Reactor

Abstract

To provide a reactor that can efficiently produce a product.SOLUTION: A reactor 1 comprises: a reaction vessel 10 which is capable of housing a solid phase B constituted of catalyst inside thereof; a gas replacement device 40 which is capable of supplying gas G to the solid phase B; an irradiation device 20 which is capable of irradiating the solid phase B with light; a gas replacement device 40 which is capable of supplying raw material gas X to the solid phase B; a distillation device 60 and a product recovery device 80 which recover a product Y produced by reaction of the raw material gas X from the reaction vessel 10; a chromaticity measuring device 50 which is capable of measuring chromaticity of the solid phase B; and a controller 90 which controls the gas replacement device 40 so as to supply the raw material gas X to the solid phase B in the case where, after performing supply of the gas G to the gas replacement device 40 and irradiation with light by the irradiation device 20, a difference between first chromaticity being the chromaticity of the solid phase B before performing irradiation with light and second chromaticity being the chromaticity of the solid phase B after performing irradiation with light becomes a predetermined difference or more, or in the case where the second chromaticity becomes a first threshold value or more.SELECTED DRAWING: Figure 1

Description

[Technical Field]

[0001] The present invention relates to a reactor technology for carrying out a chemical reaction on a reactant. [Background technology]

[0002] Conventionally, techniques for carrying out chemical reactions on reactants have been publicly known. For example, Patent Document 1 discloses a method for producing a product by a chemical reaction using two liquid phases.

[0003] However, in conventional techniques, it is necessary to replace the contents for each reaction cycle, and it is difficult to efficiently produce a product by continuously supplying raw materials and recovering the product. [Prior art documents] [Patent documents]

[0004] [Patent Document 1] Patent No. 6080281 Summary of the Invention [Problem to be solved by the invention]

[0005] The present invention has been made in view of the above circumstances, and an object of the present invention is to provide a reaction apparatus capable of efficiently producing a product. [Means for solving the problem]

[0006] The problem to be solved by the present invention is as described above, and the means for solving this problem will now be described.

[0007] That is, claim 1 provides a reaction apparatus for producing a product by reacting a raw material gas using a catalyst, the reaction apparatus comprising: a reaction vessel capable of accommodating a solid phase constituted by the catalyst inside; a gas supply device capable of supplying gas to the solid phase in preparation for the reaction of the raw material gas; an irradiation device capable of irradiating the solid phase with light in preparation for the reaction of the raw material gas; a raw material supply device capable of supplying the raw material gas to the solid phase; a product recovery device that recovers the product produced by the reaction of the raw material gas from the reaction vessel; a chromaticity measurement device capable of measuring the chromaticity of the solid phase; and a control device that controls the raw material supply device to supply the raw material gas to the solid phase when, after the gas supply device has supplied the gas and the irradiation device has irradiated the solid phase with light, a difference between a first chromaticity that is the chromaticity of the solid phase before the light irradiation and a second chromaticity that is the chromaticity of the solid phase after the light irradiation becomes equal to or greater than a predetermined difference, or when the second chromaticity becomes equal to or greater than a first threshold value.

[0008] In claim 2, the control device controls the gas supply device or the irradiation device to supply the gas or irradiate the light again if the difference between the first chromaticity and the second chromaticity is less than the predetermined difference, or if the second chromaticity is less than the first threshold value, after the gas supply device supplies the gas and the irradiation device irradiates the light.

[0009] In claim 3, the control device controls the gas supply device to supply the gas and the irradiation device to irradiate light, and then, if the difference between the first chromaticity and the second chromaticity is less than the predetermined difference or the second chromaticity is less than the first threshold, irradiate the light again, and, if, after irradiating the light, the difference between the first chromaticity and the second chromaticity is less than the predetermined difference or the second chromaticity is less than the first threshold, control the gas supply device to supply the gas again.

[0010] In claim 4, the control device controls the product recovery device to recover the product from the solid phase when, after the raw material gas is supplied by the raw material supply device, the difference between the second chromaticity and a third chromaticity, which is the chromaticity of the solid phase after the raw material gas is supplied, becomes equal to or greater than the predetermined difference, or when the third chromaticity becomes equal to or less than a second threshold value that is smaller than the first threshold value.

[0011] In claim 5, the control device controls the raw material supply device to supply the raw material gas again if, after the raw material supply device has supplied the raw material gas, the difference between the second chromaticity and the third chromaticity is less than the predetermined difference, or if the third chromaticity is greater than the second threshold value.

[0012] In claim 6, the reaction vessel can be filled with the solid phase and is provided with a rotating body that can move on a surface where the gas is supplied by the gas supply device and where light is irradiated by the irradiation device. [Effects of the Invention]

[0013] The present invention has the following effects.

[0014] In the invention according to claim 1, the product can be produced efficiently.

[0015] In the invention according to claim 2, it is possible to prevent the supply of raw material gases before the preparation for the reaction is complete.

[0016] In the invention according to claim 3, it is possible to prevent the supply of raw material gases before the reaction is fully prepared. Furthermore, by giving priority to light irradiation among light irradiation and gas supply, it is possible to prevent unnecessary gas consumption.

[0017] In the invention according to claim 4, the product can be recovered in a state where the reaction of the raw material gas has progressed sufficiently.

[0018] In the invention according to claim 5, it is possible to prevent the product from being recovered when the reaction of the raw material gas has not progressed sufficiently.

[0019] In the invention according to claim 6, the reaction efficiency can be improved. [Brief explanation of the drawings]

[0020] [Figure 1] 1 is a schematic diagram showing a reaction apparatus according to a first embodiment of the present invention. [Figure 2] FIG. 1 is a block diagram showing the configuration of a reaction apparatus. [Figure 3] A diagram showing the methanol production process. [Figure 4] 1 is a flowchart showing a reaction preparation process. [Figure 5] 1 is a flowchart showing a reaction process and a product recovery process. [Figure 6] 10(a) is a diagram showing a reaction vessel of a reaction apparatus according to another embodiment, and FIG. DETAILED DESCRIPTION OF THE INVENTION

[0021] The configuration of a reaction apparatus 1 according to a first embodiment of the present invention will be described below with reference to FIG.

[0022] The reactor 1 generates product Y through a chemical reaction of raw material gas X using a catalyst in a reaction vessel 10. In this embodiment, an example will be described in which methane is used as raw material gas X and methanol is generated as product Y. A substance that promotes the reaction of raw material gas X is used as the catalyst, and in this embodiment, zeolite is used. Zeolite is a microporous crystalline aluminosilicate. The chemical reaction in the reaction vessel 10 will be described in detail later. The reactor 1 includes a reaction vessel 10, an irradiation device 20, a heating device 30, a gas replacement device 40, a color measurement device 50, a distillation device 60, a solvent recovery device 70, a product recovery device 80, and a control device 90.

[0023] The reaction vessel 10 contains substances necessary for the reaction, such as a catalyst and raw material gas X. The shape of the reaction vessel 10 is not limited, but in this embodiment, it is formed into a hollow cylindrical shape with a bottom. The reaction vessel 10 is formed of a material that can transmit light.

[0024] As shown in FIG. 1, a "gas phase A" and a "solid phase B" are formed in the reaction vessel 10 in this order from top to bottom. The "gas phase A" is a phase composed of gas G and the like supplied from the gas replacement device 40 described below. The "solid phase B" is a phase composed of a catalyst. The solid phase B is packed into the reaction vessel 10 with a small space between them at the bottom of the reaction vessel 10. The solid phase B is preferably packed in multiple stages with gaps between them above and below to increase the surface area. Increasing the surface area of ​​the solid phase B can improve the efficiency of the reaction.

[0025] The irradiation device 20 irradiates the inside of the reaction vessel 10 with light. The irradiation device 20 is disposed to the side of the solid phase B and is configured so as to be able to irradiate the solid phase B with light. The irradiation device 20 is equipped with a light source that emits light of a wavelength required for the reaction. As the light source, an LED, halogen, or the like can be used. As the light source, various light sources that can irradiate light of a wavelength required for the reaction can be used.

[0026] The heating device 30 heats the inside of the reaction vessel 10. The heating device 30 is disposed below the solid phase B and is provided so as to be able to heat the solid phase B.

[0027] The gas replacement device 40 supplies the raw material gas X and the gas G required for preparing the reaction of the raw material gas X to the reaction vessel 10. The gas replacement device 40 replaces the gas phase A inside the reaction vessel 10 by supplying the raw material gas X and the gas G to the reaction vessel 10. In this embodiment, hydrogen and oxygen are used as the gas G. The gas replacement device 40 includes a gas phase adjustment device 41, a hydrogen intake path 42, an oxygen intake path 43, a raw material gas intake path 44, a gas supply path 45, a gas recovery path 46, and an exhaust path 47.

[0028] The gas phase adjusting device 41 adjusts the gas to be supplied into the reaction vessel 10. The gas phase adjusting device 41 is configured to be able to accommodate gases (gas G and raw material gas X).

[0029] The hydrogen intake path 42 is a path for taking in hydrogen, which is one of the gases G necessary for preparing the reaction of the raw material gas X, into the gas phase adjustment device 41. One end of the hydrogen intake path 42 is connected to a tank (not shown) filled with hydrogen. The other end of the hydrogen intake path 42 is connected to the gas phase adjustment device 41. A valve 42a that can open and close the flow path of the hydrogen intake path 42 is provided in the middle of the hydrogen intake path 42. By opening the valve 42a, hydrogen can be taken into the gas phase adjustment device 41 from the tank (not shown).

[0030] The oxygen intake path 43 is a path for taking oxygen, which is one of the gases G necessary for preparing the reaction of the raw material gas X, into the gas phase adjustment device 41. One end of the oxygen intake path 43 is connected to a tank (not shown) filled with oxygen. The other end of the oxygen intake path 43 is connected to the gas phase adjustment device 41. A valve 43a capable of opening and closing the flow path of the oxygen intake path 43 is provided in the middle of the oxygen intake path 43. By opening the valve 43a, oxygen can be taken into the gas phase adjustment device 41 from the tank (not shown).

[0031] The raw material gas intake path 44 is a path for taking in methane, which is the raw material gas X, into the gas-phase adjustment device 41. One end of the raw material gas intake path 44 is connected to a tank (not shown) filled with the raw material gas X (methane). The other end of the raw material gas intake path 44 is connected to the gas-phase adjustment device 41. A valve 44a that can open and close the flow path of the raw material gas intake path 44 is provided in the middle of the raw material gas intake path 44. By opening the valve 44a, the raw material gas X (methane) can be taken into the gas-phase adjustment device 41 from the tank (not shown).

[0032] The gas supply path 45 is a path for supplying the raw material gas X and the gas G from the gas phase adjustment device 41 to the reaction vessel 10. One end of the gas supply path 45 is connected to the gas phase adjustment device 41. The other end of the gas supply path 45 is connected to the bottom of the reaction vessel 10. Specifically, the other end of the gas supply path 45 is connected so as to communicate with the space between the bottom of the reaction vessel 10 and the solid phase B filled inside the reaction vessel 10. A pump 45a is provided in the middle of the gas supply path 45. By operating the pump 45a, the raw material gas X and the gas G can be supplied from the gas phase adjustment device 41 to the reaction vessel 10.

[0033] The gas recovery path 46 is a path for recovering gas from the reaction tank 10 to the gas phase adjustment device 41. One end of the gas recovery path 46 is connected to the reaction tank 10. Specifically, one end of the gas recovery path 46 is connected to a position corresponding to the gas phase A filled inside the reaction tank 10. The other end of the gas recovery path 46 is connected to the gas phase adjustment device 41. A valve 46a capable of opening and closing the flow path of the gas recovery path 46 is provided in the middle of the gas recovery path 46. By opening the valve 46a, gas can be recovered from the reaction tank 10 to the gas phase adjustment device 41.

[0034] The exhaust path 47 is a path for exhausting gas from the gas phase adjustment device 41 to the outside of the gas phase adjustment device 41. One end of the exhaust path 47 is connected to the gas phase adjustment device 41. The other end of the exhaust path 47 is open to the outside of the gas phase adjustment device 41.

[0035] The colorimetric measurement device 50 measures the colorimetric value (Lab value) of the surface of the solid phase B made of the catalyst. In this embodiment, a colorimeter is used as the colorimetric measurement device 50. The colorimetric measurement device 50 is disposed to the side of the solid phase B and is provided so as to be able to measure the colorimetric value of the surface of the solid phase B.

[0036] The distillation apparatus 60 is used to distill the solution recovered from the reaction tank 10. The distillation apparatus 60 is connected to the upper part of the reaction tank 10 via a solution recovery path 61. The distillation apparatus 60 can recover a mixed solution in which the product Y (methanol) is dissolved in a solvent via the solution recovery path 61. The distillation apparatus 60 can then separate the product Y (methanol) from the solvent by distilling the recovered mixed solution.

[0037] The solvent recovery device 70 recovers the solvent separated in the distillation device 60. The solvent recovery device 70 is connected to the distillation device 60 via a solvent recovery path 71. The solvent recovery device 70 can recover the solvent via the solvent recovery path 71.

[0038] The product recovery apparatus 80 recovers the product Y (methanol) separated in the distillation apparatus 60. The product recovery apparatus 80 is connected to the distillation apparatus 60 via a product recovery path 81. The product recovery apparatus 80 can recover the product Y (methanol) via the product recovery path 81.

[0039] The control device 90 shown in Fig. 2 is capable of processing various types of information. The control device 90 includes a CPU, a memory, and the like. As shown in Fig. 2, the control device 90 is electrically connected to the irradiation device 20, the heating device 30, the gas replacement device 40, the color measurement device 50, the distillation device 60, the solvent recovery device 70, and the product recovery device 80 of the reaction device 1. The control device 90 is configured to be able to acquire the measurement results of the color measurement device 50. The control device 90 is also configured to be able to control the operations of the irradiation device 20, the heating device 30, the gas replacement device 40, the distillation device 60, the solvent recovery device 70, and the product recovery device 80 based on the measurement results of the color measurement device 50.

[0040] The process of producing methanol will be explained below with reference to FIG.

[0041] First, a zeolite with ammonium groups (NH4) added to aluminum (Al) is used as a catalyst. By adding zinc nitrate (Zn(NO3)2) to solid phase B, which is made of this zeolite, the ammonium groups (NH4) in solid phase B are replaced with zinc (Zn).

[0042] Next, in a state where solid phase B is filled with hydrogen (H2), it is heated at approximately 300°C, whereby hydrogen (H) is added to zinc (Zn) in solid phase B.

[0043] Next, when solid phase B is filled with oxygen (O2), it is irradiated with light (Hv), causing a photoreaction in which the hydrogen (H) in solid phase B is replaced with oxygen (O), resulting in solid phase B containing Al-Zn-O.

[0044] In this way, the solid phase B (catalyst) is heated while filled with hydrogen (H2) and irradiated with light while filled with oxygen (O2), resulting in a composition (Al-Zn-O) to which methane can be added.

[0045] Next, methane (CH4) is supplied to the solid phase B, and a methyl group (CH3) is added to the oxygen (O) of the solid phase B.

[0046] Next, hydrogen (H) is supplied to the solid phase B, which separates the solid phase B into methanol (CHOH) and the remaining portion (Al-Zn-H). In this way, methanol can be produced and recovered.

[0047] 4 and 5, the production control of product Y (methanol) in the reaction apparatus 1 will be described. The processes from steps S11 to S26 shown in FIG. 4 correspond to a reaction preparation process for adjusting the solid phase B (catalyst) to a composition to which raw material gas X (methane) can be added. The processes from steps S27 to S31 shown in FIG. 5 correspond to a reaction process for reacting raw material gas X (methane) to produce product Y (methanol). The processes from steps S32 and S33 shown in FIG. 5 correspond to a recovery process for recovering product Y (methanol).

[0048] 4, the control device 90 operates a catalyst supply device (not shown) to fill the catalyst (zeolite) into the reaction vessel 10. The catalyst may be filled by an operator. As a result, the lower part of the reaction vessel 10 is filled with a solid phase B composed of the catalyst.

[0049] The catalyst (zeolite) may have its ammonium groups (NH4) replaced with zinc (Zn), or the ammonium groups (NH4) may be replaced with zinc (Zn) using zinc nitrate (Zn(NO3)2) in the reaction vessel 10.

[0050] After performing the process of step S11, the control device 90 proceeds to step S12.

[0051] In step S12, the control device 90 determines whether the amount of filled solid phase B has reached a specified amount. The amount of filled solid phase B is measured by any method.

[0052] If the control device 90 determines that the amount of solid phase B filled has reached the specified amount ("YES" in step S12), it proceeds to step S13. On the other hand, if the control device 90 determines that the amount of solid phase B filled has not reached the specified amount ("NO" in step S12), it returns the process to step S11. In this way, the reaction vessel 10 is filled with solid phase B until the amount of solid phase B filled reaches the specified amount.

[0053] In step S13, the control device 90 fills hydrogen (H2) into the solid phase B in the reaction tank 10. Specifically, the control device 90 opens the valve 42a and causes the gas phase adjustment device 41 to take in hydrogen via the hydrogen intake path 42. Then, the control device 90 operates the pump 45a to supply hydrogen from the gas phase adjustment device 41 to the reaction tank 10 via the gas supply path 45. In this way, the solid phase B in the reaction tank 10 is filled with hydrogen.

[0054] After performing the process of step S13, the control device 90 proceeds to step S14.

[0055] In step S14, the control device 90 determines whether the amount of hydrogen charged into the solid phase B has reached a specified amount. The specified amount of hydrogen charged is set to a charging amount necessary for the reaction of the solid phase B. The amount of hydrogen charged into the solid phase B is measured by any method.

[0056] If the control device 90 determines that the amount of hydrogen filled has reached the specified amount ("YES" in step S14), it proceeds to step S15. On the other hand, if the control device 90 determines that the amount of hydrogen filled has not reached the specified amount ("NO" in step S14), it returns the process to step S13. In this way, hydrogen is supplied to the reaction vessel 10 until the amount of hydrogen filled into the solid phase B reaches the specified amount.

[0057] In step S15, the control device 90 operates the heating device 30 to heat the solid phase B in the reaction vessel 10. The heating temperature by the heating device 30 is set to a temperature at which hydrogen can be added to the solid phase B, for example, 300°C. The heating time by the heating device 30 is also set to a time at which hydrogen can be added to the solid phase B. In this way, by heating the solid phase B in a state where the solid phase B is filled with hydrogen, hydrogen is added to the zinc (Zn) in the solid phase B.

[0058] After performing the process of step S15, the control device 90 proceeds to step S16.

[0059] In step S16, the control device 90 uses the colorimetric measurement device 50 to measure (acquire) the colorimetric value (Lab value) of the surface of the solid phase B. Here, the color of the surface of the solid phase B before oxygen is added is white. Hereinafter, the colorimetric value acquired in step S16 (the colorimetric value of the surface of the solid phase B before light irradiation in step S19, which will be described later) is referred to as the "first colorimetric value."

[0060] After performing the process of step S16, the control device 90 proceeds to step S17.

[0061] In step S17, the control device 90 fills the solid phase B in the reaction vessel 10 with oxygen (O2). Specifically, the control device 90 opens the valve 43a and causes the gas phase adjustment device 41 to take in oxygen via the oxygen intake path 43. The control device 90 then operates the pump 45a to supply oxygen from the gas phase adjustment device 41 to the reaction vessel 10 via the gas supply path 45, and opens the valve 46a to recover hydrogen (H2) into the gas phase adjustment device 41 via the gas recovery path 46. In this way, the gas phase A in the reaction vessel 10 is replaced with oxygen, and the solid phase B is filled with oxygen.

[0062] After performing the process of step S17, the control device 90 proceeds to step S18.

[0063] In step S18, the control device 90 determines whether the amount of oxygen charged into the solid phase B has reached a specified amount. The specified amount of oxygen charged is set to a charging amount necessary for the reaction of the solid phase B. The amount of oxygen charged into the solid phase B is measured by any method.

[0064] If the controller 90 determines that the amount of oxygen filled has reached the specified amount ("YES" in step S18), the process proceeds to step S19. On the other hand, if the controller 90 determines that the amount of oxygen filled has not reached the specified amount ("NO" in step S18), the process returns to step S17. In this way, oxygen is supplied to the reaction vessel 10 until the amount of oxygen filled into the solid phase B reaches the specified amount.

[0065] In step S19, the control device 90 operates the irradiation device 20 to irradiate light from the irradiation device 20 toward the solid phase B. The light irradiated from the irradiation device 20 is light of a wavelength necessary for the reaction of the solid phase B.

[0066] After performing the process of step S19, the control device 90 proceeds to step S20.

[0067] In step S20, the control device 90 determines whether the light irradiation time has reached a specified time. The specified light irradiation time is set to the irradiation time required for the reaction of the solid phase B.

[0068] When the control device 90 determines that the light irradiation time has reached the specified time ("YES" in step S20), the process proceeds to step S21. On the other hand, when the control device 90 determines that the light irradiation time has not reached the specified time ("NO" in step S20), the process returns to step S19. In this way, light is irradiated from the irradiation device 20 toward the solid phase B until the light irradiation time reaches the specified time.

[0069] In step S21, the control device 90 stops the irradiation of light by the irradiation device 20 (light irradiation).

[0070] After performing the process of step S21, the control device 90 proceeds to step S22.

[0071] In step S22, the control device 90 uses the chromaticity measuring device 50 to measure (acquire) the chromaticity (Lab value) of the surface of the solid phase B. Hereinafter, the chromaticity acquired in step S22 (the chromaticity of the surface of the solid phase B after light irradiation in step S19) will be referred to as the "second chromaticity."

[0072] After performing the process of step S22, the control device 90 proceeds to step S23.

[0073] In step S23, the control device 90 determines whether the amount of change in chromaticity of the surface of the solid phase B is equal to or greater than a specified value. More specifically, the control device 90 determines whether the amount of change in the b value, among the Lab values ​​of chromaticity of the surface of the solid phase B, is equal to or greater than a specified value.

[0074] Here, the surface color of solid phase B before oxygen is added to solid phase B (step S16) is white, but when oxygen is added to solid phase B by the photoreaction, the surface of solid phase B changes to a slightly yellowish color. When the surface color of solid phase B changes from white to yellowish, the b value in the Lab value of chromaticity increases. As an example, the b value of the surface of solid phase B before oxygen is added is 0.92, while the b value of the surface of solid phase B after oxygen is added increases to 0.97.

[0075] Therefore, in step S23, the control device 90 determines whether the difference between the b value of the first chromaticity measured in step S16 and the b value of the second chromaticity measured in step S21 (more specifically, the value obtained by subtracting the b value of the first chromaticity from the b value of the second chromaticity) is equal to or greater than a specified value. The specified value is set based on the actual b values ​​of the solid phase B before and after the addition of oxygen, and is set to, for example, 0.05.

[0076] Alternatively, in step S23, the control device 90 may determine whether the second chromaticity measured in step S22 is equal to or greater than a first threshold value. Here, the first threshold value is set based on the actual value of the b value of solid phase B after oxygen addition, and is set to, for example, 0.97. Note that when determining whether the second chromaticity is equal to or greater than the first threshold value, the process of step S16 does not need to be performed.

[0077] If the control device 90 determines that the amount of change in chromaticity of the surface of solid phase B is equal to or greater than the specified value (or the second chromaticity is equal to or greater than the first threshold value) ("YES" in step S23), the control device 90 proceeds to step S26. On the other hand, if the control device 90 determines that the amount of change in chromaticity of the surface of solid phase B is not equal to or greater than the specified value (or the second chromaticity is not equal to or greater than the first threshold value) ("NO" in step S23), the control device 90 proceeds to step S24.

[0078] In step S24, the control device 90 determines whether or not light irradiation has been re-executed by the irradiation device 20. That is, the control device 90 determines whether or not further light irradiation has been executed (whether light irradiation has been executed two or more times) after the first light irradiation for the specified time (steps S19 and S20).

[0079] If light irradiation has not been re-executed (NO in step S24), the control device 90 proceeds to step S19 and executes light irradiation for the specified time again by the irradiation device 20. On the other hand, if light irradiation has been re-executed (YES in step S24), the control device 90 proceeds to step S25.

[0080] In step S25, the control device 90 determines whether or not oxygen filling has been re-executed by the gas replacement device 40. That is, the control device 90 determines whether or not oxygen filling has been further performed (whether oxygen filling has been performed two or more times) after the first specified amount of oxygen filling (steps S17 and S18).

[0081] If oxygen filling has not been re-executed (NO in step S25), the control device 90 proceeds to step S17 and re-executes filling of a specified amount of oxygen by the gas replacement device 40. On the other hand, if oxygen filling has been re-executed (YES in step S25), the control device 90 proceeds to step S26.

[0082] In step S25, the control device 90 determines whether or not hydrogen filling has been performed again by the gas replacement device 40. That is, the control device 90 determines whether or not further hydrogen filling has been performed (whether hydrogen filling has been performed two or more times) after the first specified amount of hydrogen filling (steps S13 and S14).

[0083] The reaction preparation step is completed by the above-described processes from step S11 to step S26. By performing such a reaction preparation step, the solid phase B (catalyst) can have a composition (Al—Zn—O) to which methane, which is the raw material gas X, can be added.

[0084] 5, the control device 90 fills the solid phase B in the reaction vessel 10 with methane (CH3), which is the raw material gas X. Specifically, the control device 90 opens the valve 44a and causes the gas phase adjustment device 41 to take in methane via the raw material gas intake path 44. The control device 90 then operates the pump 45a to supply methane from the gas phase adjustment device 41 to the reaction vessel 10 via the gas supply path 45, and opens the valve 46a to recover oxygen (O2) into the gas phase adjustment device 41 via the gas recovery path 46. In this way, the gas phase A in the reaction vessel 10 is replaced with methane, and the solid phase B is filled with methane.

[0085] In step S28, the control device 90 waits for t minutes, where t minutes is set to the time required for methane to be added to the solid phase B.

[0086] After performing the process of step S28, the control device 90 proceeds to step S29.

[0087] In step S29, the control device 90 uses the chromaticity measuring device 50 to measure (acquire) the chromaticity (Lab value) of the surface of the solid phase B. Hereinafter, the chromaticity acquired in step S29 (the chromaticity of the surface of the solid phase B after the supply of methane, which is the raw material gas X) will be referred to as the "third chromaticity."

[0088] After performing the process of step S29, the control device 90 proceeds to step S30.

[0089] In step S30, the control device 90 determines whether the amount of change in chromaticity of the surface of the solid phase B is equal to or greater than a specified value. More specifically, the control device 90 determines whether the amount of change in the b value among the Lab values ​​of the surface of the solid phase B is equal to or greater than a specified value.

[0090] Here, the surface color of solid phase B after the addition of oxygen changes from white to a slightly yellowish color, but when methane is added to solid phase B, the surface color of solid phase B returns to white. When the surface color of solid phase B returns to white, the b value, which is one of the Lab values ​​of chromaticity, decreases. For example, the b value of the surface of solid phase B before the addition of methane is 0.97, while the b value of the surface of solid phase B after the addition of methane decreases to 0.92.

[0091] Therefore, in step S30, the control device 90 determines whether the difference between the b value of the second chromaticity measured in step S21 and the b value of the third chromaticity measured in step S30 (more specifically, the value obtained by subtracting the b value of the third chromaticity from the b value of the second chromaticity) is equal to or greater than a specified value. The specified value is set based on the actual b values ​​of the solid phase B before and after the addition of methane, and is set to, for example, 0.05.

[0092] Alternatively, in step S30, the control device 90 may determine whether the third chromaticity measured in step S30 is equal to or greater than a second threshold. The second threshold is set to a value smaller than the first threshold (step S22). The second threshold is set based on the actual value of the b value of the solid phase B after the addition of methane, for example, to 0.92.

[0093] If the control device 90 determines that the amount of change in chromaticity of the surface of the solid phase B is equal to or greater than the specified value (or that the third chromaticity is equal to or greater than the second threshold value) ("YES" in step S30), the control device 90 proceeds to step S31. On the other hand, if the control device 90 determines that the amount of change in chromaticity of the surface of the solid phase B is not equal to or greater than the specified value (or that the third chromaticity is not equal to or greater than the second threshold value) ("NO" in step S30), the control device 90 returns the process to step S27 and performs methane injection again.

[0094] In step S31, the control device 90 stops the blowing of the raw material gas X (methane) by the gas replacement device 40. Thereafter, the control device 90 blows hydrogen from the gas replacement device 40 into the solid phase B, thereby separating the solid phase B into methanol (CHOH) and the remaining portion (Al-Zn-H).

[0095] The reaction process is completed by the above-described processes from step S27 to step S31. By this reaction process, the raw material gas X (methane) can be reacted to produce methanol.

[0096] After performing the process of step S31, the control device 90 proceeds to step S32.

[0097] In step S32, the control device 90 operates a liquid delivery device (not shown) to supply a solvent for recovering the product Y (methanol) to the solid phase B in the reaction vessel 10. The solvent used is an organic solvent capable of dissolving methanol. The solvent may be supplied by an operator.

[0098] After performing the process of step S32, the control device 90 proceeds to step S33.

[0099] In step S33, the control device 90 distills the mixed solution in which methanol is dissolved in the solvent in the distillation device 60. Specifically, the control device 90 recovers the mixed solution in the distillation device 60 via the solution recovery path 61, and distills the recovered mixed solution in the distillation device 60. As a result, the mixed solution is separated into the solvent and methanol, and the solvent is recovered in the solvent recovery device 70 via the solvent recovery path 71, and the methanol is recovered in the product recovery device 80 via the product recovery path 81.

[0100] After performing the process of step S33, the control device 90 proceeds to step S34.

[0101] In step S34, the control device 90 determines whether the number of cycles has reached a specified number of cycles. Specifically, assuming that the processes from step S11 to S33 constitute one cycle, the control device 90 determines whether the number of cycles has reached a specified number of cycles. The specified number of cycles is set based on the target production amount of the required product Y, for example, and is set to 10 cycles.

[0102] If the number of cycles reaches the specified number of cycles (YES in step S34), the control device 90 ends the methanol production control. On the other hand, if the number of cycles does not reach the specified number of cycles (NO in step S34), the control device 90 returns to step S11 shown in FIG.

[0103] As described above, the reaction apparatus 1 according to this embodiment is configured so that the raw material gas X (methane) and the gas G (hydrogen and oxygen) required for preparing the reaction of the raw material gas X can be supplied to the reaction vessel 10 by the gas replacement device 40. The reaction apparatus 1 is also configured so that the product Y, ie, methanol, can be recovered by the distillation device 60 and the product recovery device 80. In this way, the supply of the raw material gas X and the recovery of the product Y can be performed continuously, and therefore the product Y can be produced continuously.

[0104] Furthermore, in the reaction apparatus 1 according to this embodiment, the progress of the reaction can be confirmed by checking the color of the surface of the solid phase B during the production process. If it is determined based on the color that the reaction has not progressed sufficiently, the process is not carried out further, and each process (light irradiation, oxygen filling, and hydrogen filling) is performed again as necessary. In this way, if the reaction has not progressed sufficiently, the reaction can be stably progressed by performing each process again in order.

[0105] As described above, the reaction apparatus 1 according to this embodiment has the following features: A reactor 1 for producing a product Y (e.g., methanol) by reacting a raw material gas X (e.g., methane) using a catalyst, a reaction vessel 10 capable of accommodating a solid phase B composed of the catalyst; a gas replacement device 40 (gas supply device) capable of supplying gas G (hydrogen and oxygen) to the solid phase B in preparation for the reaction of the raw material gas X; an irradiation device 20 capable of irradiating the solid phase B with light in preparation for the reaction of the raw material gas X; a gas replacement device 40 (raw material supply device) capable of supplying the raw material gas X to the solid phase B; a distillation apparatus 60 and a product recovery apparatus 80 (product recovery apparatus) for recovering the product Y produced by the reaction of the raw material gas X from the reaction tank 10; a colorimeter 50 capable of measuring the colorimeter of the solid phase B; a control device 90 that controls the gas replacement device 40 (gas supply device) to supply the raw material gas X to the solid phase B (step S27) when, after the gas replacement device 40 (gas supply device) has supplied the gas G (steps S13, S14, S17, and S18) and the irradiation device 20 has irradiated light (steps S19 and S20), a difference between a first chromaticity that is the chromaticity of the solid phase B before the light irradiation (step S16) and a second chromaticity that is the chromaticity of the solid phase B after the light irradiation (step S22) becomes equal to or greater than a predetermined difference (for example, a value obtained by subtracting the b value of the first chromaticity from the b value of the second chromaticity is 0.05 or greater) (YES in step S23), or when the second chromaticity becomes equal to or greater than a first threshold (for example, the b value of the second chromaticity is 0.97 or greater) (YES in step S23); It is equipped with the following.

[0106] By configuring in this way, the product Y can be produced efficiently. Specifically, since the supply of the raw material gas X and the recovery of the product Y can be carried out continuously, the efficiency of the production of the product Y can be improved. Furthermore, the degree of progress of the reaction of the solid phase B is determined based on the chromaticity (second chromaticity) of the surface of the solid phase B after the light irradiation, and the raw material gas X is supplied to the solid phase B only after it is determined that the reaction of the solid phase B has progressed sufficiently, so that the reaction of the raw material gas X can be stably carried out.

[0107] The control device 90 also After the gas replacement device 40 (gas supply device) supplies the gas G (steps S13, S14, S17, S18) and the irradiation device 20 irradiates light (steps S19, S20), if the difference between the first chromaticity and the second chromaticity is less than the predetermined difference (for example, the value obtained by subtracting the b value of the first chromaticity from the b value of the second chromaticity is less than 0.05) (NO in step S23), or if the second chromaticity is less than the first threshold value (for example, the b value of the second chromaticity is less than 0.97) (NO in step S23), the gas replacement device 40 (gas supply device) or the irradiation device 20 is controlled to supply the gas G (steps S13, S14, or steps S17, S18) or irradiate light (steps S19, S20) again.

[0108] By configuring in this way, it is possible to prevent the supply of the source gas X from occurring before the reaction is fully prepared. Specifically, the degree of progress of the reaction of solid phase B is determined based on the chromaticity (second chromaticity) of the surface of solid phase B after light irradiation, and if it is determined that the reaction of solid phase B has not progressed sufficiently, gas G is supplied or light is irradiated again, thereby allowing the reaction of solid phase B to progress.

[0109] The control device 90 also After the gas replacement device 40 (gas supply device) supplies the gas G (steps S13, S14, S17, S18) and the irradiation device 20 irradiates light (steps S19, S20), if the difference between the first chromaticity and the second chromaticity is less than the predetermined difference (for example, the value obtained by subtracting the b value of the first chromaticity from the b value of the second chromaticity is less than 0.05) (NO in step S23), or if the second chromaticity is less than the first threshold value (for example, the b value of the second chromaticity is less than 0.97) (NO in step S23), the light irradiation (steps S19, S20) is performed again, After the light irradiation, if the difference between the first chromaticity and the second chromaticity is less than the predetermined difference (NO in step S23), or if the second chromaticity is less than the first threshold value (NO in step S23), the gas replacement device 40 (gas supply device) is controlled to supply the gas G again (steps S13, S14, or steps S17, S18).

[0110] This configuration can prevent the supply of the raw material gas X from being performed before the reaction is fully prepared. Furthermore, by giving priority to the re-execution of light irradiation between the light irradiation and the supply of the gas G, it is possible to prevent unnecessary consumption of the gas G.

[0111] The control device 90 also After the supply of the raw material gas X by the gas replacement apparatus 40 (raw material supply apparatus) (step S27) is performed, if the difference between the second chromaticity (step S22) and the third chromaticity (step S29), which is the chromaticity of the solid phase after the supply of the raw material gas X, is equal to or greater than the predetermined difference (for example, a value obtained by subtracting the b value of the third chromaticity from the b value of the second chromaticity is 0.05 or greater) (YES in step S30), or if the third chromaticity is equal to or less than a second threshold value that is smaller than the first threshold value (for example, the b value of the third chromaticity is 0.92 or less) (YES in step S30), the distillation apparatus 60 and the product recovery apparatus 80 (product recovery apparatus) are controlled to recover the product Y from the solid phase B (steps S32 and S33).

[0112] By configuring in this way, the product Y can be recovered in a state where the reaction of the raw material gas X has progressed sufficiently. Specifically, the degree of progress of the reaction of the raw material gas X is determined based on the chromaticity (third chromaticity) of the surface of the solid phase B after the supply of the raw material gas X, and when it is determined that the reaction of the raw material gas X has progressed sufficiently, the product Y is recovered, thereby improving the efficiency of recovery of the product Y.

[0113] The control device 90 also After the supply of the raw material gas X by the gas replacement apparatus 40 (raw material supply apparatus) (step S27), if the difference between the third chromaticity and the second chromaticity is less than the predetermined difference (for example, the value obtained by subtracting the b value of the third chromaticity from the b value of the second chromaticity is less than 0.05) (NO in step S30), or if the third chromaticity is greater than the second threshold value (for example, the b value of the third chromaticity is greater than 0.92) (NO in step S30), the gas replacement apparatus 40 (raw material supply apparatus) is controlled to supply the raw material gas X again (step S27).

[0114] By configuring in this way, it is possible to prevent the product Y from being recovered in a state where the reaction of the raw material gas X has not progressed sufficiently. Specifically, the degree of progress of the reaction of the raw material gas X is determined based on the chromaticity (third chromaticity) of the surface of the solid phase B after the supply of the raw material gas X, and if it is determined that the reaction of the raw material gas X has not progressed sufficiently, the supply of the raw material gas X is performed again, thereby allowing the reaction of the raw material gas X to proceed.

[0115] Although the embodiments of the present invention have been described above, the present invention is not limited to the above-described embodiments. For example, the configuration of each part constituting the reaction apparatus 1 is not limited to the above-described ones and can be changed as appropriate.

[0116] Furthermore, in the above embodiment, an example in which methanol is produced as the product Y has been described, but the present invention is not limited to this. For example, alcohol may be used as the product Y. Furthermore, the product Y is not limited to the above example, and various substances produced by reacting the raw material gas X using a catalyst may be used.

[0117] Furthermore, in this embodiment, an example in which methane is used as the raw material gas X has been described, but the present invention is not limited to this. Various gases can be used as the raw material gas X depending on the product Y. Furthermore, in this embodiment, an example in which zeolite is used as the catalyst (solid phase B) has been described, but the present invention is not limited to this. Various catalysts can be used depending on the product Y. Furthermore, in this embodiment, an example in which hydrogen and oxygen are used as the gas G for preparing the reaction has been described, but the present invention is not limited to this. Various gases can be used depending on the catalyst (solid phase B) and the product Y.

[0118] Furthermore, in this embodiment, a colorimeter is used as the colorimeter measuring device 50 for measuring the colorimeter of solid phase B, but the method for measuring the colorimeter of solid phase B is not limited to this, and the colorimeter of solid phase B may also be measured by image processing, for example.

[0119] There may be provided a plurality of irradiation devices 20. When a plurality of irradiation devices 20 are provided, the irradiation devices 20 are provided along the periphery of the reaction vessel 10 at intervals.

[0120] 4, if oxygen filling has not been re-executed (NO in step S25), the second chromaticity measurement (step S22) may be performed after oxygen filling is re-executed (steps S17 and S18) without performing light irradiation (steps S19 to S21). Also, in the flow shown in Fig. 4, if hydrogen filling has not been re-executed (NO in step S26), the second chromaticity measurement (step S22) may be performed after hydrogen filling is re-executed (steps S13 and S14) without performing oxygen re-filling (steps S17 and S18) and light irradiation (steps S19 to S21).

[0121] Moreover, the reaction apparatus 1 may be provided with a reaction vessel 10A shown in Fig. 6 instead of the reaction vessel 10. The configuration of the reaction vessel 10A will be described below with reference to Fig. 6.

[0122] As shown in Figure 6(a), the reaction vessel 10A includes a rotor 11 and a container 12. The container 12 houses the rotor 11 and supports the rotor 11 so that it can rotate about an axis extending vertically. The container 12 is made of a material that is transparent to light.

[0123] A slit 11a that can be filled with the solid phase B is formed on the surface of the rotor 11. The slit 11a is formed so that the surface of the rotor 11 is recessed. The slit 11a is formed in a spiral shape.

[0124] By rotating the rotor 11 configured in this manner, the surfaces to which the gas G is supplied by the gas replacement device 40 and the light is irradiated by the irradiation device 20 can be shifted (moved) in order. Furthermore, when the heating device 30 is disposed to the side of the solid phase B, the surfaces to which the gas G is supplied by the gas replacement device 40, the solid phase B is heated by the heating device 30, and the light is irradiated by the irradiation device 20 can be shifted (moved) in order. This can promote the reaction. In this case, as shown in FIG. 6(b), it is preferable that the hydrogen, oxygen, and raw material gas X are each supplied to the rotor 11 from different directions (different positions in the circumferential direction). This can promote the reaction more efficiently.

[0125] As described above, the reaction vessel 10A has The solid phase B can be filled, and the gas G is supplied by the gas replacement device 40 (gas supply device), and the light is irradiated by the irradiation device 20. The rotating body 11 can move on the surface.

[0126] By configuring in this way, the reaction can be promoted. [Explanation of symbols]

[0127] 1. Reactor 10, 10A Reactor 20 Irradiation device 40 Gas replacement device 50 Color measurement device 60 Distillation Apparatus 80 Product recovery device 90 Control device

Claims

1. A reactor that produces a product by reacting a raw material gas using a catalyst, a reaction vessel capable of accommodating a solid phase constituted by the catalyst; a gas supply device capable of supplying gas to the solid phase in preparation for the reaction of the raw material gas; an irradiation device capable of irradiating the solid phase with light in preparation for a reaction of the source gas; a raw material supply device capable of supplying the raw material gas to the solid phase; a product recovery device that recovers the product produced by the reaction of the raw material gas from the reaction tank; a colorimeter capable of measuring the colorimeter of the solid phase; a control device that controls the raw material supply device to supply the raw material gas to the solid phase when, after the gas supply device has supplied the gas and the irradiation device has irradiated the light, a difference between a first chromaticity that is the chromaticity of the solid phase before the light irradiation and a second chromaticity that is the chromaticity of the solid phase after the light irradiation becomes equal to or greater than a predetermined difference, or when the second chromaticity becomes equal to or greater than a first threshold value; A reactor comprising:

2. The control device after the gas supply device has supplied the gas and the irradiation device has irradiated the light, if the difference between the first chromaticity and the second chromaticity is less than the predetermined difference, or if the second chromaticity is less than the first threshold value, controlling the gas supply device or the irradiation device to supply the gas or irradiate the light again. The reactor of claim 1.

3. The control device after the gas is supplied by the gas supply device and the light is irradiated by the irradiation device, if the difference between the first chromaticity and the second chromaticity is less than the predetermined difference or if the second chromaticity is less than the first threshold, the light is irradiated again; after the irradiation of the light, if the difference between the first chromaticity and the second chromaticity is less than the predetermined difference, or if the second chromaticity is less than the first threshold value, controlling the gas supply device to supply the gas again. The reactor of claim 1.

4. The control device after the raw material gas is supplied by the raw material supply device, when a difference between the second chromaticity and a third chromaticity, which is the chromaticity of the solid phase after the raw material gas is supplied, becomes equal to or greater than the predetermined difference, or when the third chromaticity becomes equal to or less than a second threshold value that is smaller than the first threshold value, the product recovery device is controlled to recover the product from the solid phase. The reactor of claim 1.

5. The control device after the raw material supply device has supplied the raw material gas, if the difference between the second chromaticity and the third chromaticity is less than the predetermined difference, or if the third chromaticity is greater than the second threshold value, controlling the raw material supply device to supply the raw material gas again. The reactor of claim 4.

6. The reaction vessel comprises: a rotating body that can be filled with the solid phase and can move on a surface on which the gas is supplied by the gas supply device and the light is irradiated by the irradiation device; A reactor according to any one of claims 1 to 5.

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