into the crystal lattice of the metal fine particles formed by the initial reaction. Introduce (doping). Thereby, metal fine particles of a multi-component alloy are produced. The produced liquid containing the produced metal fine particles is sent to the product tank 21 through the pipe 19. In this case, it is preferable to add and mix the fourth solution L4 obtained by mixing the chelating agent solution and the reducing agent solution to the product solution mixed by the second mixing device 13. Accordingly, the product tank 21 is provided with a stirrer 21a, and a jacket 20 is provided on the outer periphery, and the product liquid is heated or cooled as necessary.

  In the reaction system that generates gas by chemical reaction, the first and second solutions Ll and L2 can be efficiently mixed by the first mixing device 12 without being disturbed by the generated gas, and further, the reaction proceeds. It is important that the generated gas is continuously and efficiently degassed by the degassing device 14 so that no gas bubbles remain in the reaction liquid to the second mixing device 13.

  According to the chemical substance manufacturing apparatus 10 of the present invention, a closed-system mixing apparatus 12 for mixing a plurality of solutions L1 and L2 to start a reaction, and gas bubbles generated when the reaction is started by mixing are generated. Since the degassing device 14 having a gas-liquid interface to be removed from the reaction liquid LM is separated and the reaction liquid LM mixed by the mixing device 12 is sent to the degassing device 14, the mixing device 12 accompanies the reaction. Thus, mixing can be performed uniformly and efficiently without being obstructed by the gas bubbles generated. Thereby, since mixing efficiency can be raised, an unreacted substance is lost and the yield of metal fine particles can be raised.

  In addition, since the gas bubbles generated as the reaction progresses are continuously and efficiently degassed in the degassing device 14, the reaction in the course of the reaction can be stabilized and continuously degassed. As a result, the flow of the reaction liquid LM in the degassing device 14 is stabilized, so that stable liquid feeding can be performed to the subsequent process. Thereby, since the reaction liquid LM is always sent to the second mixing device 13 in a stable liquid feeding amount, the reaction liquid LM is supplied from the third preparation tank 15 with the third solution L3 added in the specified addition amount. The mixing reaction can be performed at an accurate ratio between the two. In addition, since no bubbles remain in the reaction liquid LM fed to the second mixing device 13, the second mixing device 13 can perform mixing uniformly and efficiently without being disturbed by the bubbles. Thereby, since mixing efficiency can be raised, an unreacted substance is lost and the yield of metal fine particles can be raised.

  In the present invention, for example, when the reaction rate is high and gas bubbles are generated immediately after the mixing in the first mixing device 12, the gas is discharged by the degassing device 14 after the mixing is completed by the first mixing device 12. The time until the start is preferably about 0.1 to 5 seconds, more preferably about 0.1 to 3 seconds.

  Hereinafter, the preferable aspect of the 1st and 2nd mixing apparatuses 12 and 13 and the degassing apparatus 14 in this invention is demonstrated. Of the first and second mixing devices 12 and 13, at least the first mixing device 12 is preferably a mixing device of the type described below. The description is also an example of the first mixing device 12. explain.

(A) Mixing Device The first mixing device 12 is preferably of a type that can immediately discharge the reaction liquid LM that has been mixed by instantaneous mixing, and for example, a high-pressure mixing method can be suitably used. In the following, three types of high-pressure mixing methods of a one-jet type, a T-shape / Y-shape, and a two-jet facing type will be described. In addition, as long as instantaneous mixing is possible, not only a high pressure mixing system but any mixing system may be used, for example, a static mixer or the like can be used.

a) One-Jet Type FIG. 2 is a cross-sectional view showing the concept of the one-jet type first mixing device 12.

  As shown in FIG. 2, the first mixing device 12 includes a mixer 40 having a cylindrical mixing chamber 38 (mixing field) in which the first and second solutions L1 and L2 are mixed and reacted. A first conduit 42 for introducing the first solution L1 into the mixing chamber 38 is connected to the one end side opening, and a discharge pipe 44 for the reaction liquid LM mixed and reacted in the mixing chamber 38 is connected to the other end side opening. Is done. Further, a second conduit 46 for introducing the second solution L2 into the mixing chamber 38 is connected to the side of the mixer 40 near the outlet of the first conduit 42. A first orifice 48 and a second orifice 50 are formed in the distal ends of the first conduit 42 and the second conduit 46, respectively, thereby disturbing the first conduit 42 and the second conduit 46. A first nozzle 52 and a second nozzle 54 are formed for ejecting a stream of liquid. In FIG. 2, the first solution L1 is introduced from the first conduit 42 and the second solution L2 is introduced from the second conduit 46. However, both solutions can be reversed. Further, if the connection position of the discharge pipe 44 is in the vicinity of the other end side of the mixer 40, the discharge pipe 44 may be connected to the side surface portion of the mixer 40.

  A jacket 56 through which a heat medium having a relatively large heat capacity such as water and oil flows is wound around the outer periphery of the mixer 40, and the heat medium inlet 56A and the heat medium outlet 56B of the jacket do not show the heat medium. Connected to the supply device. The mixing reaction temperature is preferably set appropriately to a predetermined temperature suitable for the initial reaction depending on the types of the first and second solutions L1 and L2.

  In addition, when preparing the 1st solution L1 by the number of multiple types of metal atoms, and mixing these multiple solutions and the 2nd solution L2, one of these solutions is a high-pressure jet of 1 MPa or more. Just flow. Therefore, a plurality of nozzle positions for ejecting the plurality of first solutions L1 may be provided on the side surface side of the mixer 40, or the plurality of first solutions L1 may be ejected in order from one nozzle position. Good. Accordingly, the number of nozzles of the straight flow high-pressure jet flow is basically one, but there may be a plurality of nozzles of cross flow orthogonal to the straight flow.

  As a method of drilling the first and second orifices 48 and 50 in the block-shaped orifice material 58, as a processing method of precisely opening an ejection hole of about 100 μm in the orifice material 58 of metal, ceramics, glass or the like. Known micro cutting processing, micro grinding processing, injection processing, micro electric discharge processing, LIGA method, laser processing, SPM processing and the like can be suitably used.

  The material of the orifice material 58 is preferably a material having good workability and a hardness close to diamond. Therefore, as materials other than diamond, those obtained by hardening various metals and metal alloys such as quenching, nitriding, and sintering can be preferably used. Ceramics can also be suitably used because of its high hardness and superior workability than diamond. In the present embodiment, an example of an orifice will be described as the throttle structure of the first nozzle 52 and the second nozzle 54. However, the orifice structure is not limited to the orifice as long as it has a function of ejecting turbulent liquid. Other methods can be used.

  The first conduit 42 and the second conduit 46 are provided with pressurizing means (not shown), and the first solution L1 and the second solution L2 are applied to the first and second nozzles 52 and 54, respectively. Pressure supplied. However, the pressure ejected from the second nozzle 54 to the mixing chamber 38 is made smaller than the pressure of the high-pressure jet stream ejected from the first nozzle 52 to the mixing chamber 38. Various means are known as pressurizing means for applying a high pressure to the liquid, and any means can be used. However, relatively easy and inexpensive means such as a plunger pump and a booster pump are available. It is preferable to use a reciprocating pump. In addition, although a high pressure cannot be generated as much as a reciprocating pump, some rotary pumps can generate a high pressure, and such a pump can be used.

  The first solution L1 is ejected from the first nozzle 52 to the mixing chamber 38 as a turbulent flow having a high pressure jet flow of 1 MPa or more and flowing into the mixing chamber 38 with a Reynolds number of 10,000 or more. The second solution L2 having a pressure lower than that of the first solution L1 is ejected from the mixing chamber 38 as an orthogonal flow substantially orthogonal to the first solution L1. In this case, even if the second solution L2 is not completely orthogonal to the first solution L1 at an angle of 900, the second solution L2 only needs to have an orthogonal velocity vector component as a main component. Thus, the first solution L1 and the second solution L2 are instantaneously and efficiently mixed under an appropriate mixing reaction temperature condition, and the reacted reaction solution LM is immediately discharged from the discharge pipe 44. In this case, the residence time in the mixing chamber 38 is preferably 5 seconds or less. As a result, fine metal particles having a fine size and good monodispersibility are formed.

  As schematically shown in FIG. 3, the mixing reaction is performed by the second solution ejected from the substantially orthogonal direction with respect to the first solution L <b> 1 to the first solution L <b> 1 having a high-speed turbulent high-pressure jet flow. By entraining so as to entrain L2, by utilizing the large eddy viscosity generated by mixing the first solution L1 and the second solution L2, high-performance mixing efficiency is obtained. The mixing chamber 38, the first and second nozzles 52 and 54, and the discharge pipe 44 of the apparatus 12 are formed to have the following relationship.

  That is, eddy viscosity needs to be formed in the mixing chamber 38, and the cylinder diameter D1 of the mixing chamber 38 is larger than the orifice diameter D2 of the first nozzle 52 and the orifice diameter D3 of the second nozzle 54. Formed. In particular, the eddy viscosity produced by the first solution L1 which is a straight flow A is important for improving the mixing efficiency, and the dimensional ratio of the cylinder diameter D1 of the mixing chamber 38 to the orifice diameter D2 of the first nozzle 52 is 1 The range of 1 to 50 times is preferable, and the range of 1.1 to 20 times is more preferable. Further, in order to make the second solution L2 that is a cross flow B orthogonal to the straight flow A easy to be caught in the solution L1 of the straight flow A, the pressure of the cross flow B is lower than the pressure of the straight flow A. Thus, it is preferable that the jet flow velocity be equal to or less than the jet flow velocity of the straight flow A. Specifically, the flow rate ratio of the jet flow velocity of the cross flow B to the jet flow velocity of the straight flow A is 0.05 to 0.4 times, more preferably 0.1 to 0.3 times.

  Further, the cross flow B is mixed in the mixing chamber 38 at a position before the eddy viscosity C formed by the straight flow A being ejected from the first nozzle 52 having a small diameter into the mixing chamber 38 having a larger diameter is maximized. The second nozzle 54 needs to be disposed between the first nozzle 52 and the maximum position of the eddy viscosity C. Therefore, it is necessary to know the position where the eddy viscosity C is maximized, but the position of the mixing chamber 38 where the eddy viscosity C is maximized is already commercially available in Japan as flow analysis software and is well known as flow analysis software. This can be grasped by performing a simulation in advance using R-flow, a numerical analysis software manufactured by R-Flow. In this case, as can be seen from FIG. 3, the position where the eddy viscosity C is maximum has a region instead of a pin point, and therefore the maximum position of the eddy viscosity C may be set to a point P that is substantially the center of the eddy viscosity C. . Therefore, the second nozzle 54 may be positioned before the point P, but more preferably, the second nozzle 54 is positioned so that the cross flow B can be ejected at the initial stage of formation of the eddy viscosity C 1.

  Further, when analyzed with the above numerical analysis software, the central point P of the city area where the eddy viscosity C appears is related to the flow velocity of the straight flow A, and the maximum flow velocity of the straight flow A (usually at the first nozzle position). This corresponds approximately to the position where the (flow velocity) decreases to 1/10. Therefore, if the position where the maximum flow velocity of the straight flow A is reduced to 1/10 is calculated and the second nozzle 4 is positioned so that the orthogonal flow B can be ejected before that point, it is also necessary to calculate the point P. Absent.

  Further, it is necessary to ensure the length L (see FIG. 2) of the mixing chamber 38 necessary for forming the maximum eddy viscosity C in the mixing chamber 38. Stagnation and backflow are likely to occur, which adversely affects the fine particle size and monodispersity of the metal fine particles. Therefore, the length L of the mixing chamber 38 is preferably 2 to 5 times the distance from the first nozzle 52 to the point P which is the maximum position of the eddy viscosity C, and more preferably 2 to 3 times.

Further, when a liquid is ejected from the first nozzle 52 or the second nozzle 54 with a high-speed flow from the first nozzle 52 or the second nozzle 54 to the larger-diameter mixing chamber 38, cavitation is likely to occur. An interface is formed, reducing the mixing efficiency. Therefore, in order to increase the mixing efficiency by using the eddy viscosity C, it is necessary to prevent the gas-liquid interface from being formed in the mixing chamber 38. Therefore, as shown in FIG. 2, the diameter D ₄ of the discharge pipe 44 is reduced by the third orifice 60 so as to be smaller than the pipe diameter D _{1 of} the mixing chamber 38, and mixing is performed with the pressure in the mixing chamber 38 increased. is required. Thereby, since cavitation can be eliminated, mixing efficiency is further improved. In order to shorten the residence time in the portion not contributing to mixing in the discharge pipe 44 as much as possible, the outlet in the mixing chamber 38 is throttled, and at least the discharge pipe 38 having an inner diameter smaller than the pipe diameter D ₁ of the mixing chamber 38 is provided. It is good to connect to the piping 30 as short as possible. In this way, by reducing the distance from the first mixing device 12 to the degassing device 14, the gas generated by the reaction in the first mixing device 12 is immediately degassed without staying in the discharge pipe 44 or the pipe 30. Degassing at the device 14 can begin.

  Further, the shape of the jet flow ejected from the first nozzle 52 into the mixing chamber 38 is regulated by the first orifice 48 provided in the first nozzle 52, and this jet flow shape affects the mixing performance. Therefore, it is preferable to appropriately use the first orifice 48 that forms a jet flow shape such as a filament shape, a conical shape, a slit shape, or a fan shape in accordance with the purpose of the mixing reaction. For example, in the case of a reaction with a very fast reaction speed on the order of milliseconds, it is necessary to eject the straight flow A and the cross flow B so that the eddy viscosity C is instantaneously maximized in the narrowest possible range. A first orifice 48 that forms a linear jet shape is preferred. Also, when the reaction rate is relatively slow, it is better to increase the entrained interface area created by the straight flow A by jetting the straight flow A and the cross flow B so that the eddy viscosity C is maximized in the widest possible range. In this case, the first orifice 48 which forms a thin jet flow shape is preferable. In the case of an intermediate reaction rate between a very high reaction rate on the order of milliseconds and a relatively low reaction rate, the first orifice 48 that forms a conical jet flow shape is preferable.

  FIGS. 4 to 7 illustrate the first orifice 48 for forming the shape of each of the thread-line shape, the conical shape, the slit shape, and the fan shape, and (a) in each figure shows the orifice at the tip. FIG. 2B is a longitudinal sectional view of the orifice, and FIG. 3C is a transverse sectional view of the orifice.

  FIG. 4 shows a first orifice 48 for ejecting the straight linear flow A to the mixing chamber 38, which is formed in a filament shape. FIG. 5 shows a first orifice 48 for ejecting a conical straight flow A to the mixing chamber 38, which is formed in a trumpet shape having an open front end. FIG. 6 shows the first orifice 48 for ejecting the straight flow A of the thin film into the mixing chamber 38, which is formed in a rectangular slit shape. FIG. 7 shows a first orifice 48 for ejecting a straight flow A of a fan-shaped thin film into the mixing chamber 38, and the tip portion is formed in a fan-like diameter.

  The first mixing device 12 of the one-jet mixing method is not limited to the above-described FIG. 2, and the first solution L1 and the second solution L2 are larger than the nozzle diameter from each nozzle. A static mixing device is used to eject the mixed reaction liquid LM from a discharge port having a diameter smaller than the diameter of the mixing field by ejecting the mixture to the mixing field, and at least one solution of the solution L1 and the solution L2 is 1 MPa or more. In a high-pressure jet flow and a turbulent flow with a Reynolds number of 10,000 or more when flowing into the mixing field, it is jetted into the mixing field, and at a position before the eddy viscosity formed by the high-pressure jet flow in the flow direction is maximized, What is necessary is just to be able to add the remaining solution at a pressure lower than the high-pressure jet stream.

b) T-shaped / Y-shaped FIGS. 8 and 9 are sectional views of the first mixing device 12 of T-shaped / Y-shaped, FIG. 8 is a T-shaped tube, and FIG. 9 is a Y-shaped tube. It is.

  As shown in FIGS. 8 and 9, the first solution L1 and the second solution L2 are fed at a pressure of 1 MPa or more at an intersection (mixing field) of very thin pipes such as a T-shaped tube and a Y-shaped tube. The two liquids are mixed instantaneously by colliding with the flow, and the reacted reaction liquid LM is discharged from the discharge pipe in a short time. That is, the first solution L1 is ejected from the first addition pipe 62 to the mixing field 64 with a high-pressure jet flow of 1 MPa or more, and the second solution L2 is ejected from the second addition pipe 66 with a high-pressure jet flow of 1 MPa or more. Both solutions are made to collide by being ejected to the mixing field 64. The reaction liquid LM that has been mixed and reacted by the energy resulting from the collision is discharged from the discharge pipe 68 in a short time. The pressures of the first solution L1 and the second solution L2 may be the same or different as long as the pressure is 1 MPa or more. A jacket 70 is wound around the outer periphery of the first addition pipe 62, the second addition pipe 66, and the discharge pipe 68, and the mixing reaction temperature with the first and second solutions L 1 and L 2 in the mixing field 64. Is controlled. 8 and 9, reference numeral 70A denotes a heat medium inlet of the jacket 70, and reference numeral 70B denotes a heat medium outlet.

  As a result, the first solution L1 and the second solution L2 are reacted instantaneously and efficiently under an appropriate mixing reaction temperature condition, and the reaction solution LM is immediately discharged from the discharge pipe 68. Metal fine particles having a fine size and good monodispersibility can be formed. In this case, the residence time is preferably 5 seconds or less.

C) Two-jet opposed type FIG. 10 shows a mixing method in which the concept of eddy viscosity is added to the T-shape, and the same members as those in FIG. In this mixing method, the first chamber L1 and the second solution L2 are mixed in a high-pressure jet flow of 1 MPa or more from the facing direction, and a mixing chamber 38 (mixing chamber) having a diameter larger than the nozzle diameter for ejecting the L1 solution and the L2 solution. The reaction liquid LM is discharged from the discharge pipe 44 having a diameter smaller than the diameter of the mixing chamber 38 by mixing with the eddy viscosity generated in both solutions.

  The first mixing device 12 in FIG. 10 has a first opening on the one end side of the mixer 40 in which a cylindrical mixing chamber 38 in which the first solution L1 and the second solution L2 are mixed and reacted is formed. A first conduit 42 for introducing the solution L1 into the mixing chamber 38 is connected, and a second conduit 46 for introducing the second solution L2 into the mixing chamber 38 is connected to the other end side opening. A discharge pipe 44 for discharging the reaction liquid LM mixed and reacted in the mixing chamber 38 from the mixing chamber 38 is connected to the central opening of the mixer 40.

  A first orifice 48 and a second orifice 50 are provided inside the distal ends of the first conduit 42 and the second conduit 46, respectively, so that the first conduit 42 and the second conduit 46 are not disturbed. A first nozzle 52 and a second nozzle 54 that inject a straight flow A1, A2 are formed. In the present embodiment, an example in which the first solution L1 is ejected from the first nozzle 52 and the second solution L2 is ejected from the second nozzle 54 will be described.

  A jacket 56 is wound around the outer periphery of the mixer 40, and the mixing reaction temperature with the first and second solutions L1, L2 in the mixer 40 is controlled in the same manner as described with reference to FIG.

Further, the pipe diameter D1 of the mixing chamber 38, the orifice diameter D ₂ of the first nozzle 52, the orifice diameter D ₃ of the second nozzle 54, and their dimensional relationship is the same as the one-jet type. Further, the method of forming the first and second orifices 48 and 50, the material of the orifice material 58, and the pressurizing means are the same as described in the one-jet type. Moreover, the shape of the straight flow A1, A2 can also be formed in the shape of each of the yarn-line shape, the conical shape, the slit shape and the fan-like shape described in the one-jet type.

  11, the one end and the other end of the mixing chamber 38 are fed from the first nozzle 52 and the second nozzle 54 to the first solution L1 and the second solution L2 by a high-pressure jet flow of 1 MPa or more. And collide in the mixing chamber 38 as turbulent straight flow A1 and A2 facing each other. By overlapping the two eddy viscosities C and D formed by the two straight flow streams A1 and A2, the solution L1 and the solution L2 are instantaneously mixed under an appropriate mixing reaction temperature condition and reacted. Is immediately discharged from the discharge pipe 44. In this case, the residence time in the mixing chamber 38 is preferably 5 seconds or less. Thereby, fine metal particles having a fine size and good monodispersibility can be formed.

  In such a mixing reaction, when the respective eddy viscosities C and D formed in the mixing chamber 38 by the two high-speed straight flow A1 and A2 of the opposing turbulent flow become maximum, the overlapping portion E becomes as large as possible. In this way, high-performance mixing efficiency is obtained. Therefore, the straight flow A1, A2 does not collide with the mixing chamber 38 immediately after jetting, and a portion E where the two eddy viscosities C, D formed in the mixing chamber 38 by the straight flow A1, A2 overlap as much as possible. It is preferable to enlarge it. For this purpose, it is preferable to appropriately set the separation distance L (see FIG. 10) between the first nozzle 52 and the second nozzle 54 facing each other, in other words, the length of the mixing field. Thus, by appropriately setting the separation distance L between the first nozzle 52 and the second nozzle 54, it is possible to reliably increase the overlapping portion E between the eddy viscosities C and D that are maximized. In addition, the two eddy viscosities C and D can be substantially completely overlapped. Therefore, it is necessary to know the position where the eddy viscosities C and D are maximized. However, the position of the mixing chamber 38 where the eddy viscosities C and D are maximized is already commercially available in Japan as flow analysis software and is good as flow analysis software. The distance from the first nozzle 52 to the eddy viscosity C and the distance from the second nozzle 54 to the eddy viscosity D are simulated in advance using a known numerical analysis software, R-Flow, manufactured by R-Flow. The distance can be grasped. In this case, as can be seen from FIG. 11, the position where the eddy viscosities C and D are maximized has not a pinpoint but a saddle region. Accordingly, the separation distance L between the first nozzle 52 and the second nozzle 54 is such that the maximum position of the eddy viscosities C and D is the points P1 and P2 that are substantially central portions of the eddy viscosities C and D, and the points P1 and P2 And the total value from the first nozzle 52 to the point P1 and the second nozzle 54 to the point P2. As another method for grasping the points P1 and P2, the points P1 and P2 at which the eddy viscosities C and D caused by the straight flow A1 and A2 become maximum are analyzed by the above numerical analysis software. This is related to the flow velocity, and corresponds approximately to the position where the maximum flow velocity of the straight flow A1, A2 (usually the flow velocity at the first or second nozzle position) is reduced to 1/10. Therefore, the points P1 and P2 may be grasped by calculating the position where the maximum flow velocity of the straight flow A1 and A2 decreases to 1/10. In this way, by making the eddy viscosities C and D overlap at the position where the eddy viscosities C and D are maximized, the contact efficiency at the liquid-liquid interface between the straight flow A1 and the straight flow A2 is increased and the mixing reaction is performed. In addition to the effect of improving the performance, there is also an effect of suppressing heat generation due to liquid-liquid friction caused by the collision between the straight flow A1 and the straight flow A2.

(B) About degassing apparatus The degassing apparatus 14 in the present invention efficiently degass gas bubbles generated with the progress of the reaction from the reaction liquid LM, thereby inhibiting the progress of the reaction and the flow of the reaction liquid LM. Any device can be used as long as it can be avoided, but a degassing device 14 to be described below can be preferably used.

a) Up-and-down meandering flow method The up-and-down serpentine-flow type degassing device 14 shown in FIGS. 12 and 13 is configured so that the liquid part 80 by the reaction liquid LM and the space part 82 in which the gas removed from the reaction liquid LM accumulates are separated. It is formed as a passage 86 having a liquid interface 84. That is, in the degassing container 88 having the inlet 88A and the outlet 88B, a plurality of weir plates 90, 90... Are provided at intervals from the bottom of the degassing container 88, and the upper end of the weir plate 90 is gas-liquid. It is formed so as to be located below the interface 84. A plurality of baffle plates 92 are provided between the barrier plates 90 so as to hang down from the ceiling plate of the degassing container 88, and the lower ends of the baffle plates 92 are separated from the bottom of the degassing container 88. Formed. As a result, as shown in FIG. 13, ascending passages 86 </ b> A and descending passages 86 </ b> B in which the reaction liquid LM continuously flows are formed continuously in the degassing vessel 88 and descend from the ascending passage 86 </ b> A. A gas-liquid interface 84 is formed at a portion where the flow is reversed in the passage 86B. The entire length of the passage 86 composed of the ascending passage 86A and the descending passage 86B needs to be long enough for degassing. An inflow pipe 94 is connected to the inlet 88A of the degassing container 88, and the inflow pipe 94 is connected to the pipe 30 (see FIG. 1) via a flange. On the other hand, an outlet pipe 96 is connected to the outlet 88B of the degassing container 88, and the outlet pipe 96 is connected to the pipe 32 (see FIG. 1) via a flange. It is necessary to connect the outflow pipe 96 so that the connection position of the outflow pipe 96 is slightly above the upper end of the dam plate 90 and to secure a height of the gas-liquid interface 84 higher than the upper end of the dam plate 90. However, when the outflow pipe 96 is provided with a valve and the outflow amount from the outflow pipe 96 is restricted by the inflow amount from the inflow pipe 94, the outflow pipe 96 may be connected to a lower position of the degassing container 88.

  According to the degassing device 14 of the vertical meandering flow system configured as described above, the reaction liquid LM mixed in the first mixing device 12 flows into the degassing device 14 from the inflow pipe 94. Then, while the reaction liquid LM alternately flows in the ascending passage 86A and the descending passage 86B, the gas bubbles 98 generated as the reaction proceeds rises toward the gas-liquid interface 84 in the passage 86, and the gas-liquid interface 84 To the space 82. In this case, it is preferable that the bottom shape of the degassing container 88 in which the flow of the reaction liquid LM is reversed from the descending passage 86B to the ascending passage 86A is formed in an arc shape. Thereby, since the flow of the reaction liquid LM flows smoothly without staying at the bottom of the degassing container 88, the bubbles 98 and the metal fine particles which are reaction products do not stagnate at the bottom. As another aspect, as shown in FIG. 14, a searcher 100 that generates a flow that prevents staying may be provided at the bottom of the ascending passage 86 </ b> A. If this stirrer 100 is provided, a reversal flow with a large force can be formed when the reaction liquid LM is reversed from the descending passage 86B to the ascending passage 86A, so that bubbles 98 and metal fine particles are trapped in the bottom of the degassing container 88. Can be prevented.

  Further, in order not to lengthen the length of the passage 86 unnecessarily, it is preferable that the height of the weir plate 90 is lowered as it goes from the inlet 88A to the outlet 88B of the degassing device 14. This is because, in the passage 86 formed in the degassing container 88, the gas generation amount from the reaction liquid LM is larger as it is closer to the inlet side, and the gas generation amount is smaller toward the outlet side. Accordingly, it is necessary to secure a longer passage length to the gas-liquid interface 84 toward the inlet side of the passage 86. If the height of the weir plate 90 is decreased from the inlet 88A to the outlet 88B of the degassing container 88, the gas The passage length to the gas-liquid interface 84 can be appropriately formed in accordance with the generation amount. As a result, it is possible to prevent the passage 86 from being lengthened unnecessarily, so that efficient degassing can be performed in a short time.

  As shown in FIGS. 12 and 13, the degassing device 14 is preferably provided with a pressure adjusting means 102 that adjusts the pressure of the space portion 82 that changes as bubbles are generated. In this case, when the pressure adjusting means 102 adjusts the pressure of the entire space portion 82 to be uniform, the communication hole 92 </ b> A may be formed in a portion corresponding to the space portion 82 of the baffle plate 92.

  The pressure adjusting means 102 is mainly connected to the pressure sensor 106 that measures the pressure in the space 82, the gas vent pipe 110 with a valve 108 that discharges the gas accumulated in the space 82, and the gas vent pipe 110. The pressure reducing means 112, a gas supply pipe 116 with a valve 114 for supplying an inert gas such as nitrogen gas to the space 82, and a control device 118 are configured. As the decompression means 112, a vacuum pump or an aspirator can be used. Then, the control device 118 adjusts the valves 108 and 114 of the gas vent pipe 110 and / or the gas supply pipe 116 based on the pressure value of the space part 82 measured by the pressure sensor 106, thereby adjusting the pressure of the space part 82. Adjust appropriately. That is, the pressure of the space portion 82 is adjusted so that the bubbles 98 in the reaction liquid LM flowing through the passage 86 of the degassing device 14 are easily degassed to the space portion 82 via the gas-liquid interface 84. In order to facilitate degassing, it is better to reduce the pressure in the space portion 82. However, if the pressure is reduced too much, the reaction liquid LM will boil and the flow will be disturbed. Therefore, when the pressure is reduced too much, the space 82 is adjusted by supplying an inert gas such as nitrogen gas. How much pressure is reduced depends on the amount of bubbles in the generated gas, the levitation force depending on the size of the bubbles, and the like, so the degree of pressure reduction may be adjusted while monitoring the degassing state. Therefore, it is preferable that the state where the bubbles 98 are removed from the reaction liquid LM flowing through the passage 86 can be observed, and the degassing container 88 is preferably formed of a transparent container.

  In this degassing, the generated gas is continuously degassed smoothly from the reaction liquid LM (so as not to disturb the flow of the liquid) while maintaining the pressure in the space 82 constant and accurately, and the flow of the reaction liquid LM is stabilized. It is very important to stabilize the reaction and to make it uniform.

  For this reason, it is preferable to use the valves 108 and 114 that open and close at a response speed of a level of 10 milliseconds or less, more preferably 5 milliseconds or less. Servovalves can be used as the valves 108 and 114 that open and close at a response speed of 5 milliseconds or less. As a result, when the measured value of the pressure sensor 106 fluctuates with respect to the preset pressure setting value of the space portion 82, the valves 108 and 114 open and close at a very fast opening / closing speed. I can not. Further, when the response speed of the valves 108 and 114 is 10 milliseconds or more, a resistor (not shown) that slows the gas release speed somewhere in the gas vent pipe 110 including the valve valves 108 and 114. May be provided to facilitate the pressure control. As the resistor, an orifice, a filter, or the like can be preferably used.

  In addition, there are cases where the reaction is a reaction that dislikes oxygen in the air, or when the gas generated by the reaction is oxygen such as hydrogen gas, it may be dangerous. In this case, since an inert gas such as nitrogen gas can be supplied from the gas supply pipe 116, the inert gas is purged from the gas supply pipe 116 into the degassing container 88 before the reactor 10 is operated. It is preferable to replace the air in the container 88 with an inert gas.

  In the present embodiment, the communication hole 92A is formed in the portion corresponding to the space portion 82 of the baffle plate 92. Pressure adjusting means 102 may be provided so that the pressure can be individually adjusted for each space 82. As described above, the closer to the inlet side of the degassing device 14, the more gas is generated from the reaction liquid LM, and the gas generation amount decreases toward the outlet side. It is necessary to quickly remove the degassed gas from the space 82 so that the pressure in the space 82 does not increase. Therefore, if the pressure can be adjusted for each space 82 divided by the baffle plates 92, the pressure in each space 82 is appropriately controlled according to the amount of gas generated, and the bubble 98 is generated for each space 82. Can form a pressure that is easily degassed.

  Further, in order to promote the degassing of the bubbles 98 from the reaction liquid LM, as shown in FIG. 13, temperature adjusting means for heating or cooling the reaction liquid LM flowing into the degassing device 14 in the middle of the inflow pipe 94. 120 is preferably provided. In this case, the entire degassing device 14 may be heated or cooled by embedding a heater or a cooling coil in the degassing container 88, the weir plate 90, and the baffle plate 92. To what degree the reaction liquid LM is heated or cooled, the temperature of the temperature adjusting means 120 or the like may be appropriately set while observing the state where the bubbles 98 are removed.

  Thus, by controlling the reaction temperature by heating or cooling the reaction liquid LM flowing in the degassing device 14, the reaction conditions can be made constant regardless of the air temperature or the room temperature. Can be kept constant regardless of the temperature. Therefore, accurate degassing treatment can be performed, and the degassing amount in the designed degassing device is accurately reproduced regardless of the season and room temperature, so the shape and capacity of the device are fixed. it can.

  In order to promote the degassing of the bubbles 98 from the reaction liquid LM, it is also a preferable method to provide an ultrasonic generator 122 as shown in FIG. Although the place where the ultrasonic generator 122 is provided is not particularly limited, for example, it may be provided outside the bottom of the degassing apparatus 14 as shown in FIG. The ultrasonic vibration frequency is preferably in the range of 1 kHz to 10 MHz, more preferably in the range of 1 kHz to 1 MHz, and particularly preferably in the range of 20 kHz to 200 kHz. The ultrasonic output is preferably in the range of 1 W to 10 kW, more preferably in the range of 10 W to 5 kW, and particularly preferably in the range of 100 W to 2 kW. Thus, by applying ultrasonic vibration to the reaction liquid LM, not only can the degassing of the bubbles 98 in the reaction liquid LM be promoted, but also the inner wall surface of the degassing container 88, the surface of the weir plate 90, and the baffle plate 92. It becomes easy to detach | desorb the bubble 98 adhering to the surface. In this case, it is better to apply a surface treatment that makes it difficult for the bubbles 98 to adhere to the inner wall surface of the degassing container 88, the surface of the dam plate 90, and the surface of the baffle plate 92, such as Teflon (trademark) processing.

  Further, in order to promote the degassing of the bubbles 98 from the reaction liquid LM, as shown in FIG. 15, the width W2 of the descending passage 86B is made larger than the width W1 of the ascending passage 86A, and the passage of the ascending passage 86A. It is preferable to make the passage sectional area of the descending passage 86B larger than the sectional area. That is, in the ascending path 86A, the flow direction of the reaction liquid LM and the rising direction of the bubbles 98 are the same, so the bubbles 98 are likely to float and separate at the gas-liquid interface 84. Since the rising direction of 98 is reversed, the bubble 98 is difficult to be lifted and separated at the gas-liquid interface 84. Therefore, in the descending passage 86B, it is necessary to make the descending flow rate of the reaction liquid LM smaller than the ascending rate of the bubbles 98. In this case, since the rising speed of the bubble 98 varies depending on the bubble diameter, it is necessary to appropriately design the descending flow speed of the descending passage 86B in accordance with the size of the bubble diameter, that is, the rising speed. 14 and 15, the pressure adjusting means 102 is omitted.

  In FIG. 16, the degassing device 14 is unitized into an inlet unit 124, an intermediate unit 126, and an outlet unit 128 so that the entire length of the passage 86 can be easily adjusted.

  As shown in FIG. 16, the inlet unit 124 has the above-described weir plate 90 standing inside the box body 130, an inflow pipe 94 connected to the lower portion of one side surface of the box body 124, and the lower portion of the other side surface. The outlet duct 132 is provided so as to project sideways. In the intermediate unit 126, the above-described weir plate 90 is erected inside the box body 134, and an inlet duct 136 protrudes laterally at a lower portion of one side surface of the box body 134, and an outlet duct 138 is formed at the lower portion of the other side surface. Is projected sideways. The outlet unit 128 has an inlet duct 142 projecting from the lower part of one side surface of the box 140 and an outflow pipe 96 connected to the upper part of the other side surface. Each unit 124, 126, 128 is formed with a communication hole 92A for equalizing the pressure in the space 82 described above. In addition, the inlet ducts 136 and 142 and the outlet ducts 132 and 238 in each unit 124, 126, and 128 are fitted in a watertight state.

  In order to assemble the degassing device 14 with the inlet unit 124, the intermediate unit 126, and the outlet unit 128, the outlet duct 132 of the inlet unit 124 and the inlet duct 136 of the intermediate unit 126 are fitted together, The outlet duct 18 and the inlet duct 142 of the outlet unit 128 are fitted. The side surfaces of the units 124, 126, and 128 that are brought together by this fitting become the baffle plate 92 described above. As a result, the degassing device 14 can be easily manufactured, and the length of the entire passage 86 in the degassing device 14 can be arbitrarily adjusted only by changing the number of intermediate units 126. When the communication hole 92A is formed in each unit 124, 126, 128, the pressure adjusting means described above may be provided in any unit. Further, when the communication hole 92A is not formed, the pressure adjusting means 102 for adjusting the pressure in the space 82 may be provided for each unit. Further, it is more preferable to provide various means and shapes for promoting degassing, such as providing the temperature adjusting means 120, the ultrasonic wave applying means 122, the stirrer 100, etc., or forming the unit bottom in an arc shape. .

b) Gas Permeation Method As shown in FIG. 17, the gas permeation method degassing apparatus 14 has an inflow pipe 94 connected to the upper part of one side surface of the degassing container 88 and an outflow pipe 96 at the lower part of the local side surface. Connected. In the degassing container 88, a degassing pipe 150 formed of a gas permeable member that allows gas to pass through without passing liquid is housed in an inverted S shape, and one end of the degassing pipe 150 is connected to the inflow pipe 94. The other end is connected to the outflow pipe 96. Further, a plurality of locations of the degassing pipe 150 are supported on the inner wall surface of the degassing container 88 via the holder 152.

The most important point in manufacturing the gas permeable degassing apparatus 14 is how to use a gas permeable member having good gas permeability. For example, Gore-Tex membrane ( Membranes with good gas permeability such as trademark are commercially available, and such membranes can be used. In addition, due to recent advances in micromachining technology, it has become possible to open extremely fine holes that do not allow liquids to pass through but allow gas to pass through hard resins such as metals and plastic resins. It is also possible to manufacture a gas permeable member. In any case, the gas permeable degassing device 14 may be any gas permeable member that allows only gas generated by the liquid-liquid reaction to permeate, regardless of technological progress. In this case, the entire degassing pipe 150 is not limited to being formed of a gas permeable member, and at least the upper part of the degassing pipe 150 may be formed of a gas permeable member. Thereby, in the degassing container 88, the degassing pipe 150 in which the gas-liquid interface between the liquid part 80 by the reaction liquid LM and the space part 82 in which the gas removed from the reaction liquid LM accumulates is formed by the gas permeable member. A degassing device 14 having a structure partitioned by is formed.

  According to the gas-permeable degassing device 14 configured as described above, the reaction liquid LM mixed in the first mixing device 12 flows into the degassing device 14 from the inflow pipe 94. Then, while the reaction liquid LM flows in the degassing pipe 150, the gas generated by the reaction rises as bubbles 98 in the reaction liquid and permeates through the degassing pipe 150 formed by the gas permeable member. Degassed to the space 82.

  In such degassing, although depending on the gas permeation performance of the gas permeable member forming the degassing pipe 150, it is preferable to provide pressure adjusting means for adjusting the pressure of the space portion 82 to depressurize the space portion 82. Since the configuration of the pressure adjusting means 102 is the same as that described in the degassing apparatus of the up and down meandering flow method, the description is omitted.

  As described above, according to the chemical substance manufacturing apparatus 10 of the present invention, the first mixing device 12 and the degassing device 14 are separated and mixed without being obstructed by the gas bubbles 98 generated by the reaction. Can be performed uniformly and efficiently, so that the reaction at the start of the reaction and in the course of the reaction can be stabilized, and stable liquid feeding can be performed to the subsequent process.

  In addition, according to the chemical substance manufacturing apparatus 10 of the present invention, by using a high-pressure mixing system as the first mixing apparatus 12, instantaneous mixing can be performed, and a reaction in which gas is generated due to the start of the reaction by mixing. The liquid LM can be immediately sent to the degasser 14. Thereby, in the 1st mixing apparatus 12, mixing is not disturbed by the bubble of gas.

  Moreover, according to the chemical substance manufacturing apparatus 10 of the present invention, the degassing apparatus 14 has the gas-liquid interface 84 between the liquid part 80 by the reaction liquid LM and the space part 82 in which the gas removed from the reaction liquid LM accumulates. Since the passage 86 is formed and the gas bubbles 98 in the reaction liquid flowing through the passage 86 are continuously removed to the space portion 82, efficient degassing using the floating force of the bubbles 98 can be performed. it can.

  Therefore, the chemical substance production apparatus 10 of the present invention is suitable for a reaction system in a flow system in which a reaction for generating a gas is performed in the flow of the reaction liquid LM. In particular, if the production apparatus 10 of the present invention is used for continuous production of magnetic particles contained in the magnetic layer of a magnetic recording medium, it is possible to make the reaction accompanied by gas generation uniform. Further, it is considered that the equilibrium of the reaction proceeds toward the reaction promoting side by continuously degassing, and the reactivity is improved, so that a quick reaction is possible, and as a result, the magnetic particles can be miniaturized. In addition, when performing liquid temperature control for degassing, the gas can be efficiently removed in the flow of continuous processing, so that the accuracy of liquid temperature control can be improved. Thereby, magnetic particles having a fine size and good monodispersibility can be produced, and a high-precision magnetic recording medium can be produced by containing the magnetic particles in the magnetic layer.

  The following operation was performed in high purity nitrogen gas.

Triammonium iron oxalate (Fe (NH ₄ ) ₃ (C ₂ O ₄ ) ₃ ) (manufactured by Wako Pure Chemical Industries) 0.46 g and potassium chloroplatinate (K ₂ PtCl ₄ ) (manufactured by Wako Pure Chemical Industries) 0.46 g And alkane solution in which 14.0 g of aerosol OT (manufactured by Wako Pure Chemical Industries) is dissolved in 80 ml of decane (manufactured by Wako Pure Chemical Industries) is added to and mixed with an aqueous solution of metal salt dissolved in 24 ml of H ₂ O (deoxygenated). Thus, a reverse micelle solution of the first solution L1 was prepared.

NaBH ₄ (manufactured by Wako Pure Chemical Industries) 0.50 g of H ₂ O (deoxygenated) dissolved in 12 ml of reducing agent aqueous solution and aerosol OT 5.4 g of decane (manufactured by Wako Pure Chemical Industries, Ltd.) 40 ml of alkane solution added The reverse micelle solution of the second solution L2 was prepared by mixing.

To a metal salt aqueous solution obtained by dissolving 0.09 g of copper chloride (CuCl ₂ · 6H ₂ O) (manufactured by Wako Pure Chemical Industries) in 2 ml of H ₂ O (deoxygenated), 3.5 g of aerosol OT (manufactured by Wako Pure Chemical Industries, Ltd.) An alkane solution dissolved in 20 ml of decane (manufactured by Wako Pure Chemical Industries, Ltd.) was added and mixed to prepare a reverse micelle solution of the third solution L3.

In an aqueous solution obtained by dissolving 0.88 g of ascorbic acid (manufactured by Wako Pure Chemical Industries) and 0.33 g of a chelating agent (DHEG) in 12 ml of H ₂ O (deoxygenated), 5.4 g of aerosol OT (manufactured by Wako Pure Chemical Industries) and olein An alkane solution obtained by dissolving 2 ml of amine (manufactured by Tokyo Chemical Industry) in 40 ml of decane (manufactured by Wako Pure Chemical Industries, Ltd.) was added and mixed to prepare a reverse micelle solution of the fourth solution LM4.

  In the method for producing fine metal particles according to the conventional method, the above four reverse micelle solutions (LM1, 2, 3, 4) were mixed as follows in a single tank. While the reverse micelle solution (L1) was stirred at a high speed with an omni mixer (manufactured by Yamato Kagaku) at 22 ° C., the reverse micelle solution (L2) was added instantaneously. Three minutes later, reverse micelle solution (L3) was further added at a rate of about 2.4 ml / min over about 10 minutes. Five minutes after the completion of the addition, the stirring was changed from the omni mixer to the magnetic stirrer and the temperature was raised to 40 ° C., and then the reverse micelle solution (L4) was added, followed by aging for 120 minutes. Thus, the obtained metal fine particles are referred to as a conventional method sample.

  On the other hand, in the chemical substance manufacturing apparatus 10 of the present invention, the reverse micelle solution (L1) and the reverse micelle solution (L2) were instantaneously mixed by the first mixing device 12 of FIG. Simultaneously with the end of mixing, the reaction liquid LM is taken out from the first mixing device 12, and the reaction byproduct gas is removed by the up-and-down meandering type degassing device 14 in FIG. 12, and the second mixing device 13 shown in FIG. The reaction solution LM was sent to. The reverse micelle solution (L3) was added to the second mixing device 13 and mixed instantaneously. The liquid from the second mixing device 13 is collected in the product tank 21, 5 minutes after the addition of the reverse micelle solution (L3) is changed to gentle stirring by the stirring blade 21 a, the temperature is raised to 40 ° C., and then reverse micelle Solution (L4) was added and aged for 120 minutes. Thus, the obtained metal fine particles are referred to as a sample according to the present invention.

Then, both the conventional method sample and the present invention method sample were cooled to room temperature, 2 ml of oleic acid (manufactured by Wako Pure Chemical Industries, Ltd.) was added, mixed, and taken out into the atmosphere. In order to destroy the reverse micelle, a mixed solution of 200 ml of H ₂ O and 200 ml of methanol was added to separate into an aqueous phase and an oil phase. A state in which the metal nanoparticles were dispersed on the oil phase side was obtained. The oil phase side was washed 5 times with a mixed solution of 600 ml of H ₂ O and 200 ml of methanol. Thereafter, 1300 ml of methanol was added to cause flocculation of the metal nanoparticles and sedimentation. After removing the supernatant, 20 ml of heptane (manufactured by Wako Pure Chemical Industries, Ltd.) was added and redispersed, and then 100 ml of methanol was added to precipitate the metal nanoparticles. This treatment was repeated twice, and finally 5 ml of octane (manufactured by Wako Pure Chemical Industries, Ltd.) was added to obtain a metal nanoparticle dispersion liquid containing FeCuPt multi-component alloy containing metal fine particles having a nano particle size.

  The yield, composition, volume average particle size and particle size distribution (variation coefficient), and coercive force of the obtained conventional metal nanoparticles and the metal nanoparticles of the present invention were measured. The composition and yield were measured by ICP spectroscopic analysis (inductively coupled high-frequency plasma spectroscopic analysis), and the volume, average particle size, and particle size distribution were determined by statistical processing by measuring particles taken by TEM. The coercive force was measured using a high sensitivity magnetization vector measuring machine manufactured by Toei Kogyo Co., Ltd. and a DATA processing apparatus manufactured by the same company under the condition of an applied magnetic field of 790 kA / m (10 kOe). The metal nanoparticles for measurement were measured using metal nanoparticles collected from the prepared metal nanoparticle dispersion, sufficiently dried, and heated in an electric furnace at 550 ° C. for 30 minutes.

  Table 1 shows the measurement results of the conventional metal nanoparticles and the metal nanoparticles of the present invention.

表１の結果から分かるように、本発明法の金属ナノ粒子は、従来法の金属ナノ粒子に比べて、小サイズで且つ単分散の粒子の良い金属ナノ粒子が得られた。また、本発明法は従来法に比べて、収率が向上すると共に、組成におけるＰｔの含有率が増加し、保磁力も大きくなった。

As can be seen from the results in Table 1, the metal nanoparticles of the method of the present invention were small and had good monodisperse metal nanoparticles compared to the metal nanoparticles of the conventional method. Further, the method of the present invention improved the yield, increased the Pt content in the composition, and increased the coercive force as compared with the conventional method.

The conceptual diagram explaining the whole structure of the manufacturing apparatus of the chemical substance of this invention Sectional drawing which shows the mixing apparatus of the one jet type high pressure mixing system in the manufacturing apparatus of the chemical substance of this invention Explanatory drawing explaining the mixing theory of the one-jet type high-pressure mixing method Explanatory drawing explaining the shape of the 1st nozzle of the mixing apparatus of a one jet type high pressure mixing system Explanatory drawing explaining another shape of the 1st nozzle Explanatory drawing explaining further another shape of the 1st nozzle Explanatory drawing explaining the other shape of the 1st nozzle Sectional view showing a T-shaped high-pressure mixing device Sectional view showing a Y-shaped high pressure mixing system Sectional view showing a two-jet opposed high-pressure mixing device Explanatory drawing explaining the mixing theory of the two-jet opposed high-pressure mixing method The perspective view which shows the degassing apparatus of the up-and-down meander flow system in the reaction apparatus of this invention Sectional drawing which shows the concept of the degassing apparatus of an up-and-down meander flow Sectional drawing of the aspect which provided the stirrer in the bottom part of the degassing apparatus of an up-and-down meandering type Cross-sectional view of the width of the ascending and descending passages of the degassing device of the up and down meandering flow system Upper / lower meandering flow type degassing unit as an exploded view Sectional view showing the concept of a gas permeation type degassing device

Explanation of symbols

DESCRIPTION OF SYMBOLS 10 ... Manufacturing apparatus, 12 ... 1st mixing apparatus, 13 ... 2nd mixing apparatus, 14 ... Degassing apparatus, 15, 16, 18 ... Preparation tank, 20 ... Heating jacket, 22, 24 ... Supply piping, 17, 26, 28 ... Supply pump, 30, 32 ... Piping, 34 ... Product tank, 36 ... Heating / cooling jacket, 38 ... Mixing chamber, 40 ... Mixer, 42 ... First conduit, 44 ... Discharge tube, 46 ... Second Conduit, 48 ... first orifice, 50 ... second orifice, 52 ... first nozzle, 54 ... second nozzle, 56 ... jacket, 58 ... orifil material, 60 ... third orifice, 62 ... first 64 ... mixing field, 66 ... second addition pipe, 68 ... discharge pipe, 70 ... jacket, 80 ... liquid part, 82 ... space part, 84 ... gas-liquid interface, 86 ... passage, 86A ... rising passage , 86B ... descending passage, 88 ... degassing capacity , 90 ... Dam plate, 92 ... Baffle plate, 92A ... Communication hole, 94 ... Inflow pipe, 96 ... Outflow pipe, 98 ... Bubble, 100 ... Stirrer, 102 ... Pressure adjusting means, 106 ... Pressure sensor, 108 ... Valve, 110 DESCRIPTION OF SYMBOLS ... Gas vent pipe, 112 ... Pressure-reducing means, 114 ... Valve, 116 ... Gas supply piping, 118 ... Control apparatus, 120 ... Temperature adjustment means, 122 ... Ultrasonic application means, 124 ... Inlet unit, 126 ... Intermediate unit, 128 ... Outlet unit, 130, 134, 140 ... box body, 132, 138 ... outlet duct, 136, 142 ... inlet duct, 150 ... degassing pipe, L1 ... first solution, L2 ... second solution, L3 ... third Solution of LM ... reaction solution

Claims (26)

In a method for producing a chemical substance that produces a chemical substance that generates gas in response to a reaction,
A first mixing step of performing a mixing reaction of a plurality of solutions in a first mixing unit of a closed system;
A degassing step of degassing a gas bubble generated from the reaction solution mixed and reacted in the first mixing step in a degassing section having a gas-liquid interface;
And a second mixing step in which an addition solution is added to the reaction solution degassed in the degassing step and a mixing reaction is performed in a second mixing unit, and the reaction solution is transferred from the first mixing step to the degassing step. And a liquid is fed to the second mixing step after completion of the degassing in the degassing step.   The method for producing a chemical substance according to claim 1, wherein a plurality of stages of mixing and degassing steps are provided in series, the first mixing step and the degassing step. In the first mixing step, a first solution containing two or more metal ions selected from groups 8, 9 and 10 of the periodic table is mixed with a second solution containing a reducing agent,
In the second mixing step, a third solution containing one or more metal ions selected from Groups 11, 12, 13, 14 and 15 of the periodic table is added to the reaction solution mixed in the first mixing step. The method for producing a chemical substance according to claim 1 or 2, wherein magnetic particles are produced as the chemical substance by adding and mixing.   The method for producing a chemical substance according to any one of claims 1 to 3, wherein instantaneous mixing is performed in at least the first mixing step of the first mixing step and the second mixing step.   The degassing part is a passage that forms the gas-liquid interface by a liquid part by the reaction liquid and a space part in which the gas removed from the reaction liquid is accumulated, and bubbles of gas in the reaction liquid flowing through the passage The method for producing a chemical substance according to any one of claims 1 to 4, wherein the chemical substance is removed in the space portion.   6. The method for producing a chemical substance according to claim 5, wherein the pressure in the space is reduced.   The passage has an ascending passage and a descending passage through which the reaction solution continuously flows, and forms the gas-liquid interface at a portion where the flow is reversed from the ascending passage to the descending passage. A method for producing 5 or 6 chemical substances.   The method for producing a chemical substance according to any one of claims 5 to 7, wherein the reaction temperature is controlled by heating or cooling the reaction liquid flowing through the degassing section.   The method for producing a chemical substance according to any one of claims 5 to 8, wherein an ultrasonic wave is applied to the reaction liquid flowing through the degassing section.   The method for producing a chemical substance according to any one of claims 5 to 9, wherein a flow rate of the reaction liquid flowing through the descending passage is slower than a rising speed of the bubbles.   The method for producing a chemical substance according to any one of claims 1 to 10, wherein an inside of the degassing part can be seen through. In the chemical substance production equipment that produces chemical substances that generate gas with the reaction,
Between the first mixing unit of a closed system that performs a mixing reaction with a plurality of solutions and the second mixing unit that performs a mixing reaction by adding an additive solution to the reaction liquid mixed in the first mixing unit. An apparatus for producing a chemical substance, comprising a degassing unit having a gas-liquid interface for removing gas bubbles generated from a reaction solution mixed and reacted in one mixing unit from the reaction solution.   At least the first mixing unit of the first mixing unit and the second mixing unit supplies at least one solution of the plurality of solutions in a high pressure jet flow of 1 MPa or more to a mixing chamber having a residence time of 5 seconds or less. 13. The chemical substance production apparatus according to claim 12, wherein the chemical substance production apparatus is a high-pressure mixing apparatus that instantaneously mixes with another solution. The degassing part is a passage that forms the gas-liquid interface by a liquid part by the reaction liquid and a space part in which the gas removed from the reaction liquid is accumulated,
A degassing vessel having an inlet and an outlet for the reaction solution;
A plurality of dam plates standing from the bottom of the degassing vessel and having an upper end located below the gas-liquid interface;
Provided between the barrier plates, the upper end is located above the gas-liquid interface and the lower end is composed of a baffle plate spaced from the bottom of the degassing container,
An ascending passage and a descending passage through which the reaction solution continuously flows are formed in the degassing container, and the gas-liquid interface is formed at a portion where the flow is reversed from the ascending passage to the descending passage. 14. The chemical substance production apparatus according to claim 12, wherein the chemical substance production apparatus is a chemical substance production apparatus.   15. The chemical substance manufacturing apparatus according to claim 14, wherein the space portion is not partitioned by the baffle plate.   16. The apparatus for producing a chemical substance according to claim 14, wherein the height of the weir plate is lowered from the entrance to the exit of the degassing vessel.   The chemical substance manufacturing apparatus according to any one of claims 14 to 16, further comprising pressure adjusting means for adjusting the pressure in the space.   The apparatus for producing a chemical substance according to any one of claims 12 to 17, wherein the degassing unit is provided with temperature adjusting means for controlling the reaction temperature by heating or cooling the reaction solution.   The apparatus for producing a chemical substance according to any one of claims 12 to 18, wherein the degassing unit is provided with an ultrasonic wave applying means for applying an ultrasonic wave to the reaction liquid.   The chemical substance manufacturing apparatus according to any one of claims 14 to 19, wherein a stirrer for forming a flow for preventing stagnation is provided at a bottom of the rising passage formed in the degassing vessel. .   21. The chemical substance manufacturing apparatus according to claim 14, wherein a cross-sectional area of the descending passage is different from that of the ascending passage.   22. The surface treatment according to claim 14, wherein the inner surface of the degassing vessel, the surface of the barrier plate, and the surface of the baffle plate are subjected to a surface treatment that prevents the gas bubbles from adhering. Chemical substance manufacturing equipment.   The chemical substance manufacturing apparatus according to any one of claims 14 to 22, wherein a bottom shape of a degassing container in which the flow of the reaction liquid is reversed from the descending passage to the ascending passage is formed in an arc shape.   Magnetic particles produced using the method for producing a chemical substance according to any one of claims 1 to 11.   Magnetic particles produced using the chemical substance producing apparatus according to any one of claims 12 to 23.   A magnetic recording medium comprising the magnetic particles according to claim 24 or 25 in a magnetic layer.

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