JP5648986B2 - Fluid processing apparatus and fluid processing method - Google Patents

Description

The present invention relates to a fluid processing apparatus and a fluid processing method for reacting at least two fluids to be processed.

Japanese Patent No. 3072467 JP-A-9-75698 Japanese Patent Laid-Open No. 11-347388 JP 2000-15073 A Japanese Patent Laid-Open No. 2001-300281 Japanese Patent Laid-Open No. 2003-47836

  A microchemical plant is a device that utilizes mixing, chemical reaction, separation, etc. in a microscale space, and has many advantages over a conventional batch-type plant using a large tank or the like. For example, it is possible to mix multiple fluids and perform chemical reactions with a small amount of sample in a short time, and because the equipment is small, if the production technology of the product can be established at the laboratory level, the equipment for mass production can be easily obtained by numbering up. Can be applied to reactions involving dangers such as explosions, can be easily adapted to the production of compounds that require high-mix low-volume production, and production volume can be easily adjusted to meet demand It can be done. For this reason, in the fields of chemical industry and pharmaceutical industry, it has been attracting attention as a suitable fluid processing apparatus for producing materials and products by mixing or reacting fluids, and its research and development has been actively conducted in recent years.

  A typical fluid processing apparatus in a microchemical plant includes a micromixer and a microreactor. Micromixers and microreactors each have a small flow channel with a flow channel width on the order of several tens of μm to 1 mm, and mixing or reacting by bringing a plurality of types of fluids led to this flow channel into contact with each other. It is what happens.

  However, in the case of using a general micromixer or microreactor, despite the advantages of microchemical devices and systems, in fact, the smaller the microchannel, the more the pressure loss becomes the fourth power of the channel. There are also problems such as being inversely proportional, that is, a liquid feeding pressure that is so large that there is no pump that actually feeds the fluid, and the phenomenon that the product clogs the flow path and the micro flow path is closed by bubbles generated by the reaction. Many. Furthermore, with regard to scale-up that has been solved by numbering-up, the number of stackable layers is actually limited to several tens, and it is easy to focus on products with high product value. The present invention has been made in view of such problems, and by reacting directly in a thin film, the temperature uniformity is high, and the uniformity in stirring of the reaction vessel is high, so that the desired reaction state can be easily achieved. It is an object of the present invention to provide a fluid processing apparatus that can be implemented and does not clog products due to self-discharge, does not require a large pressure, has high productivity, and enables conventional scale-up without numbering up.

  Specifically, the fluid processing apparatus which improved the apparatus described in patent documents 1-6 is provided.

  The apparatus described in each of the above-mentioned documents is an apparatus for stirring a liquid and liquid or a mixture of liquid and powder into a stirring tank, and generates heat or harmful by-products when mixed in advance. There is a problem that it cannot be used for a combination of substances that may cause the occurrence of the problem.

  In addition, in the inventions described in Patent Documents 1 and 2, an additive can be introduced into the stirring tank separately from the mixture, but the tip of the pipe for adding the additive is an internal space of the stirring tank. Therefore, when an additive is added to the above mixture, the additive is uniformly mixed with the above mixture, for example, the dropped additive hits the stirring blade and splashes unevenly into the stirring tank. There is a fear that it cannot be done. Therefore, when trying to react at least two fluids to be treated, such a method may not work.

The present invention provides a fluid processing apparatus in which at least two fluids to be processed including a reactant are reacted in a thin film state, which includes the following means.

Fluid treatment apparatus according to the present invention, at least the cross-sectional shape perpendicular to the central axis and agitation tank having an inner peripheral surface is circular, in the inner peripheral surface concentric with the stirring tank, the outer end of the stirring tank and a mixing tool which is attached to Mashimashi a slight gap between the inner peripheral surface, in the above stirring tank, a fluid inlet of the at least two positions, and a fluid outlet of at least one place, the fluid inlet from out one place, among the treated fluid, a first fluid to be treated containing one of the reactants is introduced into the stirring tank, from one place other than the above of the above fluid inlet, the A second treated fluid containing one of the reactants different from the reactant is introduced into the agitation tank through a flow path different from the first treated fluid .

Then, at least one of the stirring tank and the mixing tool is relative to the other, and high-speed rotation about said central axis, due to the high speed rotation, the rotation of the object to be processed fluid introduced into the agitation tank, the treated fluid is crimped to the inner peripheral surface so as to surround the center axis of the stirring tank by a centrifugal force, to form a thin film state, at least the first fluid to be treated and the second in thin film which is the formed The reactants contained in the second fluid to be treated are reacted with each other.

The “center axis” is a virtual axis. More specifically, at least a portion of the stirring tank where the fluid to be treated is a thin film is formed in a rotationally symmetric shape, and is a virtual axis that coincides with the center of symmetry. The stirrer or stirring tank rotates around this central axis. Therefore, it is not essential that an actual shaft body corresponding to the central axis exists in the stirring tank.

The film thickness of the thin film is defined by the centrifugal force, and the fluid in at least two places, the fluid inlet for the first fluid to be treated and the fluid inlet for the second fluid to be treated. The inlets are provided on both sides of the agitation tank, which are the surfaces surrounding the central axis, or are provided on the end surface and the side surfaces that intersect the central axis. .

The fluid to be treated introduced from the fluid inlet for the first fluid to be treated into the stirring tank forms the thin film state.
On the other hand, the fluid inlet for the second fluid to be processed is a portion of the inner peripheral surface of the stirring tank where the first fluid to be processed introduced into the stirring tank forms the thin film state. An opening is provided at a position away from the stirring tool in the axial direction of the central axis and at a position where the first fluid to be processed in the thin film state forms a laminar flow state.

The second treated fluid is introduced into the agitation tank along the flow direction of the treated fluid in the agitation tank, and the introduction axis with respect to the agitation tank has an axial direction of the central axis. The angle (α1) with respect to the radial direction of the stirring tank in the cross-section orthogonal is 0 ° to 90 °, and the elevation angle (β1) in the cross section along the central axis of the stirring tank is 0 ° to 90 °. It is.

  This invention can be implemented as said stirring tank being fixed and said stirring tool rotating.

The stirring tank is coordinated to the central axis is oriented vertically, the first fluid inlet for fluid to be treated is also the one provided on the lower end surface of the stirring tank it can.

The stirring tank, said central axis being coordinated so as to face the vertical direction, the discharge of each of the fluid to be treated from the stirring tank is along the flow direction of the fluid to be treated in the above stirring tank adapted, per ejection angle with respect to the stirring tank, in a horizontal section through the center of the fluid outlet, it is also desirable angle relative to the radial direction of the stirring tank ([alpha] 2) is 0 ° to 90 °.

The peripheral speed with respect to the said internal peripheral surface of the said stirring tank in the outer end of the said stirring tool can also be 5 m / s or more.
At the outer end of the mixing tool, the gap relative to the inner peripheral surface of the stirring tank can be a 3mm or less.

The present invention is a fluid treatment method in which at least two fluids containing reactants are reacted in a thin film state, and is introduced into the agitation tank accompanying the high-speed rotation using the fluid treatment device. By the rotation of the fluid to be treated, the fluid to be treated is crimped to the inner peripheral surface so as to surround the central axis of the agitation tank by centrifugal force to form the thin film state, and in the formed thin film The reactants contained in at least the first fluid to be treated and the second fluid to be treated are reacted with each other, and the thickness of the thin film is defined by the centrifugal force . The fluid treatment method is characterized in that the fluid to be treated is brought into the thin film state in the stirring tank, and the second fluid to be treated is directly added to the first fluid to be treated in the thin film state. provide.

The introduction amount of the first fluid to be treated and the second fluid to be treated, it is possible to adjust the speed and residence time of the flow of each fluid to be treated in the stirred tank.

The present invention has a stirring tank having an inner peripheral surface having a circular cross-sectional shape, and a stirring tool provided with a slight gap from the inner peripheral surface of the stirring tank, and is provided from one of the fluid inlets. is the first fluid to be treated containing one of the reactants are charged to a stirred vessel, from another one location of the fluid inlet, a second containing one different reactant with the reactant A fluid to be treated is introduced, and at least one of the stirring tank and the stirring tool rotates at a high speed with respect to the other so that the fluid to be treated is pressed against the inner peripheral surface of the stirring tank by a centrifugal force to form a thin film state. And reacting at least the reactants contained in the first treated fluid and the second treated fluid in the formed thin film, whereby the first treated fluid is characterized in that Directly put at least the other fluid to be treated directly into the thin film from an independent flow path, Since it is possible to respond, to allow high-speed homogenization of the reaction.
The apparatus of the present invention is effective in the case where molecular diffusion is important and a uniform reaction is aimed.

  In particular, at least one of the fluid inlets is opened in a portion of the inner peripheral surface of the agitation tank where the fluid to be treated introduced into the agitation tank from other than the fluid inlet forms the thin film state. . In this way, since the location where the fluid to be treated is introduced is fixed, the reaction state can be easily managed.

  In addition, since the fluid to be treated is held in the form of a thin film on the inner peripheral surface of the agitation tank, even when heating or cooling from the outer surface of the agitation tank, heat conduction is performed quickly and uniformly, which is important for reaction conditions. There are also advantages with regard to thermal factors that have a significant impact, which also allows for high speed homogenization in the reaction.

  In addition, when reacting a fluid to be processed in a thin film state, the outside of the thin film is decompressed, so that air or dissolved oxygen contained in the fluid to be processed, gases generated from the fluid to be processed, low boiling point, etc. Thus, it is possible to degas or remove the organic solvent, and the desired reaction state can be easily achieved.

  That is, in the fluid processing apparatus for reacting at least two fluids in the present invention, the premixing step that has been indispensable so far is not necessary, and the non-uniform coordination and non-uniform heat history of various reactants in the premixed state. In order to eliminate the effects of non-uniform energy drop and always provide a new reaction field, it became possible to obtain a uniform reaction product. Furthermore, the self-discharging property does not cause clogging of the product and does not require a large pressure, resulting in high productivity and scale-up.

  Hereinafter, an example of an embodiment of the present invention will be described with reference to the drawings. In each figure, “1” is a fluid processing apparatus. “2” is a stirring tank, “3” is a lid of the stirring tank 2, and a bearing and a sealing device 4 are attached to the lid 3 to support the drive shaft 5. A stirring blade 6 is fixed to the lower end of the shaft 5 as a stirring tool. “7” is a motor for driving the stirring blade 6, and the motor shaft 7-1 is connected to the shaft 5.

  In the example shown in FIG. 1, the stirring tank 2 is cylindrical, but the shape of the stirring tank 2 is not limited to this, and at least an inner peripheral surface having a circular cross-sectional shape orthogonal to the central axis. For example, it may have a conical shape, a truncated cone shape (see FIG. 4), a bullet shape, a semispherical shape, a spherical shape, or the like. When the cross-sectional shape perpendicular to the central axis is changed, such as a conical shape, as described above, the upper side may have a larger diameter as shown in FIG. The side may have a larger diameter, and the cross-sectional shape may be changed in various other patterns.

  Further, the shape of the inner peripheral surface in the cross section in the direction along the central axis may be a straight line as shown in FIG. 1 or a curve such as a parabola, and there is no problem in stirring the fluid to be processed. It can be implemented with various shapes in the range.

  In the example shown in FIG. 1, the stirring tank 2 is arranged in the vertical direction, that is, the central axis of the stirring tank 2 faces the vertical direction. However, the present invention is not limited to this. You may coordinate so that the center axis | shaft of the tank 2 may face a diagonal direction. If the fluid to be treated can be made into a thin film state in the agitation tank 2 by increasing the rotation speed of the agitator, the center axis of the agitation tank 2 is arranged so as to face the horizontal direction. May be.

  The bottom 8 which is the lower end surface of the stirring tank 2 is a fluid containing a reaction product, and a first fluid L1 for passing the first processed fluid L1 out of at least two processed fluids introduced into the stirring tank 2. One introduction pipe 11 is connected. Although not shown in the drawing, the first treated fluid L1 is passed through the first introduction pipe 11 by means such as liquid feeding by a pressure gas from a tank containing the first treated fluid L1 or a pump. The tip of the first introduction pipe 11 is open to the stirring tank 2. This portion is the first fluid inlet 11a. A first valve 11-1 is provided upstream of the first fluid inlet 11a. This 1st valve | bulb 11-1 is for adjusting the flow volume of the 1st to-be-processed fluid L1. Along with the first valve 11-1, a second valve 11-2 is provided downstream of the fluid inlet 11a in the first introduction pipe 11. The second valve 11-2 is used as a drain valve when a separate fluid is added as the first fluid to be treated L1 and fed, when the reaction process is completed, or at the time of cleaning. As described above, the first introduction path P1 for introducing the first treated fluid L1 into the stirring tank 2 is configured.

  Connected to the lower side surface portion 9a of the agitation tank 2 is a second introduction pipe 12 for passing a second treated fluid L2 different from the first treated fluid L1 out of the at least two treated fluids. . Although not shown, the second treated fluid L2 is passed through the second introduction pipe 12 by means such as liquid feeding by a pressure gas from a tank containing the second treated fluid L2 or a pump. The tip of the second introduction pipe 12 is open to the inner peripheral surface of the stirring tank 2. This portion is the second fluid inlet 12a. As described above, the second introduction path P2 that is different from the first introduction path P1 and introduces the second treated fluid L2 into the stirring tank 2 is configured.

  The upper side surface portion 9b of the agitation tank 2 is connected to a discharge pipe 13 for the fluid to be processed that has reached a desired reaction state, and the fluid to be processed is discharged from the discharge path P3. Similarly to the above, the tip of the discharge pipe 13 is open to the inner peripheral surface of the stirring tank 2. This portion is the fluid outlet 13a. Inside the agitation tank 2, as shown by the arrow in FIG. 2 (A), the fluid to be treated rises against gravity, so that the discharge pipe 13 is connected to each of the introduction pipes 11, It is provided above 12.

  In the example shown in FIG. 1, the first introduction pipe 11 is provided at the bottom 8 of the stirring tank 2, the second introduction pipe 12 is provided at the lower side surface portion 9 a of the stirring tank 2, and the discharge pipe 13 is provided in the stirring tank 2. Although provided in the upper side surface portion 9b, the present invention is not limited to the configuration of this example. For example, in order to introduce three or more fluids to be treated into the stirring tank 2, three or more introduction pipes may be provided as shown in FIGS. 4 and 5 (11, 12 ′, 12 ″ on the drawing). The plurality of fluid inlets may be provided together on the side surface of the stirring tank 2, or may be provided together on the end face of the stirring tank 2. Also, two or more discharge pipes may be provided. It may be provided.

  In this example, the inner surface of the stirring tank 2 is in a smooth surface state. By doing in this way, the flow of the to-be-processed fluid can be smoothly produced in the stirring tank 2 with rotation of the stirring blade 6, and the load of the drive motor 7 can be reduced. On the contrary, depending on the type of fluid to be treated, by providing irregularities and fixed blades on the inner surface of the agitation tank 2, the fluid to be treated in the agitation tank 2 may be turbulent to cause a turbulent flow and thereby react. It is good also as what can promote.

  The adjustment pipe 14 passes through the lid 3 via a valve 14-1. When the pressure in the stirring tank 2 is reduced, the valve 14-1 may be connected to a vacuum source. When the atmosphere in the stirring tank 2 is set to an inert gas atmosphere, the valve 14-1 is set as an inert gas source. Connect to. If these measures are unnecessary, the adjustment pipe 14 need not be installed. Further, when both decompression and inert gas atmosphere are required, a plurality of adjustment pipes 14 may be installed.

  In the example shown in FIG. 1, a flange-shaped weir plate 15 protruding inward of the stirring tank 2 is provided at a position below the discharge pipe 13. In this example, the dam plate 15 is provided so as to bisect the inner peripheral surface of the stirring tank 2, and the fluid to be treated after the reaction in the lower half of the stirring tank 2 flows from the introduction pipes 11 and 12. As the to-be-processed fluid is supplied, it moves over the barrier plate 15 and moves to the upper half of the stirring tank 2. By providing the weir plate 15 in this way, the film thickness of the fluid to be treated in the lower half of the stirring tank 2 is such that the thickness of the weir plate 15 projecting inward from the inner peripheral surface of the stirring layer 2 Match. Therefore, by adjusting the dimensions of the dam plate 15, the thin film of the fluid to be treated can be reacted with a desired film thickness. The barrier plate 15 is not essential in the present invention and may be omitted. Further, the weir plate 15 in this example is provided horizontally so as to be sandwiched between the upper half portion and the lower half portion of the stirring tank 2 as shown in the figure, but welded to the inner peripheral surface of the stirring tank 2. For example, it may be directly attached to the stirring tank 2 or may be formed integrally with the stirring tank 2. Further, the weir plate 15 may be configured to be extendable and contractible so that the projecting dimension from the inner peripheral surface of the stirring tank 2 can be changed depending on the type of fluid to be treated. Moreover, you may provide not spirally, for example, spirally.

  In the example shown in FIG. 1, the weir plate 15 is provided in one place in the stirring tank 2. However, in the case where three or more introduction pipes 12 are provided as shown in FIG. A plurality of fluids to be processed may be sequentially added in the agitation tank 2 to react with each other.

  The stirring tank 2 may be provided with a temperature adjusting mechanism for heating or cooling the fluid to be treated in the stirring tank 2 in order to obtain a temperature condition most suitable for the reaction. In the example shown in FIG. 1, the jacket 16 capable of circulating a fluid heat medium is provided on the outer surface of the agitation tank 2. However, the invention is not limited to this. An element capable of performing a cooling action may be attached to the stirring tank 2.

  In addition to the above, the agitation tank 2 may be provided with a sensor that senses temperature, pressure, and undulations and bias of the thin film.

  In this example, a stirring blade 6 is provided at the lower end of the drive shaft 5 provided concentrically with the inner peripheral surface of the stirring tank 2 as a stirring tool. The stirring blade 6 includes an arm portion 6-1 that extends from the drive shaft 5 in the radially outward direction. A projecting piece 6-2 is provided at the outer end of the arm 6-1 to improve the stirring action. In the example shown in FIG. 1, the protruding piece 6-2 on the left side of the drawing is provided so as to be folded upward from the arm portion 6-1, and the protruding piece 6-2 on the right side of the drawing is lowered from the arm portion 6-1. It is provided so as to be folded back to the side. Since this protrusion 6-2 is for forcibly moving the fluid to be treated along the inner peripheral surface of the stirring tank 2 in the circumferential direction, the outer end shape is along the inner peripheral surface of the stirring tank 2. It is desirable to provide as follows. Therefore, it can be implemented in various shapes other than those shown in the drawings. A slight gap S is provided between the outer end of the protruding piece 6-2 and the inner peripheral surface of the stirring tank 2. The gap S is 3 mm or less, preferably 2 mm or less, more preferably 1 mm or less.

When the stirring blade 6 is rotated at high speed by the drive motor 7, the first fluid L1 introduced into the stirring tank 2 from the first introduction pipe 11 belonging to the first introduction path P1 is rotated at high speed. Is pressed against the inner peripheral surface of the agitation tank 2 to form a thin film state. Here, since the first treated fluid L1 is sequentially introduced from the first introduction pipe 11 connected to the bottom 8 of the agitation tank 2, the first treated fluid in the thin film state as described above is accordingly introduced. An upward spiral flow as shown in FIG. 2A is generated in the fluid L1. The speed of the spiral flow is proportional to the introduction speed of the first treated fluid L1 into the stirring tank 2. The second treated pipe L2 that belongs to the second introduction path P2 that is a separate flow path independent of the first introduction path P1 is directly fed into the formed first treated fluid L1 in the thin film state. The desired reaction state can be achieved by introducing into the stirring tank 2 from 12. As the stirring blade 6 rotates at high speed, the first fluid L1 in the thin film state also rotates at high speed along the inner peripheral surface of the stirring tank 2, so that the above state can be sufficiently achieved in a short time.

  Here, the “high speed rotation” means a rotation speed at which the fluid to be processed can form a thin film state in the stirring tank 2 by centrifugal force. Specifically, the peripheral speed at the outer end of the stirring blade 6 is 5 m / s or more. , Preferably 10 m / s or more, more preferably 20 m / s or more.

  As described above, the second fluid inlet 12a of the second introduction pipe 12 has the first treated fluid L1 introduced from the first introduction pipe 11 to the stirring tank 2 out of the inner peripheral surface of the stirring tank 2 described above. Since the opening is formed in the portion forming the thin film state, the second processed fluid L2 is directly added to the thin film of the first processed fluid L1, and the reactants in the processed fluids L1 and L2 are directly reacted with each other. Can do.

  As described above, since the present invention enables direct reaction in a thin film, the reaction can be made uniform at high speed. In addition, the premixing process, which has been indispensable in conventional fluid processing, is unnecessary, and the effects of non-uniform coordination of reactants, non-uniform heat history, and non-uniform energy injection in the pre-mixed state are eliminated. Since a reaction field is provided, a uniform reaction product can be obtained.

  The fluid processing apparatus 1 of the present invention can adjust the flow speed and residence time of each of the fluids L1 and L2 in the agitation tank 2 according to the introduction amounts of the first fluid L1 and the second fluid L2. Thus, a desired reaction state can be easily achieved.

  When the fluid to be treated is accompanied by crystal precipitation due to reaction or the like, the precipitated crystal can have a desired particle size and particle size distribution by adjusting the rotation speed of the stirring tool.

  In addition, although this invention is mainly what each to-be-processed fluid L1, L2 reacts in a thin film, it does not exclude reaction outside the said thin film, and reaction outside a thin film in addition. May be made.

  In the example shown in FIG. 1, the stirring tank 2 is fixed and the stirring blade 6 rotates at a high speed. Conversely, the stirring blade 6 may be fixed and the stirring tank 2 may be rotated at a high speed. Alternatively, both the stirring blade 6 and the stirring tank 2 may be rotated.

  Further, in the example shown in FIG. 1, only one set of stirring blades 6 is provided, but a plurality of sets may be provided as shown in FIG. The number of arm portions 6-1 per set of stirring blades 6 may also be set as appropriate.

  In this example, the stirring blade 6 as shown in FIG. 1 was used as a stirring tool, but the stirring blade 6 is not limited to the shape having the shape of the blade, and the inner peripheral surface of the stirring tank 2 as shown in FIG. It can also be implemented as a rotating cylinder 6 ′ provided along. This rotating cylinder is hollow and has a large number of through-holes 6 ′-1, and like the stirring blade 6, the fluid to be processed can be made into a thin film state by high-speed rotation.

  In the present invention, the second treated fluid L2 is directly introduced into the first treated fluid L1 formed in the thin film state as described above from the second introducing passage P2, which is a separate flow path independent of the first introducing passage P1. Since this is the greatest feature, it will be described in more detail below.

  The relative position between the position of the stirring tool such as the stirring blade 6 in the stirring tank 2 and the introduction position where the second treated fluid L2 is directly introduced from the second introduction path P2 which is a different flow path from the first introduction path P1. The target relationship is adjusted according to the target reaction state. That is, the fluid to be processed in the state of a thin film in the vicinity of the stirrer forms a turbulent state and is effective for the purpose of reaction under uniform mixing, etc., and the thin film at a position away from the stirrer Since the fluid to be treated generally forms a laminar flow state, it is effective when the molecular diffusion is regarded as important and a uniform reaction is intended.

  Further, a second introduction pipe for introducing the second treated fluid L2 directly from the second introduction path P2 which is an independent separate flow path into the first treated fluid L1 in a thin film state in the stirring tank 2. 12 is an angle with respect to the stirring tank 2 in the horizontal section X1 (see FIG. 1) passing through the center of the second fluid inlet 12a as a reference, as shown in FIG. 2B. It is attached with α1. α1 is set to 0 ° to 90 °, more preferably 20 ° to 70 °, and the flow direction of the first treated fluid L1 in a thin film state along the inner peripheral surface of the stirring tank 2 (FIG. 2 ( The direction of introduction of the second treated fluid L2 does not face the arrow direction B) above, and the flow of the first treated fluid L1 is not disturbed more than necessary.

  The second introduction pipe 12 is attached to the stirring tank 2 with an elevation angle β1 in a vertical cross section passing through the central axis of the stirring tank and the center of the fluid inlet. β1 is set to 0 ° to 90 °, more preferably 10 ° to 50 °. When the stirring tank 2 is coordinated as shown in FIG. The flow direction of the first treated fluid L1 does not oppose the direction in which the second treated fluid L2 is introduced in the upward spiral flow direction in the stirring tank 2 (the arrow direction in FIG. 2A). Do not disturb more than necessary.

  The second introduction pipe 12 has both the directivity of the angle α1 with respect to the horizontal flow direction of the first treated fluid L1 and the directivity of both the angle β1 with respect to the vertical flow direction with respect to the stirring tank 2. Is more preferable. In this way, by setting the positional relationship in the forward direction with respect to the flow direction of the first fluid to be treated L1, the second target to be introduced from the second introduction path P2, which is a separate flow path independent of the first introduction path P1. Regarding the introduction of the processing fluid L2, the power relating to the transfer means such as a pump is reduced, and it is also effective when importance is attached to the diffusion conditions.

  And the discharge pipe 13 discharged | emitted from the stirring tank 2 after reaction to each to-be-processed fluid L1, L2 will be in a desired state in a thin film state is the radial direction of the stirring tank 2 in horizontal cross section X2 (refer FIG. 1). It is attached with an angle α2 with reference to. The ridge 2 is 0 ° to 90 °, more preferably 40 ° to 80 °. The reason is to prevent bubbles from being mixed into the processed fluid and not disturb the state of the thin film in the stirring tank 2.

  Further, in the fluid processing apparatus 1, the diameter of the second introduction pipe 12 at the second fluid inlet 12a is 20 μm to 3000 μm, preferably 50 μm to 1000 μm. As a result, even if the reaction rate is high and the reaction is accompanied by precipitation, the problem that the substance deposited near the second fluid inlet 12a does not block the second fluid inlet 12a does not occur. The spiral and laminar flow generated in the agitation tank 2 due to the flow of the second treated fluid L2 introduced from 12a is minimized. Thereby, good results can be obtained in a uniform reaction.

  Further, as described above, since the structure is very simple and there are few places where the fluid to be treated comes into contact with the fluid, the fluid treatment apparatus 1 is less likely to malfunction, the yield is improved, and the cleaning performance and sterilization are improved. Excellent in properties.

  Further, a small-diameter medium (such as a ball or a bead) made of ceramic, resin, metal, glass, or the like may be mixed in the stirring tank 2 and the fluid to be processed and the medium may be rotated at a high speed together. In particular, this has an effect of refining the precipitated crystal when the fluid to be treated is accompanied by crystal precipitation due to reaction or the like.

  Examples of fluids to be processed that are suitable for the fluid processing apparatus 1 of the present invention are illustrated below. The reaction of the reactant contained in the fluid to be treated in the agitation tank 2 is not particularly limited, but is an oxidation reaction, a reduction reaction, a neutralization reaction, a hydrolysis reaction, a dehydration reaction, a condensation reaction, a polymerization reaction. Reactions of organic compounds represented by various reactions such as substitution reaction, transfer reaction, addition reaction, coupling reaction, adsorption reaction, radical reaction, acylation reaction, nitration reaction, indole reaction, hydroxylation reaction, diazotization reaction, etc. Etc.

Of those described above, those accompanied by crystal precipitation by the reaction are not particularly limited. However, reduction reactions in the case where metal ions are reduced with a reducing agent to precipitate metal solids or metal particles, titanium tetrachloride or titanium Barium sulfate is precipitated by hydrolyzing ceramic raw materials such as isopropoxide to precipitate ceramic particles or ceramic precursors, or by mixing a solution containing barium ions and a solution containing sulfate ions. Examples thereof include neutralization reactions as typified by cases. Moreover, the case where a cation and an anion react, and a compound semiconductor particle precipitates like the compound semiconductor represented by the nanodot, the quantum dot, and the nanocrystal, etc. are mentioned. Furthermore, it can be carried out in the case of an acid pasting process in which cyan pigment particles are precipitated when a concentrated sulfuric acid solution of cyan pigment is added to water, and a solution in which drug particles are dissolved is used as the drug. When putting drug particles into a solvent with low particle solubility, that is, using a solvent (good solvent) with high solubility in a substance and a solvent (poor solvent) with low solubility in a good solvent. Etc. can also be implemented. Furthermore, in the case of precipitation using the difference in solubility, it can be carried out using the difference in solubility of the substances in each solvent as described above . For example, when the solubility changes due to temperature change, By mixing a low-temperature solution with a solution of a substance dissolved in a high temperature state, the solubility of the whole liquid is lowered and the substance can be precipitated. Other factors that change the solubility include the pH of the solution.

It is a longitudinal cross-sectional view which shows an example of embodiment of this invention. The attachment state to the stirring tank of the 2nd introduction pipe | tube based on an example of embodiment of this invention is shown, (A) is a principal part longitudinal cross-sectional view, (B) is a principal part cross-sectional view. It is a principal part cross-sectional view which shows the attachment condition to the stirring tank of the discharge pipe based on an example of embodiment of this invention. It is a longitudinal cross-sectional view which shows an example of other embodiment of this invention. It is a longitudinal cross-sectional view which shows an example of other embodiment of this invention.

DESCRIPTION OF SYMBOLS 1 Fluid processing apparatus 2 Stirrer tank 3 Stirrer tank lid 4 Sealing device 5 Drive shaft 6 Stirrer (stirrer blade)
7 Driving motor 8 Bottom of stirring tank 11 First introduction pipe 12 Second introduction pipe 13 Discharge pipe L1 First treated fluid L2 Second treated fluid P1 First introduction path P2 Second introduction path P3 Discharge path S Gap α1 Introduction angle of fluid to be treated (horizontal section)
α2 Discharge angle of fluid to be treated (horizontal section)
β1 Introduction angle (elevation angle) of fluid to be treated

Claims (8)

In a fluid processing apparatus in which at least two fluids to be processed including reactants are reacted in a thin film state,
At least a stirring tank having an inner peripheral surface having a circular cross-sectional shape orthogonal to the central axis,
In the inner peripheral surface concentric with the stirring tank, and a mixing tool which outer end is attached to Mashimashi a slight gap between the inner peripheral surface of the stirring tank,
The stirring tank includes at least two fluid inlets and at least one fluid outlet,
From one point of the said fluid inlet, of the fluid to be treated, a first fluid to be treated containing one of the reactants is introduced into the stirring vessel, one place other than the above of the above fluid inlet from the second fluid to be treated containing one different reactants and the reactants are those which introduced into the stirring vessel from different flow paths from the above first fluid to be treated,
At least one of the stirring tank and the mixing tool is relative to the other, and high-speed rotation about said central axis,
Due to the high speed rotation, the rotation of the object to be processed fluid introduced into the agitation tank, is crimped to the inner peripheral surface so as to surround the center axis of the stirring tank of the fluid to be treated in the centrifugal force, a thin film state forming a, which react the reactants to each other contained in at least the first fluid to be treated and the second fluid to be treated in a thin film which is the formed,
The film thickness of the thin film is defined by the centrifugal force ,
The at least two fluid inlets of the fluid inlet for the first fluid to be processed and the fluid inlet for the second fluid to be processed are on the side surface that is the surface surrounding the central axis in the stirring tank. Or both provided on the end surface and the side surface that intersect the central axis,
The fluid to be treated introduced from the fluid inlet for the first fluid to be treated into the stirring tank forms the thin film state,
The fluid inlet for the second treated fluid is opened to a portion of the inner peripheral surface of the stirring tank where the first treated fluid introduced into the stirring tank forms the thin film state. And in the axial direction of the central axis, provided at a position away from the stirring tool and at a position where the first fluid to be processed in the thin film state forms a laminar flow state,
The second treated fluid is introduced into the agitation tank along the flow direction of the treated fluid in the agitation tank, and the axial direction of the central axis is determined with respect to the introduction angle with respect to the agitation tank. The angle (α1) with respect to the radial direction of the stirring tank in the cross-section orthogonal is 0 ° to 90 °, and the elevation angle (β1) in the cross section along the central axis of the stirring tank is 0 ° to 90 °. fluid treatment apparatus, characterized in that it. The fluid processing apparatus according to claim 1, wherein the stirring tank is fixed, and the stirring tool rotates. The stirring tank, said central axis being coordinated so as to face the vertical direction,
The fluid processing apparatus according to claim 1 , wherein the fluid inlet for the first fluid to be processed is provided on a lower end surface of the stirring tank. The stirring tank, the central axis are coordinated so as to face the vertical direction,
Discharge of the respective fluid to be treated from the stirring tank is made along the flow direction of the fluid to be treated in the above stirring tank,
Per discharge angle with respect to the stirring tank, according to claim 1, characterized in that in a horizontal section through the center of the fluid outlet, the angle relative to the radial direction of the stirring tank ([alpha] 2) is 0 ° to 90 ° 4. The fluid processing apparatus according to any one of 3 . At the outer end of the mixing tool, the fluid processing apparatus according to claim 1, the peripheral speed relative to the inner peripheral surface of the stirring tank is characterized in that it is 5 m / s or more. At the outer end of the mixing tool, the fluid processing apparatus according to claim 1, the gap relative to the inner peripheral surface of the stirring tank is characterized in that less than 3mm. In a fluid processing method in which at least two fluids containing reactants are reacted in a thin film state,
Using the fluid treatment device according to any one of claims 1 to 6,
Due to the rotation of the fluid to be treated introduced into the stirring tank accompanying the high-speed rotation, the fluid to be treated is crimped to the inner peripheral surface so as to surround the central axis of the stirring tank by centrifugal force. The thin film state is formed, and at least the reactants contained in the first treated fluid and the second treated fluid are reacted in the formed thin film,
The film thickness of the thin film is defined by the centrifugal force ,
The first treated fluid is in the thin film state in the agitation tank, and the second treated fluid is directly added to the first treated fluid in the thin film state. Processing method. The introduction amount of the first fluid to be treated and the second fluid to be treated, according to claim 7, characterized in that to adjust the rate and residence time of the flow of each fluid to be treated in the stirred tank Fluid processing method.

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