JP2007113433A - Plunger pump system - Google Patents

Abstract

<P>PROBLEM TO BE SOLVED: To provide a plunger pump system capable of stable continuous operation while performing highly-accurate flow control by inhibiting pulsations. <P>SOLUTION: The plunger pump system 1 comprises a pair of plunger pumps 10, each of which has an individual drive 19 and which are connected in parallel between a liquid source 38 and a micro reactor 2 flow path, a flow mater 46 disposed in the micro reactor flow path, and a control unit 28 for alternately operating the pair of plunger pumps 10 for discharge at a predetermined constant feed speed. The control unit 28 adjusts the feed speed at predetermined timing based on a measurement value of the flow meter 46 when the plunger pump 10 is operated for discharge. <P>COPYRIGHT: (C)2007,JPO&INPIT

Description

  The present invention relates to a plunger pump device for feeding liquid to, for example, a microreactor.

  In recent years, a microreactor has been developed as a fluid reaction apparatus for reacting a liquid such as a reagent. In this microreactor, usually two kinds of liquids are passed through a micro flow channel to mix and react with each other. As the inner diameter of the flow path becomes smaller, the Reynolds number becomes smaller and the liquid flow becomes laminar. In order to rapidly mix the liquid in the laminar flow region, it is effective to make the inner diameter of the flow path as small as possible. This is because in the laminar flow region, molecular diffusion becomes a rate-limiting factor, and the liquid diffusion time is proportional to the square of the width of the flow path.

  In the laminar flow region, if there is a liquid concentration difference in the flow direction of the flow path, the liquid will be mixed non-uniformly. If the mixing of the liquid becomes uneven, the substance produced by the reaction further reacts with the stock solution to produce a by-product, resulting in a decrease in yield. Therefore, as a liquid feeding means for keeping the flow rate of each liquid before mixing constant, for example, a flow meter and a flow regulating valve are provided in the flow path before the chemical liquid sent out by the pressure generator enters the mixer, and the flow meter signal Thus, measures such as adjusting the valve opening to control the flow rate have been adopted.

  On the other hand, a positive displacement plunger pump is used to feed a microreactor at a high pressure. In such a positive displacement pump, a valve is not provided in the middle of the flow path, but is controlled by changing the discharge rate by changing the feed rate of the plunger. In such a case, a method of measuring the flow rate with a flow meter and performing feedback control as in the past can be considered. However, considering the accuracy and response speed of the flow meter, rough control has to be performed. In particular, since one plunger pump is intermittently operated, two units are installed in parallel and are operated by switching alternately, but flow rate fluctuation and pulsation are likely to occur at the time of switching.

  The present invention has been made in view of the above circumstances, and an object of the present invention is to provide a plunger pump device capable of stable continuous operation while performing high-precision flow rate control by suppressing pulsation.

  In order to achieve the above object, the plunger pump device according to claim 1, each having a separate driving device, a pair of plunger pumps connected in parallel between a liquid source and a microreactor flow path, and the microreactor flow A flow meter installed in the path and a control unit that alternately discharges the pair of plunger pumps at a constant predetermined feed rate, and the control unit performs the flow rate when the plunger pump is discharging. The feed rate is adjusted at a predetermined timing based on the measured value of the meter.

  In the invention according to claim 1, since the feed rate is adjusted at a predetermined timing based on the measured value of the flow meter when the plunger pump is discharging, without using complicated control means, The accuracy of the discharge amount of the plunger pump can be maintained. It is desirable to obtain the measured value by the flow meter as an average value for a predetermined time. The plunger pump may be adjusted individually, and in that case, the measurement is also performed individually.

According to a second aspect of the present invention, the plunger pump device according to the first aspect of the present invention includes a pressure sensor installed in the microreactor flow path, and the control unit performs the feeding based on an output value of the pressure sensor. It is characterized by finely adjusting the speed.
In the invention described in claim 2, since the feed rate is finely adjusted based on the output value of the pressure sensor installed in the microreactor flow path, pulsation due to various causes is suppressed.

According to a third aspect of the present invention, in the plunger pump device according to the first or second aspect, the controller controls the pair of plunger pumps to increase and decrease the speed of the pair of plunger pumps at the initial stage and the final stage, respectively. A process is performed, and one acceleration process and the other deceleration process are overlapped with each other, and the flow rate is switched and controlled.
In the invention according to claim 3, the transition from one plunger pump to the other plunger pump is performed while the flow rate is kept constant.

  According to a fourth aspect of the present invention, the plunger pump device according to the third aspect of the invention is characterized in that the feed rate is finely adjusted only for one plunger pump during the switching control.

According to a fifth aspect of the present invention, in the invention according to any one of the first to fourth aspects, the control unit is configured so that the plunger pump performs a fixed stopping process between the forward movement and the backward movement. It is characterized by controlling.
In the invention according to claim 5, since each plunger pump performs a fixed stopping process between the forward movement and the backward movement, the next operation is started after the flow in each plunger pump and the valve operation are stabilized.

  A plunger pump device according to a sixth aspect of the present invention is the invention according to any one of the first to fifth aspects, further comprising a position sensor that detects a position of the plunger of the plunger pump, and the control unit includes a position sensor of the position sensor. The feed rate is controlled based on the output.

  According to the plunger pump device according to any one of claims 1 to 6, a plunger pump device capable of stable continuous operation while performing high-precision flow rate control by suppressing pulsation without using complicated control means. Can be provided.

Embodiments of the present invention will be described below with reference to the drawings.
FIG. 1 is a diagram showing a dual plunger pump device according to an embodiment of the present invention, and is used for the purpose of, for example, discharging a chemical solution continuously to a microreactor at a constant flow rate. The plunger pump device 1 is composed of a pair of plunger pumps 10 having the same structure. Each plunger pump 10 includes a cylinder 12, a plunger 14 slidably provided in the cylinder 12, a drive device 19 that reciprocates them, and a control unit 28 that controls each part.

  Each plunger 14 is constituted by a disk-like piston 16 and a rod 18 connected thereto, and a pump chamber 17 is formed between the end portions. The rod 18 is connected to the drive device 19 through the end wall. In this embodiment, the drive device 19 has a feed screw 22 that is rotationally driven by a motor 20 and a nut 24 that is screwed to the feed screw 22, and the nut 24 is fixed to the end of the rod 18. A ball (bearing) is interposed between the feed screw 22 and the nut 24 to constitute a smooth and highly accurate linear motion mechanism called a ball screw. Further, a linear scale (position sensor) 26 for detecting the position of the nut 24 is provided, and its output is sent to the control unit 28. The control unit 28 feedback-controls the rotation of the motor 20 based on this output, and can accurately control the position and feed rate of the plunger 14.

  A seal structure is provided between the piston 16 and the inner wall of the cylinder 12. A discharge port 30 and a suction port 32 are provided on the end wall of the pump chamber 17, and these are connected to a supply line 40 connected to a discharge line 36 or a fluid tank 38 via a check valve 34, respectively. Thereby, fluid such as a chemical solution is sucked into the pump chamber from the suction port 32 by the backward movement of the plunger 14 (moving left in FIG. 1), and discharged by the forward movement of the plunger 14 (moving right in FIG. 1). It is discharged from the port 30. The material of the wetted part including the plunger 14 is preferably compatible with a corrosive or erosive chemical solution, for example, sapphire, ruby, alumina, ceramic, SUS, hastelloy, titanium. Etc. are used as appropriate.

  As shown in FIG. 2, the discharge ports 30 of the two plunger pumps 10 merge and are connected to the raw material receiving port 42 of the microreactor 2. In the microreactor 2, two raw material receiving ports 42 are provided, and these join at the mixing / reaction unit 50 via the introduction flow path 44. The introduction flow path 44 is provided with a flow meter 46 and a pressure sensor 48, respectively, and these outputs are input to the control unit 28 and used for control as described later. In FIG. 2, the control unit 28 is provided for each plunger pump device 1, but of course, one control unit 28 may be shared. Further, these control units 28 may be connected to the control device of the microreactor 2 for integrated control.

Hereinafter, the operation of the plunger pump device 1 having such a configuration will be described. The control unit 28 uses a combination of two control methods, that is, pattern control for controlling the plunger pump 10 along a predetermined pattern, and feedback control for controlling the plunger pump 10 based on the measured value of the sensor. Each of these controls the feed speed of the plunger 14, but basically the pattern control is subordinate and the feedback control is subordinate. Describing this conceptually, the overall control function F is represented by a pattern control function F1 (t) that is a function of time t and a feedback control function F2 (p) that is a function of measured pressure p.
F = F1 (t) {1 + F2 (p)} (Formula 1)
It is represented by That is, when there is no pressure fluctuation, only pattern control of F = F1 (t) is performed, and when there is a pressure fluctuation, it fluctuates at a ratio of F2 (p). How much F2 (p) contributes is determined by how the function is set, for example, it is preferably about 10% at the maximum.

  3 and 4 explain pattern control. FIG. 3 shows the operation of each plunger pump 10, and line A is a velocity diagram when the plunger 14 reciprocates once. The horizontal axis represents time as 360 degrees per cycle, and the vertical axis represents the speed of the plunger 14 (+ is the forward direction and − is the backward direction). Since the discharge amount is proportional to the speed of the plunger 14, the vertical axis also represents the discharge amount. A line B represents a change in volume of the pump chamber 17. FIG. 4 shows a state in which the two plunger pumps 10 are operating with a phase shifted by 180 degrees.

  As can be seen from these drawings, the two plunger pumps 10 are operated in an overlapping manner so that one of the two pumps 10 performs the speed increasing process and the other performs the speed reducing process at the beginning and the end of the discharge process. Thereby, in this switching process, the plunger pump 10 that performs the discharge operation is switched while the total flow rate is controlled to be constant. A short stop process is provided after the discharge operation and the suction operation of each plunger pump 10. Accordingly, after the check valve 34, 36 of the discharge port 30 or the suction port 32 is securely closed or the flow at this portion is settled, the next suction or discharge operation starts. Pulsation due to backflow or the like from the valves 34 and 36 is prevented.

In this pattern control, the steady feed speed Vc at the time of discharge is determined based on the required discharge amount and the following equation, and thereby the initial pattern function P (t) is set.
Flow rate L = Plunger cross-sectional area S x Plunger feed speed V (Formula 2)
However, the actual machine may differ from the calculation and may change with time. Therefore, an operation of adjusting the set value with the actually measured value is performed. This is not performed constantly but at an appropriate timing and frequency. This is because even if the feedback control is steadily performed, there is no effect because the response speed of the flow sensor is low, and due to the characteristics of the plunger 14, a timely adjustment is considered sufficient. Although timing and frequency are arbitrary, for example, it is performed at start-up, performed every time a certain operation time elapses, or a combination thereof.

  This adjustment process will be described with reference to the flowchart of FIG. 5 and the graph showing the change of each measured value in FIG. 6A shows an example of the change in the measured value of the flow meter 46 installed in the microreactor 2 flow path, FIG. 6B shows an example of the change in the output value of the pressure sensor 48, and FIG. 6C shows the plunger 14 One example of the change in the feed speed is shown.

  First, the control unit 28 determines whether it is the timing of the adjustment work (step 1). This is performed, for example, by detecting the presence or absence of the command signal at the time of starting, or by detecting the presence or absence of a signal that informs the operation from the timer for a predetermined time. At that timing, first, the flow rate when only the first plunger pump 10 is discharging is measured (step 2). Here, an average flow rate for a predetermined time is calculated, not an instantaneous flow rate at a certain point in time. You may make it use the average value of the flow volume of one pump in several cycles instead of one cycle.

Next, a difference ΔL between the measured flow rate and the specified flow rate is calculated, and it is determined whether or not this is larger than a preset allowable upper limit value (step 3). As shown in FIG. 6A, if it is larger than the set upper limit value, the feed rate adjustment amount is calculated (step 4), and the adjustment is made based on the calculated value (step 5). Calculation of the adjustment amount ΔV uses the following expression based on Expression 2.
Feed rate adjustment amount ΔV = flow rate difference ΔL / plunger cross-sectional area S (Formula 3)

  If ΔL is smaller than the allowable upper limit value in step 3, no adjustment is performed. Next, the measurement or adjustment operation is performed in the same manner for the second pump (steps 6 to 9), and the adjustment operation is completed. In this way, a new steady feed speed Vc is determined, and a new pattern function P (t) in which the gradient of the switching process is adjusted is determined along with this. Thereby, an accurate flow rate output in an actual machine can be achieved by a simple control method.

  In this embodiment, since adjustment is performed for each plunger pump 10, even when there is a difference in the characteristics of the two plunger pumps 10 and the flow paths, it is possible to always perform liquid feeding with no flow rate fluctuation. In addition, when there is no difference for every plunger pump 10, you may make it control two by the same pattern function. In this case, step 6 to step 9 are omitted. In step 2, it is preferable that the flow rates of the discharge operations of the two pumps are measured and averaged to obtain a measured value.

Next, the case where the feed rate is feedback controlled based on the measurement value of the pressure sensor 48 installed in the flow path of the microreactor 2 will be described with reference to FIGS. This is done by setting the control function for the overall feed rate as shown in Equation 1 below.
F = F1 (t) {1 + F2 (p)} (Formula 1)
The actual form of F (p) can be obtained, for example, by obtaining a PID control coefficient by using both experiments and theoretical analysis.

  The pressure varies depending on the length and shape of the flow path, but the pressure is constant if a constant flow rate is maintained. For this reason, since the change in pressure represents the flow rate fluctuation in the flow path, the flow rate fluctuation can be suppressed by feedback-controlling this. Further, since the response of the pressure sensor 48 is faster and more accurate than the general flow meter 46, it is suitable for suppressing fluctuations in the flow rate. In the switching process in which the two pumps operate, the control function of each pump is different in that one of P (t) is increased and the other is decreased, so that the total flow rate is maintained. The meaning of is the same.

  In the plunger pump device 1 of this embodiment, the pulsation generated when the feed of the plunger 14 is shifted due to a mechanical error, gas is mixed in the fluid, or the check valve operation becomes unstable is canceled. It is possible to control the discharge amount. For example, in FIG. 6B, the case 1 shows pressure fluctuation during steady feeding, and the case 2 shows pressure fluctuation during steady feeding, respectively, and this is detected and the feed speed is as shown in FIG. By performing feedback control, pressure fluctuations are suppressed, and fluctuations in the discharge amount are also suppressed as shown in FIG.

  In the above-described embodiment, as shown in FIG. 7A, the pressure sensor 48 is always used in both the steady discharge process in which one unit discharges and the switching process in which two units discharge. However, when the same control is simultaneously performed on the two plungers, there may be a problem that the control becomes unstable. Therefore, as shown in FIG. 7B, in the switching process, pressure feedback control may be performed on only one of the pumps. In this example, the pressure feedback control is performed for the pump in the speed increasing process in the switching process, but the reverse may be possible. Further, as shown in FIG. 7C, pressure feedback control may be performed only for the pump having the larger discharge amount.

  Next, a fluid reaction device (microreactor 2) incorporating the above-described double plunger pump device according to an embodiment of the present invention will be described. FIG. 8 to FIG. 10B are diagrams showing the overall configuration of this fluid reaction apparatus. The fluid reaction apparatus described below is an apparatus used for mixing and reacting two or more kinds of liquids.

  As shown in FIG. 8, FIG. 9, FIG. 10 (a), and FIG. 10 (b), the entire fluid reaction device is installed in one installation space and packaged. In this configuration example, the installation space is rectangular and is divided into four regions along the longitudinal direction. That is, the first region on one end side is the raw material storage unit 101 in which a plurality of storage containers 110 for storing the raw material liquid (only two storage containers 110A and 110B are shown in FIG. 8) are installed, and are adjacent thereto. The second region is a liquid distribution unit 102 in which double plunger pump devices 1A and 1B for transferring the raw material liquid in the storage container 110 are installed. A third region adjacent to the second region is a processing unit 103 having a mixing unit (mixing chip) 140 that mixes the raw material liquid and a reaction unit (reaction chip) 142 that reacts the mixed raw material liquid. . The fourth region on the other end side is a product storage unit (recovery container installation space) 104 for deriving and storing a product obtained as a result of the processing.

  In addition, the fluid reaction apparatus includes an operation control unit 106 that is a computer that controls the operation of each unit, and a heat medium controller 107 that adjusts the temperature of the processing unit 103 by flowing a heat medium through the temperature adjustment case 146. . Further, as shown in FIG. 8, the operation control unit 106 is equipped with a flow rate monitor 270 and a temperature monitor 272 that can monitor the flow rate and temperature of the liquid. In this configuration example, the operation control unit 106 and the heat medium controller 107 are separated from the fluid reaction device, but may be integrated as a matter of course. As shown in FIG. 9, a piping chamber 105 is formed in the lower floor portion of the second to fourth regions, where piping for sending a heating medium for heating or cooling to the mixing unit 140 and the reaction unit 142 is provided. Is provided. The operation control unit 106 and the control unit 28 of the plunger pump device 1 are separate, but may be integrated.

  In this way, by arranging the respective parts from the upstream side to the downstream side, the flow of the liquid can be made smooth, and the entire apparatus can be made compact. In this configuration example, each part is arranged in a straight line. However, for example, if the entire space is close to a square, each part may be configured such that the liquid flow forms a loop.

  In FIG. 9, reference numeral 250 denotes a liquid reservoir pan provided at the lower part of the apparatus, and reference numeral 252 denotes a liquid leakage sensor installed on the liquid reservoir pan 250. In this example of the apparatus, the liquid distribution unit 102, the processing unit 103, and the product storage unit 104 are partitioned by partition walls 254 and 256, and covers 258, 260, and 262 are attached to the respective parts to isolate them from the outside of the apparatus. is doing. Reference numeral 264 denotes an exhaust port, which is connected to an exhaust fan (not shown). And the toxic gas in the apparatus is prevented from leaking outside by making the pressure in the apparatus negative from the outside of the apparatus.

  Although the two storage containers 110A and 110B are installed in the raw material storage unit 101 shown in FIG. 8, three or more storage containers may be used as necessary. For example, the process can be continuously performed by storing the same liquid in two storage containers and using them alternately. Note that the raw material storage unit 101 may be provided with a cleaning liquid container 112 containing an organic solvent such as acetone for line cleaning, hydrochloric acid, pure water, or the like, or a pressure source 114 filled with nitrogen gas for purging. Further, the waste liquid container 136 may be placed in the raw material storage unit 101.

  In the liquid distribution part (introduction part) 102, plunger pump devices 1A and 1B connected to the storage containers 110A and 110B via transport pipes 121A and 121B are installed. Further, the liquid distribution unit 102 includes flow rate adjusting devices 300A and 300B, relief valves 122A and 122B, pressure measurement sensors 124A and 124B, flow path switching valves 126A and 126B, which are arranged downstream of the plunger pump devices 1A and 1B, and A backwash pump 130 is provided. The flow path switching valves 126A and 126B are connected to the cleaning liquid container 112 and the pressure source 114 in addition to the transport pipes 121A and 121B, respectively. The backwash pump 130 is used when the inside of the flow path of the mixing unit 140 or the reaction unit 142 is blocked by a product. The backwash pump 130 is connected to the cleaning liquid container 112 that stores the cleaning liquid, and is further connected to the outlet of the reaction unit 142 via the flow path switching valve 132. The cleaning liquid transferred by the backwash pump 130 flows in the opposite direction to the normal flow. That is, the cleaning liquid flows from the outlet of the reaction unit 142 toward the inlet of the mixing unit 140, passes through the flow path switching valves 126 </ b> A and 126 </ b> B, and enters the waste liquid storage container 136 from the waste liquid port 134 through a pipe (not shown).

  The backwash pump 130 is preferably a single piston pump so that the discharge pressure is high and the product can be removed by causing pulsation in the cleaning liquid. As the cleaning liquid, an organic solvent, hydrochloric acid, nitric acid, phosphoric acid, organic acid, pure water, or the like is preferably used. Examples of the organic solvent include acetone, ethanol, methanol and the like. An introduction port 240 shown in FIG. 8 is provided when pure water or hydrogen water is introduced from the outside, and can be used for cleaning instead of the cleaning liquid in the cleaning liquid container 112.

  FIG. 11 shows a mixing unit 140 for performing preheating (preliminary temperature adjustment) and mixing of the raw material liquid. The upper plate 144a, the middle plate 144b, and the lower plate 144c, which are three thin plate-like base materials, are shown. The mixing portion 140 having a total thickness of 5 mm is formed by bonding. In addition, all the flow paths described below are grooves formed on the surface of the intermediate plate 144b. The two inflow ports 147A and 147B formed through the upper plate 144a communicate with the two preheating channels 148A and 148B formed on the upper surface of the middle plate 144b, respectively. These preheating flow paths 148A and 148B each branch in the middle and expand, and merge again. Further, the preheating channels 148A and 148B communicate with the outlet channels 150A and 150B, respectively, and these outlet channels 150A and 150B communicate with the junction 152. The outlet channel 150A is formed on the upper surface of the middle plate 144b, and the outlet channel 150B is formed on the lower surface of the middle plate 144b.

  FIG. 12 is an enlarged view of the junction shown in FIG. As shown in FIG. 12, the merging portion 152 includes header portions 154 and 155 formed on the upper and lower surfaces of the intermediate plate 144b as arc-shaped grooves communicating with the outlet flow paths 150A and 150B, and the header portions 154 and 155, respectively. It has a plurality of liquid separation channels 156 and 157 extending toward the center of the arc, and a merge space 158 where these liquid separation channels 156 and 157 merge. The liquid separation channels 156 and 157 and the merge space 158 are formed on the upper surface of the intermediate plate 144b, and the liquid separation channels 156 and 157 are alternately arranged. The header portion 155 on the lower surface side and the liquid separation channel 157 communicate with each other through a communication hole 157a penetrating the intermediate plate 144b. The merge space 158 is formed so that the width gradually decreases toward the downstream side, and communicates with an outflow port 160 formed through the middle plate 144b and the lower plate 144c.

  In the example shown in FIG. 12, five separation channels 156 and four separation channels 157 are alternately arranged on the opening surface 159 on the inlet side of the merge space 158. The two types of liquids respectively flowing out from the separation flow paths 156, 157 flow downstream while forming a striped flow in the merge space 158, and are forced as the flow path width of the merge space 158 gradually decreases. Both liquids are mixed. In this example, the flow path width of the merge space 158 finally reaches 40 μm. If the processing technology accuracy is increased, the flow path width can be reduced to 10 μm.

  13A is a plan view showing the reaction part shown in FIG. 8, and FIG. 13B is a cross-sectional view of the reaction part shown in FIG. 13A. In this example, two base materials 144d and 144e are joined to form a reaction portion 142 having a thickness of 5 mm. In this reaction part 142, the reaction flow path 162 meanders, and provides a long flow path efficiently. The reaction channel 162 has connecting portions 162a and 162c connected to the inlet port 164 and the outlet port 165, and a meandering portion 162b connected to the connecting portions 162a and 162c. The width of the connecting portions 162a and 162c is narrow. The width of the meandering portion 162b is wide. Accordingly, the liquid flows rapidly at the entrance / exit portion to prevent adhesion of by-products, and flows slowly at the meandering portion 162b so that the heating and reaction time can be increased.

FIG. 14A and FIG. 14B show another example of the structure of the reaction section having a portion 163a in which the width of the reaction channel gradually decreases and a portion 163b in which the width gradually increases. In the reaction portion 142a, a reaction channel 163 is formed between the base materials 144d and 144e so that the width dimension increases or decreases in the range from the maximum a to the minimum b. The depth may be increased or decreased according to the increase or decrease of the width dimension.
In this example, the depth changes from the maximum c to the minimum d so that the cross-sectional area of the reaction channel 163 is constant.

  FIG. 14C is a cross-sectional view showing another configuration example of the reaction channel. In the reaction section 142b, the reaction channel 163c has a flat shape whose width e is larger than the depth f, and has a wide heat transfer surface intersecting the heat transfer direction (indicated by an arrow) from the thermal catalyst. Therefore, heat is effectively transmitted to the liquid in the reaction channel 163c. In addition, it is effective in order to accelerate | stimulate reaction to arrange | position an appropriate catalyst in the confluence | merging space 158 and the reaction flow paths 162,163. Such a catalyst is selected depending on the type of reaction. As for the arrangement method, for example, it can be applied to the inner surface of the channel, or can be arranged as an obstacle of the channel as described later.

  As a material for forming at least the flow path of the mixing unit 140 and the reaction unit 142, for example, SUS316, SUS304, Ti, quartz glass, Pyrex (registered trademark) glass or other hard glass, PEEK (polyetheretherketone), PE (polyethylene), Among PVC (polyvinylchloride), PDMS (Polydimethylsiloxane), Si, PTFE (polytetrafluoroethylene), and PCTFE (PolyChloroTriFluoroEthylene), a preferable one is selected in consideration of chemical resistance, pressure resistance, thermal conductivity, heat resistance, and the like. The material of the wetted part of the mixing part 140 and the reaction part 142 is preferably one that has little elution from the surface, can be modified with a surface catalyst, has a certain degree of chemical resistance, and can withstand a wide temperature range of −40 to 150 ° C. .

  FIG. 15 is a perspective view showing a configuration of a temperature adjustment case for adjusting the temperatures of the mixing unit and the reaction unit. In the following description, only the temperature adjustment case 146 for adjusting the temperature of the reaction unit 142 will be described, but the temperature adjustment case 146 for the mixing unit 140 has the same configuration, and redundant description thereof is omitted. To do. The temperature adjustment case 146 includes a case main body 172 in which a space 170 that accommodates the reaction portion 142 is formed, and a lid portion 174 that covers the space 170. Grooves 176 constituting the medium flow path are formed. A liquid supply path 178 and a drainage path 180 (see FIG. 8) communicating with the groove 176 are formed in the case main body 172. These liquid supply path 178 and the drainage path 180 are connected to the heat medium controller 107, respectively. Yes. The liquid supply path 178 communicates with the groove 176 of the lid portion 174 via the opening 179, and the drainage path 180 also communicates with the groove 176 of the lid portion 174 via an opening (not shown). In this example, the heat medium flowing through the groove 176 directly contacts the front and back surfaces of the reaction unit 142, and the reaction unit 142 is heated (or cooled) in a state of being completely accommodated in the temperature adjustment case 146.

  Although not shown, the heat medium controller 107 incorporates a control mechanism for controlling the temperature of the heat medium and a pump for transferring the heat medium. As shown in FIG. 8, the heat medium is supplied to the temperature adjustment case 146 of the mixing unit 140 and the reaction unit 142 after passing through the heat exchanger 182. The heat exchanger 182 can change the temperature of the heat medium supplied to the mixing unit 140 and the reaction unit 142 independently by changing the amount of city water for cooling, for example.

  16 (a) to 16 (d) show other examples of the temperature adjustment case 146. Here, the heat medium flow path 192 is formed inside each of the case main body 172 and the lid portion 174. FIG. Has been. As shown in FIG. 16 (c), the liquid supply path 178 has a double pipe configuration in which the tip of the liquid supply pipe 188 is inserted, and communicates with the heat medium flow path 192 through a thin communication path 190. is doing. The drainage side has the same configuration. As shown in FIG. 16 (b), the temperature adjustment case 146 that accommodates the mixing unit 140 and the temperature adjustment case 146 that accommodates the reaction unit 142 are stacked and coupled via a bolt 194, a nut 195, and a spacer 196. ing.

  FIG. 16B shows a path for supplying / discharging the liquid to / from the mixing unit 140 and the reaction unit 142 accommodated in the temperature adjustment case 146. That is, each liquid flows into and out of the mixing unit 140 through the flow passage 198 formed through the temperature adjustment case 146. In addition, the liquid is circulated between the mixing unit 140 and the reaction unit 142 through the communication passage 200 that communicates with the flow passage 198 of the temperature adjustment case 146. FIG. 16D illustrates the structure of the liquid inflow portion and the outflow portion of the reaction section 142. In order to direct the liquid flow downward, the liquid inlet of the mixing unit 140 and the reaction unit 142 is normally formed on the upper surface and the outlet is formed on the lower surface.

  As shown in FIG. 8, the outlet 202 of the reaction unit 142 is connected to the product storage unit 104 via a recovery pipe 204. In the product storage unit 104, a recovery container 208 is provided on the downstream side of the heat exchanger 206 for cooling and the flow path switching valve 132. The product storage unit 104 in which the recovery container 208 is placed is isolated so as not to be affected by temperature and the like from other regions, and to prevent toxic gas that may be generated from the product from leaking to the outside. .

  FIG. 17 shows another configuration example of the product storage unit 104, and a plurality of collection containers 208 are installed on the turntable 212. In this example, there are two collection containers 208, and the actuator 214 that moves the rotary table 212 is a 180-degree rotary actuator. Of course, the number of collection containers 208 and the types of actuators 214 can be selected as appropriate. The operation control unit 106 shown in FIG. 8 determines the replacement timing of the recovery container 208 based on a signal from the liquid level detection sensor 211b that detects the liquid level of the recovery container 208, and the flow path switching valve 132 (see FIG. 8). The liquid flow is stopped, the stop of the liquid flow is confirmed by the optical fluid detection sensor 211 a provided downstream of the recovery port 210, and the actuator 214 is operated to move the other recovery container 208 below the recovery port 210.

  Next, a process of reacting a liquid (raw material liquid) such as a chemical solution with the fluid reaction apparatus configured as described above will be described. Note that the operation of the fluid reaction apparatus is basically automatically controlled by the operation control unit 106. First, in the raw material storage part 101, it prepares in storage container 110A, 110B which stored the raw material liquid. The temperature of the heat medium is set by the heat medium controller 107, the amount of city water passing through the heat exchanger 182 is adjusted to adjust the temperature of each heat medium, and the temperature adjustment case 146 of the mixing unit 140 and the reaction unit 142 is adjusted. Heat medium is circulated to maintain a predetermined temperature. The temperature of the heat medium is measured by temperature sensors 216 and 218 provided at the inlet of the temperature adjustment case 146.

  In this example, before supplying the raw material liquid to the processing unit 103, a cleaning liquid such as pure water is supplied to the flow paths in the mixing unit 140 and the reaction unit 142 to perform cleaning in advance. While cleaning the flow path, the temperature of the cleaning liquid is measured by the temperature sensor 220 at the outlet of the mixing unit 140 and the temperature sensor 222 at the outlet of the reaction unit 142, and the temperature of the cleaning liquid is fed back to the heat medium controller 107. In this way, the mixing unit 140 and the reaction unit 142 are adjusted to a predetermined temperature.

  After the temperatures of the mixing section 140 and the reaction section 142 are adjusted and the cleaning of the flow path is completed, the flow path switching valve 132 is switched and the plunger pump devices 1A and 1B are driven to start the raw material liquid in the storage containers 110A and 110B. Each. The raw material liquid is adjusted to a predetermined flow rate by the flow rate adjusting devices 300 </ b> A and 300 </ b> B, and then reaches the recovery container 208 through the mixing unit 140, the reaction unit 142, the outlet port 202, and the recovery port 210. The flow path switching valve 132 is an automatic valve that is actuated by an actuator, and this operation can also be performed automatically.

  In the mixing unit 140, the raw material liquids are heated to a predetermined temperature in the preheating channels 148 </ b> A and 148 </ b> B (see FIG. 11), and then merged and mixed in the joining unit 152. At that time, as shown in FIG. 12, each liquid flows into the merge space 158 from the header portions 154 and 155 via the liquid separation channels 156 and 157. Since the cross section of the merge space 158 gradually decreases toward the downstream, micro-sized flows are mixed regularly and mixed rapidly according to Fick's law. In that state, when it flows into the reaction channel 162 of the reaction unit 142 maintained at a predetermined temperature, the reaction proceeds rapidly without being restricted by mass transfer or heat conduction. Therefore, it is sufficiently practical as a mass production means, and it is not necessary to carry out an explosive reaction with a high reaction rate at a low temperature. In this example, since the width of the reaction channel 162 is sufficiently wider than the width of the merge space 158, even when the reaction rate is low, the reaction can be performed over a sufficient amount of time, resulting in a high yield. Obtainable.

  The obtained product is sent from the outlet 202 of the reaction channel 162 to the heat exchanger 206 via the recovery pipe 204, cooled here, and flows into the recovery container 208 from the recovery port 210. When the storage containers 110A and 110B are emptied or the recovery container 208 is full, the operation control unit 106 stops the operation of the plunger pump devices 1A and 1B to end the processing. In this case, if an additional storage container is prepared in the raw material storage unit 101 in addition to the storage containers 110A and 110B, the flow path switching valves 126A and 126B can be switched to continuously operate without stopping. Processing is possible. In addition, when reaction takes time, it is also possible to carry out batch operation by confining the liquid in the mixing unit 140 and the reaction unit 142 for a certain period of time. Since the flow path switching valves 126A and 126B are also automatic valves, these operations can be automatically operated.

  As a method of batch operation, the plunger pump devices 1A and 1B may be temporarily stopped, or the flow switching valves 126A and 126B may be switched to stop the inflow of liquid into the processing unit 103. This eliminates the need to increase the length of the reaction channel 162 even when the reaction time of the liquid is long. In batch operation, it is preferable to perform operation control using a fullness detection means for detecting that the merge space 158 and / or the reaction flow path 162 is filled with liquid. For example, an optical fluid detection sensor as shown in FIG. 17 is used. Accordingly, when it is determined that the merge space 158 and / or the reaction channel 162 is filled with the liquid, the plunger pump devices 1A and 1B are stopped or the first channel switching valve is switched, and the liquid is set to the reaction end time. It is allowed to stay in the confluence space 158 and / or the reaction flow path 162 for a certain period of time.

  FIG. 18A and FIG. 18B show another configuration example of the merging unit in the mixing unit 140. The junction 152a is configured by disposing obstacles 224 over a predetermined distance L at a constant interval a in a Y-shaped junction space 158a. In this example, a columnar obstacle 224 having a diameter of 50 μm or less was arranged over L = 5 mm from the junction. As shown in FIG. 18B, the obstacles 224 are arranged in a staggered manner so that the adjacent obstacles 224 are shifted by half the pitch in the flow direction. As a result, the interface 125 of the liquid A and the liquid B meanders, so that the interface area (contact area) between the two liquids can be increased. In the merging portion 152b shown in FIG. 19, a row of obstacles 224 are arranged in a zigzag along the flow direction in the central portion of the merging space 158b, and the interface area can be similarly increased. This is suitable for use in the narrow merge space 158b.

  FIG. 20 shows another configuration example of the processing unit 103 of the fluid reaction device. In the processing unit 103 of FIG. 8, two systems R1 and R2 each having a combination of a mixing unit 140 and a reaction unit 142 are provided, and two types of flow path switching valves 126A and 126B of the liquid distribution unit 102 are used. The raw material liquid can be supplied to any of the systems R1 and R2. As described above, by using the two systems, the processing amount can be increased as necessary, but there are various other usage methods. For example, when the reaction product easily deposits solid particles and is easily clogged in the middle of the piping, one system is used as a spare. Further, the batch operation described above can be continuously performed by alternately switching the transfer lines by the flow path switching valves 126A and 126B. Of course, three or more transfer lines can be provided in parallel as appropriate. In this case, the flow path switching valves 126A and 126B can be automatically operated.

  FIG. 21 shows an example in which a plurality of reaction units are arranged in series in the processing unit 103. In this example, one mixing unit 140 and three reaction units 142a, 142b, and 142c are connected in series, and temperature sensors 220, 222a, 222b, and 222c are provided respectively. In this example, it is possible to independently control the temperatures of the reaction units 142a, 142b, 142c according to the stage of the reaction. This configuration is suitable for reactions that require a bold and instantaneous change in reaction time and reaction temperature, such as biochemical reactions. For example, in this system, the reaction can be performed at 100 ° C. in the reaction unit 142a and at −20 ° C. in the reaction unit 142b.

  FIG. 22 is an example in which a plurality of mixing units are provided in the processing unit 103. In this configuration example, a first mixing unit 140 and a reaction unit 142 for mixing and reacting liquid A and liquid B are provided, and a second mixing unit 140a is provided on the downstream side of the reaction unit 142. In the mixing section 140a, the third raw material liquid or the C liquid that is the reactant transported from the plunger pump 116C joins and mixes the A liquid and the B liquid. The temperatures of these two mixing units 140 and 140a and one reaction unit 142 are individually controlled. The liquid C may be a reaction terminator.

  In this configuration example, the in-line yield evaluator 226 is directly connected to the outlet 202 of the second mixing unit 140a. Thereby, the yield of the result of the chemical reaction can be confirmed in real time, and can be immediately fed back to the process parameters. The in-line yield evaluator 226 includes methods such as infrared spectroscopy, near infrared spectroscopy, and ultraviolet absorption as methods that can be measured without separating the object to be measured.

  In this configuration example, a separation and extraction unit 228 that separates unnecessary substances and necessary substances from the reaction product is further provided on the downstream side of the second mixing unit 140a. As illustrated, the separation and extraction unit 228 has a Y-shaped separation channel 234. The liquid from the second mixing unit 140a is branched into two flows by the separation channel 234, one in the channel formed by the hydrophobic wall 230 that allows only the hydrophobic molecules in the material to pass through, and the other in the material It flows into the flow path formed from the hydrophilic wall surface 232 that allows only the hydrophilic molecules inside to pass therethrough. The separated substances are recovered in the recovery containers 208 and 208a via the recovery pipes 204 and 204a, respectively. As the separation / extraction unit 228, it is possible to use a membrane or a porous frit that can adsorb only a hydrophobic substance.

  FIG. 23 shows a configuration example for continuous processing by repeating mixing / reaction and separation / extraction. That is, the mixing unit 140a that processes the liquid A and the liquid B, the reaction unit 142a, and the separation / extraction unit 228a are arranged on the upstream side, and the mixing unit 140b that processes the liquid extracted from the separation / extraction unit 228a and the liquid C The part 142b and the separation / extraction part 228b are arranged on the downstream side. Unnecessary substances after the liquid A and the liquid B react are discharged from the outlet 234a of the separation and extraction unit 228a, and unnecessary substances in the second reaction to which the liquid C is added are discharged from the discharge port 234b of the separation and extraction unit 228b. Be taken out of the system. Furthermore, a mixing unit 140c that mixes the liquid extracted from the separation / extraction unit 228b and the fourth liquid D is provided. Liquid D may be a reaction terminator or other raw material solution. An in-line yield evaluator 226 may be provided on the downstream side of the mixing unit 140c.

  FIG. 24A shows a configuration in which the respective parts in FIG. 23 are stacked. The liquid flows downward. The mixing unit 140a, the reaction unit 142a, the separation / extraction unit 228a, the mixing unit 140b, the reaction unit 142b, the separation / extraction unit 228b, and the mixing unit 140c are accommodated in the temperature adjustment case 146, respectively, and further, a bolt 194, a nut 195, and a spacer 196. Are stacked at a predetermined interval. The movement of the liquid between each part is performed via the communication path 200 (refer FIG.11 (b)). The accuracy of temperature control is improved by interposing air between each part so as not to be affected by the heat of other parts by utilizing the heat insulation of air. As shown in FIG. 24B, it is preferable to cover each temperature adjustment case 146 with a heat insulating material such as a clean silicon member 236 containing bubbles.

  The fluid introduced into the fluid reaction apparatus is liquid or gas, and the substance to be recovered is liquid, gas, solid or a mixture thereof. When the introduced substance is a solid such as powder, a powder dissolver can be installed in the raw material reservoir 101. FIG. 25 is a configuration example of the raw material reservoir 101 when one of the two raw material liquids is a solution in which powder is dissolved and the other is originally liquid. The raw material powder and the solvent are introduced from the raw material inlet 242 of the powder dissolver 240. In this example, the raw material powder is dissolved by heating by the heater 244 and stirring by the stirrer 246, and the generated raw material liquid is mixed by the plunger pump 116A from the pipe 249 drawn into the take-out port 148, and the mixing unit 140 and the reaction unit. 142 is sent.

It is a figure which shows the plunger pump apparatus of one Embodiment of this invention. It is a figure which shows the connection of a plunger pump apparatus and a microreactor. It is a graph which shows the pattern of the feed rate of one plunger pump. It is a graph which shows the pattern of the feed rate of the whole plunger pump apparatus. It is a flowchart explaining adjustment operation | movement of a feed rate. It is a graph explaining control of feed speed. It is a graph explaining the control action in other embodiments. It is a schematic diagram which shows the whole fluid reaction apparatus. It is a perspective view which shows the structure of the whole fluid reaction apparatus of FIG. FIG. 10A is a plan view showing the overall configuration of the fluid reaction apparatus of FIG. 8, and FIG. 10B is a front view. FIG. 11A is a plan view showing the configuration of the mixing section, and FIG. 11B is a cross-sectional view. It is a figure which expands and shows the confluence | merging part of a mixing part. FIG. 13A is a plan view showing the structure of the reaction section, and FIG. 13B is a cross-sectional view. 14A is a longitudinal sectional view showing another configuration of the reaction unit, FIG. 14B is a cross-sectional view taken along line XVIII-XVIII in FIG. 14A, and FIG. 14C is still another configuration of the reaction unit. FIG. It is a perspective view which shows the structure of a temperature adjustment case. 16 (a) is a plan sectional view of the processing section, FIG. 16 (b) is a side sectional view, FIG. 16 (c) is a partially enlarged view of FIG. 16 (a), and FIG. 16 (d) is FIG. FIG. It is a figure which shows the other structure of a product storage part. FIG. 18A is a plan view showing another configuration of the merging portion, and FIG. 18B is an enlarged view of the main portion of FIG. It is a top view which shows other structure of a confluence | merging part. It is a schematic diagram which shows the other structure of a fluid reaction apparatus. It is a schematic diagram which shows the other structure of a fluid reaction apparatus. It is a schematic diagram which shows the other structure of a fluid reaction apparatus. It is a schematic diagram which shows the other structure of a fluid reaction apparatus. It is a perspective view which shows the structure of the process part of FIG. It is a schematic diagram which shows the other structure of a fluid reaction apparatus.

Explanation of symbols

DESCRIPTION OF SYMBOLS 1 Plunger pump apparatus 2 Microreactor 10 Plunger pump 12 Cylinder 14 Plunger 16 Piston 17 Pump chamber 18 Rod 19 Drive apparatus 20 Motor 22 Feed screw 24 Nut 26 Linear scale 28 Control part 30 Discharge port 32 Suction port 34 Check valve 36 Discharge line 38 Fluid tank 40 Supply line 42 Raw material receiving port 44 Introduction flow path 46 Flow meter 48 Pressure sensor 50 Mixing / reaction section

Claims (6)

A pair of plunger pumps each having a separate drive and connected in parallel between the liquid source and the microreactor flow path;
A flow meter installed in the microreactor channel;
A controller that alternately discharges the pair of plunger pumps at a constant predetermined feed rate;
The said control part adjusts the said feed rate at predetermined | prescribed timing based on the measured value of the said flow meter when the said plunger pump is performing discharge operation, The plunger pump apparatus characterized by the above-mentioned. A pressure sensor installed in the microreactor channel;
The plunger pump device according to claim 1, wherein the control unit finely adjusts the feed rate based on an output value of the pressure sensor.   The controller performs a speed increasing process and a speed reducing process for each of the pair of plunger pumps at an initial stage and a final stage of the discharge operation, and the flow rate is constant so that one speed increasing process and the other speed reducing process overlap each other. 3. The plunger pump device according to claim 1, wherein the switching control is performed as it is.   4. The plunger pump device according to claim 3, wherein during the switching control, fine adjustment of the feed speed is performed only for one plunger pump. 5.   5. The plunger pump device according to claim 1, wherein the control unit controls the plunger pump to perform a certain stopping process between the forward movement and the backward movement. The position sensor which detects the position of the plunger of the said plunger pump is provided, The said control part controls feed speed based on the output of this position sensor, The Claim 1 thru | or 5 characterized by the above-mentioned. Plunger pump device.

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