CIRCULATION ELEMENT AND REACTION TANK

Abstract

This circulation element, which forms a reaction vessel together with a first reaction unit and a second reaction unit, is provided between: the first reaction unit, inside which a first catalytic layer is provided and which is provided with a first supply port for supplying a raw material solution to the first catalytic layer from above and a first drain port for causing a reaction solution prepared from the raw material solution that has flowed down the first catalytic layer to flow down, and the second reaction unit, which has a second catalytic layer provided inside it, with a second supply port for supplying a reaction solution to the second catalytic layer from above and a second drain port for causing the reaction solution that has flowed down the second catalytic layerflows outward, and is provided below the first reaction unit. The circulation element comprises: a flow path forming member for forming a flow path to cause the reaction solution to flow down from the inside of the first reaction unit to the inside of the second reaction unit; and a liquid removal unit for removing the reaction solution to the outside of the flow path and / or a fixing unit for fixing an analyzer for analyzing the reaction solution in the flow path.

Description

Technical field

[0001] The present invention relates to a flow element forming a reaction vessel which causes a supplied raw material liquid to pass through a catalyst layer and flow off as reaction liquid, and to a reaction vessel. State of the art

[0002] In the design of a device for manufacturing a pharmaceutical product, a test is performed to determine the reaction rate in the presence of a catalyst for a raw material liquid containing a pharmaceutical raw material. This test is carried out, for example, with a test apparatus comprising a column, which is a reaction vessel filled with a catalyst layer, and a mechanism for supplying the raw material liquid to the column. During the test, the column assumes a position where an internal flow path extends vertically. The supply mechanism introduces the raw material liquid from above the column. This raw material liquid reacts upon contact with the catalyst layer and flows below the column as the reaction liquid. The temperature within the column is adjusted concurrently with the supply of the raw material liquid.The reaction fluid obtained when the column interior is in a stable state is sampled. The temperature setting within the column, as described above, is achieved, for example, by placing the column in a heating / cooling device.

[0003] This experiment is described in more detail below. A large number of columns, each with different feed fluid residence times, are manufactured in the same way as the column described above. This means that the manufactured columns have different feed fluid residence times (and also different reaction times of the feed fluid in the presence of the catalyst). Specifically, for example, columns with the same flow path diameter but different lengths are produced. An operator exchanges the columns one after the other in the test setup, and the sampling procedure described above is performed with each column exchange.The concentration of the pharmaceutical raw material remaining in each extracted reaction liquid is determined using an analytical instrument, and the reaction rate described above is calculated based on the residence time of each reaction liquid in the column and the determined concentration of the pharmaceutical raw material.

[0004] Determining the reaction rate using the test described above is time-consuming and laborious, as it requires the operator to exchange the columns and wait each time for the column interior to reach a stable state before the columns are exchanged. Patent reference 1 discloses a reaction analysis system comprising a mixer to which two fluids are fed, a reaction tube through which a fluid flowing through the mixer passes, and a plurality of temperature measuring units that measure the temperature of the fluid in the flow paths before and after the mixer. The reaction analysis system estimates a reaction parameter indicating a reaction state of the fluid based on the temperature measured by each temperature measuring unit.However, this system has a different configuration than the test device described above, which causes a reaction between the raw material liquid and the catalyst layer, and is not a technique that can solve the problem described above. Bibliography Patent literature

[0005] Patent Literature 1: JP 2021-159910 A Brief description of the invention: Technical problem

[0006] The present invention was made in view of such circumstances, and one objective of the present invention is to provide a technique that enables a simple analysis of reaction liquids with different reaction times from one another when a raw material liquid is caused to pass through a catalyst layer in a reaction vessel to obtain a reaction liquid for analysis. Solution to the problem

[0007] The present invention (first invention) relates to a flow element forming a reaction vessel which allows a supplied raw material liquid to pass through a catalyst layer and flow out as reaction liquid, together with a first reaction unit and a second reaction unit, The flow element is provided between the first reaction unit and the second reaction unit, the first reaction unit being provided internally with a first catalyst layer and containing a first inlet opening for supplying the feedstock liquid to the first catalyst layer from above and a first outlet opening to allow reaction liquid generated from the feedstock liquid flowing down the first catalyst layer to flow downwards, the second reaction unit being provided internally with a second catalyst layer, containing a second inlet opening for supplying the reaction liquid to the second catalyst layer from above and a second outlet opening to allow the reaction liquid flowing down the second catalyst layer to flow outwards, and being provided below the first reaction unit. the flow element contains: a flow path forming part that creates a flow path causing the reaction fluid to flow down from the interior of the first reaction unit to the interior of the second reaction unit; and a liquid sampling device configured to extract the reaction fluid to outside the flow path, and a mounting part provided in the flow path forming part to attach an analyzer configured to analyze the reaction fluid in the flow path from outside the flow path.

[0008] The second invention is the flow element according to the first invention, wherein the liquid extraction device is provided, and the liquid extraction device a liquid intake configured to receive a portion of the reaction fluid flowing through the flow path, and a sampling port provided in the flow path forming part to extract the reaction fluid from the fluid intake to the outside of the flow path.

[0009] The third invention is the flow element according to the second invention, which also has a part for opening and closing the extraction opening.

[0010] The fourth invention is the flow element according to the second or third invention, wherein the flow path forming part is provided with a side tube, one end of which is open at a position above the liquid intake in the flow path and the other end of which is open on the outside of the flow path to form the extraction orifice, and The part for opening / closing is a valve that is provided in the side pipe.

[0011] The fifth invention is the flow element according to the fourth invention, wherein in a state where one direction of formation of the flow path is a vertical direction, the side pipe is inclined downwards from the outside of the flow path in the direction of the flow path.

[0012] The sixth invention is the flow element according to one of the second to fifth inventions, wherein the liquid intake forms a recess that stores the raw material liquid.

[0013] The seventh invention is the flow element according to the sixth invention, wherein a blocking part that blocks part of the flow path, is provided above the recess, and the blocking part is provided in a position that, viewed from the recess, is offset in a direction of formation of the flow path.

[0014] The eighth invention is the flow element according to one of the second to seventh inventions, wherein the flow path forming part is provided with a mounting part for mounting a measuring instrument from the outside of the flow path.

[0015] The ninth invention is the flow element according to the eighth invention, wherein the measuring instrument is a thermometer, and The mounting part is a connecting hole that links the flow path and the outside of the flow path to bring the thermometer into the flow path by inserting the thermometer from the outside of the flow path.

[0016] The present invention (tenth invention) relates to a reaction vessel in which a supplied raw material liquid flows through a catalyst layer and flows out as reaction liquid, wherein the reaction vessel contains: a first reaction unit which is provided inside with a first catalyst layer and includes a first feed opening for supplying the raw material liquid to the first catalyst layer from above and a first drain opening to allow a reaction liquid generated from the raw material liquid flowing down the first catalyst layer to flow downwards; a second reaction unit, which is provided internally with a second catalyst layer, which includes a second inlet opening for supplying the reaction fluid to the second catalyst layer from above and a second outlet opening for allowing the reaction fluid flowing down the second catalyst layer to flow outwards, and is provided below the first reaction unit; and The system comprises a flow element provided between the first reaction unit and the second reaction unit, a flow path forming part that creates a flow path causing the reaction fluid to flow downwards from the interior of the first reaction unit towards the second feed port, a fluid extraction device configured to extract the reaction fluid to the outside of the flow path, or a mounting part provided in the flow path forming part to attach an analyzer configured to analyze the reaction fluid in the flow path from outside the flow path.

[0017] The eleventh invention is the reaction vessel according to the tenth invention, wherein the liquid extraction device is provided, and the liquid extraction device contains: a liquid intake configured to receive a portion of the reaction fluid flowing through the flow path, and a sampling port provided in the part of the flow path that forms the part that conveys the reaction fluid from the fluid intake to the outside of the flow path.

[0018] The twelfth invention is the reaction vessel according to the eleventh invention, wherein a plurality of sets of the first reaction units and the flow path forming parts, each connected to a bottom of the first reaction unit, are provided, and the second reaction unit is connected to a bottom of a composite formed by connecting the sets together in a longitudinal direction, and The reaction fluid is supplied to the first reaction units of the second and subsequent sets from a top side of the assembly, instead of the raw material fluid.

[0019] The thirteenth invention is the reaction vessel according to the eleventh or twelfth invention, wherein the first reaction unit, the second reaction unit and the flow path forming part are each a cylindrical body and are connected to each other, a first flange connected to a lower section-side flange formed at a lower end section of the first reaction unit, provided at an upper end section of the flow path forming part, and a second flange, connected to an upper section-side flange formed at an upper end section of the first reaction unit or an upper end section of the second reaction unit, is provided at a lower end section of the flow path forming part.

[0020] The fourteenth invention is the reaction vessel according to the thirteenth invention, wherein a gasket is provided between the lower section-side flange and the first flange and between the upper section-side flange and the second flange, and The seal is provided with a grid to separate the flow path and the interior of the first reaction unit or the interior of the second reaction unit.

[0021] The fifteenth invention is the reaction vessel according to one of the eleventh to fourteenth claims, wherein in one flow direction of the reaction fluid, a length of a first flow path that accommodates the first catalyst layer in the first reaction unit is smaller than a length of a second flow path that accommodates the second catalyst layer in the second reaction unit. Advantageous effects of the invention

[0022] The present invention enables a simple analysis of reaction liquids with different reaction times when a raw material liquid is passed through a catalyst layer in a reaction vessel to obtain a reaction liquid for analysis. Brief description of the drawings Fig. Figure 1 is a configuration diagram of a catalytic reactor for the production of a pharmaceutical product according to an embodiment of the present invention. Fig. Figure 2 is a longitudinal side view of a reaction vessel that forms the test apparatus. Fig. Figure 3 is a perspective view of a flow element that forms the reaction vessel. Fig. Figure 4 is a perspective longitudinal section view of the flow element. Fig. Figure 5 is a schematic view of another example of a reaction vessel. Fig. Figure 6 is a longitudinal side view of another example of the reaction vessel. Fig. Figure 7 is a perspective longitudinal section view showing another example of a flow element. Fig. Figure 8 is a schematic view showing another example of a flow element. Fig. Figure 9 is a longitudinal section side view showing a modification of the flow element. Description of the embodiments

[0023] A catalytic reactor 1 with a reaction vessel 2 according to an embodiment of the present invention is described with reference to a configuration diagram of Fig. 1 described. The catalytic reactor 1 is a test device for the production of a pharmaceutical product, as described in the prior art section. The structure of the catalytic reactor 1 is described in an overview below. The reaction vessel 2, which forms the catalytic reactor 1, is designed as a vertically elongated cylindrical column. A flow path 21 in the reaction vessel 2 is filled with a catalyst to form a catalyst layer 30.

[0024] A raw material liquid containing a pharmaceutical raw material is fed into the reaction vessel 2 from above, flowing down the flow path 21 and passing through the catalyst layer 30. During its passage through the catalyst layer 30, the pharmaceutical raw material in the raw material liquid undergoes a chemical reaction due to the action of the catalyst layer 30, and the raw material liquid flows out of a lower section of the reaction vessel 2 as a reaction liquid containing a reaction product. In the present embodiment, hydrogen gas (H₂) is added to the reaction vessel 2 in addition to the raw material liquid, and a hydrogenation reaction is carried out as the chemical reaction described above. Nitrogen gas (N₂), used to adjust the concentration of the hydrogen gas, is also introduced into the reaction vessel 2.

[0025] Four of the aforementioned catalyst layers 30 are provided at intervals in the flow path 21. From another perspective, one can say that a catalyst layer in the reaction vessel 2 is subdivided into four layers in the direction of formation of the flow path 21, and each of the subdivided layers forms the catalyst layer 30. A liquid intake 53 is provided between the catalyst layer 30 and the catalyst layer 30, which receives and retains a portion of the reaction liquid flowing to the outside of the reaction vessel 2.

[0026] Since the catalyst layers 30 and the liquid intake 53 are provided as described above, the reaction fluid flowing from the lower section of the reaction vessel 2 and the reaction fluid drawn from each of the liquid intake 53 have different contact times with the catalyst layer 30 (i.e., different reaction times in the presence of the catalyst forming the catalyst layer 30) compared to each other. An operator can calculate the rate of the hydrogenation reaction of the pharmaceutical feedstock by taking samples of these reaction fluids and determining the concentration of the remaining pharmaceutical feedstock. As described later, the reaction vessel 2 is configured so that the operator can draw off the reaction fluid contained in each liquid intake 53 from the outside of the reaction vessel 2.In addition to the reaction fluid contained in the liquid samples 53, the reaction fluid flowing from the lower end of the reaction vessel 2 also serves as a sampling target.

[0027] In this description, the feedstock liquid flowing through the catalyst layer 30 is referred to as the reaction liquid. If, for example, the feedstock liquid is fed into the reaction vessel 2 under conditions of low reactivity, it may be retained in an unreacted state in the liquid intake 53 or flow out of the lower section of the reaction vessel 2. This feedstock liquid is also referred to as the reaction liquid. That is to say, the reaction liquid in this description contains a liquid with the same composition as the feedstock liquid before it is fed into the reaction vessel 2.

[0028] The following describes the construction of the catalytic reactor 1 in more detail. The catalytic reactor 1 includes a treatment fluid supply mechanism 7 and a gas supply mechanism 8. The treatment fluid supply mechanism 7 comprises a feed pipe 71, a pump 72, a valve 73, and a reservoir 74. A downstream end of the feed pipe 71 is connected to the reaction vessel 2, and the pump 72 and the valve 73 are located, in that order, on the upstream end of the feed pipe 71. The reservoir 74 is connected to the upstream end of the feed pipe 71 and stores the feed fluid. The feed fluid is supplied to the reaction vessel 2 at a predetermined rate by the pump 72, which operates in a state where the valve 73 is open.

[0029] The gas supply mechanism 8 comprises a gas supply pipe 81, gas supply pipes 82 and 83, valves 84 and 85, an H2 gas storage section 86, and an N2 gas storage section 87. A downstream end of the gas supply pipe 81 is connected to a section between the downstream end of the feedstock-liquid supply pipe 71 and the pump 72. The gas supply pipe 81 branches on the upstream side, forming the gas supply pipes 82 and 83. An upstream end of the gas supply pipe 82 is connected to the H2 gas storage section 86 via the valve 84, and an upstream end of the gas supply pipe 83 is connected to the N2 gas storage section 87 via the valve 85. The H2 gas storage part 86 and the N2 gas storage part 87 are formed, for example, by a gas cylinder.During the supply of the raw material liquid into the reaction vessel 2 by the pump 72, the valves 84 and 85 are opened to direct the H2 gas and the N2 gas into the supply pipe 71 for the raw material liquid. This supplies the raw material liquid together with the H2 gas and the N2 gas to the reaction vessel 2.

[0030] Reaction vessel 2 is also referred to as Fig. Figure 2, which shows a longitudinal side view, is described in more detail. When reaction vessel 2 is used (i.e., when the feedstock liquid is added), it is heated or cooled, for example, by placing it in a heating / cooling device, similar to the column described in the prior art section. In a heating case, for example, a furnace can be used as the heating / cooling device. The following description assumes that reaction vessel 2 is in such a state. Therefore, the description of the position and orientation of reaction vessel 2 and each element that forms reaction vessel 2 describes the position and orientation assumed when reaction vessel 2 is in use.

[0031] The reaction vessel 2 contains four reaction units 3, each housing the catalyst layer 30, and three flow elements 5, each housing the liquid intake 53. A schematic diagram of the reaction units 3 and the flow elements 5 is described below. Each reaction unit 3 contains a tube wall 31 forming a cylindrical body. The inner surface of the tube wall 31 is configured as a flow path 32 for the feedstock liquid or the reaction liquid, and the catalyst layer 30 is provided within this flow path 32. Each flow element 5 contains a tube wall 51 forming a cylindrical body. The tube wall 51 is a flow path-forming component. The inner surface of the tube wall 51 is configured as a flow path 52 for the reaction liquid, and the liquid intake 53 is provided within this flow path 52.Flow paths 32 and 52, for example, have the same diameter as each other.

[0032] The tube walls 31 of the four reaction units 3 and the tube walls 51 of the three flow elements 5 are connected such that their central axes are aligned in plan view and extend vertically, forming the cylindrical reaction vessel 2 as described above. By connecting the tube walls 31 and 51, the flow paths 32 of the reaction units 3 and the flow paths 52 of the flow elements 5 are connected to form the flow path 21 of the reaction vessel 2 described above, and the direction of formation of the flow path 21 (which is also the direction of formation of the flow paths 32 and 52) lies along the vertical axis. The reaction units 3 and the flow elements 5 are arranged alternately in the vertical direction, and an upper and a lower section of the reaction vessel 2 are each formed by the reaction unit 3.Therefore, each of the three flow elements 5 is positioned such that it is enclosed between the reaction units 3 from above and below. For the sake of simplicity, the reaction units 3 are sometimes referred to as 3A, 3B, 3C, and 3D from above, and the flow elements 5 are sometimes referred to as 5A, 5B, and 5C from above to distinguish them from one another.

[0033] The reaction units 3 are described in detail below. Reaction unit 3A is provided with an upper cover 33, which closes an upper opening of the flow path 32. The downstream end of the feed tube for the feed liquid 71 is connected to the upper cover 33, and the feed liquid is directed into the reaction vessel 2 through a through-hole 33A provided in the upper cover 33. Reaction unit 3D is also provided with a lower cover 34 to close a lower opening of the flow path 32. An upstream end of a drain tube 35 is connected to the lower cover 34, and the reaction liquid flows through a through-hole 34A provided in the lower cover 34 into the drain tube 35. The outflowing reaction liquid is taken by the operator and used to calculate the reaction rate mentioned above.Furthermore, the drain pipe 35 is equipped with a thermometer 23 for measuring the temperature in the drain pipe 35. The thermometer 23 is described together with the thermometers 23 provided in the flow elements 5.

[0034] Reaction units 3A to 3D are similarly configured, except that the upper lid 33 and the lower lid 34 are provided in reaction units 3A and 3D, respectively. Consequently, the reaction fluid flows similarly in each of reaction units 3A to 3D, differing only in the time (reaction time) during which the reaction fluid taken from each location is in contact with the catalyst layer 30. The flow path 32 of each reaction unit 3 is filled with the catalyst from an upper end section to a lower end section to form the catalyst layer 30 described above, and the feedstock fluid or reaction fluid flows downwards through a space within the catalyst of the catalyst layer 30.Since the reaction units 3A to 3D have the same configuration except for the difference in the presence or absence of the upper lid 33 and the lower lid 34, as described above, the reaction units 3A to 3D also have the same volume of the catalyst layer 30.

[0035] An upper and a lower section of the tube wall 31, which is a cylindrical body, project towards the outside of the cylindrical body to form flanges 37. The upper flange 37 of reaction unit 3A and the lower flange 37 of reaction unit 3D are each connected to the upper cover 33 and the lower cover 34, respectively. The other flanges 37 of reaction units 3A to 3D are connected to flanges 63 or 64, which will be described later and are provided in the flow elements 5.

[0036] The following section describes the flow elements 5, also with reference to a perspective view of Fig. 3 and a perspective longitudinal section view of Fig. As described in section 4, since no catalyst layer 30 is provided, each flow element 5 does not contribute to the hydrogenation reaction of the pharmaceutical raw material. Therefore, the flow element 5 only needs to retain the reaction fluid through the liquid intake 53 and allow the operator to take samples. Consequently, the flow element 5 is configured as a short tube to prevent an increase in the size of the reaction vessel 2 and has a shorter tube length than the tube length of the reaction unit 3.

[0037] The liquid intake 53 is described. The liquid intake 53 contains side walls 54A and 55A as well as longitudinal walls 54B and 55B and is configured to form a recess 54 and two recesses 55. The recesses 54 and 55 open upwards and are positioned at the same level in the flow path 52. The recesses 54 and 55 have different shapes, and recess 54 is inserted between the recesses 55 from the left and right. The depths of the recesses 54 and 55 are chosen to be relatively small so that the reaction liquid in the recesses 54 and 55 is replaced when the reaction liquid is continuously supplied, as described later in a test procedure.

[0038] The recesses 54 and 55 are described in more detail below. A horizontal, plate-shaped partition is provided to divide the flow path 52 vertically, and two slot-shaped through-holes extending from front to back are formed at a distance from left to right, so that the partition is divided into three sections. The subdivided partitions form the side walls 54A and 55A of the recesses 54 and 55, and the side walls are arranged in the left-right order 55A, 54A, 55A. A right end and a left end of the side wall 54A are extended vertically upwards to form the longitudinal walls 54B, and the respective longitudinal walls 54B and the pipe wall 51 form a side wall of the recess 54. In addition, a right end of the left side wall 54A and a left end of the right side wall 54A are each extended vertically upwards to form the longitudinal wall 54B.The longitudinal wall 54B and the pipe wall 51 form a side wall of the recess 55.

[0039] Longitudinal walls 54B and 55B face each other, with a gap 56 between them. A portion of the reaction fluid in the flow path 52 falls into the recesses 54 and 55 to accumulate there, and a portion of the accumulated reaction fluid overflows from the recesses 54 and 55 and flows downwards through the gap 56. Another portion of the reaction fluid falls directly into the gap 56 in the flow path 52 and flows downwards through the gap 56.

[0040] Furthermore, the flow element 5 is provided with a side tube 61 that penetrates the tube wall 51. Therefore, one end of the side tube 61 opens into the flow path 52 and the other end opens onto the outside of the flow path 52. The side tube 61 and the liquid intake 53 form a liquid sampling device for taking samples. The side tube 61 is a straight tube that slopes downwards from the outside of the tube wall 51 towards the flow path 52. One end of the side tube 61 opens at a point above the liquid intake 53 in the flow path 52. A section of the side tube 61 on the outside of the tube wall 51 forms a sampling port for taking and sampling the reaction fluid from the recesses 54 and 55, and a valve 62 is provided in this section. When the operator opens and closes valve 62, the dispensing port is opened and closed.Valve 62 is closed to prevent foreign substances from being mixed into the reaction vessel 2 during the supply of the raw material liquid, and valve 62 is opened at the time of withdrawal of the reaction liquid from the liquid intake 53.

[0041] The following describes the sampling procedure from the liquid intake 53. The operator inserts a syringe 22 from the outside of the reaction vessel 2 into the side tube 61, with the valve 62 open. A syringe needle is inserted into the recess 54 or the recess 55 to draw up and withdraw the reaction liquid. A curved needle, such as the one shown in [reference missing], can be used as the syringe needle. Fig. 2 shown, used to penetrate into the recesses 54 and 55.

[0042] To facilitate the insertion of the syringe into the recesses 54 and 55 with the top open, as described above, the side tube 61 is inclined such that it is located on the side of the flow path 52 below the side tube 61 on the outside of the flow path 52, as described above. Inclining the side tube 61 in this way is also advantageous because it prevents the reaction fluid from accumulating in the side tube 61. More precisely, if the side tube 61 is horizontal or inclined such that it is positioned on the outside of the flow path 52 below the side tube 61 on the side of the flow path 52, the reaction fluid flowing through the flow path 52 will flow into the side tube 61 to collect there.

[0043] If the reaction fluid accumulates in this way, it will flow out of the side tube 61 from the reaction vessel 2 at the time the valve 62 is opened for sampling. Therefore, it is necessary to collect the reaction fluid with a tool and remove it before sampling. Furthermore, the reaction fluid supplied to the flow path 52 before the interior of the reaction vessel 2 reaches a stable state remains in the side tube 61, depending on its length and angle of inclination, until the valve 62 is opened. That is, the reaction fluid continues to be supplied to the flow path 52, and new reaction fluid flows into the side tube 61 near the flow path 52 to replace the existing reaction fluid. However, this exchange does not occur outside the flow path 52, and the reaction fluid supplied before the steady state stagnates.In this case, there is a risk that the reaction fluid will adhere to and remain on the side tube 61 before reaching a stable state, even after the valve 62 has been opened for sampling. Furthermore, when the syringe 22 is inserted into the side tube 61, the reaction fluid adheres to the syringe needle, which is inserted into the recesses 54 and 55, and is drawn in along with the reaction fluid in the recesses 54 and 55. As described above, from the perspective of reducing labor and improving the accuracy of detecting the concentration of the pharmaceutical raw material in the reaction fluid, it is advantageous for the side tube 61 to be inclined such that it is positioned on the side of the flow path 52 below the side tube 61 on the outside of the flow path 52, thus preventing the accumulation of the reaction fluid.

[0044] An upper and a lower section of the tube wall 51, which is a cylindrical body, project towards the outside of the cylindrical body to form the flanges 63 and 64, respectively. In each of the flanges 63 (a first flange) and 64 (a second flange), an annular groove 65 is formed along an opening of the flow path 52 to surround the opening, and an annular seal 66 is provided in the groove 65. The seal 66 is provided with a grid 67, and the grid 67 is tensioned such that it vertically subdivides a circular area surrounded by the seal 66. The grid 67 can be configured so that it is not connected to the seal 66 but can be separated from it.

[0045] The flanges 63 and 64 of the flow elements 5 and the flanges 37 of the reaction units 3A to 3D are each connected to the intervening seal 66, thus preventing leakage of the reaction fluid between the reaction unit 3 and the flow element 5. Because the seal 66 and the respective flanges 63, 64, and 37 are arranged in this way, the grid 67 separates the flow path 32 of the reaction unit 3 (i.e., the interior of the reaction unit 3) from the flow path 52 of the flow element 5. The grid 67 prevents the catalyst forming the catalyst layer 30 from moving into the reaction unit 3, which is distinct from the reaction unit 3 where the catalyst is supplied, or from the flow element 5.

[0046] Furthermore, a through-hole 68 is provided in the pipe wall 51 of the flow element 5. The through-hole 68 is a connecting hole that links the flow path 52 and the outside of the flow path 52, and the thermometer 23 is inserted from the outside of the pipe wall 51 through the through-hole 68 into the flow path 52. The through-hole 68 thus forms a mounting point for the thermometer 23, which is a measuring instrument, on the flow element 5. The thermometer 23 measures the temperature of the flow path 52. Therefore, a total of four thermometers are provided in the device, including the thermometers 23 of the flow elements 5A to 5C and the thermometer 23 of the drain pipe 35.The thermometers 23 are positioned to correspond to reaction units 3A to 3D, and the operator can monitor the temperatures at the outlets of reaction units 3A to 3D using the temperatures detected by the corresponding thermometers 23 to determine whether the interior of reaction vessel 2 is in a stable state. The thermometer 23 located below and closest to the predetermined reaction unit 3 is the thermometer corresponding to the outlet of reaction unit 3. Therefore, the thermometers 23 of the flow elements 5A, 5B, and 5C and of the drain pipe 35 correspond to the outlets of reaction units 3A, 3B, 3C, and 3D, respectively.

[0047] Each thermometer 23 can be positioned in the flow path 32 of the reaction unit 3. However, in this case, the thermometer 23 enters the catalyst layer 30. This causes the flow of the reaction fluid in one region around the thermometer 23 to differ from the flow of the reaction fluid in another region of the flow path 32, resulting in a deviation of the reaction time in the reaction unit 3 from the intended time and potentially reducing the accuracy of the calculated reaction rate. Therefore, a configuration in which the thermometer 23 is positioned in the flow element 5, where the catalyst layer 30 is not located, is preferable from the perspective of accurately calculating the reaction rate.

[0048] Reaction unit 3 and the flow element 5 provided at the bottom of reaction unit 3 are combined as a set. That is, reaction unit 3A and flow element 5A, reaction unit 3B and flow element 5B, and reaction unit 3C and flow element 5C are each combined as a set and are positioned next to each other in the vertical direction rather than the longitudinal direction. When the three adjacent sets are combined as a composite, reaction vessel 2 has a configuration in which reaction unit 3D is provided adjacent to the bottom of the composite.

[0049] The reaction units 3A to 3C, which form the sets, correspond to first reaction units, and the upper and lower end sections of the flow paths 32 of reaction units 3A to 3C are configured as first inlet ports and first outlet ports, respectively. The reaction unit 3D, which does not form a set, corresponds to a second reaction unit, and the upper and lower end sections of the flow path 32 of reaction unit 3D are configured as second inlet ports and second outlet ports, respectively.Since the raw material liquid in contact with the catalyst layer 30 is referred to as the reaction liquid, as described above, the raw material liquid is fed from above to the first feed port of reaction unit 3A, which forms the first batch, and the reaction liquid is fed from above to reaction units 3B and 3C, which form the second and subsequent batches, and to reaction unit 3D, which forms the second reaction unit. The reaction liquid can flow out of reaction vessel 2 (into drain pipe 35) through the second drain port of reaction unit 3D.The catalyst layers 30 provided in reaction units 3A to 3C are first catalyst layers; the catalyst layer provided in reaction unit 3D is a second catalyst layer; the flow paths 32 of reaction units 3A to 3C correspond to first flow paths, and the flow path 32 of reaction unit 3D corresponds to a second flow path. The lower flanges 37 of reaction units 3A to 3C correspond to the lower section-side flanges. The upper flanges 37 of the first reaction units (reaction units 3A to 3C) and the second reaction unit (reaction unit 3D) correspond to the upper section-side flanges.

[0050] A test procedure using the catalytic reactor 1 is described. The reaction vessel 2 is stored in the heating / cooling device, and the interior of the heating / cooling device is set to a predetermined temperature. The treatment liquid feed mechanism (7) and the gas feed mechanism (8) supply the feedstock liquid, H₂ gas, and N₂ gas into the reaction vessel 2. The feedstock liquid passes through the catalyst layer 30 of the reaction unit 3 to become the reaction liquid, and the reaction liquid flows down the flow path 21 in the reaction vessel 2 and out of the reaction vessel 2 into the drain pipe 35.

[0051] As described above, as the reaction fluid flows in the reaction vessel 2, it is directed into the recesses 54 and 55 and the fluid intake 53 in the flow element 5, where it is stored. Since the raw material fluid continues to be supplied to the reaction vessel 2, some of the reaction fluid accumulated in the recesses 54 and 55 overflows and flows through the gap 56 between them into the lower reaction unit 3. Because the recesses 54 and 55 are relatively shallow, the overflowing reaction fluid, as described above, traps the reaction fluid located at the bottom of the recesses 54 and 55. Thus, while the reaction fluid remains stored in the recesses 54 and 55, it is continuously replaced by new reaction fluid.

[0052] When a predetermined time has elapsed since the start of the supply of the raw material liquid and each gas to the reaction vessel 2, and the operator confirms that the temperature recorded by each thermometer 23 is a suitable temperature, the operator determines that the interior of the reaction vessel 2 has reached a stable state and stops the supply of the raw material liquid and each gas to the reaction vessel 2. The operator takes samples of the reaction liquid flowing from the drain pipe 35 by any method and takes samples of the reaction liquids from the liquid collection pots 53 of the flow elements 5A to 5C according to the method described above.Since there is a possibility that the reaction liquid may fall into the flow paths 52 of the flow elements 5A to 5C even after the supply of the raw material liquid to the reaction vessel 2 from above has been stopped, sampling from the liquid samplers 53 is carried out quickly. The concentration of the pharmaceutical raw material in each sampled reaction liquid is determined using an analyzer.

[0053] Reaction units 3A to 3D have the same volume of catalyst layer 30. Therefore, if the reaction time of the reaction fluid drawn from the drain pipe 35 is X, the reaction times of the reaction fluids drawn from the flow elements 5A, 5B, and 5C can be described as 1 / 4X, 2 / 4X, and 3 / 4X, respectively, due to the different number of catalyst layers 30 through which the reaction fluid flows. The rate of the hydrogenation reaction of the pharmaceutical raw material is determined from these four differing reaction times and the concentration of the pharmaceutical raw material, which is determined from each sample of the reaction fluid.

[0054] As described above, samples of the four reaction liquids, which have different reaction times, can be easily taken from the catalytic reactor 1 without having to exchange the reaction vessel 2, as described in the prior art section. This reduces the time and effort required to determine the rate of the hydrogenation reaction mentioned above. Suppose the liquid sampling device (the liquid intake 53 and the side tube 61) for carrying out the sampling is provided in the reaction unit 3 instead of in the flow element 5. In this case, as in the case described above where the thermometer 23 is provided in the reaction unit 3, the flow of the reaction liquid in the catalyst layer 30 fluctuates, and as a result, the accuracy of the calculated reaction rate may decrease.Since the flow element 5 is provided in the reaction vessel 2 with the liquid intake 53 and the side tube 61, the reaction rate can be accurately calculated from the obtained samples of the reaction liquids, in addition to the effect that the samples of the four reaction liquids can be easily obtained.

[0055] Although the flow path 21 of the reaction vessel 2 is described as running along the vertical axis, the flow path 21 can be inclined with respect to the vertical axis as long as there are no problems with the flow of the reaction liquid and its storage in the liquid reservoir 53. The number of flow elements 5 and the number of reaction units 3 that form the reaction vessel of the present invention are not limited to the example described above. In particular, the number of sets of the flow elements 5 and the reaction units 3 described above can be any number. For example, the number of sets is not limited to a plurality of sets, but can be a single set. That is, the reaction vessel can be formed from only one flow element 5 and two reaction units 3 that sandwich the flow element 5.Furthermore, the reaction vessel 2 is not limited to a cylindrical body, but can also be a square cylindrical body.

[0056] Furthermore, the lower end section of the reaction vessel according to the present invention is not limited to being formed by the reaction unit 3 and can be formed by the flow element 5. Specifically, for example, a flow element 5D is provided such that it adjoins the reaction unit 3D of the reaction vessel 2 described above from below. The lower lid 34, to which the drain pipe 35 is connected, is provided on a lower section of the flow element 5D instead of on the lower section of the reaction unit 3D. Instead of taking the reaction fluid from the drain pipe 35, sampling is carried out from the flow element 5D.

[0057] Furthermore, the volumes of the catalyst layers 30 in the respective reaction units 3 can differ. In such a configuration, for example, the flow paths 32 of the respective reaction units 3 have the same diameter but different lengths in the flow direction of the reaction fluid. In particular, the lengths of the flow paths 32 are shown in a schematic view of Fig. 5 3A < 3B < 3C < 3D, which is an example of such a configuration. Therefore, in the Fig. In the example shown in Figure 5, the first flow path of each of the first reaction units has a shorter length than the second flow path of the second reaction unit, and among the first flow paths of the plurality of first reaction units, the uppermost first flow path has a shorter length. By configuring the respective flow paths 32, the lengths of the catalyst layers 30 in the formation direction of the flow paths 32 are also 3A < 3B < 3C < 3D. In the early phase of the reaction, the rate of reaction progress may be higher (i.e., the concentration change of the pharmaceutical raw material is greater) than in the later phase of the reaction. In this case, according to this configuration, the number of tests to be performed can be reduced by using raw material samples of different concentrations in the respective samples obtained.

[0058] During the test, the reaction vessel 2 is not limited to being located in the heating / cooling device. To regulate the temperature of the reaction vessel 2 when it is not located in the heating / cooling device, a jacket 38 can, for example, be provided on the reaction unit 3, as shown in Fig. Figure 6 shows the casing 38 being provided to surround the pipe wall 31 between the upper flange 37 and the lower flange 37, and a fluid flow path is formed within the casing 38. A fluid supply pipe and a fluid outlet pipe are each connected to an upstream and a downstream end of the flow path, respectively. A fluid, heated to a predetermined temperature by a fluid supply source, is fed into the flow path of the casing 38 through the supply pipe and discharged through the outlet pipe. An arrow near the casing 38 in the drawing indicates the direction of fluid flow. When such a fluid flows into the reaction vessel 2 during the supply of the feed fluid, the temperature of the flow path 32 of the reaction unit 3 can be adjusted. The flow path, the fluid supply source, the supply pipe, and the outlet pipe within the casing 38 are not shown.

[0059] A modification of the flow element 5 is described below. The liquid receptacle 53 provided in the flow element 5 can have any shape and is not limited to forming the recesses 54 and 55 described above. For example, a horizontal plate can be provided as the liquid receptacle in the flow path 52, and after the feed of the raw material liquid has ceased, the operator can aspirate the liquid droplets remaining on the horizontal plate to perform a sampling. However, to enable the extraction of a sufficient quantity of reaction liquid, it is advantageous to form a recess as the liquid receptacle. Although the side tube 61 penetrates the tube wall 51 of the flow element 5, the present invention is also not limited to such an arrangement.For example, a through-hole can be formed in the tube wall 51, which serves as a sampling opening for the reaction fluid, and the through-hole can be closed by a removable cover from the outside of the tube wall 51.

[0060] The flow element 5 can be provided with a blocking part 57, which is shown in a longitudinal side view. Fig. Figure 7 shows that two of the blocking parts 57 are positioned above the recesses 54 and 55 in the flow path 52, extending in the front-back direction to block a portion of the flow path 52. These blocking parts 57 are spaced at the same height from each other in the left-right direction. Each of the two blocking parts 57 is formed in a horizontal plate shape, and a front and a rear end of each blocking part 57 are held in contact with the pipe wall 51. Viewed in the direction of formation (vertical direction) of the flow path 52, the blocking part 57 covers the entire gap 56 immediately below it.Therefore, the blocking part 57 is positioned offset from the recesses 54 and 55 in the direction of flow formation, over the entire area where the liquid intake 53 is not provided. One end and the other end of the left and right ends of the blocking part 57 are arranged to overlap with the end of recess 54 and the end of recess 55, respectively. In the flow path 52, the reaction fluid either flows directly to recesses 54 and 55, or it flows onto the blocking parts 57 and then to the ends of the blocking parts 57 in order to flow to recesses 54 and 55.

[0061] It is described why the blocking parts 57 are provided. The reaction vessel 2 can be used for various reactions, and different types of liquid feedstocks can be used. Depending on the feedstock liquid to be used and the environment in which the test is carried out, the feedstock liquid undergoes a reaction in contact with the catalyst layer 30 and a non-catalytic thermal decomposition reaction in a state in which it is not in contact with the catalyst layer 30.If the blocking elements 57 are not provided in the case of the non-catalytic thermal decomposition reaction, which proceeds as described above, the rate of progression of the non-catalytic thermal decomposition reaction differs between the reaction fluid that flows down to the fluid intake 53, stagnates in the recesses 54 and 55, and is then fed to the gap 56 of the flow path 52, and the reaction fluid that flows directly to the gap 56. That is, the reaction fluids, in which the reactions do not proceed uniformly, are mixed in each flow element 5 and fed to the lower unit. In this case, the accuracy of the calculated reaction rate may decrease. However, in a case where such a non-catalytic thermal decomposition reaction does not occur, it is not necessary to include the blocking elements 57 in the flow path 52. Fig. 4 to provide the blocking parts 57 and the like as shown. The blocking parts 57 are not limited to a horizontal plate, but can have any shape, e.g. an inclined plate.

[0062] An inline analyzer that analyzes the components of the reaction fluid can also be connected externally to the pipe wall 51 of the flow element 5. The analyzer is shown in a schematic view of Fig. This analyzer optically detects the concentration of the pharmaceutical raw material in the reaction liquid, e.g., using transmitted and scattered light, and includes a light source 91 and a detector 92 that receives the transmitted and scattered light. The branch tubes 93 and 94, which are short tubes, are connected to a side wall of the tube wall 51 and are open at the flow path 52, so that they face each other. Flanges 95 are formed at the end sections of the branch tubes 93 and 94 on the side opposite the flow path 52. The light source 91 and the detector 92 are connected to one flange 95 and the other flange 95, respectively, by means of a fastening such as a screw. The flanges 95 thus form a fastening element of the analyzer to the tube wall 51 from the outside of the flow path 52.In the above configuration, the detector 92 is illuminated by the light source 91 through the flow path 52 (indicated in the drawing by a dashed arrow), thereby analyzing the components of the reaction fluid flowing down the flow path 52.

[0063] Suppose the analyzer is a probe type configured to measure absorbance and similar parameters, with the probe being inserted from the outside through the through-hole 68 into the flow path 52, similar to the thermometer 23, and the concentration of the pharmaceutical product being determined based on the measurement result. In a case where the analyzer is configured as described above, the through-hole 68, into which the probe is inserted, forms the mounting part.

[0064] As described above, an area where the catalyst layer 30 is not provided is formed as a flow element 5 in the reaction vessel 2, and this area is used as a location for the liquid extraction device, comprising the liquid intake 53 and the side tube 61, or for the analyzer. In the case where the liquid extraction device is provided, it prevents the liquid extraction device from influencing the flow of the reaction liquid in the catalyst layer 30 as described above. On the other hand, in the case where the Fig. The analytical device shown in Figure 8 prevents the analysis from becoming impossible due to the blockage of the optical path by the catalyst layer 30. As described above, the flow element 5 also serves as the area in which the thermometer 23, a measuring instrument for monitoring the condition in the reaction vessel 2, is installed, thus preventing the thermometer 23 from influencing the liquid flow in the catalyst layer 30. The measuring instrument is not limited to the thermometer 23 but could, for example, be a pressure gauge for monitoring the pressure in the flow path 52. The pressure gauge can be provided by making the through-hole 68 in the tube wall 51 and inserting the pressure gauge from the outside of the tube wall 51 into the through-hole 68, as was done when mounting the thermometer 23.The thermometer 23 or the pressure measuring instrument can be provided in the flow element 5 both when the liquid sampling device is provided in the flow element 5 and when the analyzer is provided in the flow element 5.

[0065] Fig.Figure 9 is a longitudinal side view showing a flow element 50, which is a further modification of the flow element 5. The flow element 50 is provided in the reaction vessel 2 in place of the flow element 5. The flow element 50 is described below with regard to one difference from the flow element 5. The flow path 52 is not provided with the side walls 54A and 55A and the longitudinal walls 54B and 55B, and the recesses 54 and 55 are not formed. Instead, a drain-side pipe 41 is provided, which penetrates the pipe wall 51 of the flow element 5. The drain-side pipe 41 is a straight pipe that is inclined upward from the outside of the pipe wall 51 toward the flow path 52 and is open in the flow path 52.Part of the reaction fluid supplied to flow path 52 flows through the side of the outlet pipe 41 to the lower reaction unit 3, and another part of the reaction fluid flows into the outlet pipe 41 and out of reaction vessel 2. Thus, when the feedstock fluid is supplied to reaction vessel 2, the reaction fluid flows out of the outlet pipe 41 in addition to the outlet pipe 35. When the interior of reaction vessel 2 reaches a stable state, the operator takes samples of each of the reaction fluids flowing out of the outlet pipe 35 and the outlet pipe 41.

[0066] As described above, the outflow-side pipe 41 forms the liquid intake and the discharge port for the reaction liquid in the flow element 50 and is configured such that the absorbed reaction liquid can flow to the outside of the reaction vessel 2 without being stored in the flow path 52. Therefore, the liquid intake in the present invention is not limited to the configuration in which the reaction liquid is stored in the flow path 52. However, the amount of reaction liquid flowing through each reaction unit 3 is different, and there is a possibility that the reactivity of the pharmaceutical raw material varies in each reaction unit 3.This means that, since there is a possibility that the concentration of the remaining pharmaceutical raw material may differ between the extracted reaction liquids due to the reaction time and other factors, it is preferable that the liquid intake be configured to store the reaction liquid in the flow path 52 as in the liquid intake 53 described above, in order to increase the accuracy of the test.

[0067] A valve can be provided in the outflow-side pipe 41 outside the flow path 52. This valve can be closed to store the reaction fluid while the feedstock fluid is supplied to the reaction vessel 2 and opened at the time of sampling. However, as described in the description of the side pipe 61, it can be difficult to replace the accumulated reaction fluid in such a configuration. Therefore, it is advantageous to provide a recess, such as the fluid intake 53, in the reaction vessel 2 as a fluid intake, which causes the stored reaction fluid to remain in the flow path 52. That is, the stored reaction fluid preferably remains in the flow path 52 and does not move out of it.

[0068] Although reaction vessel 2, in which the hydrogenation reaction is carried out, has been described as an example, it is not limited to carrying out such a reaction. It could be a vessel in which a variety of liquids are mixed to carry out a chemical reaction in the presence of a catalyst, or a vessel in which a thermal decomposition reaction is carried out in the presence of a catalyst. While it has been described that the feedstock liquid contains the pharmaceutical raw material, the feedstock liquid could contain any compound. Therefore, the present technology is not limited to the field of pharmaceutical manufacturing.

[0069] The embodiments disclosed herein serve in every respect for illustration and do not constitute a limitation. The embodiments described above may be omitted, replaced, modified, or combined in various ways without deviating from the scope and spirit of the appended claims. Reference symbol list 2 reaction vessel 21 Flow path 3 reaction unit 30 catalyst layer 5 Flow element 51 Pipe wall 52 Flow path 53 Fluid intake 61 side tube QUOTES INCLUDED IN THE DESCRIPTION

[0000] This list of documents cited by the applicant was automatically generated and is included solely for the reader's convenience. The list is not part of the German patent or utility model application. The DPMA accepts no liability for any errors or omissions. Cited patent literature

[0000] JP 2021-159910 A

[0005]

Claims

[1] Flow element forming a reaction vessel which causes a supplied raw material liquid to pass through a catalyst layer and flow out as a reaction liquid, together with a first reaction unit and a second reaction unit, wherein the flow element is provided between the first reaction unit and the second reaction unit, wherein the first reaction unit is provided inside with a first catalyst layer and comprising a first inlet opening for supplying the feedstock liquid to the first catalyst layer from above and a first outlet opening to allow a reaction liquid generated by the feedstock liquid to flow down the first catalyst layer, wherein the second reaction unit is provided inside with a second catalyst layer, comprising a second inlet opening for supplying the reaction liquid to the second catalyst layer from above and a second outlet opening to allow the reaction liquid flowing down the second catalyst layer to flow outwards, and the second reaction unit is provided below the first reaction unit. the flow element includes: a flow path forming part that creates a flow path causing the reaction fluid to flow downwards from an inside of the first reaction unit towards an inside of the second reaction unit; and a liquid sampling device and a mounting part, wherein the liquid sampling device is configured to extract the reaction fluid to an outside of the flow path, and the mounting part is provided in the flow path forming part to attach an analyzer configured to analyze the reaction fluid in the flow path from the outside of the flow path. [2] Flow element according to claim 1, wherein the liquid extraction device is provided, and the liquid extraction device contains: a liquid intake configured to capture a portion of the reaction fluid flowing down the flow path, and a sampling port provided in the flow path forming part to extract the reaction fluid from the fluid intake to outside the flow path. [3] Flow element according to claim 2, further comprising an opening / closing part configured to open and close the extraction port. [4] Flow element according to claim 3, wherein the flow-forming part is provided with a side tube, one end of which is open at a position above the liquid intake in the flow path and the other end of which is open on the outside of the flow path to form the extraction orifice, and The part used for opening / closing is a valve that is provided in the side pipe. [5] Flow element according to claim 4, wherein in a state where one direction of formation of the flow path is a vertical direction, the side pipe is inclined downwards from the outside of the flow path in the direction of the flow path. [6] Flow element according to claim 2, wherein the liquid intake forms a recess in which the raw material liquid is stored. [7] Flow element according to claim 6, wherein a blocking part that blocks part of the flow path, is provided above the recess, and the blocking part is provided in a position that, viewed from the recess, is offset in a direction of formation of the flow path. [8] Flow element according to claim 2, wherein the flow path forming part is provided with a mounting part for mounting a measuring instrument from outside the flow path. [9] Flow element according to claim 8, wherein the measuring instrument is a thermometer, and The mounting part is a connecting hole that links the flow path and the outside of the flow path to bring the thermometer into the flow path by inserting the thermometer from the outside of the flow path. [10] Reaction vessel which causes a supplied raw material liquid to pass through a catalyst layer and flow out as a reaction liquid, wherein the reaction vessel comprises: a first reaction unit which is provided inside with a first catalyst layer and includes a first feed opening for supplying the raw material liquid to the first catalyst layer from above and a first drain opening to allow a reaction liquid generated from the raw material liquid flowing down the first catalyst layer to flow downwards; a second reaction unit, which is provided internally with a second catalyst layer, has a second inlet opening for supplying the reaction fluid to the second catalyst layer from above and a second outlet opening for the reaction fluid flowing down the second catalyst layer to the outside, and is provided below the first reaction unit; and A flow element provided between the first reaction unit and the second reaction unit, comprising: a flow path forming part that creates a flow path causing the reaction fluid to flow downwards from an inside of the first reaction unit towards the second feed opening, and a fluid extraction device and a mounting part, wherein the fluid extraction device is configured to extract the reaction fluid to an outside of the flow path, and the mounting part is provided in the part forming the flow path to attach an analyzer configured to analyze the reaction fluid in the flow path from the outside of the flow path. [11] Reaction vessel according to claim 10, wherein the liquid extraction device is provided, and the liquid extraction device contains: a liquid intake configured to receive a portion of the reaction fluid flowing through the flow path, and a sampling port provided in the flow path forming part to extract the reaction fluid from the fluid intake to outside the flow path. [12] Reaction vessel according to claim 11, wherein a plurality of sets of the first reaction units and the flow path forming parts, each connected to a bottom of the first reaction unit, are provided, and the second reaction unit is connected to a bottom of a composite formed by connecting the sets together in a longitudinal direction, and The reaction liquid, instead of the raw material liquid, is supplied to the first reaction units of the second and subsequent sets from a top side in the assembly. [13] Reaction vessel according to claim 12, wherein the first reaction unit, the second reaction unit and the flow path forming part are each a cylindrical body and are connected to each other, a first flange, connected to a lower section-side flange formed at a lower end section of the first reaction unit, is provided at an upper end section of the flow path forming part, and a second flange, connected to an upper section-side flange formed at an upper end section of the first reaction unit or an upper end section of the second reaction unit, is provided at a lower end section of the flow path forming part. [14] Reaction vessel according to claim 12, wherein a gasket is provided between the lower section-side flange and the first flange and between the upper section-side flange and the second flange, and The seal is provided with a grid to separate the flow path and the interior of the first reaction unit or the interior of the second reaction unit. [15] Reaction vessel according to claim 11, wherein in one flow direction of the reaction fluid, the length of a first flow path that accommodates the first catalyst layer in the first reaction unit is smaller than the length of a second flow path that accommodates the second catalyst layer in the second reaction unit.

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