Reaction device

The reaction apparatus addresses the challenge of reactant concentration measurement in two-phase chemical reactions by using a detection unit to separate and measure reactant concentrations, ensuring timely replenishment and maintaining optimal levels for efficient production.

JP2025147932APending Publication Date: 2025-10-07DAIWA HOUSE INDUSTRY CO LTD +1
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Patent Information

Application Number
JP2024048448
Authority / Receiving Office
JP · JP
Patent Type
Applications
Current Assignee / Owner
Filing Date
2024-03-25
Publication Date
2025-10-07

AI Technical Summary

Technical Problem

Existing methods for chemical reactions using two liquid phases struggle with accurately measuring reactant concentrations during the reaction, leading to inefficiencies due to improper timing of raw material replenishment, which can result in either low or excessive reactant concentrations.

Method used

A reaction apparatus with a detection unit that separates and measures the concentration of reactants in separate liquid phases within a reaction vessel, allowing for accurate detection and replenishment of reactants based on real-time consumption data.

Benefits of technology

Enables precise monitoring of reactant consumption, maintaining optimal reactant concentrations and enhancing reaction efficiency by ensuring timely replenishment, thereby improving production efficiency.

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Abstract

To provide a reaction device that can accurately detect the consumption amount of reactants while continuing the reaction in a reaction vessel.SOLUTION: A reaction device 100 for reacting a first reactant and a second reactant in a solution including a first solution S1 and a second solution S2 to generate a product, comprises: a reaction vessel 1 that can form therein a first liquid phase composed of the first solution S1 containing the first reactant and a second liquid phase composed of the second solution S2 containing the second reactant; a stirrer 2 that mixes the first solution S1 and the second solution S2 together to generate a mixing solution inside the reaction vessel 1; and a detection unit 30 for detecting the consumption amount of the first reactant or the second reactant inside the reaction vessel 1 by separating the mixed solution introduced from the reaction vessel 1 into the first liquid phase and the second liquid phase and measuring the concentration of the first reactant in the first liquid phase or the second reactant in the second liquid phase.SELECTED DRAWING: Figure 1
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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] In the invention described in Patent Document 1, an aqueous phase in which substances used in a chemical reaction are dissolved in water and an organic phase in which raw materials are dissolved in an organic solvent are placed in a reaction vessel, and light is irradiated onto each liquid phase to cause a chemical reaction and produce a product. In such a method of producing a product using two liquid phases (aqueous phase and organic phase), the raw materials are consumed as the product is produced, so it is necessary to replenish the reaction vessel with raw materials.

[0004] In this case, considering production efficiency, it is desirable to replenish raw materials while the reaction is continuing. However, when two solutions (water and organic solvent) are being stirred to promote the reaction, it is difficult to accurately measure the concentration of the raw materials in the solution. If the concentration of the raw materials in the solution cannot be accurately measured, it becomes difficult to set the appropriate timing for replenishment of the raw materials. Specifically, if the interval between replenishment of raw materials is too long, the concentration of the raw materials in the reaction vessel will be low for a long time, resulting in a decrease in reaction efficiency. On the other hand, if the interval between replenishment of raw materials is too short, the concentration of the raw materials in the reaction vessel will become too high. Therefore, it is desirable to accurately grasp the concentration of the raw materials (reactants) in the reaction vessel, and therefore the consumption of the raw materials, while the reaction is continuing in the reaction vessel. [Prior art documents] [Patent documents]

[0005] [Patent Document 1] Patent No. 6080281 Summary of the Invention [Problem to be solved by the invention]

[0006] The present invention has been made in view of the above circumstances, and the problem to be solved by the present invention is to provide a reaction apparatus that can accurately detect the consumption amount of reactants while the reaction is continued in the reaction vessel. [Means for solving the problem]

[0007] The problem to be solved by the present invention is as described above, and the means for solving this problem will now be described.

[0008] That is, claim 1 provides a reaction apparatus for producing a product by reacting a first reactant and a second reactant in a solution containing a first solution and a second solution, the reaction apparatus comprising: a reaction vessel capable of forming a first liquid phase constituted by the first solution containing the first reactant and a second liquid phase constituted by the second solution containing the second reactant; a mixing device for mixing the first solution and the second solution to produce a mixed solution inside the reaction vessel; and a detection unit for separating the mixed solution introduced from the reaction vessel into the first liquid phase and the second liquid phase, and detecting the consumption amount of the first reactant or the second reactant inside the reaction vessel by measuring the concentration of the first reactant in the first liquid phase or the second reactant in the second liquid phase.

[0009] In claim 2, the detection unit comprises a circulation unit that forms a flow path for the mixed solution introduced from the reaction vessel, a first valve that is provided upstream of the circulation unit and opens and closes the flow path, and a second valve that is provided downstream of the circulation unit and opens and closes the flow path.

[0010] In claim 3, the detection unit is provided in the middle of the flow section and comprises a storage section that stores the first liquid phase when the mixed solution separates into the first liquid phase and the second liquid phase, an emitter that can irradiate light toward the first liquid phase stored in the storage section, and a light-receiving section that can receive light that is irradiated from the emitter and passes through the first liquid phase, and calculates the absorbance of the first solution that constitutes the first liquid phase stored in the storage section based on the amount of light irradiated from the emitter and the amount of light received by the light-receiving section, and measures the concentration of the first reactant in the first liquid phase stored in the storage section based on the calculated absorbance.

[0011] In claim 4, the detection unit is provided in the middle of the flow section and includes a storage section that stores the first liquid phase when the mixed solution separates into the first liquid phase and the second liquid phase, and measures the concentration of the first reactant in the first liquid phase stored in the storage section based on the color difference between the first liquid phase containing the first reactant at a specified concentration and the first liquid phase stored in the storage section.

[0012] In claim 5, the reaction vessel is provided with a replenishing unit that replenishes the first reactant or the second reactant inside the reaction vessel based on the consumption amount of the first reactant or the second reactant detected by the detection unit. [Effects of the Invention]

[0013] The present invention has the following effects.

[0014] According to claim 1, the consumption amount of the reactant (the first reactant or the second reactant) can be detected with high accuracy while the reaction is continued in the reaction vessel.

[0015] In claim 2, the mixed solution can be separated into the first liquid phase and the second liquid phase in the detection unit with a simple configuration.

[0016] According to claim 3, the consumption amount of the reactant (first reactant) can be detected with high accuracy using a simple configuration.

[0017] According to claim 4, the consumption amount of the reactant (first reactant) can be detected with high accuracy using a simple configuration.

[0018] In claim 5, the reactant (first reactant) inside the reaction vessel can be maintained at an optimum concentration. [Brief explanation of the drawings]

[0019] [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 schematic diagram showing a reactor with a stirring device in operation. [Figure 3] FIG. 1 is a schematic diagram showing the configuration of a detection device. [Figure 4] FIG. 2 is a schematic diagram showing the configuration of a refilling device. [Figure 5] 10 is a flowchart showing raw material replenishment control. [Figure 6] (a) A diagram showing the detection device when the valve is open, (b) A diagram showing the detection device when the valve is closed and the liquid is separated into a first liquid phase and a second liquid phase, and (c) A diagram showing the detection device when light is irradiated from the light-emitting unit. DETAILED DESCRIPTION OF THE INVENTION

[0020] The configuration of a reaction apparatus 100 according to a first embodiment of the present invention will be described below with reference to FIGS.

[0021] The reaction device 100 produces a product through a chemical reaction of reactants in a liquid contained inside a reaction vessel 1. In this embodiment, an example in which methanol is produced as the product will be described as an example. The reactants include a first reactant and a second reactant. The first reactant is used to oxidize the second reactant. In this embodiment, sodium chlorite is used as the first reactant, and methane is used as the second reactant. In this specification, a decomposition product of the first reactant (e.g., chlorine dioxide) may also be referred to as the first reactant (sodium chlorite).

[0022] The liquids used in the reaction include a first solution S1 and a second solution S2, which are two types of liquids with different specific gravities. More specifically, the second solution S2 has a higher specific gravity than the first solution S1. Therefore, as shown in FIG. 1, the first solution S1 and the second solution S2 are separated in the reaction vessel 1 so that the second solution S2 is located below the first solution S1. As the first solution S1, a solution in which the solubility of the product is greater than that of the second solution S2 is used. As the second solution S2, a solution in which the solubility of the second reactant is greater than that of the first solution S1 is used. As the first solution S1, a solution in which the solubility of the first reactant is greater than that of the second solution S2 is used. As the first solution S1, for example, water is used. As the second solution S2, for example, a fluorous solvent is used.

[0023] The reaction apparatus 100 according to this embodiment can obtain a product by a chemical reaction between a first reactant and a second reactant in a liquid contained in a reaction vessel 1. A detailed description of the chemical reaction in the reaction vessel 1 will be given later. The reaction apparatus 100 includes a reaction vessel 1, a stirring device 2, an irradiation device 3, a detection device 4, a replenishment device 5, and a control device 6.

[0024] The reaction vessel 1 accommodates a first reactant (sodium chlorite), a second reactant (methane), a first solution S1, and a second solution S2. The shape of the reaction vessel 1 is not limited, but in this embodiment, it is formed into a hollow rectangular parallelepiped shape capable of accommodating the first reactant, the second reactant, the first solution S1, and the second solution S2 therein. The reaction vessel 1 is formed of a material that is resistant to the first reactant, the second reactant, the first solution S1, and the second solution S2.

[0025] As shown in FIG. 1, a "first liquid phase" and a "second liquid phase" are formed inside the reaction vessel 1, in this order from top to bottom. The "first liquid phase" is a phase (aqueous phase) composed of the first solution S1. The "second liquid phase" is a phase (solvent phase) composed of the second solution S2. In the state where the first and second liquid phases are separated, the first reactant (sodium chlorite) is contained in the first liquid phase, and the second reactant (methane) is contained in the second liquid phase.

[0026] The agitator 2 agitates the first solution S1 and the second solution S2 in the reaction vessel 1. The agitator 2 is provided inside the reaction vessel 1. The agitator 2 is equipped with a propeller or the like that rotates around a rotation axis whose axis is oriented in the vertical direction. Note that the agitator 2 is not limited to one equipped with a propeller, and various configurations that can agitate the first solution S1 and the second solution S2 can be employed. The agitator 2 can mix the first solution S1 and the second solution S2 by operating. Mixing the first solution S1 and the second solution S2 increases the contact area between the first solution S1 and the second solution S2, thereby accelerating the reaction. Note that the interior of the reaction vessel 1 separates again into the first liquid phase and the second liquid phase when a predetermined time has elapsed after agitation has stopped.

[0027] The irradiation device 3 irradiates light into the inside of the reaction vessel 1. The irradiation device 3 is disposed on the side of the reaction vessel 1 and is set up so as to irradiate light onto the solutions (first solution S1 and second solution S2) contained inside the reaction vessel 1. The irradiation device 3 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.

[0028] The reaction vessel 1, the stirring device 2, and the irradiation device 3 configured as above generate a product inside the reaction vessel 1. The process of generating a product in the reaction device 100 will be described below with reference to Figures 1 and 2. The detection device 4, the replenishing device 5, and the control device 6 will be described later.

[0029] A first liquid phase composed of a first solution S1 and a second liquid phase composed of a second solution S2 are formed in the reaction vessel 1 from the top to the bottom. A first reactant (sodium chlorite) is dissolved in the first solution S1 (first liquid phase), and a second reactant (methane) is dissolved in the second solution S2 (second liquid phase).

[0030] When the agitator 2 is operated, the first solution S1 and the second solution S2 are mixed, and a mixed solution is generated inside the reaction vessel 1 as shown in FIG. 2. In this state, the irradiation device 3 is operated to irradiate the mixed solution with light. As a result, the first reactant (sodium chlorite) becomes a radical (chlorine radical), and the radical (chlorine radical) oxidizes the second reactant (methane). This produces a product (methanol). Due to the difference in solubility between the first solution S1 and the second solution S2, the product (methanol) moves to the first liquid phase (not shown) above the mixed solution and is recovered by a recovery device (not shown). In this way, the reaction device 100 can produce and recover the product (methanol).

[0031] Here, as the production of the product progresses, the reactants are consumed along with the production of the product, and therefore it is necessary to replenish the raw materials (reactants) inside the reaction vessel 1. For this reason, the reaction apparatus 100 is provided with a detection device 4, a replenishment device 5, and a control device 6 as components for replenishing the first reactant (sodium chlorite) inside the reaction vessel 1.

[0032] The detection device 4 recovers the mixed solution from the reaction vessel 1 and detects the concentration of the first reactant (sodium chlorite) contained in the recovered mixed solution. The detection device 4 is provided outside the reaction vessel 1. The detection device 4 includes a recovery path 10, a detection-side pump 20, a detection unit 30, and a return path 40.

[0033] The recovery path 10 is a path for recovering the solution from inside the reaction vessel 1. One end of the recovery path 10 is connected to the reaction vessel 1 at a position where the mixed solution can be recovered. The other end of the recovery path 10 is connected to the detection unit 30, which will be described later.

[0034] The detection-side pump 20 pumps the solution in the reaction vessel 1 downstream. The detection-side pump 20 is provided midway along the recovery path 10. When the detection-side pump 20 is operated, it can recover the mixed solution in the reaction vessel 1 via the recovery path 10 and supply it to the detection unit 30 side, which will be described later.

[0035] The detection unit 30 detects the concentration of the first reactant (sodium chlorite) contained in the mixed solution recovered from the reaction vessel 1. The detection unit 30 is connected to the recovery path 10. The configuration of the detection unit 30 will be described in detail later.

[0036] The return path 40 is a path for returning the solution that has flowed through the detection unit 30 to the reaction vessel 1. One end of the return path 40 is connected to the detection unit 30. The other end of the return path 40 is connected to the reaction vessel 1 at a position higher than the position where the recovery path 10 and the reaction vessel 1 are connected.

[0037] The configuration of the detection unit 30 will be described below with reference to Fig. 3. The detection unit 30 includes a flow section 31, a storage section 32, an upstream valve 33, a downstream valve , a light emitter 35, and a light receiver .

[0038] The circulating section 31 is a part that constitutes a path for the solution recovered from the reaction vessel 1. The circulating section 31 is formed in a cylindrical shape that allows the solution to flow inside. The circulating section 31 is provided with its longitudinal direction oriented approximately vertically. The lower end of the circulating section 31 is connected to the recovery path 10. The upper end of the circulating section 31 is connected to the return path 40. Inside the circulating section 31 thus provided, the solution flows from the recovery path 10 (upstream side) below to the return path 40 (downstream side) above.

[0039] The storage section 32 is a section in which the solution recovered from the reaction vessel 1 is stored. The storage section 32 is made of a light-transmitting material. The storage section 32 is formed in a hollow rectangular parallelepiped shape. The storage section 32 is provided above (near the upper end of) the flow-through section 31 so as to communicate with the flow-through section 31.

[0040] The upstream valve 33 opens and closes the flow path of the solution. The upstream valve 33 is provided at the connection between the recovery path 10 and the circulating section 31. The upstream valve 33 thus provided can switch between allowing and disallowing the flow of the solution from the recovery path 10 to the circulating section 31.

[0041] The downstream valve 34 opens and closes the flow path of the solution. The downstream valve 34 is provided at the connection between the circulating section 31 and the return path 40. The downstream valve 34 thus provided can switch between allowing and disallowing the flow of the solution from the circulating section 31 to the return path 40.

[0042] The light-emitting unit 35 is a part configured to be able to emit light and irradiate it. The light-emitting unit 35 is provided on the side of the storage unit 32 so as to be able to irradiate light toward the storage unit 32. More specifically, the light-emitting unit 35 is disposed at a position facing the side surface of the storage unit 32, which is formed in a rectangular parallelepiped shape, and is provided so that the light irradiated from the light-emitting unit 35 is perpendicular to the side surface of the storage unit 32. This makes it possible to suppress refraction of the light irradiated from the light-emitting unit 35.

[0043] The light receiving unit 36 ​​is a part that receives light from the light emitting unit 35. The light receiving unit 36 ​​is provided on a side of the storage unit 32 (the side opposite to the light emitting unit 35) so as to be able to receive light irradiated from the light emitting unit 35 towards the storage unit 32. More specifically, the light receiving unit 36 ​​is disposed at a position facing one of the side surfaces of the storage unit 32 formed in a rectangular parallelepiped shape, the side surface opposite to the side surface on the light emitting unit 35 side.

[0044] The mixed solution is recovered from the reaction vessel 1 by the recovery path 10, the detection-side pump 20, and the detection unit 30 configured as described above, and the concentration of the first reactant (sodium chlorite) contained in the recovered mixed solution is detected (the detection method will be described later). After the concentration of the first reactant is detected, the mixed solution is returned to the reaction vessel 1 via the return path 40.

[0045] 1 and 4 replenishes a raw material (first reactant) into the reaction vessel 1. The replenishment device 5 includes a raw material adjusting section 50, a supply path 60, a replenishment-side pump 70, and a replenishment-side valve 80.

[0046] The raw material adjusting section 50 is a section for preparing a replenishment raw material (first reactant). As shown in Fig. 4, the raw material adjusting section 50 includes a raw material tank 51, an acid tank 52, an adjusting tank 53, a first pump 54, and a second pump 55.

[0047] The raw material tank 51 is configured to be able to store a raw material (first reactant (sodium chlorite)). The acid tank 52 is configured to be able to store an acid for adjusting the pH of the first reactant. In this embodiment, hydrochloric acid is stored in the acid tank 52. The adjustment tank 53 is connected to the raw material tank 51 via a first pump 54, and is configured to be able to receive the first reactant (sodium chlorite) from the raw material tank 51 by operating the first pump 54. In addition, the adjustment tank 53 is connected to the acid tank 52 via a second pump 55, and is configured to be able to receive hydrochloric acid from the acid tank 52 by operating the second pump 55.

[0048] When the raw material (first reactant) is supplied into the reaction vessel 1 by the replenishing device 5 configured as described above, first, a predetermined amount of the first reactant (sodium chlorite) is charged from the raw material tank 51 into the adjustment tank 53. Then, hydrochloric acid is charged from the acid tank 52 into the adjustment tank 53 in an amount sufficient to adjust the pH of the first reactant charged into the adjustment tank 53 to a predetermined value (for example, pH 1 to 2). In this way, an appropriate amount of hydrochloric acid is added to the first reactant (sodium chlorite) in the adjustment tank 53, thereby adjusting the first reactant (sodium chlorite) to a strong acidity (for example, pH 1 to 2).

[0049] The supply path 60 is a path for supplying the first reactant (sodium chlorite) from the raw material adjusting section 50 to the reaction vessel 1. One end of the supply path 60 is connected to the adjustment tank 53. The other end of the supply path 60 is connected to the reaction vessel 1 at a position higher than the position where the return path 40 and the reaction vessel 1 are connected (see FIG. 1).

[0050] The refilling pump 70 sends the first reactant (sodium chlorite) in the adjustment tank 53 to the reaction vessel 1. The refilling pump 70 is provided in the middle of the supply path 60. When the refilling pump 70 is operated, the first reactant (sodium chlorite) in the adjustment tank 53 can be supplied to the reaction vessel 1 via the supply path 60.

[0051] The refill-side valve 80 opens and closes the flow path of the solution. The refill-side valve 80 is provided in the middle of the supply path 60, more specifically, downstream of the refill-side pump 70 (closer to the reaction vessel 1). The refill-side valve 80 thus provided can switch between allowing and disallowing the flow of the first reactant (sodium chlorite) from the adjustment tank 53 to the reaction vessel 1.

[0052] The raw material adjusting section 50 configured as described above prepares a raw material (first reactant) with adjusted pH, and by operating the refilling side pump 70 with the refilling side valve 80 open, the first reactant (sodium chlorite) can be supplied into the reaction vessel 1 via the supply path 60.

[0053] The control device 6 shown in FIG. 1 controls the operations of the detection device 4 and the replenishment device 5. The control device 6 is electrically connected to the detection device 4 so as to be able to acquire the detection results of the detection device 4. The control device 6 is also electrically connected to the replenishment device 5 so as to be able to control the operation of the replenishment device 5. The control device 6 can control the operation of the replenishment device 5 based on the detection results of the detection device 4.

[0054] 5 and 6, a method for detecting the concentration of the first reactant (sodium chlorite) by the detection unit 30 will be described. The flow shown in FIG. 5 shows the replenishment control of the raw material (first reactant), which is repeatedly executed at predetermined intervals (for example, every minute). The replenishment control of the raw material shown in FIG. 5 is executed while the reaction is in progress in the reaction vessel 1. In other words, the replenishment control of the raw material shown in FIG. 5 is executed when the agitator 2 is operating and a mixed solution is generated inside the reaction vessel 1.

[0055] In step S11, the control device 6 introduces the solution into the detection unit 30. Specifically, the control device 6 operates the detection-side pump 20 while opening the upstream valve 33 and downstream valve 34 of the detection unit 30, thereby drawing the mixed solution inside the reaction vessel 1 into the detection unit 30. The mixed solution drawn (introduced) into the detection unit 30 flows through the circulating unit 31 and is returned to the inside of the reaction vessel 1 via the return path 40 (see FIG. 6(a)).

[0056] After performing the process of step S11, the control device 6 proceeds to step S12.

[0057] In step S12, the control device 6 closes the upstream valve 33 and the downstream valve 34 of the detection unit 30 and stops the detection-side pump 20. Closing the upstream valve 33 and the downstream valve 34 stops the flow of the mixed solution from the recovery path 10 to the detection unit 30 and from the detection unit 30 to the return path 40. At this time, the flow unit 31 and the storage unit 32 are filled with the mixed solution.

[0058] After performing the process of step S12, the control device 6 proceeds to step S13.

[0059] In step S13, the control device 6 determines whether a predetermined time has elapsed since the process of step S12 was performed. Here, the "predetermined time" is set to the time (e.g., 10 seconds) required for the mixed solution to separate into the first liquid phase and the second liquid phase in the circulating section 31 and the storage section 32. Since the mixed solution needs to be quickly separated into the first liquid phase and the second liquid phase in the circulating section 31 and the storage section 32, the circulating section 31 and the storage section 32 are formed to have a relatively small capacity.

[0060] If the control device 6 determines that the predetermined time has elapsed ("YES" in step S13), it proceeds to step S14. On the other hand, if the control device 6 determines that the predetermined time has not elapsed ("NO" in step S13), it executes the process of step S13 again. That is, the control device 6 cannot proceed to the next process until the determination in step S13 is "YES."

[0061] After a predetermined time has elapsed since the process of step S12, the first solution S1 and the second solution S2 separate into two layers due to the difference in specific gravity between them, with the first solution S1 located above the second solution S2. That is, in the detection unit 30 (the flow-through unit 31 and the storage unit 32), the mixed solution introduced from the reaction vessel 1 separates into a first liquid phase composed of the first solution S1 and a second liquid phase composed of the second solution S2 (see FIG. 6(b)). Because the first liquid phase is located above the second liquid phase, the inside of the storage unit 32 provided near the upper end of the flow-through unit 31 is filled with the first liquid phase (first solution S1). At this time, the first reactant (sodium chlorite) is present in the first liquid phase due to the difference in solubility.

[0062] In step S14, the control device 6 causes the light-emitting unit 35 to emit light toward the light-receiving unit 36 ​​(see FIG. 6(c)). The light emitted from the light-emitting unit 35 passes through the first liquid phase (first solution S1) contained in the container 32 and is received by the light-receiving unit 36. The control device 6 calculates the absorbance of the first solution S1 contained in the container 32 based on the amount of light emitted from the light-emitting unit 35 and the amount of light received by the light-receiving unit 36.

[0063] After performing the process of step S14, the control device 6 proceeds to step S15.

[0064] In step S15, based on the absorbance calculated in step S14, the control device 6 calculates the concentration of the first reactant (sodium chlorite) in the first liquid phase (first solution S1) contained in the container 32. Specifically, the control device 6 can calculate the concentration of the first reactant by comparing the absorbance calculated in step S14 with pre-stored data indicating the relationship between the absorbance and the concentration of the first reactant.

[0065] After performing the process of step S15, the control device 6 proceeds to step S16.

[0066] In step S16, the control device 6 supplies the first reactant (sodium chlorite) from the replenishment device 5 to the reaction vessel 1. Specifically, based on the concentration of the first reactant calculated in step S15, the control device 6 supplies the first reactant from the replenishment device 5 to the reaction vessel 1 necessary to return the concentration of the first reactant (sodium chlorite) inside the reaction vessel 1 to a specified concentration. Here, the "specified concentration" is set to a value that can maintain sufficient reaction efficiency inside the reaction vessel 1 and does not cause an excess of the first reactant (sodium chlorite) inside the reaction vessel 1. In this way, the amount of first reactant (sodium chlorite) consumed in the production of the product (methanol) is replenished inside the reaction vessel 1.

[0067] After performing the process of step S16, the control device 6 ends the flow of FIG.

[0068] As described above, in the method for producing a product using two liquid phases, the solution is stirred to promote the reaction. Therefore, the solution (mixed solution) in the reaction vessel 1 is a mixture of the first solution S1 (water) and the second solution S2 (fluorous solvent), making it very difficult to measure the concentration of the first reactant (sodium chlorite) in the solution.

[0069] Therefore, in the reaction device 100 according to this embodiment, a detection unit 30 is provided outside the reaction vessel 1, the mixed solution is introduced from the reaction vessel 1 into the detection unit 30, and the concentration of the first reactant (sodium chlorite) is measured in a state where the mixed solution is separated into a first liquid phase and a second liquid phase in the detection unit 30. This makes it possible to measure the concentration of the first reactant with high accuracy, and therefore to detect the consumption amount of the first reactant inside the reaction vessel 1 with high accuracy.

[0070] Then, by appropriately supplying the raw material (first reactant) from the replenishing device 5 to the reaction vessel 1 based on the detection result of the detection unit 30, the reaction can be continued while maintaining the concentration of the first reactant (sodium chlorite) inside the reaction vessel 1 at an optimum concentration. Therefore, sufficient reaction efficiency can be maintained, and the first reactant (sodium chlorite) inside the reaction vessel 1 can be prevented from becoming excessive.

[0071] Furthermore, in the reaction apparatus 100 according to this embodiment, the consumption amount of the first reactant (sodium chlorite) can be grasped while the reaction continues inside the reaction vessel 1 without stopping the stirring by the stirring device 2. This makes it possible to shorten the time required to produce the product, thereby improving production efficiency.

[0072] Furthermore, if the stirring by the stirrer 2 is stopped and the concentration of the solution inside the reaction vessel 1 is measured directly, the larger the volume of the solution, the longer the time required for two-phase separation and the longer the time required to detect the concentration of the first reactant. On the other hand, in the reaction device 100 according to this embodiment, by introducing the solution into the small-capacity detection unit 30, the time required for separation can be significantly reduced, and ultimately the time required to detect the concentration of the first reactant can be reduced. Furthermore, by arranging the longitudinal direction (flow direction) of the flow unit 31 of the detection unit 30 to be oriented vertically, the solution can be easily separated.

[0073] As described above, the reaction device 100 according to this embodiment has the following features: A reactor 100 for reacting a first reactant (e.g., sodium chlorite) and a second reactant (e.g., methane) in a solution containing a first solution S1 and a second solution S2 to produce a product (e.g., methanol), a reaction vessel 1 in which a first liquid phase constituted by the first solution S1 containing the first reactant and a second liquid phase constituted by the second solution S2 containing the second reactant can be formed; an agitator 2 (mixer) that mixes the first solution S1 and the second solution S2 to generate a mixed solution inside the reaction vessel 1; a detection unit (30) that separates the mixed solution introduced from the reaction vessel (1) into the first liquid phase and the second liquid phase, and detects the consumption amount of the first reactant or the second reactant inside the reaction vessel (1) by measuring the concentration of the first reactant in the first liquid phase or the second reactant in the second liquid phase; It is equipped with the following.

[0074] With this configuration, the consumption amount of the reactant (first reactant or second reactant) can be detected with high accuracy while the reaction in the reaction vessel 1 continues.

[0075] In addition, the detection unit 30 a flow section 31 that forms a flow path for the mixed solution introduced from the reaction vessel 1; an upstream valve 33 (first valve) provided upstream of the flow passage portion 31 and configured to open and close the flow path; a downstream valve 34 (second valve) provided downstream of the flow passage portion 31 and configured to open and close the flow path; It is equipped with the following.

[0076] With this configuration, the mixed solution can be separated into the first liquid phase and the second liquid phase in the detection unit 30 with a simple configuration.

[0077] In addition, the detection unit 30 a storage section (32) provided in the middle of the flow section (31) and configured to store the first liquid phase when the mixed solution is separated into the first liquid phase and the second liquid phase; a light-emitting unit (35) capable of irradiating light toward the first liquid phase contained in the container (32); a light receiving unit (36) capable of receiving light irradiated from the light emitting unit (35) and passing through the first liquid phase; Equipped with The absorbance of the first solution S1 constituting the first liquid phase contained in the reaction vessel 1 is calculated based on the amount of light irradiated from the light-emitting unit 35 and the amount of light received by the light-receiving unit 36, and the concentration of the first reactant in the first liquid phase contained in the container 32 is measured based on the calculated absorbance.

[0078] With this configuration, the consumption amount of the reactant (first reactant) can be detected with high accuracy using a simple configuration.

[0079] Moreover, the reaction device 100 according to this embodiment has the following features: The reaction vessel 1 is provided with a replenishment device 5 (replenishment unit) that replenishes the first reactant or the second reactant inside the reaction vessel 1 based on the consumption amount of the first reactant or the second reactant detected by the detection unit 30.

[0080] By configuring in this way, the reactant (first reactant) inside the reaction vessel 1 can be maintained at an optimum concentration.

[0081] 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 device 100 is not limited to the above-described ones and can be changed as appropriate.

[0082] Furthermore, in the above embodiment, an example was shown in which a first liquid phase is formed on the upper side and a second liquid phase is formed on the lower side in the reaction vessel 1, but this is not limited to such an embodiment, and the first liquid phase may be formed on the lower side and the second liquid phase on the upper side.

[0083] In the above embodiment, an example in which methanol is produced as a product is described, but the present invention is not limited to this. For example, alcohol may be used as a product. In addition, the product is not limited to the above example, and various substances produced by chemical reactions using two liquid phases (aqueous phase and solvent phase) may be used.

[0084] In addition, although the present embodiment illustrates an example in which sodium chlorite is used as the first reactant and methane is used as the second reactant, the present invention is not limited to this example. Various substances can be used as the first reactant and the second reactant depending on the product.

[0085] In this embodiment, water is used as the first solution S1, but the present invention is not limited to this. Various aqueous solutions that form an aqueous phase can be used as the first solution S1. In this embodiment, a fluorous solvent is used as the second solution S2, but the present invention is not limited to this. Various solvents that form a solvent phase can be used as the second solution S2.

[0086] In this embodiment, the replenishing device 5 replenishes (supplies) the raw material (first reactant) into the reaction vessel 1 via the adjustment tank 53, but the raw material may be directly supplied from the raw material tank 51 into the reaction vessel 1. In this case, hydrochloric acid is also directly supplied from the acid tank 52 into the reaction vessel 1.

[0087] In this embodiment, the replenishing device 5 replenishing the first reactant (sodium chlorite) into the reaction vessel 1, but it may also replenishing the second reactant (methane). In addition, both a replenishing device for replenishing the first reactant (sodium chlorite) and a replenishing device for replenishing the second reactant (methane) may be provided.

[0088] Furthermore, in this embodiment, the replenishment of the first reactant from the replenishment device 5 to the reaction vessel 1 is performed each time the concentration of the first reactant is calculated by the detection unit 30, but it may also be performed when the calculated concentration of the first reactant falls below a predetermined threshold value.

[0089] Furthermore, in this embodiment, in the detection unit 30, the recovery path 10 is provided at the lower end of the circulation section 31, and the return path 40 (downstream side) is provided at the upper end of the circulation section 31, but the positional relationship between the upstream and downstream sides in the detection unit 30 is not limited to this, and for example, the recovery path 10 may be provided at the upper end of the circulation section 31, and the return path 40 (downstream side) may be provided at the lower end of the circulation section 31.

[0090] In addition, in this embodiment, the solution that has passed through the detection unit 30 is returned to the reaction vessel 1, but it does not necessarily have to be returned to the reaction vessel 1.

[0091] Furthermore, in this embodiment, the concentration of the first reactant is measured based on the absorbance of the first liquid phase (first solution S1) contained in the detection unit 30, but the method of measuring the concentration of the first reactant in the detection unit 30 is not limited to this, and any method can be adopted.

[0092] For example, the concentration of the first reactant in the first liquid phase (first solution S1) contained in the container 32 may be measured based on the color difference between the first liquid phase containing the specified concentration of the first reactant and the first liquid phase contained in the container 32. Specifically, when the first reactant is sodium chlorite, the aqueous phase containing the strongly acidic sodium chlorite is yellow, and the solvent phase is colorless and transparent. As chlorine dioxide, a decomposition product of sodium chlorite, is consumed and its amount decreases, the color of the aqueous phase becomes lighter and approaches colorless and transparent. Therefore, the concentration of sodium chlorite may be measured by installing a camera near the container 32 and observing the color change of the aqueous phase using images captured by the camera. Alternatively, the concentration of sodium chlorite may be measured by installing a color difference meter near the container 32 and observing the color change of the aqueous phase using the color difference meter.

[0093] As another method for measuring the concentration of the first reactant (sodium chlorite) in the detection unit 30, a pair of current-carrying electrodes may be installed in the storage unit 32, and the concentration of the first reactant may be measured by measuring the electrical conductivity of the solution stored in the storage unit 32. Furthermore, when the solution stored in the storage unit 32 contains a reactant that is corrosive to metals, such as sodium chlorite, the concentration of sodium chlorite may be measured by measuring the electrical conductivity of the solution using an electromagnetic induction method, which can be implemented by covering the liquid-contacting parts of the storage unit 32 with a corrosion-resistant material.

[0094] As described above, the detection unit 30 a storage section (32) provided in the middle of the flow section (31) and configured to store the first liquid phase when the mixed solution is separated into the first liquid phase and the second liquid phase; The concentration of the first reactant in the first liquid phase contained in the storage section 32 is measured based on the color difference between the first liquid phase containing the first reactant at a specified concentration and the first liquid phase contained in the storage section 32.

[0095] With this configuration, the consumption amount of the reactant (first reactant) can be detected with high accuracy using a simple configuration. [Explanation of symbols]

[0096] 1 reaction vessel 2 Stirring device 5 Refilling device 30 Detection unit 31 Distribution Department 32 Storage section 33 Upstream valve 34 Downstream valve 35 Light-emitting part 36 Light receiving part

Claims

1. A reactor for reacting a first reactant and a second reactant in a solution comprising a first solution and a second solution to produce a product, a reaction vessel in which a first liquid phase constituted by the first solution containing the first reactant and a second liquid phase constituted by the second solution containing the second reactant can be formed; a mixer that mixes the first solution and the second solution to generate a mixed solution inside the reaction vessel; a detection unit that separates the mixed solution introduced from the reaction vessel into the first liquid phase and the second liquid phase, and detects the consumption amount of the first reactant or the second reactant inside the reaction vessel by measuring the concentration of the first reactant in the first liquid phase or the second reactant in the second liquid phase; Equipped with Reactor.

2. The detection unit a flow section that forms a flow path for the mixed solution introduced from the reaction vessel; a first valve provided upstream of the flow passage portion and configured to open and close the flow passage; a second valve provided downstream of the flow passage portion and configured to open and close the flow passage; Equipped with The reactor of claim 1.

3. The detection unit a storage section provided in the middle of the flow section and configured to store the first liquid phase when the mixed solution is separated into the first liquid phase and the second liquid phase; a light emitting unit capable of irradiating light toward the first liquid phase contained in the container; a light receiving unit capable of receiving light irradiated from the light emitting unit and passing through the first liquid phase; Equipped with calculating an absorbance of the first solution constituting the first liquid phase contained in the container based on the amount of light irradiated from the light-emitting unit and the amount of light received by the light-receiving unit, and measuring a concentration of the first reactant in the first liquid phase contained in the container based on the calculated absorbance; The reactor of claim 2.

4. The detection unit a storage section provided in the middle of the flow section and configured to store the first liquid phase when the mixed solution separates into the first liquid phase and the second liquid phase; measuring the concentration of the first reactant in the first liquid phase contained in the container based on a color difference between the first liquid phase containing the first reactant at a specified concentration and the first liquid phase contained in the container; The reactor of claim 2.

5. a replenishing unit that replenishes the first reactant or the second reactant inside the reaction vessel based on the consumption amount of the first reactant or the second reactant detected by the detection unit; A reactor according to any one of claims 1 to 4.

Citation Information

Patent Citations

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