JP2015123383A - Continuous reaction unit, and method for continuous crystallization reaction of inorganic particle - Google Patents

Abstract

PROBLEM TO BE SOLVED: To provide a small-sized processing unit having a sufficient throughput with uniform contact processing characteristics.SOLUTION: In a reactor 10, a swirling flow of liquid is created. Injection liquids A and B are injected into a contact field in the reactor 10 at a position away from the inner surface of the reactor 10 toward the center, so as to be subjected to contact processing.

Description

  The present invention relates to a continuous reaction apparatus for circulating a contact treatment liquid and performing a reaction, and a continuous reaction crystallization method for inorganic particles.

  There are an unlimited number of operations for obtaining a product or an intermediate product through industrial treatment such as liquid-liquid reaction, gas-liquid reaction, catalytic reaction, or the like, or generation of particles by crystallization treatment.

  For example, as shown in FIG. 13, for example, A component, B component or C component is put into stirring contact processing tank 1 and stirred by stirring blade 3 with stirring motor 2 to promote reaction of each component. It is common to make it. At an appropriate time, the product liquid is withdrawn from the discharge port 5, and then target crystallized particles are obtained by, for example, filtration, washing and drying. 4 is a baffle.

However, in this processing mode, a large contact processing tank 1 is required and stirring is performed by the stirring blade 3 for uniform reaction and processing, but there is a limit to expecting high uniformity.
On the other hand, as a processing method, when each component is charged into the contact processing tank 1 and then stirred, the production efficiency is poor. Therefore, the continuous production method in which each component is continuously added during stirring can provide high efficiency, but it is difficult to set the conditions for contact treatment (such as controlling the amount of input over time), and a uniform product can always be obtained efficiently. It is not something that can be done.
As an attempt to improve these, a microreactor with a flow path of 1 mm or less has been proposed, but the production volume is low and problems with continuous production due to blockage of the flow path have been pointed out. Few.

  Patent Document 1 discloses a technique for bringing a component into contact with another component in the process of moving the component in a cyclone system.

JP-A-4-240288

  However, the prior art is a component separation technique and is not intended for reaction or treatment.

  In the contact processing field including the chemical industry, there is a great demand for a reaction apparatus that exhibits a sufficient throughput while exhibiting a uniform contact processability even though it is a small processing apparatus.

  Therefore, a main problem of the present invention is to provide a reactor and a continuous reaction crystallization method for inorganic particles that exhibit a sufficient throughput while exhibiting a uniform contact processability even though they are small processing apparatuses. .

The present invention that has solved this problem is as follows.
[Invention of Claim 1]
A reactor having one end and the other end; injection means for injecting the reaction liquid into the reactor; and extracting the contact treatment liquid from the other end of the reactor, and at least the extracted contact treatment liquid Circulating means for returning a part to the one end of the reactor,
The liquid flow in the reactor is swirled by returning the contact treatment liquid, and the swirl is configured to contact the reaction liquid injected by the injection means.
A continuous reaction apparatus comprising pressure increasing means for increasing the pressure in the reactor from normal pressure.

[Invention of Claim 2]
The continuous reaction apparatus according to claim 1, wherein the reaction liquid is injected at a position closer to the center than the inner surface of the reactor.

(Function and effect)
In a field that shows a swirling flow as a liquid flow, the flow in the central vortex part or the inner peripheral part in the vicinity of the central cavity part like a tornado has a disturbed flow such as high mass transfer / stirring mixing effect that affects the reaction. large. This portion becomes an abrupt diffusion field of the injection solution containing the reactant or gas to be injected, and a homogeneous reaction is possible.
Furthermore, since the outer peripheral portion of the swirl flow is in contact with the wall surface of the flow path, the swirl flow on the outer periphery serves as a reactant supply body, and abrupt changes in material and heat are mitigated. Since it functions as a barrier against the reactants of the injected injection material (liquid, gas, solid), it prevents the reactant from adhering to the inner surface of the reactor and the inner surface of the flow path and is stable for a long time The present inventor tried to develop a reaction processing apparatus that uses a tube reactor as an apparatus that exhibits a sufficient throughput even though it is a small processing apparatus. However, in certain types of reaction processing material systems, fine showers (primary nuclei) adhere to the walls of the flow channel, and then crystals grow from this as the nuclei, blocking the flow and long-term stable operation. Some cases were difficult to do.

  As a countermeasure, it is conceivable to arrange reaction paths in parallel and, if clogging occurs, switch to the other reaction path for circulation, and clean the reaction path in which clogging occurred. However, it was judged that a change in particle size due to discontinuous operation should be avoided even in a short time of switching, and that a new mechanism is necessary to withstand stable operation over a long period of time.

  On the other hand, according to the present invention, the liquid flow in the reactor is a swirl flow by returning the contact treatment liquid, and the swirl flow is brought into contact with the reaction liquid injected by the injection means. It was found that this could be solved.

  On the other hand, although the target aggregated particles can be generated by performing the contact treatment at normal pressure, a treatment substance is obtained by providing a pressure-increasing means for raising the pressure in the reactor above normal pressure and performing the reaction under the action of pressure. It has been found that the reaction is further promoted or suppressed. This is because the dielectric constant of the liquid increases with increasing pressure, and ionic substances are likely to solvate. This change in dielectric constant affects the reaction rate such as nucleation and primary particle growth. Conceivable.

[Invention of Claim 3]
The contact field in the reactor between the returned contact treatment liquid and the injected reaction liquid is defined as a region on the center side from the inner surface of the swirling flow reactor generated in the reactor. The continuous reaction apparatus according to claim 1, wherein the reaction solution is brought into contact.

(Function and effect)
When a liquid is circulated through the reactor and a return flow of the circulating liquid is caused to flow into the reactor to generate a swirling flow, a cylindrical body having a thickness where the outer peripheral portion of the swirling flow is on the inner surface of the reactor Forming part. As a result, a phenomenon occurs in which the cylindrical body part functions as a barrier (barrier) against the reaction with the newly injected liquid, and the contact field is set to the central region from the inner surface of the swirling flow reactor. The reaction solution was brought into contact in this contact field. As a result, it is possible to alleviate temperature changes accompanying heat absorption and heat generation due to the reaction and to prevent the reactants from adhering to the inner surface of the flow path.

[Invention of Claim 4]
2. The continuous reaction apparatus according to claim 1, wherein the inner surface of the reactor is tapered from one end side toward the other end portion, and the contact treatment liquid inflow position is at one end portion in the longitudinal direction of the reactor.

(Function and effect)
The reactor may have a cylindrical shape with a uniform inner radius, but a reactor whose inner surface is tapered from one end to the other end in the longitudinal direction is suitable for generating a swirling flow. .
In addition, it is desirable for the reactor to ensure a certain long space along the longitudinal direction in order to lengthen the contact field of the swirl flow. In view of this, it is a preferred embodiment that the liquid is allowed to flow from one end portion in the longitudinal direction of the reactor and to flow out from the other end portion in the longitudinal direction.

[Invention of Claim 5]
The continuous reaction apparatus according to claim 1, further comprising a pressure adjusting means and a circulation pump in this order in a circulation path through which the contact treatment liquid extracted from the other end of the reactor is returned to the one end.

(Function and effect)
As a pressure increasing means for raising the pressure in the reactor from the normal pressure, the pressure adjusting means and the circulation pump are arranged in this order in the circulation path in which the contact treatment liquid extracted from the other end of the reactor is returned to the one end. It can be configured by having it, and the configuration is simple and the pressure in the reactor can also be adjusted. Further, when an external treatment tank is installed between the pressure adjusting means and the circulation pump, the circulation pump can be driven stably.

[Invention of Claim 6]
A circulation path through which the contact treatment liquid extracted from the other end of the reactor is returned to the one end has a pressure regulating valve, a circulation pump, and a pressure gauge in this order. The continuous reaction apparatus according to claim 1, wherein the pressure adjusting valve adjusts the pressure based on the pressure.

(Function and effect)
The pressure distribution in the reactor can be easily adjusted. If the inlet pressure is adjusted, the pressure distribution is known in advance, so that the pressure in the reaction field in contact with the reaction solution can be monitored.

[Invention of Claim 7]
A pressure regulating valve, a pressure reservoir for temporarily storing the contact treatment liquid, a circulation pump, and a pressure gauge are arranged in this order on the circulation path through which the contact treatment liquid extracted from the other end is returned to the one end. The compressor or pressurizing cylinder for pressurizing the inside thereof is connected to the pressure reservoir, and the compressor or the pressurizing cylinder adjusts the pressure based on the pressure of the circulation path by the pressure gauge. Continuous reactor.

(Function and effect)
The inside of the pressure reservoir is pressurized by a compressor or a pressurizing cylinder, whereby the pressure in the reactor can be increased from the normal pressure.
[Invention of Claim 8]
A pressure regulating valve, a pressure reservoir for temporarily storing the contact treatment liquid, a circulation pump, and a pressure gauge are arranged in this order on the circulation path through which the contact treatment liquid extracted from the other end is returned to the one end. A compressor or a pressurizing cylinder is connected to the pressure reservoir, and the contact treatment liquid is continuously or intermittently extracted from the circulation path based on the pressure of the pressure reservoir by the pressure gauge. The continuous reaction apparatus of Claim 1 which provided the pressure control system to perform.
(Function and effect)
By keeping the pressure in the pressure reservoir constant, the pressure in the reaction field is kept constant, fluctuations in the reaction liquid injection pressure are reduced, and reaction liquid injection control can be stabilized.

[Invention of Claim 9]
The continuous reaction apparatus according to claim 1, wherein the reactors for providing the contact field are arranged in series.

(Function and effect)
When it is desired to increase the throughput, it is desirable to arrange the reactors in series. By arranging in series, it is possible to increase the amount of injected liquid by the number of stages without increasing the amount of circulating return liquid, increasing the production volume and reducing the internal capacity of the apparatus relative to the production volume, As a result, it is possible to save space and reduce apparatus cost. Here, “the capacity of the device relative to the production volume is reduced” means that the capacity of the circulation pump and the flow path part remains constant and only the capacity of the reactor and the pipe connecting them is injected. This means that the overall capacity of the apparatus can be reduced compared to the production volume. Further, “reducing the internal volume of the apparatus” also has the effect of shortening the residence time of the reactants in the apparatus, and as a result, the residence time can be controlled to reduce the diameter.
Furthermore, according to such a configuration, by adjusting the reaction rate expressed in a form such as generation of nuclei and growth of particles by using a high pressure in the former stage and a low pressure in the latter stage, it is possible. For species of reactants, it is a very suitable means.

[Invention of Claim 10]
The continuous reaction apparatus according to claim 1, wherein the injection direction with respect to the contact field of the reaction solution is directed in the downstream direction of the swirl flow or from the one end side to the other end part.

(Function and effect)
The injection direction with respect to the contact field of the injection liquid may be in the upstream direction of the swirling flow of the liquid, but is in the direction downstream in the streamline direction of the swirling flow of the liquid or from the one end side toward the other end. The amount of reaction solution injected can be controlled more smoothly.

[Invention of Claim 11]
A reactor having one end and the other end; injection means for injecting the reaction liquid into the reactor; and extracting the contact treatment liquid from the other end of the reactor, and at least the extracted contact treatment liquid Circulating means for returning a part to the one end of the reactor,
Furthermore, it has a pressure raising means for raising the pressure in the reactor from the normal pressure,
The liquid flow in the reactor is swirled by returning the contact treatment liquid, the reaction liquid injected by the injection means is brought into contact with the swirl flow, the reaction is performed, and reaction crystallization of inorganic particles is performed. A continuous reaction crystallization method for inorganic particles.

(Function and effect)
There exists an effect similar to Claim 1.

  As described above, according to the present invention, there is an advantage that a sufficient amount of processing can be achieved and a uniform contact processing property can be exhibited even though the processing device is small.

It is a schematic diagram of the 1st example of the present invention. It is a schematic diagram of the reactor of the 1st example. It is a cross-sectional schematic diagram of the upper end part of a reactor. It is an explanatory outline figure of the generation form of swirl flow. It is a schematic diagram of the example of serial arrangement of a reactor. It is a schematic diagram of other embodiment. It is a schematic diagram of another embodiment. It is a schematic diagram of the other reactor example. It is a schematic diagram of the example of another form of a reactor. An example of a block unit reactor is shown, (a) is a plan view and (b) is a front view. It is a vorticity distribution map at 55 kPa. It is a vorticity distribution map in 147kPa. It is a schematic diagram of a prior art example.

Next, the form for implementing this invention is demonstrated.
As will be described later, the scope of application of the present invention is wide. However, a comprehensive description of various examples may cause confusion, so an example of the apparatus will be described with an example, and another application range will be described later.

A typical example of the present invention is a continuous reaction apparatus for obtaining agglomerated particles of metal particles. One specific example is intended to produce aggregated particles using Ni and Co transition metals.
According to the present invention, a method for injecting an injection solution containing an inorganic substance to be injected at a position closer to the center than the inner surface of the reactor in the contact field of the swirling flow in the reactor and performing the contact treatment is generally widely used. Since it can be applied to the case where aggregated particles are obtained from an inorganic substance, metals other than the transition metal and other inorganic substances may be targeted.

1 to 4 show a first example of the present invention, in which a liquid flow in the reactor 10 is a swirl flow, and an injection liquid containing an inorganic substance to be injected is contacted in the reactor 10. In FIG. 2 and FIG. 4 conceptually indicated by the symbol Q, the injection is performed at the center side position from the inner surface of the reactor 10 to perform the contact treatment.
In the illustrated example, A liquid, B liquid, and C liquid are injected as an injection liquid containing an inorganic substance to be injected. Although not shown, a gas (inert gas such as nitrogen gas or carbon dioxide gas) can be injected in parallel.
The first example of the present invention is an example in which the injection direction with respect to the contact field of the injection liquid containing the inorganic substance to be injected is directed to the downstream direction of the swirling flow of the liquid.
Although the illustrated reactor 10 is in the horizontal direction, it may be in the vertical direction because it does not affect the flow in principle.

The illustrated reactor 10 circulates the liquid through the circulation paths 11 and 14 (the extraction path 11 and the return path 14) by the circulation pump 13, and allows the return liquid of the circulating liquid to flow into the reactor 10. A swirl flow is generated. Reference numeral 15 denotes a temperature controller for heating or cooling the liquid provided as necessary.
As shown in the drawing, the reactor 10 has a tapered inner surface from one end side in the longitudinal direction to the other end, and the inflow position including the inlet 10X for returning the circulating fluid is the reactor. 10 at one end in the longitudinal direction, and as shown in FIG. 3, the return liquid is allowed to flow in substantially the tangential direction in a form along the inner peripheral surface thereof. Thereby, a swirl flow R is formed.
The outflow position including the outflow port 10Y of the contact processing liquid after the contact processing is performed is the other end portion in the longitudinal direction.

The contact treatment liquid is guided to the temporary storage device 20, and the contact treatment liquid is stabilized and particles are settled in the temporary storage device 20. The final contact treatment liquid 10 </ b> Z is used as an overflow liquid from the temporary storage device 20. Or it is transferred to the subsequent productization means (not shown) by the extraction pump 22. 21 is a take-off valve. 23 is an adjustment stirrer.
The remaining liquid is returned to the reactor 10 by the circulation pump 13 via the return path 14.

A pressure indicator 12A is provided at the inlet portion of the reactor 10, and a pressure adjustment valve 12B is provided at the outlet portion. By narrowing the valve opening degree of the pressure adjustment valve 12B with respect to the discharge pressure of the circulation pump 13, The pressure in the reactor 10 is in a pressurized state.
Then, the pressure in the reactor 10 is adjusted by adjusting the valve opening degree of the pressure adjusting valve 12B based on the current pressure by the pressure indicator 12A.
The pressure in the reactor 10 is preferably 0.01 to 1.0 MPa, particularly 0.05 to 0.3 MPa at the inlet portion of the reactor 10.

The liquid flow in the reactor 10 becomes a swirl flow R, but there is a tendency that a hollow portion V (see FIG. 4) is formed at the center of the vortex. In particular, the flow in the inner peripheral portion in the vicinity of the vortex center of the swirling flow R is remarkably faster than the average flow velocity, and the flow disturbance is large.
When the injection liquids A to C containing the metal to be injected are injected at such positions, the injection liquid diffuses rapidly and a homogeneous reaction is possible.
Therefore, as shown in FIG. 2, it is desirable to prevent each of the infusion solutions A to C until they are discharged from their tips using the infusion tubes 16A, 16B.
Furthermore, it is desirable to insert the guide tube 17 so as not to be affected by the swirling flow R.

  Here, the injection positions of the injection liquids A to C containing the inorganic substance to be injected may be injected at a position closer to the center than the inner wall surface of the reactor 10 in the contact area in the reactor 10. As indicated by position 4, the radius is preferably within 2/3 of the radius r, preferably within 1/2.

  As shown in the example of FIG. 5, the reactors 10, 10... That provide the contact field can be arranged in series.

On the other hand, as shown in FIG. 6, a sealed pressure reservoir 30 is provided, and this is pressurized by the compressor 24 to pressurize the inside of the reactor 10.
Also in this example, a pressure indicator 12A is provided at the inlet portion of the reactor 10, and a pressure adjustment valve 12B is provided at the outlet portion. The valve opening degree of the pressure adjustment valve 12B with respect to the discharge pressure of the circulation pump 13 is provided. By reducing the pressure, the pressure in the reactor 10 is in a pressurized state.
Further, the pressure reservoir 30 is also provided with a pressure indicator 30A, and by adjusting the valve opening degree of the pressure regulating valve 12B based on the current pressure by the pressure indicator 30A and the pressure indicator 12A, A controller 50 for adjusting the pressure is provided.

  A part of the liquid in the pressure reservoir 30 is sent into the adjustment tank 20 via the transfer path 16 by the extraction pump 22A, and the particle size and the like are adjusted, and finally the subsequent product is extracted by the extraction pump 22A. Is transferred to a converting means (not shown).

  The remaining liquid in the pressure reservoir 30 is returned to the reactor 10 by the circulation pump 13 via the return path 14.

  On the other hand, as shown in FIG. 7, the pressure regulating valve 12 </ b> B, the pressure regulating valve 12 </ b> B, the pressure reservoir 30 that temporarily stores the contact processing liquid, and the pressure gauge that indicates the pressure in the pressure reservoir 30 as shown in FIG. 7. 30A and a circulation pump 13 are arranged in this order, and a compressor 24 or a pressure cylinder for pressurizing the inside thereof is connected to the pressure reservoir 30, and contact is made from a circulation path based on the pressure of the pressure reservoir 30 by the pressure gauge 30A. It is desirable to provide a pressure control system having a controller 51 that continuously or intermittently extracts the processing liquid and controls the pressure in the pressure reservoir 30 to be constant. The specific control operation can be performed on the extraction pump 22A or the extraction valve 22C.

In the reactor 10 of the above example, the one whose inner surface is tapered from the one end side in the longitudinal direction toward the other end is suitable for generating a swirl flow, but the inner space has a uniform radius. It may be in a shape.
Further, as shown in FIG. 8, a rotating cylinder or a fixed cylinder 40 is provided in the reactor 10, and the injection liquids A and B containing the metal to be injected are introduced into the tangential direction of the inner wall surface through the injection pipes 42 and 43. The effluent after the contact treatment is made to flow out from the outflow pipe 44 at the other end.

  In the example shown in FIGS. 1 to 4 in which the inner space includes a cylindrical portion having a uniform radius and a tapered portion, the change position from the cylindrical portion to the tapered portion can be selected as appropriate. However, the inflow port 10X for the contact treatment liquid is preferably in the cylindrical part for generating a spiral flow.

In the embodiment shown in FIG. 2, the injection solution is injected on the relatively downstream side of the reactor 10. However, as shown in FIG. 9, the guide tube 17 is shortened and the injection solution A to C solution injection tube 16A is used. 16B... May be provided on the upstream side. Alternatively, the guide tube may be eliminated and an injection tube may be provided at the end. Further, as shown in FIG. 2, the injection tubes 16 </ b> A, 16 </ b> B...
According to the form shown in FIG. 9, since the reaction length in the swirl flow field can be earned, the adhesion of the material in the flow path on the downstream side is drastically reduced.

The metal agglomerated particles obtained by the production method of the present invention can be produced as a battery material.
The electrical characteristics can be improved by using, for example, battery agglomerated particles, which are obtained by the present invention, having a small particle size, a uniform particle size, and an excellent spherical metal shape.

The apparatus according to the present invention can be formed of an appropriate material. In particular, the reactor 10 in which a flow path is processed into a plastic molded article can be used. An example of the block unit reactor is shown in FIG. The reactor can have an appropriate dimensional relationship depending on the processing material and liquid.
However, the diameter of the contact field that forms the swirl flow on the basis of the dimensions shown in FIG. 10 from the viewpoint of obtaining a small processing apparatus that exhibits a sufficient throughput and that exhibits uniform contact processability. The ratio of the main-flow inlet diameter D1 that forms the swirling flow with respect to D2 is preferably D2 / D1 = 2.5-10. When this ratio is small, the generation of the swirling flow is not sufficient, and when it is excessively large, the speed becomes slow and the swirling flow becomes unstable.
In order to generate a swirl flow stably, it is desirable that the ratio of the diameter D3 of the extraction portion to the diameter D2 of the contact field forming the swirl flow is D2 / D3 = 0.5-10. .
Further, in order to ensure the contact reaction time, it is desirable that the ratio of the length H in the flow path direction to the diameter D2 of the contact field forming the swirling flow is H / D2 = 1 to 10.

By the way, the present invention efficiently performs mass transfer and chemical reaction in a reaction field that is controlled by mass transfer rather than reaction, and can be used regardless of inorganic reaction or organic reaction.
It can also be used as a liquid-liquid mixing device such as application of this device in liquid-liquid extraction, water-oil emulsion, and the like.
In addition, it is an apparatus that can be used for processes other than liquid-liquid reactions such as gas-liquid reactions and reactions (coating) on the surface of solid particles.

  In order to obtain a swirl flow with less power, a liquid viscosity of 1000 cP or less, particularly 100 cP or less is desirable.

Next, examples and comparative examples will be shown to clarify the effects of the present invention.
Example 1
In the apparatus of the embodiment of FIGS. 1 to 4, the operating conditions are as follows: reactor inlet pressure 110 kPa, flow rate 30 L / min, temperature 45 ° C., total apparatus capacity 5 L, nickel sulfate 1.24 mol / L and cobalt sulfate 0.23 mol / An aqueous solution adjusted to L was poured into the reactor at 76 g / min and 25 wt% sodium hydroxide at 30 g / min, and obtained after 6 hr while adding 25 wt% aqueous ammonia to the reactor at 5 g / min. Samples were evaluated by SEM photographs and the like.
(Example 2)
The same procedure as in Example 1 was performed except that the reactor inlet pressure was changed to 50 kPa.
(Example 3)
As operating conditions, the reactor inlet pressure was 110 kPa, the flow rate was 7 L / min, the temperature was 45 ° C., the total volume of the apparatus was 1 L, ferrous sulfate was 0.55 mol / L, manganese sulfate was 0.09 mol / L, and zinc sulfate was 0.08 mol / The aqueous solution adjusted to L was injected into the reactor at 29 g / min and caustic soda at 8 g / min, and samples obtained after 3 hours were evaluated.
Example 4
The same procedure as in Example 3 was performed except that the reactor inlet pressure was changed to 50 kPa.
<Discussion>
(1) In any case of Example 1 and Example 2, the particle diameter was small and suitable agglomerated particles could be obtained.
(2) In the sample evaluation, the packing density of the agglomerated particles was used as an evaluation item, and 10 g of a sample dried at 24 hr and 105 ° C. was put into a 25 ml graduated cylinder, and this was placed on the vibration plate for 1 minute to be sufficiently uniform. It is a measure of the bulk of the time. At this time, the rotation speed of the vibration motor was 2500 rpm.
Packing density of Example 1: 1.32 g / ml, Packing density of Example 2: 1.2 g / ml, Packing density of Example 3: 0.7 g / ml, Packing density of Example 4: 0.55 g / ml ml.
From this result, it was found that the packing density of the aggregated particles can be clearly changed by the pressure in the reactor.
(3) When the change in the vorticity in the reactor was measured according to the pressure, the results shown in FIGS. 11 and 12 were obtained.

It can be applied to various uses in addition to the positive electrode active material for lithium ion batteries. Examples are listed as follows.
1) Emulsion fuel production 2) Small-diameter particle production Nanoparticle crystal growth, etc. 3) Diazo compound production 4) Catalytic reaction 5) Other reaction processes in microreactors a Gas-liquid interface reaction Fluorination reaction with fluorine gas Carbon monoxide Carbonylation reaction by gas b Liquid-liquid interface reaction Nitration reaction (organic phase / water phase)
Ester reduction Diazo coupling c Solid-liquid interface reaction Solid-supported catalyst reaction Air-liquid-solid interface reaction Hydrogenation reaction

DESCRIPTION OF SYMBOLS 10 ... Reactor, 10X ... Inlet, 10Y ... Outlet, 11, 14 ... Circulation path, 16A, 16B ... Injection pipe, 17 ... Guide pipe, 20 ... Reservoir, 40 ... Rotating cylinder, A, B, C ... Infusion solution.

Claims (11)

A reactor having one end and the other end; injection means for injecting the reaction liquid into the reactor; and extracting the contact treatment liquid from the other end of the reactor, and at least the extracted contact treatment liquid Circulating means for returning a part to the one end of the reactor,
The liquid flow in the reactor is swirled by returning the contact treatment liquid, and the swirl is configured to contact the reaction liquid injected by the injection means.
A continuous reaction apparatus comprising pressure increasing means for increasing the pressure in the reactor from normal pressure.   The continuous reaction apparatus according to claim 1, wherein the reaction liquid is injected at a position closer to the center than the inner surface of the reactor.   The contact field in the reactor between the returned contact treatment liquid and the injected reaction liquid is defined as a region on the center side from the inner surface of the swirling flow reactor generated in the reactor. The continuous reaction apparatus according to claim 1, wherein the reaction solution is brought into contact.   2. The continuous reaction apparatus according to claim 1, wherein the inner surface of the reactor is tapered from one end side toward the other end portion, and the contact treatment liquid inflow position is at one end portion in the longitudinal direction of the reactor.   The continuous reaction apparatus according to claim 1, further comprising a pressure adjusting means and a circulation pump in this order in a circulation path through which the contact treatment liquid extracted from the other end of the reactor is returned to the one end.   A circulation path through which the contact treatment liquid extracted from the other end of the reactor is returned to the one end has a pressure regulating valve, a circulation pump, and a pressure gauge in this order. The continuous reaction apparatus according to claim 1, wherein the pressure adjusting valve adjusts the pressure based on the pressure.   A pressure adjusting valve, a pressure reservoir for temporarily storing the contact treatment liquid, and a pressure in the pressure reservoir are provided in a circulation path through which the contact treatment liquid extracted from the other end is returned to the one end. A pressure gauge for instructing and a circulation pump are provided in this order, and a compressor or a pressure cylinder for pressurizing the inside thereof is connected to the pressure reservoir, and the compressor or the pressure cylinder is based on a pressure signal of the pressure reservoir by the pressure gauge. The continuous reaction apparatus according to claim 1, wherein the pressure is adjusted.   A pressure regulating valve, a pressure reservoir for temporarily storing the contact treatment liquid, a circulation pump, and a pressure gauge are arranged in this order on the circulation path through which the contact treatment liquid extracted from the other end is returned to the one end. A compressor or a pressurizing cylinder is connected to the pressure reservoir, and the contact treatment liquid is continuously or intermittently extracted from the circulation path based on the pressure of the pressure reservoir by the pressure gauge. The continuous reaction apparatus of Claim 1 which provided the pressure control system to perform.   The continuous reaction apparatus according to claim 1, wherein the reactors for providing the contact field are arranged in series.   The continuous reaction apparatus according to claim 1, wherein an injection direction with respect to the contact field of the reaction solution is directed from the one end side to the other end part. A reactor having one end and the other end; injection means for injecting the reaction liquid into the reactor; and extracting the contact treatment liquid from the other end of the reactor, and at least the extracted contact treatment liquid Circulating means for returning a part to the one end of the reactor,
Furthermore, it has a pressure raising means for raising the pressure in the reactor from the normal pressure,
The liquid flow in the reactor is swirled by returning the contact treatment liquid, the reaction liquid injected by the injection means is brought into contact with the swirl flow, the reaction is performed, and reaction crystallization of inorganic particles is performed. A continuous reaction crystallization method for inorganic particles.