JP2007038058A - Liquid treatment apparatus and liquid feeding method - Google Patents

Abstract

<P>PROBLEM TO BE SOLVED: To provide generation of air bubbles at the inside of a liquid at introduction of the liquid into a flow passage structure body in a liquid treatment apparatus having the flow passage structure body. <P>SOLUTION: The liquid treatment apparatus 1 is provided with a micro-reactor 2 formed with a fine flow passage reaching from an introduction port to a discharge port; a feeding pipe 31 and a discharge pipe 41 connected to the introduction port and the discharge port of the micro-reactor 2 respectively; a liquid feeding pump 32 for feeding chemicals to the micro-reactor 2 through the feeding pipe 31; and a pressure-reduction pump 43 connected to the discharge pipe 41. At introduction of the chemicals into the micro-reactor 2, A control part 12 drives/controls the liquid feed pump 32 and/or the pressure reduction pump 43 and a difference of a first pressure of the chemicals in the feeding pipe 31 and a second pressure of a gas in the discharge port is maintained to a pressure difference or lower at which the air bubbles are not generated at the inside of the chemicals. Thereby, generation of the air bubbles at the inside of the chemicals can be prevented in the liquid treatment apparatus 1. <P>COPYRIGHT: (C)2007,JPO&INPIT

Description

  The present invention relates to a liquid processing apparatus that processes a liquid by flowing a predetermined liquid through a flow path structure, and a technique for supplying the liquid into the flow path structure in the liquid processing apparatus.

  Conventionally, in a field such as a chemical synthesis reaction or a biochemical reaction, a micro flow channel has been used as a micro container for processing a small amount of sample fluid (for example, applying heat or reacting by irradiating light). A microreactor, which is a provided channel structure, is used. In a microreactor, it is known that it is easily realized to process a minute amount of raw material on the order of microliters under a certain condition, contamination of impurities is suppressed, and safety is ensured. A general microreactor is formed by superimposing another member on a substrate having a fine groove formed on the main surface.

  By the way, in the microreactor, the air dissolved in the chemical solution to be treated is deposited and adheres and stays as bubbles on the wall surface of the flow path, so that the chemical solution cannot be stably supplied into the microreactor. The reaction may vary. Normally, the flow rate of the chemical solution is slowed down in the microchannel of the microreactor, and the contact area with the bubble wall surface is larger than the area occupied by bubbles attached to the wall surface in the cross section perpendicular to the channel. It is not easy to peel off and push away. Accordingly, in Patent Document 1, a branch path is formed in which a degassing partition wall having a water impermeability and a gas permeability is provided at the branch point while branching from the micro flow path in the microreactor, and the pressure in the branch path is reduced. Thus, a technique for degassing the liquid in the fine channel has been disclosed.

Note that Patent Document 2 discloses a technique in which a plurality of fluids respectively supplied from a plurality of supply units in a microreactor are caused to flow into a common common part by suction from a separately provided suction unit. 3 discloses a technique for producing high-concentration ozone water by adjusting the pressure of ozone gas in the microreactor in the high-concentration ozone water production apparatus. Moreover, in patent document 4, when sending a liquid to a 1st flow path through the 3rd flow path branched from a 2nd flow path inside a microreactor, a 2nd flow path and a 1st flow path The air phase reaches the inlet of the third flow path by sending the liquid by pushing it out with air in the second flow path while maintaining the pressure difference with the flow path within a predetermined pressure range. In such a case, a technique for preventing air in the second flow path from entering the first flow path while stopping the inflow of the liquid into the first flow path is disclosed.
JP 2002-18271 A JP 2002-236131 A JP 2003-210956 A JP 2005-17057 A

  By the way, in the microreactor, when the state of the wall surface of the flow path of the chemical solution is rough or the flow path is branched, the flow of the chemical solution is introduced when the chemical solution is introduced into the microreactor by being pushed by a pump. Is disturbed and gas (for example, air) in the vicinity of the interface at the tip of the chemical solution is taken into the chemical solution. That is, in addition to the air dissolved in the chemical solution generated as bubbles, gas may be taken into the chemical solution as bubbles and the bubbles may stay in the fine flow path. It becomes difficult to stably supply the chemical solution into the microreactor for processing. In order to prevent the gas from being taken in as bubbles, it is conceivable to introduce the chemical solution into the microreactor at a low speed, but it takes a long time to introduce the chemical solution into the microreactor. Even when the technique of Patent Document 1 is used, it is not possible to prevent the gas from being taken into the chemical liquid as bubbles as described above when the chemical liquid is introduced into the microreactor. Furthermore, when the microreactor and the surrounding structure are complicated, such as when the chemical liquid is processed by irradiating light to the micro flow path of the microreactor, it is difficult to adopt the method of Patent Document 1. Therefore, a new method capable of appropriately supplying a chemical solution into the microreactor is required.

  The present invention has been made in view of the above problems, and an object of the present invention is to appropriately supply a liquid into a flow channel structure in a liquid processing apparatus having the flow channel structure.

  The invention according to claim 1 is a liquid processing apparatus that performs processing on the liquid by flowing a predetermined liquid through the flow channel structure, and a flow in which a fine flow path from the inlet to the outlet is formed. A path structure, a supply pipe connected to the introduction port, a liquid feeding mechanism for supplying a predetermined liquid to the flow path structure via the supply pipe, and a discharge pipe connected to the discharge port A pressure reducing mechanism connected to the discharge pipe, a first pressure gauge for acquiring a first pressure of fluid in the supply pipe, a second pressure gauge for acquiring a second pressure of fluid in the discharge port, and the flow A controller that controls a difference between the first pressure and the second pressure by drivingly controlling the liquid feeding mechanism and / or the pressure reducing mechanism when supplying the liquid into the path structure; .

  Invention of Claim 2 is the liquid processing apparatus of Claim 1, Comprising: The said control part is said 1st pressure and said 2nd at the time of the introduction of the liquid to the inside of the said flow-path structure. The difference from the pressure is maintained below the pressure difference at which bubbles are generated inside the liquid.

  Invention of Claim 3 is the liquid processing apparatus of Claim 2, Comprising: The said control part is a said 1st from completion of introduction of the liquid to the inside of the said flow-path structure until completion of introduction. The difference between the pressure and the second pressure is maintained below the pressure difference at which bubbles are generated inside the liquid.

  A fourth aspect of the present invention is the liquid processing apparatus according to any one of the first to third aspects, wherein a valve is provided in the supply pipe, and the first pressure gauge is configured such that a liquid is the valve. In the closed state in which the valve before passing is closed, the pressure of the gas on the liquid feeding mechanism side of the valve is acquired as the first pressure, and the control unit preliminarily acquires the first pressure gauge of the supply pipe. The liquid is introduced to a position between the liquid delivery mechanism and the liquid feeding mechanism, and the pressure reducing mechanism is driven in the closed state, whereby the second pressure is made lower than the first pressure, and then the valve Is opened to depressurize the liquid feeding mechanism side of the valve and activate the liquid feeding mechanism.

  The invention according to claim 5 is the liquid processing apparatus according to claim 4, wherein a difference between the first pressure and the second pressure immediately before the valve is opened from the closed state is 0. 9 atmospheres or less.

  A sixth aspect of the present invention is the liquid processing apparatus according to the fifth aspect, wherein the pressure reduction in the vicinity of the interface of the tip of the liquid in the supply pipe is completed within 2 seconds after the opening of the valve is started.

  A seventh aspect of the present invention is the liquid processing apparatus according to any one of the first to sixth aspects, further comprising a degassing module for degassing the liquid on the liquid feeding mechanism side of the first pressure gauge. .

  The invention according to claim 8 is the liquid processing apparatus according to any one of claims 1 to 7, wherein the liquid supply tank stores liquid before being supplied to the flow path structure by the liquid feeding mechanism. And a liquid temperature adjusting unit that lowers the temperature of the liquid flowing into the flow path structure at a time lower than the temperature of the liquid in the liquid supply tank when the liquid is introduced into the flow path structure. Is further provided.

  A ninth aspect of the present invention is the liquid processing apparatus according to any one of the first to eighth aspects, further comprising a flow rate adjusting unit that adjusts a flow rate of the liquid flowing into the flow path structure. .

  A tenth aspect of the present invention is the liquid processing apparatus according to any one of the first to ninth aspects, wherein the flow path structure is vibrated when the liquid is supplied into the flow path structure. A vibration imparting unit for imparting is further provided.

  An eleventh aspect of the invention is the liquid processing apparatus according to any one of the first to tenth aspects, further comprising a structure temperature adjusting unit that adjusts the temperature of the flow path structure.

  The invention according to claim 12 is the liquid processing apparatus according to any one of claims 1 to 11, further comprising a light irradiation unit that irradiates light to the flow channel structure, At least in part, the light from the light irradiation unit is guided to the internal microchannel.

  A thirteenth aspect of the present invention is the liquid processing apparatus according to any one of the first to twelfth aspects, wherein the decompression mechanism is a pump capable of sucking both gas and liquid.

  The invention according to claim 14 is the liquid processing apparatus according to any one of claims 1 to 12, wherein the liquid detection unit detects the outflow of the liquid from the flow path structure to the discharge pipe, and A liquid storage tank that stores the liquid discharged from the discharge pipe, and the discharge pipe branches from the detection position by the liquid detection unit on the liquid storage tank side and is connected to the pressure reducing mechanism A switching valve that switches between a path, a path from the discharge port to the pressure reducing mechanism, and a path from the discharge port to the liquid storage tank, and the control unit detects the outflow of liquid by the liquid detection unit. Immediately thereafter, the switching valve is controlled to guide the liquid to the liquid storage tank.

  A fifteenth aspect of the present invention is the liquid processing apparatus according to any one of the first to thirteenth aspects, wherein each of the flow path structure, the supply pipe, the discharge pipe, the first pressure gauge, and A plurality of processing units including the second pressure gauge; a plurality of supply pipes of the plurality of processing units are coupled and connected to the liquid feeding mechanism; and a plurality of discharge pipes of the plurality of processing units are coupled. Connected to the decompression mechanism.

  A sixteenth aspect of the present invention is the liquid processing apparatus according to any one of the first to thirteenth aspects, each of which includes the liquid feeding mechanism, the flow channel structure, the supply pipe, the discharge pipe, A plurality of processing units including a first pressure gauge and a second pressure gauge are provided, the plurality of processing units are connected in series, and the two processing units adjacent to each other are connected to the supply pipe of the downstream processing unit The liquid feeding mechanism thus performed operates as the pressure reducing mechanism connected to the discharge pipe of the upstream processing unit, and the pressure reducing mechanism is separately connected to the discharge pipe of the most downstream processing unit.

  The invention according to claim 17 is the liquid processing apparatus according to any one of claims 1 to 16, wherein the flow path structures are a plurality of flow path structures connected in series or in parallel. The temperatures of the plurality of flow path structures are individually adjusted.

  According to an eighteenth aspect of the present invention, there is provided a flow channel structure in which a fine flow channel extending from the inlet to the outlet is formed, a supply pipe connected to the inlet, and a predetermined liquid to the supply pipe. A liquid feeding mechanism that supplies the fluid to the flow path structure, a discharge pipe connected to the discharge port, a pressure reducing mechanism connected to the discharge pipe, and a first pressure of the fluid in the supply pipe. In a liquid processing apparatus comprising a first pressure gauge and a second pressure gauge that acquires a second pressure of the fluid at the discharge port, a liquid supply method for supplying a liquid into the flow path structure, The first pressure and the first pressure are controlled by driving and controlling the liquid feeding mechanism and / or the pressure-reducing mechanism substantially in parallel with the step of sending the liquid into the flow path structure and the step of sending the liquid. And a step of controlling the difference between the two pressures.

  According to the present invention, the liquid can be appropriately supplied into the flow channel structure by controlling the difference between the first pressure and the second pressure when supplying the liquid into the flow channel structure. .

  In the invention of claim 2, the liquid is maintained by maintaining the difference between the first pressure and the second pressure below the pressure difference at which bubbles are generated in the liquid when the liquid is introduced into the flow path structure. The difference between the pressure at the tip of the gas and the pressure of the gas in the vicinity of the interface between the tips can be made equal to or less than the pressure difference at which bubbles are generated in the liquid, so that bubbles can be prevented from being generated in the liquid.

  Further, in the invention of claim 4, when the liquid is introduced into the flow path structure by reducing the pressure of the gas downstream of the liquid tip immediately before the liquid is introduced into the flow path structure, It is possible to suppress the gas in the vicinity of the interface of the liquid tip from being taken in as bubbles in the liquid.

  In the invention of claim 7, it is possible to prevent the generation of bubbles in the liquid by reducing the amount of gas dissolved in the liquid. In the invention of claim 8, the solubility of the gas in the liquid By raising, it is possible to prevent bubbles from being generated in the liquid in the flow channel structure.

  In the invention of claim 10, when the liquid is supplied to the inside of the channel structure, the channel structure should be generated by generating bubbles in the liquid or by taking the gas into the liquid as bubbles. Even when bubbles remain attached to the wall surface of the fine flow path of the body, the bubbles can be peeled off and removed by applying vibration to the flow path structure.

  In the inventions of claims 11 and 17, the liquid processing apparatus can perform processing depending on the temperature of the flow path structure, and in the invention of claim 12, the liquid processing apparatus performs processing involving light irradiation. be able to.

  In the invention of claim 13, the configuration of the liquid processing apparatus can be simplified, and in the invention of claim 14, the liquid can be prevented from flowing into the pressure reducing mechanism.

  According to the fifteenth aspect of the invention, it is possible to increase the amount of liquid processed in the liquid processing apparatus. The chemical solution can be easily supplied to the plurality of flow channel structures.

  FIG. 1 is a diagram showing a configuration of a liquid processing apparatus 1 according to the first embodiment of the present invention. The liquid processing apparatus 1 processes a chemical solution by flowing a predetermined chemical solution through a flow channel structure in which a micro flow channel is formed.

  The liquid processing apparatus 1 in FIG. 1 includes a main body 11 and a control unit 12 connected to the main body 11. The main body 11 includes a microreactor device (hereinafter simply referred to as “microreactor”) 2 that is a flow channel structure in which a fine flow channel from an inlet to an outlet is formed. A valve is provided at the inlet of the microreactor 2. A supply pipe 31 having 311 is connected. A liquid feed pump 32 is connected to the side of the supply pipe 31 opposite to the microreactor 2, and the chemical liquid stored in the chemical liquid supply tank 33 by the liquid feed pump 32 is supplied into the microreactor 2 through the supply pipe 31. . Further, a discharge pipe 41 is connected to the discharge port of the microreactor 2, and a gas-liquid separation unit 42 capable of separating the gas and liquid flowing out from the discharge pipe 41 is provided on the opposite side of the discharge pipe 41 from the microreactor 2. The gas-liquid separator 42 has a product storage tank 421 that forms a closed space, and an exhaust pipe 431 connected to the decompression pump 43 is provided above the product storage tank 421. A branch passage 432 that is opened to the atmosphere is provided in the exhaust pipe 431 via a switching valve 433. The switching valve 433 reduces the pressure in the product storage tank 421 by the decompression pump 43 and the product storage tank 421 from the branch passage 432. The inside of the atmosphere can be switched. In a state where the pressure reducing pump 43 and the product storage tank 421 communicate with each other by the switching valve 433, the pressure reducing pump 43 is connected to the discharge pipe 41 through the exhaust pipe 431 and the product storage tank 421.

  In the supply pipe 31, a first pressure gauge 51 that acquires the pressure of the fluid in the supply pipe 31 (hereinafter referred to as “first pressure”) is provided on the upstream side of the valve 311 (that is, the liquid feed pump 32 side). . The discharge pipe 41 is provided with a second pressure gauge 52 that acquires the pressure of the fluid in the discharge pipe 41 (hereinafter referred to as “second pressure”). A flow meter (for example, a differential pressure flow meter, a Kalman flow meter, or an ultrasonic flow meter) 411 that acquires the flow rate of the fluid in the discharge pipe 41 is attached to the liquid separation unit 42 side. The first and second pressures acquired by the first and second pressure gauges 51 and 52 and the flow rate acquired by the flow meter 411 are output to the control unit 12. Each of the first and second pressure gauges 51 and 52 can acquire gas and liquid pressures.

  As shown in FIG. 1, in the vicinity of the microreactor 2, a vibration applying unit 61 that applies ultrasonic vibration to the microreactor 2, a reactor temperature adjusting unit 62 that adjusts the temperature of the microreactor 2, and a power supply unit 631 are connected. In addition, a light irradiation unit 63 that irradiates light (for example, ultraviolet rays) of a predetermined wavelength toward the microreactor 2 is provided. The light irradiation unit 63 is provided with an illuminance meter 632, and from the power supply unit 631 to the light irradiation unit 63 according to the output of the illuminance meter 632 so that the intensity of light from the light irradiation unit 63 is constant. The supplied power (actually the inverter output) is adjusted. In addition, what has a motor is provided as the vibration provision part 61, and the vibration (or mechanical vibration using a fluid) which arises by rotation of a motor may be provided to the microreactor 2. FIG. In this case, the vibration imparting unit 61 imparts vibration to the microreactor 2 substantially using magnetism.

  FIG. 2 is a plan view showing the microreactor 2, and FIG. 3 is a longitudinal sectional view showing the configuration in the vicinity of the microreactor 2. As shown in FIG. 2, the introduction port 21 and the discharge port 22 described above are formed in the microreactor 2, and the introduction port 21 and the discharge port 22 have a substantially triangular cross section parallel to the XY plane in FIG. 2 are respectively connected to the introduction part 211 and the discharge part 221 (in FIG. 2, the flow path in the microreactor 2 is illustrated by broken lines). A plurality of microchannels 23 extending in the X direction are formed between the introduction part 211 and the discharge part 221. The cross section of the fine channel 23 is, for example, a rectangle having a width and a height of 1 mm. In FIG. 3, only five fine flow paths 23 are shown, but actually, a large number of fine flow paths 23 are formed as shown in FIG.

  As shown in FIG. 3, the microreactor 2 has a plate-shaped reactor main body 24 formed of metal, and each of the reactor main body 24 on the (+ Z) side surface (upper surface) in FIG. A plurality of grooves 241 that form the bottom and side surfaces of the microchannel 23 and extend in the X direction are formed. A diffusion plate 25 that diffuses and transmits light is attached to the upper surface of the reactor main body 24, and an O-ring 26 is provided between the diffusion plate 25 and the reactor main body 24 at the outer edge of the diffusion plate 25. The diffusion plate 25 is made of Teflon (registered trademark) resin, and the opening on the (+ Z) side of the groove 241 is closed by the diffusion plate 25 to form the fine flow path 23. In the microreactor 2, a glass plate 64 is provided on the opposite side of the diffusion plate 25 from the reactor main body 24, and light emitted from the light irradiation unit 63 passes through the glass plate 64 and the diffusion plate 25 to the internal fine flow path 23. Evenly guided. In the present embodiment, light is irradiated to the entire microchannel 23, but depending on the design of the microreactor 2 and the processing with respect to the chemical solution, the light from the light irradiation unit 63 may enter the microchannel 23 only in part of the microreactor 2. You may be guided. That is, in the liquid processing apparatus 1, the light from the light irradiation unit 63 is guided to the internal microchannel 23 in at least a part of the microreactor 2.

  Further, a heat exchanger 621 of the reactor temperature adjustment unit 62 is provided in contact with the lower surface of the microreactor 2 on the (−Z) side of the microreactor 2, and the glass plate 64, the microreactor 2, and the heat exchanger 621 are fixed by the fixing unit 65. It is sandwiched in the Z direction. The heat exchanger 621 is formed with a heat medium flow path whose temperature is controlled externally. In the microreactor 2, for example, when the reaction heat of the chemical solution is generated in the fine flow path 23, the generated heat is transferred to the metal. It is absorbed by the heat exchanger 621 through the reactor body 24 formed in the above manner. The reactor temperature control unit 62 has a temperature sensor and a heater or Peltier element that is in contact with the microreactor 2 in addition to the one having the heat exchanger 621, or a microwave or laser. The microreactor 2 may be heated. In addition, the microreactor 2 is immersed in a container in which a liquid heat medium is held, and the heat medium is circulated while temperature-controlling outside, or the heat medium is directly temperature-controlled in the container by a heater or a Peltier element. Thus, the temperature of the microreactor 2 may be adjusted. Further, the microreactor may be formed of various materials other than metal, regardless of organic materials or inorganic materials such as glass, ceramic, silicon, resin, and the like.

  In the microreactor 2 of FIG. 3, the diffusion plate 25 is elastically deformed to achieve good adhesion between the diffusion plate 25 and the reactor main body 24, and the liquid flowing in one microchannel 23 is transferred to another microchannel 23 or microreactor. 2 is prevented from leaking outside. Further, in the microreactor 2, the O-ring 26 is also used, so that the liquid is prevented from leaking to the outside even if the liquid having a high viscosity is caused to flow at a high pressure through the fine flow path 23.

  In the liquid processing apparatus 1 of FIG. 1, each configuration of the main body 11 (liquid feeding pump 32, first pressure gauge 51, valve 311, vibration applying section 61, reactor temperature adjustment section 62, light irradiation section 63, second pressure gauge 52. The flow meter 411, the switching valve 433, and the pressure reducing pump 43) are connected to the control unit 12, and under the control of the control unit 12, the chemical solution is flowed into the microreactor 2 and predetermined processing is performed on the chemical solution.

  Next, the operation when the liquid processing apparatus 1 flows a predetermined chemical solution into the microreactor 2 to process the chemical solution will be described with reference to FIG. Actually, an experiment as a preliminary preparation is performed in order to acquire a predetermined condition relating to the processing on the chemical liquid. Details of the preliminary preparation will be described in detail after the description of the processing on the chemical liquid in the liquid processing apparatus 1. . In the following description, the flow path of the chemical solution from the supply pipe 31 to the discharge pipe 41 via the microreactor 2 is generically referred to as a chemical solution path.

  In the liquid processing apparatus 1, for example, the chemical liquid is stored in the chemical liquid supply tank 33 under atmospheric pressure, and the liquid feed pump 32 is disposed below the liquid level of the chemical liquid supply tank 33 with respect to the vertical direction. Also, a valve 311 is disposed on the upper side, and the valve 311 is opened and the switching valve 433 is opened to the branch path 432 side to bring the gas (air) in the chemical path to atmospheric pressure so that the tip of the chemical ( That is, the most downstream portion of the chemical solution is introduced in advance to a position between the first pressure gauge 51 and the liquid feed pump 32. In addition, a check valve is provided in the liquid feeding pump, and the tip of the chemical liquid may be introduced to a position between the first pressure gauge 51 and the liquid feeding pump 32 by driving the liquid feeding pump for a short time. .

  Subsequently, the valve 311 is closed, and the switching valve 433 is switched to the decompression pump 43 side. In this state, the control unit 12 starts driving the decompression pump 43 that is the decompression mechanism. Thus, in the closed state in which the valve 311 is closed, the downstream side of the valve 311 in the chemical solution path (a part of the supply pipe 31, the inside of the microreactor 2, the discharge pipe 41, the inside of the product storage tank 421, and the exhaust pipe) 431) is depressurized (step S11).

  In the first pressure gauge 51 and the second pressure gauge 52, the first pressure and the second pressure are repeatedly acquired every minute time, and the liquid is fed more than the valve 311 in the supply pipe 31 by driving the pressure reducing pump 43. The first pressure of the gas on the pump 32 side is lower than the second pressure of the gas in the discharge pipe 41. Further, the pressure on the microreactor 2 side of the valve 311 in the supply pipe 31 is also substantially the same as the second pressure in the discharge pipe 41 (more precisely, due to the pressure loss in the micro flow path 23 of the microreactor 2, the supply pipe 31 The pressure on the microreactor 2 side of the inner valve 311 is slightly larger than the second pressure in the discharge pipe 41.) In the liquid processing apparatus 1, the rotational speed of the decompression pump 43 is controlled by the control unit 12, so that the decompression speed (change amount of pressure per unit time) and the ultimate pressure due to decompression can be controlled within a certain range. However, the pressure reduction speed and the ultimate pressure may be controlled by separately providing a valve (so-called pressure regulating valve) capable of adjusting the pressure in the discharge pipe 41 and controlling the pressure regulating valve.

  The controller 12 obtains a difference between the first pressure and the second pressure every minute time (step S12), and compares this difference with a set pressure difference described later (step S13). When the difference between the first pressure and the second pressure becomes equal to or larger than the set pressure difference (step S13), the valve 311 is opened by the control unit 12, and the feed pump 32 side (upstream side) of the valve 311 in the supply pipe 31 is opened. ) Is depressurized (step S14). At this time, after the opening of the valve 311 is started, the pressure reduction in the vicinity of the interface of the distal end portion of the chemical solution in the supply pipe 31 (that is, the interface on the valve 311 side of the chemical solution) in the supply pipe 31 is completed after the opening of the valve 311 is completed. The opening operation of the valve 311 (or the degree of opening of the valve 311) is controlled so that the gas pressures upstream and downstream of the valve 311 in the supply pipe 31 become substantially the same in the set pressure reduction time. In the liquid processing apparatus 1, the first pressure is slightly higher than the second pressure immediately after the pressure reduction in the vicinity of the interface at the tip of the chemical solution is completed. The set pressure difference and the set pressure reduction time will be described in detail after explanation of the overall operation in the liquid processing apparatus 1.

  When the pressure reduction in the vicinity of the interface at the front end of the chemical solution in the supply pipe 31 is completed (or almost in parallel with the pressure reduction), the liquid delivery pump 32 that is a liquid delivery mechanism is activated in the liquid processing apparatus 1 to deliver the chemical solution. Is started (step S15). As a result, the tip of the chemical solution moves through the supply pipe 31 toward the microreactor 2, passes through the position of the valve 311, and is then introduced into the microreactor 2 through the inlet 21. When the tip of the chemical solution passes through the position of the first pressure gauge 51 during the movement of the tip of the chemical solution in the supply pipe 31, the pressure of the chemical solution in the supply pipe 31 is set as the first pressure by the first pressure gauge 51. Will be acquired.

  In the liquid processing apparatus 1, when the feeding of the chemical solution by the liquid feeding pump 32 is started, the control of the difference between the first pressure and the second pressure by the control unit 12 is started (step S16). Specifically, the control unit 12 controls the drive of the liquid feed pump 32 and the decompression pump 43 based on the first pressure and the second pressure that are sequentially acquired, so that the pressure of the chemical liquid in the supply pipe 31 is the first. The difference between the pressure and the second pressure, which is the pressure of the gas in the discharge pipe 41, is controlled within a range that is greater than or equal to the preset pressure difference and less than or equal to a predetermined upper limit pressure difference that is greater than the preset pressure difference. Here, the upper limit pressure difference is a bubble having a diameter larger than a predetermined value among bubbles formed by precipitation of gas dissolved in the chemical solution due to pressure fluctuation in the chemical solution (hereinafter simply referred to as “ It is calculated | required by the prior preparation mentioned later as a pressure difference which produces | generates "precipitation bubble". The upper limit pressure difference will be described in detail after the description of the overall operation in the liquid processing apparatus 1 as with the set pressure difference and the set pressure reduction time.

  As described above, immediately before the valve 311 is opened, the difference between the first pressure of the gas upstream of the valve 311 of the supply pipe 31 and the second pressure of the discharge pipe 41 is substantially the same as the set pressure difference ( Or a value slightly higher than the set pressure difference) so that the difference between the first pressure and the second pressure does not exceed the upper limit pressure difference. It can be said that the control of the difference between the first pressure and the second pressure starts immediately before the introduction of the chemical solution into the microreactor 2.

  Inside the microreactor 2, the tip of the chemical solution flows into the inside of the fine channel 23 through the inlet 21 and the inlet 211, passes through the microchannel 23, and then passes through the outlet 221 and the outlet 22. Then, it is led to the discharge pipe 41 and the introduction of the chemical solution into the microreactor 2 is completed. Here, in the fine flow path 23 inside the microreactor 2, pressure loss occurs with the chemical solution being introduced and the gas downstream of the tip portion of the chemical solution, so that the pressure of the chemical solution at the tip portion and the interface between the tip portion of the chemical solution The difference between the pressure of the gas nearby is the first pressure that is the pressure of the chemical in the supply pipe 31 (substantially, the pressure of the chemical in the inlet 21) and the second pressure that is the pressure of the gas in the outlet 22. It becomes smaller than the difference. In other words, when the chemical solution is introduced into the microreactor 2, the difference between the pressure of the chemical solution at the tip portion and the pressure of the gas near the interface of the tip portion of the chemical solution is smaller than the upper limit pressure difference. As a result, the difference between the pressure of the chemical solution at the tip and the pressure of the gas near the interface of the tip of the chemical is larger than the upper limit pressure difference, thereby preventing the generation of precipitated bubbles inside the chemical.

  Further, when the tip of the chemical solution from the supply pipe 31 to the discharge pipe 41 is moved, it is affected by the state of the wall surface of the chemical solution flow path (for example, when the inner surface of the supply pipe 31 or the fine flow path 23 is rough). ) In the vicinity of the inlet 21 or in the vicinity of the inlet from the inlet 211 to the microchannel 23, the flow at the tip of the chemical is disturbed, so that the gas near the interface of the tip is taken into the chemical as bubbles. Even if this happens, the gas pressure (atmospheric pressure) in the vicinity of the interface at the tip of the chemical solution is reduced, so that the gas uptake in the chemical solution is suppressed compared to when the pressure reduction is not performed.

  In the liquid processing apparatus 1, the supply of the chemical solution to the microreactor 2 is continued by the liquid feed pump 32 even after the introduction of the chemical solution to the microreactor 2 is completed. And when the front-end | tip part of a chemical | medical solution reaches | attains the flowmeter 411, the control part 12 will switch the switching valve 433 to the branch path 432 side, and the pressure reduction pump 43 will also stop while making the inside of the product storage tank 421 atmospheric pressure. The tip of the chemical liquid is further moved by the operation of the liquid feed pump 32 and reaches the product storage tank 421, and the chemical liquid is stored in the product storage tank 421. In the following description, the continuous supply of the chemical solution to the microreactor 2 after the introduction of the chemical solution is referred to as continuous supply.

  When the chemical solution is continuously supplied to the microreactor 2, processing involving light irradiation by the light irradiation unit 63 on the chemical solution and processing depending on the temperature of the microreactor 2 by the reactor temperature adjustment unit 62 are performed in the microreactor 2 ( In step S17), the chemical solution (product) having undergone these processes is stored in the product storage tank 421. The processing for the chemical solution in the microreactor 2 may also be performed when the chemical solution is introduced into the microreactor 2.

  In the microreactor 2, a certain amount of light is imparted to the chemical solution by the light irradiation unit 63, thereby suppressing generation of unreacted materials due to insufficient light amount and by-products due to excessive light amount in processing involving light irradiation. Moreover, in the microreactor 2, since the reaction of the chemical solution under a constant temperature environment is realized by the reactor temperature control unit 62, generation of the by-product due to temperature fluctuation during the reaction is suppressed and generated. The purity of the product can be improved. 3 is formed of a Teflon (registered trademark) resin exhibiting good lubricity, and thus a frictional force generated between the chemical solution and the side surface of the fine channel 23 on the diffusion plate 25 side. The pressure loss of the chemical solution due to the above is reduced, and the chemical solution can be smoothly flowed into the fine flow path 23 without using a high-performance liquid feed pump or increasing the pressure of the chemical solution.

  In the liquid processing apparatus 1, the chemical liquid pressure in the supply pipe 31 (substantially, the chemical liquid pressure at the inlet 21) is controlled by driving the liquid feed pump 32 even during continuous supply of the chemical liquid to the microreactor 2. Is controlled so that the difference between the first pressure acquired as the pressure and the second pressure acquired as the pressure of the chemical solution at the discharge port 22 does not exceed the upper limit pressure difference. It is possible to prevent the generation of precipitated bubbles inside the chemical liquid due to a decrease in pressure exceeding.

  In the present embodiment, the decompression pump 43 is stopped immediately after the introduction of the chemical solution, but the decompression pump 43 is continuously driven even during the continuous supply of the chemical solution, and the liquid feed pump 32 and the decompression pump 43 are driven and controlled. Thus, the difference between the first pressure and the second pressure may be controlled. In this case, the liquid feed pump 32 may be temporarily stopped. That is, in the liquid processing apparatus 1, the control unit 12 controls the drive of the liquid feeding pump 32 and / or the decompression pump 43 to control the difference between the first pressure and the second pressure. In the liquid processing apparatus 1, even if the microreactor 2 has a very long fine flow path 23, the liquid supply pump 32 excessively supplies the chemical solution by driving the decompression pump 43 during the continuous supply of the chemical solution. The chemical solution can be smoothly and continuously supplied into the microreactor 2 without increasing the pressure.

  Further, the control unit 12 monitors the state of the flow path of the microreactor 2 (for example, whether the fine flow path 23 is blocked) by checking the difference between the first pressure and the second pressure. In addition, by providing a flow meter on the upstream side of the microreactor 2, it is also possible to use the flow meter and the downstream flow meter 411 for monitoring, for example, leakage of a chemical solution in the microreactor 2.

  Furthermore, in the liquid processing apparatus 1, in the unlikely event that the chemical solution is introduced into the microreactor 2 from when the chemical solution starts to be discharged from the microreactor 2 to the discharge pipe 41, and then continuously supplied, Is taken in as bubbles in the chemical solution, or when bubbles are deposited in the chemical solution and remain attached to the wall surface of the microchannel 23 in the microreactor 2, the microreactor is applied by the vibration applying unit 61. By constantly applying ultrasonic vibration to 2, the bubbles can be peeled off to remove (purge) the chemical. As a result, the chemical solution can be flowed at a substantially constant flow rate in each fine channel 23 to perform uniform processing on the chemical solution.

  In this manner, when the chemical treatment is performed in the liquid processing apparatus 1 and a necessary amount of product is stored in the product storage tank 421, the first pressure and the second pressure by the control unit 12 are reduced. While the difference control is finished (step S18), the sending of the chemical solution by the liquid feed pump 32 is also stopped (step S19), and the processing in the liquid processing apparatus 1 is finished.

  Next, the upper limit pressure difference, the set pressure difference, and the set pressure reduction time that are determined in advance by a predetermined experiment that is a preliminary preparation will be described. FIG. 5 is a diagram illustrating a configuration of the experimental apparatus 10 prepared when determining the upper limit pressure difference, the set pressure difference, and the set pressure reduction time.

  In the experimental apparatus 10, similarly to the liquid processing apparatus 1, the microreactor 2 and the liquid feed pump 32 are connected to the upstream side of the microreactor 2 by a supply pipe 31 having a valve 311. Connected to. A discharge pipe 41 is connected to the downstream side of the microreactor 2, and a syringe 71 having a cylinder and a piston is detachably connected to the opposite side of the discharge pipe 41 from the microreactor 2. Further, a second pressure gauge 52 is provided in the discharge pipe 41. Thus, the experimental apparatus 10 has a simplified configuration of the liquid processing apparatus 1.

  When the experimental apparatus 10 shown in FIG. 5 is prepared, first, the valve 311 is opened, and the syringe 71 is removed from the discharge pipe 41, and then the chemical solution (however, a predetermined gas ( Saturation) An alternative liquid whose solubility is equivalent to that of the chemical solution may be used, and water at 25 ° C. is used here.) Is introduced, and the introduction part 211 (see FIG. 2) of the microreactor 2 is substantially It is filled. At this time, the tip of the chemical solution is set to a position slightly entering the fine flow path 23, and the second pressure acquired by the second pressure gauge 52 is atmospheric pressure (here, 1 atm (atm)). . Then, the syringe 71 is attached to the tip of the discharge pipe 41, and the gas on the downstream side of the drug solution (that is, a part inside the microreactor 2 and the discharge pipe 41) is decompressed using the syringe 71. Thereby, in the process of step S14 of FIG. 5 in the liquid processing apparatus 1, a state approximately equivalent to the state in which the valve 311 is opened and the vicinity of the interface at the tip of the chemical solution in the supply pipe 31 is decompressed is in the microreactor 2. Realized.

  In this experiment for determining the upper limit pressure difference, the set pressure difference, and the set pressure reduction time, the ultimate pressure of the gas after the pressure reduction by the syringe 71 is changed to a plurality of target pressures, and until the target pressure is reached after the start of pressure reduction. The time (hereinafter referred to as “arrival time”) is also changed in several ways. Here, the target atmospheric pressure is set to 0.5, 0.2, 0.1, 0.05 atm, and the arrival time for each target atmospheric pressure is set to 1, 2, 4 seconds (i.e., 1, 1, The piston is pulled to reach each target pressure in 2 or 4 seconds.) Then, when the pressure is reduced by the syringe 71, the inside of the introducing portion 211 is observed to measure the size (diameter) of bubbles generated inside the drug solution. In the microreactor 2, the inside of the introduction part 211 can be observed through the diffusion plate 25.

  FIG. 6 is a diagram showing the relationship between the arrival time with respect to each target atmospheric pressure and the size (diameter) of the bubble to be measured. In FIG. 6, a target pressure of 0.5 atm is indicated by diamonds, a target pressure of 0.2 atm is square, a target pressure of 0.1 atm is indicated by triangles, and a target pressure of 0.05 atm is indicated by circles. . From FIG. 6, it can be seen that the smaller the target atmospheric pressure, the larger the diameter of bubbles generated inside the chemical solution. In other words, the larger the pressure difference before and after decompression, the larger the diameter of the generated bubbles. Also, when viewed at the same target atmospheric pressure, the bubble diameter becomes smaller as the arrival time is shorter.

  By the way, the width and height of the fine flow path 23 of the general microreactor 2 are both about 1 mm, and if bubbles with a diameter larger than 1 mm are generated in the introduction part 211, the fine flow paths 23 are generated by the bubbles. There is a possibility that the inlet portion 211 side of the liquid will be blocked (the same applies to the case where bubbles are generated in the fine flow path 23). Therefore, it is important that the diameter of bubbles generated inside the chemical solution is 1 mm or less. In FIG. 6, when the target pressure is 0.5 atm, the bubble diameter is 1 mm or less when the arrival time is 1, 2, or 4 seconds, and when the target pressure is 0.2 atm, the arrival time is 3 seconds. Hereinafter, when the target pressure is 0.1 atm, the bubble diameter is 1 mm or less if the arrival time is 2 seconds or less. That is, as long as the target pressure after depressurization from the state of 1 atm is 0.1 atm or more and the time to reach the target pressure is 2 seconds or less, the diameter of the generated bubbles may be 1 mm or less. It becomes possible. When the pressure difference is 0.5 atm, the diameter of the generated bubbles is 0.3 mm or less even when the arrival time is 4 seconds.

  In the liquid processing apparatus 1 of FIG. 1, when the pressure on the downstream side of the valve 311 is reduced in the closed state where the valve 311 is closed and then the pressure on the upstream side of the valve 311 is reduced by opening the valve 311, it is usually in a short time. Therefore, when the first pressure of the gas upstream of the valve 311 is 1 atm, the second pressure immediately before the valve 311 is opened from the closed state of the valve 311 is 0.1 atm. That is, by setting the difference between the first pressure and the second pressure to 0.9 atm or less, the pressure of the gas in the vicinity of the interface at the front end of the chemical solution is surely reduced to 0. It is realized that the diameter of the bubbles generated in the chemical solution in the supply pipe 31 is 1 mm or less when the pressure is 1 atm or more. On the other hand, when a bubble with a small diameter adheres to the wall surface of the microchannel, the contact area with the wall surface of the bubble is generally larger than the area occupied by the bubble in the cross section perpendicular to the channel. Depending on the design, it may be difficult to peel off and remove from the wall surface, and there may be variations in the flow rate of the chemical solution between the plurality of fine channels due to the influence of attached bubbles. In FIG. 6, when the target atmospheric pressure is 0.1 atm or more and the arrival time is less than 1 second, it is assumed that the size of the generated bubbles is very small. Therefore, in the liquid processing apparatus 1 of FIG. In order to prevent the generation of bubbles and make the flow rate constant in the plurality of fine channels 23, the time from the start of opening the valve 311 to the completion of the pressure reduction near the interface at the tip of the chemical solution is 1 second or more It is preferable that However, even in this case, from the viewpoint of setting the difference between the first pressure and the second pressure immediately before the valve 311 is opened from the closed state to 0.9 atm or less and the diameter of the generated bubbles to 1 mm or less, the valve 311 It is important that the time from the start of opening until the decompression of the vicinity of the interface of the chemical solution in the supply pipe 31 is completed is within 2 seconds.

  By the way, as mentioned above, it is considered that the lower the gas pressure in the vicinity of the interface of the tip of the chemical solution, the better, from the viewpoint of suppressing the gas from being taken in as bubbles in the chemical solution. In addition, the bubbles that are actually captured as the precipitated bubbles have a diameter larger than an arbitrary value (however, the value is equal to or less than the width and height of the microchannel 23 of the microreactor 2). Therefore, based on the above experimental results, the upper limit for opening the valve 311 so that the diameter of the generated bubbles is not larger than the size that can be regarded as the precipitated bubbles and the generation of bubbles having an extremely small diameter is prevented. And a set pressure reduction time are determined. Actually, a value that is somewhat smaller than this pressure difference is set so that the difference between the first pressure and the second pressure does not exceed the upper limit pressure difference even if a slight time delay occurs in the opening operation of the valve 311. Determined as pressure difference.

  In this experiment, when the chemical solution is introduced into the microreactor 2 in the liquid processing apparatus 1 of FIG. 1, a gas pressure difference in the vicinity of the interface at the tip of the chemical solution before and after the opening of the valve 311 and the chemical solution are generated. Although the relationship with the bubble size is substantially acquired, the pressure at the tip of the chemical and the pressure of the gas near the interface at the tip of the chemical at the time of introduction and continuous supply of the chemical into the microreactor 2 Similarly, the relationship between the difference and the size of bubbles generated in the chemical solution can be considered. Therefore, when the chemical solution is introduced into the microreactor 2 in the liquid processing apparatus 1 of FIG. 1, the chemical solution at the tip is maintained by maintaining the difference between the first pressure of the chemical solution and the second pressure of the gas below the upper limit pressure difference. The difference between the pressure of the gas and the pressure of the gas in the vicinity of the interface at the tip is equal to or less than the pressure difference at which the precipitation bubbles are generated, so that the formation of the precipitation bubbles at the tip of the chemical can be prevented. Even during continuous supply, by maintaining the difference between the first pressure of the chemical solution and the second pressure of the chemical solution below the upper limit pressure difference, it is possible to prevent the generation of precipitated bubbles caused by fluctuations in the pressure of the chemical solution it can. The experimental results shown in FIG. 6 are for water. However, when a chemical solution having a relatively high viscosity is used, the size of generated bubbles is generally small. Further, if the set pressure difference, the set pressure reduction time, and the upper limit pressure difference are substantially obtained, the above experiment may be performed by another simple method under the same conditions.

  As described above, in the liquid processing apparatus 1 of FIG. 1, immediately before the chemical solution is introduced into the microreactor 2, the chemical solution is driven by driving the decompression pump 43 in a state where the valve 311 before the chemical solution passes is closed. The gas on the downstream side of the valve 311 on the path is decompressed, and the pressure on the downstream side of the valve 311 on the chemical liquid path is made lower than the first pressure on the upstream side of the valve 311. Thereby, compared with the case where such pressure reduction is not performed, it is possible to prevent the gas in the vicinity of the interface at the tip of the chemical solution from being taken into the chemical solution as bubbles when the chemical solution is introduced into the microreactor 2. Further, the liquid feed pump 32 and / or the decompression pump 43 are driven and controlled immediately before the introduction of the chemical liquid into the microreactor 2 until the introduction is completed and during the continuous supply of the chemical liquid, and the first pressure, the second pressure, By maintaining the difference between the pressure difference below the upper limit pressure difference, it is possible to prevent the generation of precipitated bubbles inside the chemical solution. As described above, in the liquid processing apparatus 1, when the chemical liquid is supplied into the microreactor 2 (that is, immediately before the chemical liquid is introduced into the microreactor 2, during the introduction, and during the continuous supply), the first pressure and the second pressure Is controlled, the chemical solution is appropriately supplied into the microreactor 2 to stably perform the treatment on the chemical solution.

  Here, it is conceivable to apply the technique of the above-described Patent Document 1 to provide a degassing partition wall so as to face the entire fine flow path in the microreactor, and to remove bubbles in the fine flow path. Since there is a certain limit to the pressure resistance of the degassing partition wall, it is difficult to supply the chemical solution into the microreactor when processing a highly viscous chemical solution. On the other hand, in the liquid processing apparatus 1, since the generation of bubbles and precipitated bubbles due to gas intake is suppressed by controlling the difference between the first pressure and the second pressure, a high-viscosity chemical solution is applied to the microreactor 2 at a certain high pressure. Can be supplied within. Further, in the liquid processing apparatus 1, it is possible to introduce the chemical into the microreactor 2 in a short time (to make the microreactor 2 liquid-tight) by increasing the flow rate of the chemical at the time of introduction into the microreactor 2.

  In the liquid processing apparatus 1, a chemical liquid process depending on the temperature of the microreactor 2 is performed by the reactor temperature adjustment unit 62, and a chemical liquid process involving light irradiation is realized by the light irradiation unit 63. Here, suppose that FIG. As shown in A, when a relatively deep groove portion 241a is formed in the reactor main body 24 and the groove portion 241a is closed by a general glass plate 25a, a region where the light from the light irradiation portion 63 is not irradiated. (A region to which cross-hatching is added in FIG. 7A) exists, and it becomes impossible to uniformly perform the process related to the light irradiation on the chemical solution flowing through the fine channel 23 (inside the groove portion 241a). . On the other hand, in the liquid processing apparatus 1, FIG. As shown in B, the light from the light irradiation unit 63 is diffused by the diffusion plate 25 and irradiated to the fine flow path 23 (inside the groove 241a), so that the microreactor 2 can irradiate the chemical liquid with light. Such processing can be performed uniformly.

  FIG. 8 is a view showing a main body 11a of a liquid processing apparatus according to another example. In the discharge pipe 41 of the liquid processing apparatus of FIG. 8, the end portion on the opposite side to the microreactor 2 is connected to the product storage tank 44 and on the downstream side of the flow meter 411 (on the opposite side to the microreactor 2). A branch path 412 that branches and is connected to the decompression pump 43 is provided. A switching valve 413 is attached to a branch point of the discharge pipe 41, and a path from the discharge port of the microreactor 2 to the decompression pump 43 and a route from the discharge port to the product storage tank 44 are switched by the switch valve 413. Other configurations are the same as those of the liquid processing apparatus 1 of FIG. However, in the liquid processing apparatus of FIG. 8 (and the liquid processing apparatuses of FIGS. 9 to 11 and FIGS. 14 to 17 described later), the configuration relating to the processing in the microreactor 2 (vibration applying unit 61, reactor temperature adjusting unit 62 and The illustration of the light irradiation unit 63) is omitted as appropriate.

  In the processing in the liquid processing apparatus of FIG. 8, the valve 311 is closed while the chemical solution is introduced to the position between the first pressure gauge 51 and the liquid feed pump 32, and the discharge port is opened by the switching valve 413. The controller 12 (see FIG. 1) starts driving the decompression pump 43 while acquiring the first pressure and the second pressure in this state, and the downstream side of the chemical solution path valve 311 is decompressed. (FIG. 4: Step S11). When the difference between the first pressure and the second pressure is equal to or greater than the set pressure difference (steps S12 and S13), the valve 311 is opened and the liquid feed pump 32 side (upstream side) of the valve 311 is depressurized (step S14). . Subsequently, when the liquid feed pump 32 is activated, the delivery of the chemical liquid is started (step S15), and the control of the difference between the first pressure and the second pressure by the control unit 12 is also started (step S16). The chemical solution is introduced into the microreactor 2 while preventing gas in the vicinity of the interface of the tip portion of the chemical solution from being taken in as bubbles in the chemical solution or generating precipitated bubbles.

  And when the front-end | tip part of a chemical | medical solution is discharged | emitted from the microreactor 2 and reaches | attains the flowmeter 411, the pressure reduction pump 43 will be stopped and the switching valve 413 will be switched to the product storage tank 44 side, and a chemical | medical solution will be in a product storage tank. To 44. This prevents the chemical liquid from flowing into the decompression pump 43. In addition, a predetermined process is performed on the chemical solution inside the microreactor 2 (step S17), and the chemical solution is continuously supplied, whereby a necessary amount of the processed chemical solution ( When the product is stored, the control of the difference between the first pressure and the second pressure by the control unit 12 is terminated (step S18), and the delivery of the chemical solution is stopped (step S19). The process ends.

  As described above, in the liquid processing apparatus of FIG. 8, immediately after the chemical solution is introduced into the microreactor 2 and the outflow of the chemical solution from the microreactor 2 to the discharge pipe 41 is detected by the flow meter 411 serving as the liquid detection unit. The switching valve 413 is controlled to guide the chemical liquid to the product storage tank 44. Here, when the gas-liquid separator 42 is used as in the liquid processing apparatus 1 of FIG. 1, the chemical valve does not flow into the decompression pump 43, so that the switching valve 413 is unnecessary, and the control associated therewith is also omitted. On the other hand, since the product storage tank 421 is a part of the gas-liquid separator 42, the replacement of the product storage tank 421 becomes complicated. On the other hand, in the liquid processing apparatus of FIG. 8, the product storage tank 44 can be easily replaced by simply removing it from the discharge pipe 41. The above-described configuration in which the switching valve 413 switches between the path from the discharge port of the microreactor 2 to the decompression pump 43 and the path from the discharge port to the product storage tank 44 is described later with reference to FIGS. It may be provided in the liquid processing apparatus of FIG.

  FIG. 9 is a diagram showing a main body 11b of a liquid processing apparatus according to still another example. In the liquid processing apparatus of FIG. 9, a deaeration module 34 that degass the liquid is provided closer to the liquid feed pump 32 than the first pressure gauge 51 of the supply pipe 31, and the deaeration module 34 connects the deaeration exhaust pipe 341. Via the switching valve 433 of the exhaust pipe 431 via the pressure reducing pump 43 side. Other configurations are the same as those of the liquid processing apparatus 1 of FIG.

  In the process in the liquid processing apparatus of FIG. 9, the valve 311 is closed while the chemical liquid is introduced to the position between the first pressure gauge 51 and the deaeration module 34, and the pressure reducing pump 43 is switched by the switching valve 433. Is communicated with the product storage tank 421. In this state, the controller 12 (see FIG. 1) starts driving the decompression pump 43, whereby the downstream side of the valve 311 in the chemical solution path is decompressed (FIG. 4: step S11), and the deaeration module 34 The deaeration of the liquid existing inside is started. When the difference between the first pressure and the second pressure is equal to or greater than the set pressure difference (steps S12 and S13), the valve 311 is opened and the liquid feed pump 32 side (upstream side) of the valve 311 is depressurized (step S14). . Subsequently, when the liquid feed pump 32 is activated, the delivery of the chemical liquid is started and the chemical liquid is introduced into the microreactor 2 (step S15), and the difference between the first pressure and the second pressure by the control unit 12 is determined. Is also started (step S16). And when the front-end | tip part of a chemical | medical solution reaches | attains the flowmeter 411, the inside of the product storage tank 421 will be open | released by air | atmosphere by the switching valve 433. FIG. At this time, the control unit 12 keeps the decompression pump 43 driven, so that degassing of the chemical solutions sequentially supplied to the microreactor 2 is continued.

  Inside the microreactor 2, a predetermined process is performed on the sequentially supplied chemicals (step S 17), and the processed chemicals (that is, products) are guided to the product storage tank 421 and stored. The When a necessary amount of product is stored in the product storage tank 421, the control of the difference between the first pressure and the second pressure by the control unit 12 is finished, and the liquid feed pump 32 and the decompression pump 43 are stopped. Then, the delivery of the chemical liquid is stopped, and the processing in the liquid processing apparatus is finished (steps S18 and S19).

  As described above, in the liquid processing apparatus of FIG. 9, the chemical solution supplied to the microreactor 2 is degassed by the degassing module 34. As a result, when the chemical solution is introduced into the microreactor 2, the amount of gas dissolved in the chemical solution is reduced, and the temperature of the chemical solution rises due to the influence of reaction heat in the microreactor 2, etc., and precipitation bubbles are likely to be generated in the chemical solution. Even if it is a state, it can prevent that a precipitation bubble generate | occur | produces. The degassing module 34 may also be provided in the liquid processing apparatus of FIG. 8 (and the liquid processing apparatuses of FIGS. 14 to 17 described later).

  FIG. 10 is a view showing a main body 11c of a liquid processing apparatus according to still another example. The supply pipe 31 of the liquid processing apparatus of FIG. 10 is provided with a degassing module 34 similar to the liquid processing apparatus of FIG. 9, and the microreactor 2 is interposed between the degassing module 34 and the first pressure gauge 51. And a flow rate adjusting unit (for example, a mass flow controller) 35 having a flow meter is attached. Further, the end of the supply pipe 31 opposite to the microreactor 2 is connected to the chemical liquid supply tank 33, and a gas supply pipe 362 having a pressure adjustment valve 361 is connected to the upper part of the chemical liquid supply tank 33. The gas supply pipe 362 is connected to the high-pressure gas supply unit 363, and the liquid supply gas is supplied into the chemical solution supply tank 33 at a predetermined pressure by the pressure adjustment valve 361, whereby the chemical solution in the chemical solution supply tank 33 is obtained. Is fed to the supply pipe 31. That is, in the main body 11 c, the liquid supply mechanism 36 that supplies the chemical solution to the microreactor 2 through the supply pipe 31 is realized by the pressure adjustment valve 361, the gas supply pipe 362, and the high-pressure gas supply unit 363. 1, 8, and 9 (and the liquid processing apparatuses in FIGS. 11, 14, and 17, which will be described later), a liquid feeding mechanism 36 may be provided instead of the liquid feeding pump 32. Good.

  In the processing in the liquid processing apparatus of FIG. 10, for example, the downstream side of the chemical solution path valve 311 is depressurized while the chemical solution is introduced to a position between the deaeration module 34 and the flow rate adjustment unit 35 (FIG. 4: Step S11). ) When the difference between the first pressure and the second pressure is equal to or greater than the set pressure difference (steps S12 and S13), the valve 311 is opened and the upstream side of the valve 311 in the supply pipe 31 is depressurized (step S14). At this time, pressure reduction near the interface of the chemical solution is performed via the flow rate adjusting unit 35.

  Then, the liquid feeding mechanism 36 is activated to start delivery of the chemical liquid (step S15), and the control of the difference between the first pressure and the second pressure by the control unit 12 (see FIG. 1) is also started (step S16). ). When the chemical solution is introduced into the microreactor 2, the flow rate of the chemical solution is gradually increased to a predetermined value by the flow rate adjusting unit 35, and then adjusted to be constant. When the tip of the chemical solution is discharged from the discharge port of the microreactor 2 to the discharge pipe 41 and reaches the flow meter 411, the inside of the product storage tank 421 is opened to the atmosphere by the switching valve 433. At this time, the chemical liquid is continuously degassed by continuing to drive the decompression pump 43. The tip of the chemical solution is guided to the product storage tank 421.

  In the liquid processing apparatus, the supply of the chemical solution to the microreactor 2 is continued, and within the microreactor 2, a predetermined process is performed on the sequentially supplied chemical solutions (step S17), and the processed chemical solution (that is, the product). Is stored in the product storage tank 421. At this time, even if chemical leakage occurs in the microreactor 2, the control unit 12 compares the flow rate indicated by the flow rate adjustment unit 35 with the flow rate indicated by the flow rate meter 411, thereby leaking the chemical solution. Is detected, a warning indicating leakage of the chemical solution is displayed on the display unit of the control unit 12, and the liquid feed pump 32 is stopped. In the microreactor 2, when a process involving irradiation of light from the light irradiation unit 63 (see FIG. 1) is performed on the chemical liquid, the chemical liquid is adjusted according to the intensity of light acquired by the illuminometer 632. The flow rate per unit time of the chemical solution in the microchannel 23 of the microreactor 2 may be adjusted by the flow rate adjusting unit 35 so that the amount of light applied is constant.

  When a necessary amount of product is stored in the product storage tank 421, the control of the difference between the first pressure and the second pressure by the control unit 12 is finished and the delivery of the chemical solution by the liquid feed pump 32 is stopped. (Steps S18 and S19). Further, the driving of the decompression pump 43 is also stopped, and the processing in the liquid processing apparatus is finished.

  As described above, in the liquid processing apparatus of FIG. 10, the flow rate adjusting unit 35 that adjusts the flow rate of the chemical solution flowing into the microreactor 2 is provided. As a result, when the chemical solution is introduced into the microreactor 2, it is suppressed that the chemical solution suddenly flows into the microreactor 2 and the flow is disturbed at the tip portion of the chemical solution, and the gas in the vicinity of the interface at the tip portion of the chemical solution is suppressed. It can further be suppressed that it is taken in as a bubble. In the liquid processing apparatus of FIG. 10, it is possible to control the difference between the first pressure and the second pressure by driving and controlling the flow rate adjusting unit 35 during the continuous supply of the chemical solution to the microreactor 2. . Further, the flow rate adjusting unit 35 may be provided in the liquid processing apparatus of FIGS. 1, 8, and 9 (and FIGS. 14, 15, and 17).

  FIG. 11 is a view showing a main body 11d of a liquid processing apparatus according to still another example. In the liquid processing apparatus of FIG. 11, the supply pipe 31 is connected to the liquid feed pump 32 on the side opposite to the microreactor 2 (upstream side). Or, it is connected to a rinsing liquid supply tank 372 side for storing a rinsing liquid (for example, acetone). The chemical solution supply tank 33 is provided with a tank temperature adjustment unit 331 that keeps the temperature of the internal chemical solution constant. Further, in the supply pipe 31, the liquid temperature for adjusting the temperature of the liquid flowing in the supply pipe 31 and the deaeration module 34 connected to the auxiliary pump 342 separately prepared in order from the liquid feed pump 32 side to the microreactor 2. Adjustment unit 38, temperature sensor 53 that acquires the temperature of the liquid in the supply pipe 31, auxiliary pressure gauge 54 that acquires the pressure of the liquid or gas in the supply pipe 31, filter 39, flow rate adjustment unit 35, and first pressure gauge 51 And a valve 311 is provided. In the liquid processing apparatus, when the chemical liquid is supplied to the microreactor 2, a difference between the pressure of the chemical liquid acquired by the auxiliary pressure gauge 54 and the pressure of the chemical liquid acquired by the first pressure gauge 51 is obtained. When the difference is equal to or greater than a predetermined value, a warning requesting replacement of the filter 39 is displayed on the display unit of the control unit 12 (see FIG. 1).

  A suction pump 46 (for example, a plunger pump) capable of sucking both gas and liquid is provided on the opposite side of the discharge pipe 41 from the microreactor 2, and the suction pump 46 is switched to a product storage tank by a switching valve 471. It is connected to the 44 side or the rinsing liquid recovery tank 472 side that recovers the rinsing liquid that has flowed through the microreactor 2. The product storage tank 44 is provided with a tank temperature adjustment unit 441 that keeps the temperature of the internal product constant. The discharge pipe 41 includes a second pressure gauge 52, a flow meter 411, a liquid temperature adjusting unit 48 that adjusts the temperature of the liquid flowing in the discharge pipe 41 in order from the microreactor 2 side toward the suction pump 46, and a discharge pipe. A temperature sensor 54 is provided for acquiring the temperature of the liquid in 41.

  In the process in the liquid processing apparatus of FIG. 11, the liquid feed pump 32 is connected to the chemical liquid supply tank 33 side by the switching valve 371 so that the chemical liquid is positioned between the liquid feed pump 32 and the first pressure gauge 51 (for example, the liquid temperature The valve 311 is closed in this state, and the suction pump 46 is communicated with the product storage tank 44 by the switching valve 471. And the control part 12 starts the drive of the suction pump 46 which is a pressure reduction mechanism (FIG. 4: step S11). At this time, the inside of the product storage tank 44 is open to the atmosphere, and the downstream side of the chemical liquid path valve 311 is depressurized by the suction pump 46. In addition, by driving the auxiliary pump 342, the liquid flowing in the supply pipe 31 in the degassing module 34 can be degassed.

  When the difference between the first pressure and the second pressure is equal to or greater than the set pressure difference (steps S12 and S13), the valve 311 is opened and the liquid feed pump 32 side (upstream side) of the valve 311 is depressurized (step S14). . Subsequently, the feeding of the chemical liquid is started by activating the liquid feeding pump 32, and the chemical liquid moves toward the microreactor 2 and is introduced into the microreactor 2 (step S15). Further, the control of the difference between the first pressure and the second pressure by the control unit 12 is started (step S16). At this time, the temperature of the chemical solution flowing (introduced) into the microreactor 2 by the liquid temperature control unit 38 is higher than the temperature of the chemical solution in the chemical solution supply tank 33 before being supplied to the microreactor 2 by the liquid feed pump 32. Is further reduced, the gas (saturated) solubility in the liquid is increased, and the generation of precipitated bubbles in the chemical solution in the microreactor 2 is further prevented. In addition, since the chemical liquid is filtered by the filter 39, even if an unnecessary substance is mixed in the chemical liquid, the inflow of the unnecessary substance into the microreactor 2 is prevented, and the chemical liquid is processed in the microreactor 2. It is prevented that troubles occur.

  When the discharge of the chemical solution from the microreactor 2 is detected by the flow meter 411, the suction pump 46 is stopped and the chemical solution in the discharge pipe 41 is guided to the product storage tank 44. In the liquid processing apparatus, the supply of the chemical solution is continued, and a predetermined process is performed on the supplied chemical solution in the microreactor 2 (step S17), so that a product obtained by the process is stored in the product storage tank 44. Is done. At this time, the product is adjusted to a predetermined temperature (for example, cooled) in the supply pipe 31 by the liquid temperature adjustment unit 48, and the product temperature is also kept constant by the tank temperature adjustment unit 441 in the product storage tank 44. Therefore, even if the product is altered by temperature, it is possible to prevent the quality of the product from being deteriorated. If there is a possibility that condensation may occur in the supply pipe 31 or the discharge pipe 41 due to the temperature adjustment of the chemical solution or product, a heat insulating material is wound around these pipes to suppress condensation or to prevent condensation on the pipe. A system for detecting and notifying the operator or a drainage unit for discharging condensed water is provided. In addition, the liquid temperature control sections 38 and 48 provided in the supply pipe 31 and the discharge pipe 41 center on the supply pipe 31 or the discharge pipe 41 that uses a heat exchanger, a heater, or a Peltier element, or that is made of metal. The supply pipe 31 or the discharge pipe 41 may be heated by applying a high-frequency current to the coil wound as follows.

  In the liquid processing apparatus of FIG. 11, even when the chemical solution is continuously supplied, the control unit 12 controls the liquid feed pump 32 to control the difference between the first pressure and the second pressure, thereby preventing the generation of precipitated bubbles. The If necessary, the suction pump 46 is continuously driven even during the continuous supply of the chemical liquid, and the liquid feed pump 32 and the suction pump 46 are driven to control the difference between the first pressure and the second pressure. In this case, the liquid feed pump 32 may be temporarily stopped. That is, in the liquid processing apparatus 1, the control unit 12 drives and controls the liquid feed pump 32 and / or the suction pump 46 to control the difference between the first pressure and the second pressure.

  When a required amount of product is stored in the product storage tank 44, the switching valve 371 of the supply pipe 31 is on the rinsing liquid supply tank 372 side, and the switching valve 471 of the discharge pipe 41 is on the rinsing liquid recovery tank 472 side. Each can be switched. Thereby, in the liquid processing apparatus, the cleaning of the chemical solution path from the supply pipe 31 to the discharge pipe 41 via the microreactor 2 is performed. Thereafter, the control of the difference between the first pressure and the second pressure by the controller 12 is stopped (may be stopped before the rinsing liquid is supplied) (step S18), and the liquid feed pump 32 is stopped to perform liquid processing. The process in the apparatus ends (step S19).

  When processing depending on the temperature of the chemical solution is performed in the liquid processing apparatus, the processing by the liquid temperature adjusting unit 38 that lowers the temperature of the chemical solution flowing into the microreactor 2 is lower than the temperature of the chemical solution in the chemical solution supply tank 33. This is performed only at the time of introduction of the chemical solution, and at the subsequent continuous supply of the chemical solution, the chemical solution in the supply pipe 31 and the microreactor 2 is set to a temperature suitable for producing a desired product. In this case, when the switching valve 471 is switched, a product (a product generated from the chemical liquid that has flowed into the microreactor 2 at a temperature at which precipitation bubbles are not easily generated) acquired when the chemical liquid is introduced is rinsed with the rinse liquid recovery tank 472. Then, by switching the switching valve 471 again, only the product generated during the continuous supply of the chemical solution is stored in the product storage tank 44.

  As described above, in the liquid processing apparatus of FIG. 11, the temperature of the chemical solution is set lower than the temperature of the chemical solution in the chemical solution supply tank 33 when the chemical solution is introduced into the microreactor 2. Thereby, when supplying a chemical | medical solution to the inside of the micro reactor 2, it can further prevent that a bubble generate | occur | produces in the chemical | medical solution resulting from the fluctuation | variation of the pressure of a chemical | medical solution. The liquid temperature adjustment unit 38 is configured so that the temperature of the chemical liquid flowing into the microreactor 2 can be lower than the temperature of the chemical liquid in the product storage tank 44, as long as the temperature of the chemical liquid is reduced. 11 may be arranged at a position different from that in FIG. Further, the liquid temperature adjusting unit 38 may be provided in the liquid processing apparatus of FIGS. 1 and 8 to 10 (and FIGS. 14 to 17).

  In the liquid processing apparatus, by providing a suction pump 46 capable of sucking both gas and liquid, a gas-liquid separation unit 42 is provided as in the liquid processing apparatus 1 of FIG. 1, or the liquid processing of FIG. It is possible to simplify the configuration of the liquid processing apparatus without separately providing the configuration (branch path 412 and switching valve 413) necessary for using the decompression pump 43 capable of sucking only gas as in the apparatus. Further, in the liquid processing apparatus of FIGS. 1 and 8 to 10 (and FIGS. 14 to 16), a suction pump 46 may be provided instead of the decompression pump 43. In the liquid processing apparatus shown in FIG. 11, the rinsing liquid is supplied to the microreactor 2 before the chemical liquid is supplied, and the rinsing liquid is filled into the microreactor 2 by using the above-described method when the rinsing liquid is introduced. The liquid to be used may be switched to the chemical liquid. In the liquid processing apparatus, a metering pump having a flow rate control function is provided in place of the liquid feed pump 32, and the flow rate of the chemical solution flowing into the microreactor 2 can be adjusted while omitting the flow rate adjusting unit 35. is there.

  Next, the case where only the valve 311 is omitted in the liquid processing apparatus of FIG. 11 will be described according to the processing flow of FIG. In the processing in this liquid processing apparatus, the suction pump 46 is communicated with the product storage tank 44 by the switching valve 471 in a state where the chemical liquid is introduced to the position between the first pressure gauge 51 and the liquid feeding pump 32, and the control is performed. The unit 12 starts driving the suction pump 46 (step S11).

  Here, in the liquid processing apparatus in which the valve 311 of the supply pipe 31 is omitted, when the suction pump 46 is driven, changes in the first pressure and the second pressure when the below-described chemical solution is not supplied will be described. . FIG. 12 is a diagram showing changes in the first pressure and the second pressure when no chemical solution is supplied. In FIG. 12, the triangle indicates the first pressure, and the diamond indicates the second pressure. As shown in FIG. 12, in the microreactor 2 used in the present embodiment, a relatively large pressure loss occurs in the fine flow path 23, so that immediately after the start of decompression by the suction pump 46, There is a large difference between the second gas pressure and the first gas pressure in the supply pipe 31.

  Actually, the control unit 12 obtains the difference between the first gas pressure in the supply pipe 31 and the second gas pressure in the discharge pipe 41 every minute time (step S12), and the first pressure and the second pressure are calculated. When the difference becomes a predetermined pressure difference (for example, 0.2 atm) smaller than the upper limit pressure difference (step S13), the liquid feed pump 32 is activated and the delivery of the chemical liquid is started (step S15). ), The control of the difference between the first pressure and the second pressure by the controller 12 is started (step S16). Note that the process of opening the valve 311 in step S14 of FIG. 4 is omitted.

  FIG. 13 is a diagram illustrating changes in the first pressure and the second pressure. In FIG. 13, the triangle indicates the first pressure, and the diamond indicates the second pressure. Further, the time indicated by the reference numeral T1 in FIG. 13 is the time when the liquid feeding pump 32 is activated and the liquid feeding is started (actually, about 0.3 seconds from the start of decompression). rear). When the feeding of the chemical liquid is started, the gas in the chemical liquid path is compressed by the movement of the tip of the chemical liquid, but the supply pipe 31 is decompressed from the downstream side while driving and controlling the suction pump 46, The difference between the first pressure and the second pressure is kept constant.

  At the time denoted by reference numeral T2 in FIG. 13, the tip of the chemical solution passes through the position of the first pressure gauge 51, the pressure acquisition target by the first pressure gauge 51 is switched to the chemical solution, and the first pressure starts from 1 atm. It rises to about 1.6 atm and then becomes constant. At this time, also in the discharge pipe 41 provided with the second pressure gauge 52, the gas in the chemical liquid path is compressed by the movement of the chemical liquid, and the second pressure is changed to the first pressure by temporarily reducing the suction amount by the suction pump 46. It rises in the same way while keeping the difference from the pressure constant. After that, the liquid feed pump 32 and the suction pump 46 are driven and controlled by the control unit 12 so that the difference between the first pressure and the second pressure is substantially constant. As a result, when the chemical solution is introduced into the microreactor 2, the gas in the vicinity of the interface at the tip of the chemical solution is prevented from being taken in as bubbles in the chemical solution or the generation of precipitated bubbles.

  In the liquid processing apparatus, the supply of the chemical solution is continued, and the control unit 12 controls the difference between the first pressure and the second pressure, thereby preventing the generation of precipitated bubbles even during the continuous supply of the chemical solution to the microreactor 2. The Further, a predetermined process is performed on the chemical solution inside the microreactor 2 (step S17), and when a necessary amount of product is stored in the product storage tank 44, the first pressure by the control unit 12 is stored. And the control of the difference between the second pressure and the second pressure are finished (step S18), the sending of the chemical solution by the liquid feed pump 32 is stopped, and the processing in the liquid processing apparatus is finished (step S19).

  As described above, in the liquid processing apparatus in which the valve 311 of the supply pipe 31 is omitted, the second pressure is reduced due to the pressure loss of the gas in the microchannel 23 in the microreactor 2 immediately before the chemical solution is introduced into the microreactor 2. It is made lower than the first pressure. Then, when the difference between the first pressure and the second pressure becomes a predetermined pressure difference smaller than the upper limit pressure difference, the liquid feed pump 32 is activated and the introduction of the chemical liquid is started. However, by driving and controlling the liquid feed pump 32 and the suction pump 46, the difference between the first pressure and the second pressure is kept constant at the pressure difference. Thereby, it is possible to prevent the gas in the vicinity of the interface at the tip of the chemical solution from being taken in as bubbles in the chemical solution or the generation of precipitated bubbles.

  In the liquid processing apparatus described above, one type of chemical solution is supplied to the microreactor 2 to perform processing on the chemical solution. However, depending on the design of the microreactor, a process of mixing a plurality of types of chemical solutions may be performed. In addition, it is possible to connect a plurality of microreactors 2 to perform more advanced processing on a chemical solution. Hereinafter, an example of such a liquid processing apparatus will be described.

  FIG. 14 is a view showing a main body 11e of a liquid processing apparatus according to still another example. The liquid processing apparatus of FIG. 14 is provided with a plurality of (three) microreactors (however, the reference numerals 2a, 2b, and 2c are attached to the right side from the leftmost microreactor in FIG. 14). The microreactors 2 a to 2 c are accommodated in one casing 91. Specifically, the leftmost microreactor 2a in FIG. 14 is provided with two inlets, and a supply pipe 31 is connected to each inlet. A chemical solution supply tank 33 is connected to the opposite side of each supply pipe 31 from the microreactor 2a via a liquid feed pump 32. Between the liquid feed pump 32 of the supply pipe 31 and the microreactor 2a, the liquid feed pump 32 side is connected. A first pressure gauge 51 and a valve 311 are provided in order. One chemical solution supply tank 33 stores a predetermined liquid monomer, and the other chemical solution supply tank 33 stores a polymerization initiator for the monomer.

  The microreactor 2a is provided with one discharge port, and each of the other two microreactors 2b and 2c is provided with one introduction port and one discharge port. A connecting pipe 92 (for example, an inner pipe) is provided between the outlet of the microreactor 2a and the inlet of the central microreactor 2b and between the outlet of the central microreactor 2b and the inlet of the rightmost microreactor 2c. A 1/16 inch diameter stainless steel (SUS316) is attached. Each microreactor 2a to 2c has a reactor temperature control unit having a temperature sensor (note that reference numerals 62a, 62b, and 62c are attached to the right side from the leftmost reactor temperature control unit in FIG. 14). It is provided so as to abut on the main body 24 (see FIG. 3). Each of the microreactors 2a to 2c (the reactor main body 24) is made of a metal having a good thermal conductivity such as stainless steel (SUS316), for example, and the temperature of the microreactors 2a to 2c is adjusted by the reactor temperature control units 62a to 62c. Is adjusted efficiently.

  In the housing 91, the microreactors 2a to 2c and the corresponding reactor temperature control units 62a to 62c are covered with a heat insulating material 931, and a heat insulating partition wall 932 is provided between the two adjacent microreactors 2a to 2c. . Thereby, the plurality of microreactors 2 a to 2 c are respectively disposed in a plurality of spaces (chambers) formed by being partitioned by the heat insulating partition walls 932 in the housing 91. Each space is provided with an intake port 94 and an exhaust port 95 to be individually ventilated. A discharge pipe 41 is connected to the discharge port of the rightmost microreactor 2c. In addition, about each structure provided in the discharge pipe 41, it is the same as that of the liquid processing apparatus 1 of FIG.

  In the processing in the liquid processing apparatus of FIG. 14, as in the liquid processing apparatus 1 of FIG. 1, the chemical liquid path (in this case, the resin monomer and the polymerization is performed by driving the decompression pump 43 in the closed state where each valve 311 is closed. The chemical liquid paths of the initiator are actually reduced to one downstream of each valve 311 of the microreactor 2a (FIG. 4: step S11). At this time, the pressures acquired by the two first pressure gauges 51 are both the same pressure (for example, atmospheric pressure). When the difference between the first pressure and the second pressure is equal to or greater than the set pressure difference (steps S12 and S13), the two valves 311 are opened simultaneously, and the liquid feed pump 32 side (upstream side) of the valve 311 is depressurized ( Step S14). Then, the liquid feed pumps 32 are simultaneously activated to start the delivery of the monomer and the polymerization initiator, and are introduced into the microreactor 2a from different inlets (step S15). Further, the control unit 12 (see FIG. 1) starts to control the difference between the first pressure and the second pressure in one supply pipe 31 and the difference between the first pressure and the second pressure in the other supply pipe 31. (Step S16).

  In the microreactors 2a to 2c, a predetermined process is performed on the monomer (step S17). Specifically, the microreactor 2a is heated to about 50 ° C. by the reactor temperature control unit 62a, and the monomer and the polymerization initiator are mixed in the microreactor 2a under this temperature environment (that is, the microreactor 2a is mixed with the mixer). As a role.) Subsequently, the mixed liquid is introduced into the central microreactor 2 b through the connection pipe 92. The microreactor 2b is heated to about 200 ° C. by a reactor temperature control unit 62b having a ceramic heater, for example, and the polymerization of the monomer is promoted in the microreactor 2b. Then, the polymerized liquid (polymer) is introduced into the microreactor 2c, and the polymerization reaction is stopped, for example, by holding the microreactor 2c at about 30 ° C. by the reactor temperature control unit 62c having a Peltier element. A certain liquid is discharged from the discharge port to the discharge pipe 41 and stored in the product storage tank 421. When a necessary amount of product is stored in the product storage tank 421, the control of the difference between the first pressure and the second pressure by the control unit 12 is finished (step S18), and the chemical solution by the liquid feed pump 32 is discharged. The delivery is stopped and the processing in the liquid processing apparatus is finished (step S19).

  As described above, in the liquid processing apparatus of FIG. 14, the plurality of microreactors 2 a to 2 c are connected in series, and the temperatures of the plurality of microreactors 2 a to 2 c are individually adjusted. Thereby, when supplying the chemical liquid to the microreactors 2a to 2c, the gas in the vicinity of the interface at the tip of the chemical liquid is prevented from being taken in as bubbles in the chemical liquid, and the generation of precipitated bubbles is prevented, and the plurality of microreactors 2a In each of ˜2c, the temperature-dependent treatment can be performed on the mixed liquid. In the liquid processing apparatus, each microreactor 2a-2c is covered with a heat insulating material 931, and is placed in a space formed by a heat insulating partition wall 932, and each space is individually ventilated, so that the microreactor 2b is heated to a high temperature. Polymerization of the monomer is promoted by heat from the other microreactors 2a and 2c, resulting in low uniformity of molecular weight of the polymer after production, particularly having a fine flow path, and mixing at low temperature is required. It is prevented that excessive polymerization occurs in the microreactor 2a to be closed and the flow path is blocked. In the case where there is no effect on the processing in each of the microreactors 2a to 2c, it is possible to provide only the heat insulating material 931 and omit the heat insulating partition 932. Moreover, in the liquid processing apparatus of FIG. 14, the influence of the heat from the outside with respect to the process target liquid may be suppressed by winding a heat insulating material around the supply pipe 31, the connection pipe 92, and the discharge pipe 41. Furthermore, the monomer and the polymerization initiator may be delivered by a syringe pump.

  FIG. 15 is a diagram showing a part of a main body 11f of a liquid processing apparatus according to still another example. The liquid processing apparatus of FIG. 15 includes a plurality (three) of microreactors 2d each provided with a reactor temperature control unit 62, and each microreactor 2d has two inlets and one outlet. The liquid processing apparatus includes two supply pipes 31 and one discharge pipe 41. One supply pipe 31 branches on the microreactor 2d side and is connected to one introduction port of each microreactor 2d. It branches on the microreactor 2d side and is connected to the other inlet of each microreactor 2d. Further, the discharge pipe 41 branches on the microreactor 2d side and is connected to the discharge port of each microreactor 2d. The configuration on the upstream side of the branch point of each supply pipe 31 and the configuration on the downstream side of the branch point of the discharge pipe 41 are the same as those of the liquid processing apparatus of FIG.

  In the liquid processing apparatus of FIG. 15 as well, by performing the same processing as that of the liquid processing apparatus of FIG. It is possible to perform a temperature-dependent process on the chemical solution supplied in each of the plurality of microreactors 2d while preventing the intake or generation of precipitated bubbles. As described above, by individually adjusting the temperatures of the plurality of microreactors 2d connected in parallel, the temperature of each microreactor 2d can be adjusted with higher accuracy, and the quality of the product can be improved. It becomes.

  Note that the plurality of microreactors 2a to 2c connected in series in the liquid processing apparatus of FIG. 14 constitute one microreactor group, and each microreactor 2d in the liquid processing apparatus of FIG. 15 is replaced with this microreactor group and connected in parallel. More advanced processing may be performed on the chemical solution using a plurality of microreactor groups. Further, in the liquid processing apparatus of FIGS. 1 and 8 to 11 (and FIGS. 16 and 17 described later), a plurality of microreactors connected in series or in parallel as in the liquid processing apparatuses of FIGS. And the temperatures of the plurality of microreactors may be individually adjusted.

  FIG. 16 is a view showing a main body 11g of a liquid processing apparatus according to the second embodiment of the present invention. In the liquid processing apparatus of FIG. 16, a plurality of microreactors 2 are arranged in parallel, a supply pipe 31 is connected to the introduction port of each microreactor 2, and a discharge pipe 41 is connected to the discharge port. The supply pipe 31 is provided with a flow rate adjusting unit 35, a first pressure gauge 51, and a valve 311 in order from the upstream side (opposite side to the microreactor 2), and the discharge pipe 41 is provided with the second in order from the upstream side (microreactor 2 side). A pressure gauge 52 and a flow rate adjustment unit 45 are provided. As described above, in the liquid processing apparatus of FIG. 16, the microreactor 2, the supply pipe 31, the discharge pipe 41, the first and second pressure gauges 51 and 52, and the flow rate adjustment units 35 and 45 are configured as one processing unit 13. The processing units 13 are arranged in parallel. In the plurality of processing units 13, the plurality of supply pipes 31 are combined and connected to the liquid feed pump 32, and the plurality of discharge pipes 41 are combined and connected to the decompression pump 43.

  In the processing in the liquid processing apparatus of FIG. 16, the chemical solution may be positioned between the first pressure gauge 51 and the liquid feeding pump 32 (either before or after branching to the plurality of supply pipes 31. ), The controller 12 (see FIG. 1) closes the valve 311 of each processing unit 13 and starts driving the decompression pump 43 (FIG. 4: step S11). In the liquid processing apparatus, the control unit 12 (see FIG. 1) individually drives and controls the plurality of downstream flow rate adjustment units 45, whereby the first pressures acquired by the first pressure gauges 51 in all the processing units 13 are obtained. And the second pressure acquired by the second pressure gauge 52 become substantially equal to or larger than the set pressure difference at the same time (steps S12 and S13), and then all the valves 311 are opened at the same time so (Upstream side) is depressurized (step S14). Subsequently, the feeding of the chemical liquid is started by activating the liquid feeding pump 32 (step S15), and the control of the difference between the first pressure and the second pressure in each processing unit 13 by the control unit 12 is also started. (Step S16). In the control of the difference between the first pressure and the second pressure, drive control of the flow rate adjusting units 35 and 45 may be performed together with the liquid feed pump 32 and the pressure reducing pump 43.

  The chemical solution is introduced into each microreactor 2 and then discharged to the discharge pipe 41. Then, when the outflow of the chemical solution from the microreactor 2 to the discharge pipe 41 is detected in all the flow rate adjusting sections 45, the decompression pump 43 is stopped and the path is switched by the switching valve 413, and the plurality of discharge pipes 41 are discharged. The chemical solution is guided to the product storage tank 421. In the liquid processing apparatus, the supply of the chemical solution to the microreactor 2 is continued, and a predetermined process is performed on the chemical solution inside the microreactor 2 (step S17), and the processed chemical solution (product) is stored in the product storage tank. It is stored at 421.

  At this time, the pressure loss in the flow of the chemical solution is different in each of the plurality of microreactors 2, but the flow rate of the chemical solution flowing to the microreactor 2 is made constant by each flow rate adjusting unit 35. Product can be produced. In addition, since the control unit 12 monitors the pressure indicated by the first and second pressure gauges 51 and 52 and the flow rate indicated by the flow meters included in the flow rate adjustment units 35 and 45 for each processing unit 13, the microreactor 2 even when an abnormality occurs in the flow path in 2 (for example, when leakage occurs in the microreactor 2 or when the flow path is likely to be clogged), it becomes possible to detect an abnormality at an early stage. Quality degradation can be suppressed. When an abnormality occurs in the flow path in the microreactor 2 as described above, the supply pipe 31 and the discharge pipe 41 are blocked by the flow rate adjusting units 35 and 45 of the processing unit 13 including the microreactor 2 in which the abnormality has occurred. Thereby, the production | generation of the product using the other microreactor 2 can be performed continuously.

  In the liquid processing apparatus, when a necessary amount of product is stored in the product storage tank 421, the control of the difference between the first pressure and the second pressure is finished (step S18), and the delivery of the chemical solution is stopped. (Step S19), the processing in the liquid processing apparatus ends.

  As described above, in the liquid processing apparatus of FIG. 16, a plurality of processing units 13 each having the microreactor 2, the supply pipe 31, the discharge pipe 41, and the first and second pressure gauges 51 and 52 are provided. The processing unit 13 is connected to one liquid feed pump 32 and one pressure reduction pump 43. As a result, when supplying the chemical solution to the microreactor 2, gas in the vicinity of the interface at the tip of the chemical solution is taken in as bubbles in the chemical solution, or precipitation bubbles are generated in the chemical solution. The amount of chemical solution can be increased.

  In the liquid processing apparatus of FIG. 16, a plurality of microreactors each having two inlets and one outlet may be used. In this case, a supply pipe 31 having a flow rate adjusting unit 35, a first pressure gauge 51, and a valve 311 is connected to one introduction port of each microreactor, and these supply pipes 31 are coupled to one liquid feed pump 32. Connected. Further, a supply pipe 31 having a flow rate adjusting unit 35, a first pressure gauge 51, and a valve 311 is connected to the other inlet of each microreactor, and these supply pipes 31 are combined to form another liquid feed pump. 32. In such a liquid processing apparatus, for example, water is sent out by one liquid feed pump 32 and oil is sent out by the other liquid feed pump 32 to produce an emulsion as a product (that is, the microreactor is a mixer). As a role.)

  By the way, when producing an emulsion by mixing water and oil, the temperature of the mixer has a great influence on the quality of the emulsion. Therefore, in general, an appropriate mixer temperature in the production of an emulsion is determined by experiments. The In this case, the quality of the resulting emulsion is usually confirmed by stabilizing the temperature of the mixer that mixes the water and oil and then delivering water and oil to determine the appropriate mixer temperature. It takes a long time. In addition, enormous time is required to determine appropriate conditions such as the mixing ratio of water and oil and the flow rate of liquid in the mixer.

  On the other hand, in the liquid processing apparatus that can be used for the production of the emulsion, for example, while the temperature of one microreactor is set to 50 ° C. by the reactor temperature adjustment unit 62, two flow rate adjustment units 35 connected to the microreactor are provided. By controlling, water and oil are mixed at a mixing ratio of 1: 2 to obtain a product. At this time, for the other microreactors, the flow rate adjusting units 35 and 45 are closed so that the liquid does not flow into the microreactor. Subsequently, in another microreactor previously stabilized at a temperature of 50 ° C., a product is obtained by mixing water and oil at a mixing ratio of 1: 1, and collected in another product storage tank 421. Is done. Thereafter, in a further microreactor previously stabilized at a temperature of 100 ° C., water and oil are mixed at a mixing ratio of 1: 1 to obtain a product. In this way, the liquid processing apparatus can acquire products manufactured under a plurality of conditions in a short time, and determine various conditions suitable for manufacturing a high-quality emulsion in a short time. Is possible.

  FIG. 17 is a view showing a part of the main body 11h of the liquid processing apparatus according to the third embodiment of the present invention. In the liquid processing apparatus of FIG. 17, a plurality of processing units (two processing units 13a and 13b in FIG. 17) each having a supply pipe 31, a discharge pipe 41 and a microreactor 2 are provided in series, and each of the processing units 13a and 13b In the supply pipe 31, a liquid feed pump 32, a first pressure gauge 51, and a valve 311 are provided in order from the upstream side to the downstream side, and a second pressure gauge 52 is attached to the discharge pipe 41. In the two processing units 13a and 13b adjacent to each other, the liquid feed pump 32 of the other processing unit 13b is connected to the downstream side of the discharge pipe 41 of the upstream processing unit 13a. Further, a chemical supply tank 33 is connected to the liquid feed pump 32 of the upstream processing unit 13a, and a suction pump 46 capable of sucking both gas and liquid is decompressed to the discharge pipe 41 of the downstream processing unit 13b. Connected as a mechanism.

  Next, processing in the liquid processing apparatus of FIG. 17 will be described according to FIG. First, in the upstream processing unit 13a, the chemical solution is introduced to the position between the first pressure gauge 51 and the liquid feed pump 32, the valve 311 of the processing unit 13a is closed, and the downstream side processing unit 13a is closed. The valve 311 of the processing unit 13b is opened. Then, the control unit 12 (see FIG. 1) starts driving the liquid feeding pump 32 and the suction pump 46 of the processing unit 13b, and downstream of the valve 311 of the processing unit 13a in the chemical liquid path from the chemical liquid supply tank 33 to the suction pump 46. The side is depressurized (FIG. 4: step S11). When the difference between the first pressure and the second pressure in the processing unit 13a is equal to or larger than the set pressure difference (steps S12 and S13), the valve 311 of the processing unit 13a is opened and the liquid feed pump 32 side (upstream side) of the valve 311 is opened. ) Is depressurized (step S14). Subsequently, the liquid feeding pump 32 of the processing unit 13a is activated to introduce the chemical into the microreactor 2 on the upstream side (step S15). In addition, when the control unit 12 starts controlling the difference between the first pressure and the second pressure in the processing unit 13a (step S16), the leading end of the chemical solution is introduced when the chemical solution is introduced into the microreactor 2 of the processing unit 13a. It is possible to prevent gas in the vicinity of the interface of the part from being taken in as bubbles in the chemical solution and generation of precipitated bubbles. Thereafter, the chemical solution is discharged to the discharge pipe 41 of the processing unit 13a, and the tip of the chemical solution reaches the position of the liquid feed pump 32 of the processing unit 13b on the downstream side.

  Actually, a flow meter is provided between the liquid feed pump 32 of the processing unit 13b and the first pressure gauge 51, and when it is confirmed that the tip of the chemical solution has moved to this position, the processing unit The liquid feed pumps 32 of 13a and 13b are temporarily stopped, the valve 311 of the processing unit 13b is closed, and the downstream side of the valve 311 of the processing unit 13b in the chemical solution path is depressurized (that is, with respect to the processing unit 13b). (Step S11 in FIG. 4 is performed). When the difference between the first pressure and the second pressure in the processing unit 13b becomes equal to or larger than the set pressure difference (steps S12 and S13), the valve 311 of the processing unit 13b is opened and the liquid feed pump 32 side of the valve 311 ( The pressure on the upstream side is reduced (step S14). Subsequently, the liquid feed pump 32 of the processing units 13a and 13b is activated to introduce the tip of the chemical into the microreactor 2 of the processing unit 13b (step S15), and the control unit 12 in the processing unit 13b. Control of the difference between the first pressure and the second pressure is also started (step S16). And the front-end | tip part of a chemical | medical solution is discharged | emitted to the discharge pipe 41 of the processing unit 13b, and is guide | induced to the product storage tank not shown through the suction pump 46. FIG.

  In the liquid processing apparatus, different processing is performed in each of the two microreactors 2 connected in series (step S17), and the products after processing by the microreactors 2 of the two processing units 13a and 13b are product storage tanks. It is stored at. When a desired amount of product is acquired, the control of the difference between the first pressure and the second pressure in the processing units 13a and 13b is finished (step S18), the delivery of the chemical solution is also stopped, and the liquid processing apparatus. The process in is finished (step S19).

  As described above, in the liquid processing apparatus of FIG. 17, a plurality of processing units 13 a each including the liquid feed pump 32, the microreactor 2, the supply pipe 31, the discharge pipe 41, and the first and second pressure gauges 51 and 52. 13b are connected in series, and in two processing units 13a and 13b adjacent to each other, the liquid feed pump 32 connected to the supply pipe 31 of the downstream processing unit 13b is connected to the discharge pipe 41 of the upstream processing unit 13a. The suction pump 46 is separately connected to the discharge pipe 41 of the processing unit 13b on the downstream side. Here, in the case where a pump is not provided between two microreactors 2 connected in series, if the chemical liquid is caused to flow only by the upstream liquid feed pump, it is necessary to increase the pressure of the chemical liquid, which is an expensive pump. Depending on the type of chemical solution, the solute dissolved in the solvent is likely to precipitate, making it difficult to produce the desired reaction uniformly. There is also a possibility of end. In addition, when flowing a high-viscosity chemical solution, an excessive load is applied to the upstream microreactor. On the other hand, in the liquid processing apparatus of FIG. 17, by providing a pump between two microreactors 2 connected in series, even when a highly viscous chemical solution is allowed to flow, the chemical solution is set to an excessively high pressure. The chemical solution can be easily supplied to the plurality of microreactors 2 arranged in series using a relatively inexpensive pump.

  Although the embodiments of the present invention have been described above, the present invention is not limited to the above-described embodiments, and various modifications can be made.

  In the first to third embodiments, if the control of the difference between the first pressure and the second pressure by the control unit 12 is performed when supplying the chemical liquid to the inside of the microreactor, the chemical microreactor 2 may be performed just before the introduction to 2, at the time of introduction, or at the time of continuous supply.

  When a plurality of microreactors 2 are connected in series as in the liquid processing apparatus shown in FIG. 14, depending on the design of the liquid processing apparatus, the connection pipe 92 may be omitted and the microreactors 2 may be connected almost directly. . For example, as shown in FIG. 18, the introduction port of another microreactor 2 is directly connected to the discharge port of one microreactor 2 using a dedicated connector, and a plurality of microreactors 2 are connected to each other to form one microreactor group. It may be 20. In this case, the supply pipe 31 is connected to the introduction port of the most upstream microreactor 2 and the discharge pipe 41 is connected to the discharge port of the most downstream microreactor 2 to constitute a liquid processing apparatus. Here, when a tube is provided between two microreactors 2 adjacent to each other, depending on the type of treatment for the chemical solution, heat insulation is provided to prevent a temperature drop of the chemical solution due to heat dissipation in the tube. Although necessary, in the microreactor group 20 shown in FIG. 18, a tube between the microreactors 2 can be omitted, and a compact liquid processing apparatus can be realized.

  In the third embodiment, two processing units 13a are connected in series. However, in the liquid processing apparatus, three or more processing units 13a may be connected in series. In this case, in two processing units adjacent to each other among the three or more processing units, the liquid feed pump 32 connected to the supply pipe 31 of the downstream processing unit is connected to the discharge pipe 41 of the upstream processing unit. Thus, the suction pump 46 (or the decompression pump 43) is separately connected to the discharge pipe 41 of the most downstream processing unit 13b.

  Further, in the liquid processing apparatus in the above embodiment, a plurality of reactor temperature adjustment units 62 are provided for one microreactor 2, and a plurality of portions of the microreactor 2 are adjusted to different temperatures by the plurality of reactor temperature adjustment units 62, respectively. May be.

  The liquid processing apparatus in the first to third embodiments can be used for various purposes. For example, a liquid processing apparatus using a microreactor used for mixing two kinds of liquids can be used for a mixer portion of a fluid analysis instrument. Of course, by using a microreactor provided with three or more inlets, the liquid processing apparatus may be used for mixing and reaction of three or more kinds of fluids. The liquid processing apparatus can also be used for a fuel cell. When used as a fuel cell, the microreactor is formed with two fine channels facing each other with a functional membrane such as an ion exchange membrane interposed therebetween.

It is a figure which shows the structure of the liquid processing apparatus which concerns on 1st Embodiment. It is a top view which shows a microreactor. It is a longitudinal cross-sectional view which shows the structure of a microreactor vicinity. It is a figure which shows the flow of the operation | movement which flows a chemical | medical solution to a microreactor and performs a process to a chemical | medical solution. It is a figure which shows the structure of the apparatus for experiment. It is a figure which shows the relationship between the arrival time with respect to target air pressure, and the bubble size. It is a figure which shows a mode that light is irradiated to a microchannel. It is a figure which shows a mode that light is irradiated to a microchannel. It is a figure which shows the other example of a liquid processing apparatus. It is a figure which shows the further another example of a liquid processing apparatus. It is a figure which shows the further another example of a liquid processing apparatus. It is a figure which shows the further another example of a liquid processing apparatus. It is a figure which shows the change of a 1st pressure and a 2nd pressure. It is a figure which shows the change of a 1st pressure and a 2nd pressure. It is a figure which shows the further another example of a liquid processing apparatus. It is a figure which shows the further another example of a liquid processing apparatus. It is a figure which shows a part of structure of the liquid processing apparatus which concerns on 2nd Embodiment. It is a figure which shows a part of structure of the liquid processing apparatus which concerns on 3rd Embodiment. It is a figure which shows a mode that microreactors are connected.

Explanation of symbols

DESCRIPTION OF SYMBOLS 1 Liquid processing apparatus 2,2a-2d Microreactor 12 Control part 13,13a, 13b Processing unit 21 Inlet 22 Outlet 23 Fine flow path 31 Supply pipe 32 Liquid feed pump 33 Chemical liquid supply tank 34 Deaeration module 35 Flow rate adjustment part 36 Liquid feeding mechanism 38 Liquid temperature adjustment part 41 Discharge pipe 43 Decompression pump 44 Product storage tank 46 Suction pump 51 First pressure gauge 52 Second pressure gauge 61 Vibration applying part 62, 62a to 62c Reactor temperature adjustment part 63 Light irradiation part 311 Valve 411 Flow meter 412 Branch 413 Switching valve S15, S16 Step

Claims (18)

A liquid processing apparatus for processing a liquid by flowing a predetermined liquid through a flow channel structure,
A flow path structure in which a fine flow path from the inlet to the outlet is formed,
A supply pipe connected to the inlet;
A liquid feeding mechanism for supplying a predetermined liquid to the flow path structure via the supply pipe;
A discharge pipe connected to the discharge port;
A pressure reducing mechanism connected to the discharge pipe;
A first pressure gauge for obtaining a first pressure of fluid in the supply pipe;
A second pressure gauge for obtaining a second pressure of the fluid at the outlet;
A controller that controls a difference between the first pressure and the second pressure by drivingly controlling the liquid feeding mechanism and / or the pressure reducing mechanism when supplying the liquid into the flow path structure; ,
A liquid processing apparatus comprising: The liquid processing apparatus according to claim 1,
The control unit maintains a difference between the first pressure and the second pressure below a pressure difference at which bubbles are generated inside the liquid when the liquid is introduced into the flow path structure. A liquid processing apparatus. The liquid processing apparatus according to claim 2,
The pressure difference between the first pressure and the second pressure is the pressure difference at which bubbles are generated inside the liquid until the control unit completes the introduction from just before the liquid is introduced into the flow path structure. A liquid processing apparatus, characterized by being maintained below. A liquid processing apparatus according to any one of claims 1 to 3,
A valve is provided in the supply pipe;
In the closed state in which the valve is closed before liquid passes through the valve, the first pressure gauge acquires the gas pressure on the liquid feeding mechanism side of the valve as the first pressure,
The control unit introduces a liquid to a position between the first pressure gauge and the liquid feeding mechanism in the supply pipe in advance, and drives the pressure reducing mechanism in the closed state, whereby the second A liquid processing apparatus, wherein the pressure is lower than the first pressure, and then the valve is opened to depressurize the liquid feeding mechanism side of the valve and activate the liquid feeding mechanism. The liquid processing apparatus according to claim 4,
The liquid processing apparatus, wherein a difference between the first pressure and the second pressure immediately before the valve is opened from the closed state is 0.9 atm or less. The liquid processing apparatus according to claim 5,
2. A liquid processing apparatus according to claim 1, wherein the pressure reduction in the vicinity of the interface of the tip of the liquid in the supply pipe is completed within 2 seconds after the opening of the valve. A liquid processing apparatus according to any one of claims 1 to 6,
The liquid processing apparatus according to claim 1, further comprising a degassing module for degassing the liquid on the liquid feeding mechanism side of the first pressure gauge. A liquid processing apparatus according to any one of claims 1 to 7,
A liquid supply tank for storing liquid before being supplied to the flow path structure by the liquid feeding mechanism;
A liquid temperature adjusting unit that lowers the temperature of the liquid flowing into the flow path structure when the liquid is introduced into the flow path structure, than the temperature of the liquid in the liquid supply tank;
A liquid processing apparatus further comprising: A liquid processing apparatus according to any one of claims 1 to 8,
A liquid processing apparatus, further comprising a flow rate adjusting unit that adjusts a flow rate of the liquid flowing into the flow path structure. A liquid processing apparatus according to any one of claims 1 to 9,
A liquid processing apparatus, further comprising: a vibration applying unit that applies vibration to the flow channel structure when the liquid is supplied into the flow channel structure. A liquid processing apparatus according to any one of claims 1 to 10,
A liquid processing apparatus, further comprising a structure temperature adjusting unit that adjusts a temperature of the flow path structure. A liquid processing apparatus according to any one of claims 1 to 11,
A light irradiating unit for irradiating light to the flow channel structure;
In at least a part of the flow channel structure, light from the light irradiation unit is guided to the internal micro flow channel. A liquid processing apparatus according to any one of claims 1 to 12,
The liquid processing apparatus, wherein the pressure reducing mechanism is a pump capable of sucking both gas and liquid. A liquid processing apparatus according to any one of claims 1 to 12,
A liquid detector that detects the outflow of liquid from the flow path structure to the discharge pipe;
A liquid storage tank for storing the liquid discharged from the discharge pipe;
Further comprising
The discharge pipe is
A branch path that branches from the detection position by the liquid detection unit on the liquid storage tank side and is connected to the decompression mechanism;
A switching valve that switches between a path from the discharge port to the pressure reducing mechanism and a path from the discharge port to the liquid storage tank;
Have
The liquid processing apparatus, wherein the control unit controls the switching valve to guide the liquid to the liquid storage tank immediately after the liquid detection unit detects the outflow of the liquid. The liquid processing apparatus according to claim 1,
Each includes a plurality of processing units including the flow channel structure, the supply pipe, the discharge pipe, the first pressure gauge, and the second pressure gauge,
A plurality of supply pipes of the plurality of processing units are combined and connected to the liquid feeding mechanism, and a plurality of discharge pipes of the plurality of processing units are combined and connected to the pressure reducing mechanism. apparatus. The liquid processing apparatus according to claim 1,
Each includes a plurality of processing units including the liquid feeding mechanism, the flow channel structure, the supply pipe, the discharge pipe, the first pressure gauge, and the second pressure gauge,
The plurality of processing units are connected in series, and in two adjacent processing units, the liquid feeding mechanism connected to the supply pipe of the downstream processing unit is connected to the discharge pipe of the upstream processing unit. The liquid processing apparatus according to claim 1, wherein the operation as the reduced pressure mechanism is performed, and the reduced pressure mechanism is separately connected to the discharge pipe of the most downstream processing unit. A liquid processing apparatus according to any one of claims 1 to 16,
The flow channel structure is a plurality of flow channel structures connected in series or in parallel,
The liquid processing apparatus, wherein temperatures of the plurality of flow channel structures are individually adjusted. A flow channel structure in which a fine flow channel from the introduction port to the discharge port is formed, a supply pipe connected to the introduction port, and a predetermined liquid to the flow channel structure through the supply pipe A liquid feeding mechanism to supply, a discharge pipe connected to the discharge pipe, a pressure reducing mechanism connected to the discharge pipe, a first pressure gauge for obtaining a first pressure of fluid in the supply pipe, and the discharge pipe And a second pressure gauge for acquiring a second pressure of the fluid in the liquid processing apparatus, the liquid supply method for supplying the liquid into the flow path structure,
Delivering liquid into the flow channel structure;
Controlling the difference between the first pressure and the second pressure by driving and controlling the liquid feeding mechanism and / or the pressure reducing mechanism substantially parallel to the step of delivering the liquid;
A liquid supply method comprising:

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