WO2022118695A1 - 有機ハイドライド製造装置、水除去装置および水除去方法 - Google Patents

有機ハイドライド製造装置、水除去装置および水除去方法 Download PDF

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Publication number
WO2022118695A1
WO2022118695A1 PCT/JP2021/042828 JP2021042828W WO2022118695A1 WO 2022118695 A1 WO2022118695 A1 WO 2022118695A1 JP 2021042828 W JP2021042828 W JP 2021042828W WO 2022118695 A1 WO2022118695 A1 WO 2022118695A1
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Prior art keywords
cathode
container
anode
water
liquid
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PCT/JP2021/042828
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English (en)
French (fr)
Japanese (ja)
Inventor
康太 三好
秀緒 大津
宏紀 土門
淳 角南
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Eneos Corp
De Nora Permelec Ltd
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Eneos Corp
De Nora Permelec Ltd
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Priority to EP21900450.4A priority Critical patent/EP4257731A4/en
Priority to AU2021392237A priority patent/AU2021392237A1/en
Priority to US18/255,643 priority patent/US20240102192A1/en
Priority to CN202180080512.1A priority patent/CN116529426A/zh
Priority to JP2022566851A priority patent/JPWO2022118695A1/ja
Publication of WO2022118695A1 publication Critical patent/WO2022118695A1/ja
Anticipated expiration legal-status Critical
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    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
    • C25B3/00—Electrolytic production of organic compounds
    • C25B3/20—Processes
    • C25B3/25—Reduction
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
    • C25B15/00—Operating or servicing cells
    • C25B15/02—Process control or regulation
    • C25B15/023—Measuring, analysing or testing during electrolytic production
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
    • C25B15/00—Operating or servicing cells
    • C25B15/08—Supplying or removing reactants or electrolytes; Regeneration of electrolytes
    • C25B15/083—Separating products
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
    • C25B15/00—Operating or servicing cells
    • C25B15/08—Supplying or removing reactants or electrolytes; Regeneration of electrolytes
    • C25B15/085—Removing impurities
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
    • C25B15/00—Operating or servicing cells
    • C25B15/08—Supplying or removing reactants or electrolytes; Regeneration of electrolytes
    • C25B15/087—Recycling of electrolyte to electrochemical cell
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
    • C25B3/00—Electrolytic production of organic compounds
    • C25B3/01—Products
    • C25B3/03—Acyclic or carbocyclic hydrocarbons
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
    • C25B9/00—Cells or assemblies of cells; Constructional parts of cells; Assemblies of constructional parts, e.g. electrode-diaphragm assemblies; Process-related cell features
    • C25B9/17—Cells comprising dimensionally-stable non-movable electrodes; Assemblies of constructional parts thereof
    • C25B9/19—Cells comprising dimensionally-stable non-movable electrodes; Assemblies of constructional parts thereof with diaphragms
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
    • C25B9/00—Cells or assemblies of cells; Constructional parts of cells; Assemblies of constructional parts, e.g. electrode-diaphragm assemblies; Process-related cell features
    • C25B9/17—Cells comprising dimensionally-stable non-movable electrodes; Assemblies of constructional parts thereof
    • C25B9/19—Cells comprising dimensionally-stable non-movable electrodes; Assemblies of constructional parts thereof with diaphragms
    • C25B9/23—Cells comprising dimensionally-stable non-movable electrodes; Assemblies of constructional parts thereof with diaphragms comprising ion-exchange membranes in or on which electrode material is embedded

Definitions

  • the present invention relates to an organic hydride manufacturing apparatus, a water removing apparatus, and a water removing method.
  • an organic hydride having an anode electrode that generates protons from water, a cathode electrode that hydrogenates an organic compound (hydrogenated product) having an unsaturated bond, and an electrolytic tank having a diaphragm separating the anode electrode and the cathode electrode.
  • a manufacturing apparatus is known (see, for example, Patent Document 1).
  • protons are generated by oxidation of water at the anode electrode, the protons move to the cathode electrode side through the diaphragm, and the hydrogenated product is hydrogenated by the protons at the cathode electrode, so that the organic hydride is produced. Hydride is manufactured.
  • the generation of protons and the hydrogenation of the hydride can be performed in a one-step process. Therefore, the manufacturing process of the organic hydride can be simplified as compared with the case where hydrogen is produced by water electrolysis or the like and the organic hydride is produced by a two-step process in which the hydrogenated product is chemically hydrogenated in a reactor such as a plant. Alternatively, the production efficiency of organic hydride can be increased. In addition, since the high-pressure container for storing hydrogen, which is required when producing hydrogen by water electrolysis, can be omitted, the equipment cost is expected to be significantly reduced.
  • the present invention has been made in view of such a situation, and one of the objects thereof is to provide a technique for suppressing the overflow of organic hydride and hydride while suppressing the increase in size of the organic hydride production apparatus. be.
  • One aspect of the present invention is an organic hydride manufacturing apparatus.
  • This device has an anode electrode that oxidizes water in the anode solution to generate protons, an anode chamber that houses the anode electrode, a cathode electrode that hydrogenates the hydride in the cathode solution with protons to generate organic hydride, and a cathode.
  • An electrolytic tank having a cathode chamber for accommodating an electrode, a diaphragm for partitioning the anode chamber and the cathode chamber and moving protons together with accompanying water from the anode chamber side to the cathode chamber side, and at least organic hydride and accompanying water discharged from the cathode chamber.
  • a water removing device for removing the accompanying water from the contained cathode solution includes a container that stores the cathode liquid sent out from the cathode chamber, a drainage pipe that is connected to the container and discharges the accompanying water, and a detector that detects that a predetermined amount of accompanying water has accumulated in the container. It is provided in the drainage pipe, and it is possible to switch between the regulated state that regulates drainage from the drainage pipe and the execution state that executes drainage, and the switching unit that switches from the regulated state to the execution state based on the detection result of the detection unit. Have.
  • Another aspect of the present invention is a water removing device.
  • This device has an anode electrode that oxidizes water in the anode solution to generate protons, an anode chamber that houses the anode electrode, a cathode electrode that hydrogenates the hydride in the cathode solution with protons to generate organic hydride, and a cathode. Containing at least organic hydride and accompanying water delivered from the cathode chamber containing the electrodes and the cathode chamber of the electrolytic tank having a diaphragm that separates the anode chamber and the cathode chamber and transfers protons with the accompanying water from the anode chamber side to the cathode chamber side.
  • a container for storing the cathode solution a drain pipe connected to the container to discharge the accompanying water, a detection unit for detecting that a predetermined amount of the accompanying water has accumulated in the container, and a drain pipe provided in the drain pipe. It is possible to switch between a regulated state that regulates drainage and an execution state that executes drainage, and includes a switching unit that switches from the regulated state to the execution state based on the detection result of the detection unit.
  • Another aspect of the present invention is a water removing method.
  • the anode electrode that oxidizes water in the anode solution to generate protons the anode chamber that houses the anode electrode, the cathode electrode that hydrogenates the hydride in the cathode solution with protons to generate organic hydride, and the cathode.
  • This includes storing the cathode solution in a container and discharging the accompanying water from the container when it is detected that a predetermined amount of accompanying water has accumulated in the container.
  • the present invention it is possible to suppress the overflow of organic hydride and the hydride to be hydrogenated while suppressing the increase in size of the organic hydride production apparatus.
  • FIG. 1 is a schematic diagram of the organic hydride manufacturing apparatus 1 according to the embodiment.
  • the organic hydride production apparatus 1 includes an electrolytic cell 2, a power source 4, a first distribution mechanism 6, a second distribution mechanism 8, a control unit 10, and a water removing device 12.
  • the electrolytic cell 2 is an electrolytic cell that produces organic hydride ⁇ by hydrogenating the hydride ⁇ by an electrochemical reduction reaction.
  • the electrolytic cell 2 has an anode electrode 14, an anode chamber 16, a cathode electrode 18, a cathode chamber 20, and a diaphragm 22.
  • the anode electrode 14 is an electrode (anode) that oxidizes water in the anode liquid La to generate a proton (H + ).
  • the anode electrode 14 is arranged so as to be in contact with one main surface of the diaphragm 22.
  • the anode electrode 14 has a metal such as iridium (Ir), ruthenium (Ru), platinum (Pt), or a metal oxide thereof as an anode catalyst.
  • the anode catalyst is dispersed, supported or coated on a substrate having electron conductivity.
  • the base material is composed of a material containing a metal as a main component, such as titanium (Ti) or stainless steel (SUS). Examples of the form of the base material include woven fabric and non-woven fabric sheets, meshes, porous sintered bodies, foam molded bodies (foams), expanded metals, and the like.
  • the thickness of the anode electrode 14 including the anode catalyst and the substrate is not particularly limited, but is, for example, 0.05 to 1 mm.
  • the thickness of the anode electrode 14 is set to 0.05 mm or more, the amount of catalyst required for the electrolytic reaction can be obtained more reliably. Further, by setting the thickness of the anode electrode 14 to 1 mm or less, it is possible to prevent the diffusivity of the anode liquid La from being excessively lowered.
  • the anode catalyst may be coated on a base material to form a catalyst layer.
  • the thickness of the catalyst layer is not particularly limited, but is, for example, 0.1 to 50 ⁇ m.
  • the anode electrode 14 may have a layer structure obtained by directly coating the main surface of the diaphragm 22 with an anode catalyst.
  • the thickness of the layer constituting the anode electrode 14 is not particularly limited, but is, for example, 0.1 to 50 ⁇ m.
  • the anode electrode 14 is housed in the anode chamber 16.
  • the space in the anode chamber 16 other than the anode electrode 14 constitutes a flow path of oxygen generated by the anode liquid La and the electrode reaction.
  • the cathode electrode 18 is an electrode (cathode) that produces organic hydride ⁇ by hydrogenating the hydride ⁇ in the cathode liquid Lc with a proton.
  • the cathode electrode 18 is arranged so as to be in contact with the other main surface of the diaphragm 22 (the main surface opposite to the anode electrode 14).
  • the cathode electrode 18 has a catalyst layer 18a and a diffusion layer 18b.
  • the catalyst layer 18a is arranged so as to be in contact with the diaphragm 22.
  • the catalyst layer 18a has, for example, platinum, ruthenium, or the like as a cathode catalyst. Further, the catalyst layer 18a has a catalyst carrier that supports a cathode catalyst.
  • the catalyst carrier is composed of an electron conductive material such as porous carbon, porous metal, and porous metal oxide.
  • the thickness of the catalyst layer 18a is not particularly limited, but is, for example, 20 to 50 ⁇ m. By setting the thickness of the catalyst layer 18a to 20 ⁇ m or more, the amount of catalyst required for the electrolytic reaction can be obtained more reliably. Further, by setting the thickness of the catalyst layer 18a to 50 ⁇ m or less, it is possible to suppress the excessive decrease in the diffusivity of the hydride ⁇ .
  • the diffusion layer 18b is arranged so as to be in contact with the surface of the catalyst layer 18a opposite to the diaphragm 22.
  • the diffusion layer 18b is a layer that uniformly diffuses the liquid hydride ⁇ supplied from the outside into the catalyst layer 18a. Further, the organic hydride ⁇ produced in the catalyst layer 18a is discharged from the catalyst layer 18a via the diffusion layer 18b.
  • the diffusion layer 18b is made of a conductive material such as carbon or metal. Further, the diffusion layer 18b is a porous body such as a sintered body of fibers or particles and a foam molded body. Specific examples of the material constituting the diffusion layer 18b include a carbon woven fabric (carbon cloth), a carbon non-woven fabric, and carbon paper.
  • the thickness of the diffusion layer 18b is not particularly limited, but is, for example, 200 to 700 ⁇ m. By setting the thickness of the diffusion layer 18b to 200 ⁇ m or more, the diffusibility of the hydride ⁇ can be more reliably enhanced. Further, by setting the thickness of the diffusion layer 18b to 700 ⁇ m or less, it is possible to prevent the electrical resistance from becoming excessive.
  • the cathode electrode 18 is housed in the cathode chamber 20.
  • the space in the cathode chamber 20 other than the cathode electrode 18 constitutes a flow path of the hydride ⁇ and the organic hydride ⁇ generated by the electrode reaction.
  • the anode chamber 16 and the cathode chamber 20 are separated by a diaphragm 22.
  • the diaphragm 22 is arranged between the anode electrode 14 and the cathode electrode 18.
  • the diaphragm 22 is composed of a solid polymer electrolyte membrane having proton conductivity.
  • the solid polymer electrolyte membrane is not particularly limited as long as it is a material that conducts protons, and examples thereof include a fluorine-based ion exchange membrane having a sulfonic acid group such as Nafion (registered trademark).
  • the diaphragm 22 moves protons from the anode chamber 16 side to the cathode chamber 20 side with water ( H2O ).
  • water that moves with protons is referred to as accompanying water W.
  • the thickness of the diaphragm 22 is not particularly limited, but is, for example, 5 to 300 ⁇ m. By setting the thickness of the diaphragm 22 to 5 ⁇ m or more, the desired strength of the diaphragm 22 can be obtained more reliably. Further, by setting the thickness of the diaphragm 22 to 300 ⁇ m or less, it is possible to suppress the ion transfer resistance from becoming excessive.
  • the reaction that occurs when toluene (TL) is used as an example of the hydride ⁇ in the electrolytic cell 2 is as follows.
  • the obtained organic hydride ⁇ is methylcyclohexane (MCH).
  • Electrode reaction at the anode electrode 2H 2 O ⁇ O 2 + 4H + + 4e -
  • water is electrolyzed at the anode electrode 14, and oxygen gas, protons, and electrons are generated.
  • the protons travel through the diaphragm 22 toward the cathode electrode 18.
  • the electrons flow into the positive electrode of the power supply 4.
  • Oxygen gas is discharged to the outside through the anode chamber 16.
  • methylcyclohexane is produced by the reaction of toluene, electrons supplied from the negative electrode of the power source 4, and protons arriving through the diaphragm 22. Therefore, according to the organic hydride production apparatus 1, the electrolysis of water and the hydrogenation reaction of the hydride ⁇ can be performed in one step.
  • the power supply 4 is a DC power supply that supplies electric power to the electrolytic cell 2. By supplying electric power from the power source 4, a predetermined electrolytic voltage is applied between the anode electrode 14 and the cathode electrode 18 of the electrolytic cell 2.
  • the power supply 4 receives electric power from the electric power supply unit 24 and supplies electric power to the electrolytic cell 2.
  • the power supply unit 24 can be configured by a renewable energy power generation device such as a wind power generation device 26 or a solar power generation device 28.
  • the power supply unit 24 may include a power generation device that uses renewable energy other than wind power and solar power, such as a geothermal power generation device, a wave power generation device, a temperature difference power generation device, and a biomass power generation device. Further, the power supply unit 24 is not limited to a power generation device that generates power by using renewable energy.
  • the first distribution mechanism 6 is a mechanism for distributing the anode liquid La containing water to the anode chamber 16.
  • the first distribution mechanism 6 has an anodic liquid tank 30, an anodic liquid circulation path 32, an anodic liquid circulation device 34, and an anodic liquid gas-liquid separation unit 36.
  • the anolyte tank 30 stores the anolyte La supplied to the anolyte chamber 16.
  • Examples of the anode liquid La include a solution having a predetermined ionic conductivity such as a sulfuric acid aqueous solution, a nitric acid aqueous solution, and a hydrochloric acid aqueous solution, pure water, ion-exchanged water, and the like.
  • the anolyte tank 30 and the anolyte chamber 16 are connected by an anolyte circulation path 32.
  • the anode liquid circulation path 32 includes an anode inlet pipe 32a for supplying the anode liquid La in the anode liquid tank 30 to the anode chamber 16 and an anode outlet pipe 32b for returning the anode liquid La sent out from the anode chamber 16 to the anode liquid tank 30.
  • the anode liquid circulation device 34 is provided in the middle of the anode inlet pipe 32a as an example. By driving the anolyte liquid circulation device 34, the anolyte liquid La flows in the anolyte liquid circulation path 32. As a result, the anode liquid La circulates between the anode liquid tank 30 and the anode chamber 16.
  • the anode liquid circulation device 34 for example, various pumps such as a gear pump and a cylinder pump, a natural flow type device, and the like can be used.
  • the anode liquid-gas-liquid separation unit 36 is provided in the middle of the anode outlet pipe 32b. At the anode electrode 14, oxygen is generated by the electrode reaction. Therefore, the anode liquid La recovered from the anode chamber 16 contains gaseous oxygen and dissolved oxygen in addition to unreacted water. The gaseous oxygen is separated from the anolyte liquid La in the anolyte liquid gas-liquid separation unit 36 and taken out of the system. The anodic solution La from which oxygen has been separated is recovered in the anolyte tank 30.
  • the anode inlet pipe 32a is connected to the lower portion of the anode chamber 16 in the vertical direction
  • the anode outlet pipe 32b is connected to the upper portion of the anode chamber 16 in the vertical direction.
  • the anode liquid La in the anode liquid tank 30 is pumped up by the anode liquid circulation device 34 and enters the anode chamber 16.
  • the anode liquid La in the anode chamber 16 is pushed out to the anode outlet pipe 32b by the flow of the anode liquid La entering the anode chamber 16, and flows down to the anode liquid gas-liquid separation unit 36 by gravity.
  • the anolyte La is placed under atmospheric pressure in the anolyte gas-liquid separation unit 36.
  • the anolyte liquid La in the anolyte liquid gas-liquid separation unit 36 flows into the anolyte liquid tank 30 in a natural flow manner as the liquid level in the anolyte liquid tank 30 drops.
  • the anode inlet pipe 32a may be connected to the upper part of the anode chamber 16 in the vertical direction. In this case, the anode liquid La enters the anode chamber 16 from the upper part in the vertical direction. That is, the anode liquid La may be supplied to the anode chamber 16 as a downward flow instead of an upward flow.
  • the second distribution mechanism 8 is a mechanism for distributing the cathode liquid Lc containing the hydride ⁇ to the cathode chamber 20.
  • the second distribution mechanism 8 has a cathode liquid tank 38, a cathode liquid circulation path 40, a cathode liquid circulation device 42, and a cathode liquid gas-liquid separation unit 44 (gas-liquid separation tower).
  • the cathode liquid tank 38 stores the cathode liquid Lc supplied to the cathode chamber 20.
  • the cathode liquid Lc stored in the cathode liquid tank 38 contains the hydride ⁇ at least before the start of operation of the organic hydride production apparatus 1.
  • the hydrogenated product ⁇ is a compound that is hydrogenated by an electrochemical reduction reaction in the electrolytic cell 2 to become organic hydride ⁇ , that is, a dehydrogenated product of organic hydride ⁇ .
  • the hydride ⁇ and the organic hydride ⁇ are preferably liquid at 20 ° C. and 1 atm.
  • the hydride ⁇ and the organic hydride ⁇ are organic compounds capable of adding / desorbing hydrogen by reversibly causing a hydrogenation reaction / dehydrogenation reaction.
  • the hydride ⁇ and the organic hydride ⁇ have a lower specific density than water.
  • the hydride ⁇ and the organic hydride ⁇ have low compatibility with water and form an interface IF with the accompanying water W.
  • the detection unit 52 which will be described later, is composed of a sensor that detects the interface IF based on the difference in buoyancy (specific gravity) applied to the float, there is a difference in specific gravity with respect to the accompanying water W to the extent that this sensor can detect it.
  • Certain hydride ⁇ and organic hydride ⁇ are selected.
  • examples of the hydride ⁇ include aromatic compounds having a liquid specific density of 0.6 to 0.9 g / cm 3 .
  • the detection unit 52 is composed of a sensor that detects the interface IF based on the difference in capacitance (relative permittivity)
  • the relative permittivity is set with respect to the accompanying water W to the extent that this sensor can detect it.
  • Dielectric ⁇ and organic hydride ⁇ with differences are selected.
  • examples of the hydride ⁇ include aromatic compounds having a relative permittivity of 1 to 50.
  • hydride ⁇ examples include alkylbenzenes such as benzene and toluene, and nitrogen-containing aromatic compounds such as pyridine and pyrazine.
  • the cathode liquid tank 38 and the cathode chamber 20 are connected by a cathode liquid circulation path 40.
  • the cathode liquid circulation path 40 includes a cathode inlet pipe 40a that supplies the cathode liquid Lc in the cathode liquid tank 38 to the cathode chamber 20, and a cathode outlet pipe 40b that returns the cathode liquid Lc sent out from the cathode chamber 20 to the cathode liquid tank 38.
  • the concentration of the hydride ⁇ of the cathode liquid Lc flowing through the cathode liquid circulation path 40 decreases with the lapse of the operating time of the organic hydride manufacturing apparatus 1, in other words, as the number of times of circulation increases, and the concentration of the organic hydride ⁇ . Is rising.
  • the cathode liquid circulation device 42 is provided in the middle of the cathode inlet pipe 40a as an example. By driving the cathode liquid circulation device 42, the cathode liquid Lc flows in the cathode liquid circulation path 40. As a result, the cathode liquid Lc circulates between the cathode liquid tank 38 and the cathode chamber 20.
  • the cathode liquid circulation device 42 for example, various pumps such as a gear pump and a cylinder pump, a natural flow type device, and the like can be used.
  • the cathode liquid-gas-liquid separation unit 44 is provided in the middle of the cathode outlet pipe 40b.
  • hydrogen is produced by a side reaction. This side reaction is more likely to occur as the concentration of the hydride ⁇ supplied to the cathode electrode 18 decreases. In other words, the ratio of side reactions to all electrode reactions at the cathode electrode 18 increases. Therefore, the cathode liquid Lc recovered from the cathode chamber 20 contains gaseous hydrogen and dissolved hydrogen in addition to the unreacted hydride ⁇ and the generated organic hydride ⁇ . The gaseous hydrogen is separated from the cathode liquid Lc at the cathode liquid gas-liquid separation unit 44 and taken out of the system. The cathode liquid Lc from which hydrogen is separated is recovered in the cathode liquid tank 38.
  • the cathode inlet pipe 40a is connected to the lower portion of the cathode chamber 20 in the vertical direction
  • the cathode outlet pipe 40b is connected to the upper portion of the cathode chamber 20 in the vertical direction.
  • the cathode liquid Lc in the cathode liquid tank 38 is pumped up by the cathode liquid circulation device 42 and enters the cathode chamber 20.
  • the cathode liquid Lc in the cathode chamber 20 is pushed out to the cathode outlet pipe 40b by the flow of the cathode liquid Lc entering the cathode chamber 20, and flows down to the cathode liquid gas-liquid separation unit 44 by gravity.
  • the cathode liquid Lc is placed under atmospheric pressure in the cathode liquid gas-liquid separation unit 44.
  • the cathode liquid Lc in the cathode liquid gas-liquid separation unit 44 flows into the cathode liquid tank 38 in a natural flow manner as the liquid level in the cathode liquid tank 38 decreases.
  • the cathode inlet pipe 40a may be connected to the upper part of the cathode chamber 20 in the vertical direction. In this case, the cathode liquid Lc enters the cathode chamber 20 from the upper part in the vertical direction. That is, the cathode liquid Lc may be supplied to the cathode chamber 20 as a downward flow instead of an upward flow.
  • the control unit 10 controls the operation of the organic hydride manufacturing apparatus 1.
  • the control unit 10 is realized by elements and circuits such as a computer CPU and memory as a hardware configuration, and is realized by a computer program or the like as a software configuration, but in FIG. 1, it is realized by their cooperation. It is drawn as a functional block. It is well understood by those skilled in the art that this functional block can be realized in various ways by a combination of hardware and software.
  • a signal indicating the voltage of the electrolytic cell 2, the potential of the anode electrode 14, or the potential of the cathode electrode 18 is input to the control unit 10 from the sensor 46 provided in the electrolytic cell 2.
  • the sensor 46 can detect the potential of each electrode and the voltage of the electrolytic cell 2 by a known method.
  • the sensor 46 is composed of a known voltmeter or the like. Note that FIG. 1 schematically shows the sensor 46.
  • the sensor 46 may include a current detection unit that detects a current flowing between the anode electrode 14 and the cathode electrode 18.
  • the control unit 10 controls the power supply 4, the anode liquid circulation device 34, the cathode liquid circulation device 42, and the like based on the detection result of the sensor 46.
  • the water removing device 12 is a device that removes the accompanying water W from the cathode liquid Lc. As described above, the accompanying water W moves to the cathode chamber 20 from the anode chamber 16 side. Therefore, the cathode liquid Lc sent out from the cathode chamber 20 contains not only the hydride ⁇ and the organic hydride ⁇ but also the accompanying water W. The water removing device 12 removes the accompanying water W from the cathode liquid Lc.
  • the water removing device 12 has a container 48, a drain pipe 50, a detection unit 52, and a switching unit 54.
  • the container 48 stores the cathode liquid Lc delivered from the cathode chamber 20.
  • the container 48 of the present embodiment is provided in the middle of the cathode outlet pipe 40b. Further, the container 48 also serves as a cathode liquid-gas-liquid separation unit 44. Therefore, an exhaust port 48a for discharging hydrogen in the cathode liquid Lc is provided in the upper part of the container 48 in the vertical direction.
  • the cathode liquid Lc stored in the container 48 contains the hydride ⁇ , the organic hydride ⁇ , and the accompanying water W.
  • the hydride ⁇ and the organic hydride ⁇ have a lighter specific gravity than the accompanying water W and have incompatibility with the accompanying water W. Therefore, the cathode liquid Lc is divided into a lower layer (aqueous layer) containing the accompanying water W and an upper layer (oil layer) containing the hydride ⁇ and the organic hydride ⁇ in the container 48.
  • the drain pipe 50 is connected to the container 48 and discharges the accompanying water W accumulated in the container 48.
  • One end of the cathode outlet pipe 40b is connected to the container 48.
  • the other end of the cathode outlet pipe 40b is connected to the cathode liquid tank 38.
  • one end of the drain pipe 50 is connected to the container 48.
  • the connection position C1 of the drain pipe 50 to the container 48 (cathode liquid-gas-liquid separation unit 44) is arranged vertically below the connection position C2 of the cathode outlet pipe 40b to the container 48.
  • the detection unit 52 detects that a predetermined amount of accompanying water W has accumulated in the container 48.
  • the "predetermined amount” can be appropriately set based on empirical knowledge or experiments.
  • the detection unit 52 of the present embodiment includes an interface sensor that detects the interface IF between the layer containing the hydride ⁇ and the organic hydride ⁇ in the cathode liquid Lc and the layer containing the accompanying water W.
  • a known interface sensor such as a float type interface sensor, a capacitance type interface sensor, a conductivity type interface sensor, or the like can be used for the detection unit 52. Further, a person skilled in the art can appropriately select a combination of the types of the hydride ⁇ and the organic hydride ⁇ and the detection method of the interface sensor.
  • the detection position of the interface IF of the detection unit 52 is set vertically below the connection position C2 of the cathode outlet pipe 40b. Further, the detection position of the interface IF is set vertically above the connection position C1 of the drain pipe 50.
  • the detection unit 52 may be arranged inside the container 48. Further, when the container 48 does not interfere with the detection of the interface IF (for example, when the container 48 is made of a material capable of detecting the capacitance inside the container from the outside of the container), the detection unit 52 is placed outside the container 48. It may be arranged. By detecting the interface IF, the detection unit 52 can detect that a predetermined amount of accompanying water W has accumulated in the container 48. When the detection unit 52 detects the interface IF, the detection unit 52 transmits a control signal to the switching unit 54.
  • the switching unit 54 is provided in the drain pipe 50.
  • the switching unit 54 includes a mechanism capable of switching between a regulated state for restricting drainage from the drainage pipe 50 and an execution state for executing drainage from the drainage pipe 50.
  • the switching unit 54 of the present embodiment is composed of a valve.
  • a valve constituting the switching unit 54 for example, a known solenoid valve or the like can be used.
  • the valve constituting the switching unit 54 is a normally closed type solenoid valve that closes when the power is not supplied and opens when the power is turned on. When the switching unit 54 is closed, the discharge of the accompanying water W from the drainage pipe 50 is restricted.
  • the switching unit 54 When the switching unit 54 is opened, the accompanying water W is allowed to be discharged from the drain pipe 50 (draining of the accompanying water W is executed).
  • the switching unit 54 opens the valve based on the detection result of the detection unit 52. That is, when the water level (interface IF) of the accompanying water W rises to the detection position of the detection unit 52, the switching unit 54 becomes energized and opens in response to the control signal from the detection unit 52, and the accompanying water W automatically opens. Is discharged from the container 48.
  • the amount of accompanying water W accumulated in the container 48 by the opening of the switching unit 54 is determined according to the size of the container 48 and the detection position of the interface IF.
  • the switching unit 54 closes the valve after a predetermined time has passed since the valve was opened to regulate drainage.
  • the valve opening time of the switching unit 54 is adjusted so that the interface IF closes before reaching the connection position C1 of the drain pipe 50.
  • the valve opening time can be set in advance based on the amount of accompanying water W accumulated in the container 48 when the switching unit 54 is opened, the drainage speed from the drain pipe 50, and the like. This makes it possible to prevent the hydride ⁇ and the organic hydride ⁇ from being discharged from the drain pipe 50.
  • the valve closing of the switching unit 54 may be realized by the control of the detection unit 52, or may be realized by a timer or the like that stops the energization of the switching unit 54 after a predetermined time has elapsed. ..
  • the opening and closing of the switching unit 54 may be controlled as follows. That is, the detection unit 52 has two interface sensors, and one interface sensor is arranged below the other interface sensor. The interface IF detection position on the upper interface sensor is set below the connection position C2, and the interface IF detection position on the lower interface sensor is set above the connection position C1.
  • the detection unit 52 has two interface sensors, and one interface sensor is arranged below the other interface sensor.
  • the interface IF detection position on the upper interface sensor is set below the connection position C2
  • the interface IF detection position on the lower interface sensor is set above the connection position C1.
  • the switching portion 54 is opened, the accompanying water W is discharged, and the interface IF is lowered.
  • the switching unit 54 closes.
  • This control also can prevent the hydride ⁇ and the organic hydride ⁇ from being discharged from the drain pipe 50.
  • the cathode liquid Lc circulates between the cathode liquid tank 38 and the cathode chamber 20.
  • the cathode liquid Lc sent out from the cathode chamber 20 does not have to be returned to the cathode liquid tank 38.
  • the cathode liquid Lc sent out from the cathode chamber 20 may be stored in an organic hydride tank (not shown) after passing through the cathode liquid gas-liquid separation unit 44.
  • the cathode liquid Lc sent out from the cathode chamber 20 contains the unreacted hydride ⁇ .
  • the cathode liquid Lc sent out from the cathode chamber 20 does not contain the hydride ⁇ . ..
  • the organic hydride production apparatus 1 may have a plurality of electrolytic cells 2.
  • each electrolytic cell 2 is oriented so that the arrangement of the anode chamber 16 and the cathode chamber 20 is the same, and the electrolytic cells 2 are laminated with a current-carrying plate sandwiched between the adjacent electrolytic cells 2.
  • the current-carrying plate is made of a conductive material such as metal.
  • the electrolytic cells 2 may be connected in parallel, or a series connection and a parallel connection may be combined.
  • the switching unit 54 may be configured by a pump. In this case, the switching unit 54 is driven by receiving the control signal from the detection unit 52 to execute drainage. Further, the switching unit 54 stops driving when a predetermined time has elapsed from the execution of drainage to regulate drainage.
  • the organic hydride production apparatus 1 includes an electrolytic cell 2 and a water removing apparatus 12.
  • the anode electrode 14 that oxidizes water in the cathode solution La to generate protons
  • the anode chamber 16 that houses the anode electrode 14, and the hydride ⁇ in the cathode solution Lc are hydrogenated with protons.
  • the cathode electrode 18 that generates the organic hydride ⁇ , the cathode chamber 20 that houses the cathode electrode 18, and the anode chamber 16 and the cathode chamber 20 are partitioned, and protons are transferred from the anode chamber 16 side to the cathode chamber 20 side together with the accompanying water W. It has an anode 22 and.
  • the water removing device 12 has a container 48 for storing the cathode liquid Lc sent out from the cathode chamber 20, a drainage pipe 50 connected to the container 48 and discharging the accompanying water W, and a predetermined amount of the accompanying water W accumulated in the container 48. It is possible to switch between the detection unit 52 that detects the fact and the regulated state that regulates the drainage from the drainage pipe 50 and the execution state that executes the drainage, which is provided in the drainage pipe 50, and is based on the detection result of the detection unit 52.
  • It has a switching unit 54 for switching from the regulated state to the execution state, and removes the accompanying water W from the cathode liquid Lc containing at least the organic hydride ⁇ and the accompanying water W sent out from the cathode chamber 20.
  • the organic hydride manufacturing apparatus 1 includes a water removing device 12 that detects that a predetermined amount of accompanying water W has accumulated in the container 48 and automatically drains the water. Then, when the detection unit 52 detects that a predetermined amount of the accompanying water W has accumulated in the container 48, the accompanying water W is discharged from the container 48.
  • the container downstream side container
  • the cathode liquid Lc such as the cathode liquid gas-liquid separation unit 44
  • the downstream container is used so that the entire amount of the accompanying water W generated by the operation of the organic hydride manufacturing apparatus 1 can be stored. It is necessary to increase the volume.
  • the water removing device 12 drains water every time the accompanying water W reaches a predetermined amount, the size required for the container 48 included in the water removing device 12 can be reduced. In addition, it is possible to avoid increasing the size of the container on the downstream side. Therefore, it is possible to suppress the increase in size of the organic hydride production apparatus 1.
  • the organic hydride manufacturing apparatus 1 of the present embodiment is connected to the cathode liquid tank 38 for storing the cathode liquid Lc supplied to the cathode chamber 20, the cathode liquid tank 38 and the cathode chamber 20, and is contained in the cathode liquid tank 38.
  • the cathode inlet pipe 40a that supplies the cathode liquid Lc to the cathode chamber 20, and the cathode outlet pipe 40b that is connected to the cathode chamber 20 and the cathode liquid tank 38 and returns the cathode liquid Lc sent out from the cathode chamber 20 to the cathode liquid tank 38.
  • the accompanying water W may be sent to the cathode chamber 20 via the cathode liquid circulation path 40.
  • the accompanying water W is sent into the cathode chamber 20
  • the amount of the accompanying water W that reaches the reaction field of the cathode electrode 18 increases, and the reduction reaction of the hydride ⁇ may be inhibited.
  • the organic hydride production apparatus 1 of the present embodiment includes the water removing apparatus 12, it is possible to suppress the inhibition of the reduction reaction of the hydride ⁇ by the accompanying water W. Therefore, the production efficiency of the organic hydride can be effectively improved.
  • the organic hydride manufacturing apparatus 1 includes a cathode liquid circulation apparatus 42 provided in the middle of the cathode inlet pipe 40a.
  • the container 48 of the water removing device 12 is provided in the middle of the cathode outlet pipe 40b.
  • the flow of the cathode liquid Lc tends to be gentler in the cathode outlet pipe 40b in which the cathode liquid circulation device 42 is not provided, as compared with the cathode inlet pipe 40a in which the cathode liquid circulation device 42 is provided.
  • the water removing device 12 can be installed in the region where the flow of the cathode liquid Lc is likely to be gentler, and the accompanying water W can be more stably stored in the bottom of the container 48. be able to. Therefore, the removal efficiency of the accompanying water W can be improved.
  • the container 48 of the present embodiment also serves as the cathode liquid-gas-liquid separation unit 44.
  • the cathode liquid-gas-liquid separation unit 44 As a result, it is possible to suppress an increase in cost associated with the installation of the water removing device 12 as compared with the case where the container 48 is separately provided. In addition, it is possible to further suppress the increase in size of the organic hydride production apparatus 1.
  • the detection unit 52 of the present embodiment has an interface IF between the layer containing at least the organic hydride ⁇ in the cathode liquid Lc and the layer containing the accompanying water W (when the cathode liquid Lc contains the hydride ⁇ ).
  • the accompanying water W accumulated in the container 48 can be easily detected. Therefore, the configuration of the water removing device 12 can be simplified.
  • FIG. 2 is a schematic view of a part of the organic hydride manufacturing apparatus 1 according to the modified example.
  • the electrolytic cell 2, the power supply 4, the first distribution mechanism 6, the control unit 10, and the power supply unit 24 in this modification have the same configurations as those in the embodiment.
  • the second distribution mechanism 8 has a cathode liquid tank 38, a cathode liquid circulation path 40, a cathode liquid circulation device 42, and a cathode liquid gas-liquid separation unit 44.
  • the water removing device 12 is provided in the cathode liquid / gas / liquid separating unit 44, but in this modification, the water removing device 12 is provided in the cathode liquid tank 38. Except for this point, each configuration of the second distribution mechanism 8 is the same as that of the embodiment.
  • the water removing device 12 has a container 48, a drain pipe 50, a detection unit 52, and a switching unit 54.
  • the container 48 of this modification also serves as a cathode liquid tank 38.
  • the cathode liquid Lc stored in the container 48 contains the hydride ⁇ , the organic hydride ⁇ , and the accompanying water W.
  • the cathode liquid Lc is divided into a lower layer containing the accompanying water W and an upper layer containing the hydride ⁇ and the organic hydride ⁇ in the container 48.
  • connection position C1 of the drain pipe 50 to the container 48 (cathode liquid tank 38) is arranged vertically below the connection position C3 of the cathode inlet pipe 40a to the container 48. Further, naturally, the connection position C1 is arranged vertically below the connection position of the cathode outlet pipe 40b with respect to the container 48.
  • the detection unit 52 detects that a predetermined amount of accompanying water W has accumulated in the container 48.
  • the detection unit 52 is composed of an interface sensor.
  • the detection position of the interface IF of the detection unit 52 is set vertically below the connection position C3 of the cathode inlet pipe 40a. Further, the detection position of the interface IF is set vertically above the connection position C1 of the drain pipe 50.
  • the switching unit 54 is provided in the drain pipe 50 and can switch between a regulated state for restricting drainage from the drain pipe 50 and an execution state for executing drainage from the drain pipe 50.
  • the switching unit 54 of this modification is composed of a valve as in the embodiment, and opens the valve based on the detection result of the detection unit 52. That is, when the water level of the accompanying water W rises to the detection position of the detection unit 52, the switching unit 54 becomes energized and opens in response to the control signal from the detection unit 52, and the accompanying water W automatically becomes the container 48. Is discharged from. Further, as an example, the switching unit 54 closes when a predetermined time has elapsed from the opening of the valve. As in the embodiment, opening / closing control of the switching unit 54 using two interface sensors can also be adopted. Further, the switching unit 54 may be configured by a pump.
  • the organic hydride production apparatus 1 according to the present modification can also obtain the same effect as the organic hydride production apparatus 1 according to the embodiment.
  • An exhaust port 48a may be provided in the container 48 constituting the cathode liquid tank 38, and the container 48 of the water removing device 12 may also serve as the cathode liquid tank 38 and the cathode liquid gas-liquid separation unit 44.
  • the anolyte liquid gas-liquid separation unit 36 and the anolyte liquid tank 30 may be integrated.
  • the embodiments may be specified by the items described below.
  • a cathode chamber (20) that houses the cathode electrode (18) and an anode chamber (20) that partitions the anode chamber (16) and the cathode chamber (20).
  • a switching unit (54) for switching to an execution state is provided. Water removal device (12).
  • a cathode chamber (20) that houses the cathode electrode (18) and an anode chamber (20) that partitions the anode chamber (16) and the cathode chamber (20).
  • the cathode solution (Lc) containing water (W) is stored in the container (48), and the cathode solution (Lc) is stored in the container (48). This includes discharging the accompanying water (W) from the container (48) when it is detected that a predetermined amount of the accompanying water (W) has accumulated in the container (48). Water removal method.
  • the present invention can be used for an organic hydride manufacturing apparatus, a water removing apparatus, and a water removing method.

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Automation & Control Theory (AREA)
  • Analytical Chemistry (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Sustainable Development (AREA)
  • Electrolytic Production Of Non-Metals, Compounds, Apparatuses Therefor (AREA)
  • Water Treatment By Electricity Or Magnetism (AREA)
  • Removal Of Specific Substances (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
  • Water Treatment By Sorption (AREA)
PCT/JP2021/042828 2020-12-03 2021-11-22 有機ハイドライド製造装置、水除去装置および水除去方法 Ceased WO2022118695A1 (ja)

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EP21900450.4A EP4257731A4 (en) 2020-12-03 2021-11-22 Apparatus for producing organic hydride, water removal device, and water removal method
AU2021392237A AU2021392237A1 (en) 2020-12-03 2021-11-22 Organic hydride production apparatus, water removal device, and water removal method
US18/255,643 US20240102192A1 (en) 2020-12-03 2021-11-22 Organic hydride production device, water removal device, and water removal method
CN202180080512.1A CN116529426A (zh) 2020-12-03 2021-11-22 有机氢化物制造装置、水去除装置以及水去除方法
JP2022566851A JPWO2022118695A1 (https=) 2020-12-03 2021-11-22

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JP2000297392A (ja) * 1999-04-12 2000-10-24 Japan Organo Co Ltd ガス溶解水製造装置
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CN116529426A (zh) 2023-08-01
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AU2021392237A9 (en) 2024-09-12
JPWO2022118695A1 (https=) 2022-06-09
US20240102192A1 (en) 2024-03-28

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