WO2018221036A1 - Méthode de production d'hydrure de magnésium, système de production d'énergie utilisant de l'hydrure de magnésium, et appareil de production d'hydrure de magnésium - Google Patents

Méthode de production d'hydrure de magnésium, système de production d'énergie utilisant de l'hydrure de magnésium, et appareil de production d'hydrure de magnésium Download PDF

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WO2018221036A1
WO2018221036A1 PCT/JP2018/015418 JP2018015418W WO2018221036A1 WO 2018221036 A1 WO2018221036 A1 WO 2018221036A1 JP 2018015418 W JP2018015418 W JP 2018015418W WO 2018221036 A1 WO2018221036 A1 WO 2018221036A1
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Prior art keywords
magnesium
product
plasma
hydrogen
reaction chamber
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PCT/JP2018/015418
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English (en)
Japanese (ja)
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力 滝沢
峯夫 森元
坂本　雄一
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株式会社エスイー
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Priority claimed from JP2017227963A external-priority patent/JP6471211B2/ja
Application filed by 株式会社エスイー filed Critical 株式会社エスイー
Priority to KR1020197035694A priority Critical patent/KR102111622B1/ko
Priority to MYPI2020002269A priority patent/MY176543A/en
Priority to EP18810561.3A priority patent/EP3632842A4/fr
Priority to US16/617,436 priority patent/US11643704B2/en
Priority to MA47828A priority patent/MA47828B1/fr
Publication of WO2018221036A1 publication Critical patent/WO2018221036A1/fr

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    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B6/00—Hydrides of metals including fully or partially hydrided metals, alloys or intermetallic compounds ; Compounds containing at least one metal-hydrogen bond, e.g. (GeH3)2S, SiH GeH; Monoborane or diborane; Addition complexes thereof
    • C01B6/04—Hydrides of alkali metals, alkaline earth metals, beryllium or magnesium; Addition complexes thereof
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B5/00—General methods of reducing to metals
    • C22B5/02—Dry methods smelting of sulfides or formation of mattes
    • C22B5/12—Dry methods smelting of sulfides or formation of mattes by gases
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M8/00—Fuel cells; Manufacture thereof
    • H01M8/06—Combination of fuel cells with means for production of reactants or for treatment of residues
    • H01M8/0606—Combination of fuel cells with means for production of reactants or for treatment of residues with means for production of gaseous reactants
    • H01M8/065—Combination of fuel cells with means for production of reactants or for treatment of residues with means for production of gaseous reactants by dissolution of metals or alloys; by dehydriding metallic substances
    • H—ELECTRICITY
    • H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
    • H05H—PLASMA TECHNIQUE; PRODUCTION OF ACCELERATED ELECTRICALLY-CHARGED PARTICLES OR OF NEUTRONS; PRODUCTION OR ACCELERATION OF NEUTRAL MOLECULAR OR ATOMIC BEAMS
    • H05H1/00—Generating plasma; Handling plasma
    • H05H1/24—Generating plasma
    • H05H1/46—Generating plasma using applied electromagnetic fields, e.g. high frequency or microwave energy
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/30—Hydrogen technology
    • Y02E60/50—Fuel cells
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P70/00—Climate change mitigation technologies in the production process for final industrial or consumer products
    • Y02P70/50—Manufacturing or production processes characterised by the final manufactured product

Definitions

  • the present invention relates to a method for producing magnesium hydride and the like, a power generation system using magnesium hydride, and a production apparatus for magnesium hydride and the like.
  • a typical example of such clean energy is nuclear power generation, but it not only has the potential to pollute the environment with radioactive waste generated during operation, but once an accident occurs, the damage is significant.
  • the current situation is that a policy not to construct a nuclear power plant has been proposed.
  • clean energy includes renewable energy such as solar power generation and wind power generation.
  • renewable energy such as solar power generation and wind power generation.
  • the amount of power generation depends on the weather, there is a problem that stable power supply is difficult.
  • Patent Document 1 discloses that magnesium hydride is regenerated again from magnesium hydroxide, which is a by-product after separating hydrogen from magnesium hydride and generating power in a fuel cell or the like. .
  • Patent Document 1 specifically, magnesium hydroxide is heated and dehydrated to obtain magnesium oxide, and the first procedure is performed in a plasma flame of a plasma torch having a temperature of about 2000 (K).
  • a method of performing a third procedure for producing magnesium hydride from magnesium is disclosed.
  • Patent Document 1 describes that when hydrogen is supplied in the second procedure, metal magnesium becomes magnesium hydroxide due to a reversible reaction during cooling. It is considered that the second procedure is performed using gas as methane. When methane is used as a reducing agent, there is a problem that carbon dioxide, which causes global warming, is generated.
  • Patent Document 2 discloses a method of generating metallic magnesium by performing a reduction reaction by exposing anhydrous magnesium halide to low-temperature plasma generated under a reduced pressure of atmospheric pressure or lower.
  • JP 2011-32131 A Japanese Unexamined Patent Publication No. 2016-216780
  • magnesium hydroxide is mainly produced, but even if magnesium hydride reacts with water to produce magnesium oxide,
  • the reaction formula is as follows. Since 4 mol of hydrogen is generated with respect to 2 mol of magnesium hydride, the amount of generated hydrogen is doubled as compared with the case of metallic magnesium. 2MgH 2 + 2H 2 O ⁇ 2MgO + 4H 2 Moreover, magnesium hydride has a high reaction rate even when it is reacted with low-temperature water.
  • magnesium hydride having a large amount of hydrogen generation and a high hydrogen generation rate is preferable.
  • the present invention has been made in view of such circumstances, and a method for producing magnesium hydride with high production efficiency free of carbon dioxide, a power generation system free of carbon dioxide and radiation using magnesium hydride, and magnesium hydride.
  • An object of the present invention is to provide a manufacturing apparatus.
  • the present invention is grasped by the following composition in order to achieve the above-mentioned object.
  • the method for producing magnesium hydride according to the present invention includes a step of irradiating a magnesium compound different from the magnesium hydride with hydrogen plasma, and an adhesion for adhering the magnesium hydride disposed within the range where the hydrogen plasma exists. Depositing the magnesium product containing magnesium hydride on the means, and the surface temperature of the attaching means is kept below a predetermined temperature at which the magnesium hydride precipitates.
  • the magnesium compound is a magnesium compound having no oxygen atom.
  • the magnesium compound is magnesium halide.
  • the magnesium compound is magnesium chloride.
  • the recovering procedure may be carried out without stopping the irradiation of the hydrogen plasma to the magnesium compound, and into the take-out chamber where the magnesium product can be taken out from the apparatus that irradiates the hydrogen plasma.
  • a procedure for moving the magnesium product adhering to the adhering means to a position where the exfoliated magnesium product can be accommodated, and exfoliating the magnesium product from the adhering means so as to be accommodated in the take-out chamber And a procedure for causing
  • the power generation system of the present invention is a power generation system using magnesium hydride, a procedure for generating a magnesium product containing magnesium hydride from a magnesium compound different from the magnesium hydride, and the magnesium product.
  • a procedure for generating hydrogen from the hydrogen a procedure for supplying the generated hydrogen to a power generation unit to perform power generation, a procedure for generating the magnesium compound from a by-product containing magnesium after generating the hydrogen, including.
  • the magnesium compound is magnesium chloride
  • the by-product contains magnesium hydroxide or magnesium oxide
  • the procedure for producing the magnesium compound includes the by-product, hydrochloric acid, And a procedure for obtaining a hydrate of magnesium chloride and a procedure for dehydrating the hydrate.
  • the apparatus for producing magnesium hydride of the present invention comprises a microwave generating means for generating a microwave supplied into a reaction chamber, a hydrogen supply means for supplying hydrogen into the reaction chamber, and the hydrogen in the reaction chamber.
  • Cooling means for keeping the surface temperature of the surface on which the material is deposited below a predetermined temperature at which the magnesium hydride precipitates.
  • the range in which the hydrogen plasma exists is a range in which the hydrogen plasma having a plasma density that can be visually observed exists.
  • a peeling means for peeling the magnesium product from the adhesion means, and without stopping the irradiation of the hydrogen plasma to the magnesium compound A take-out chamber capable of taking out the magnesium product, and the peeling means is located at a position where the peeled magnesium product is accommodated in the take-out chamber when the magnesium product is peeled off from the attaching means. It is provided and the said adhesion means can move the said magnesium product adhering to the position where the said magnesium product is peeled by the said peeling means.
  • a window of a dielectric material provided in a portion where the microwave is incident into the reaction chamber is provided, and the hydrogen plasma is formed on the surface of the window.
  • a microwave surface wave hydrogen plasma with high density and low electron temperature is generated.
  • the production method of the present invention is a method for producing a product obtained by treating a raw material containing metal atoms with plasma to obtain a product different from the raw material, wherein the raw material is vaporized to substantially remove oxygen atoms.
  • the surface temperature is maintained at a temperature within a predetermined temperature range suitable for the precipitation of the product.
  • the plasma is a microwave surface wave plasma.
  • the production apparatus of the present invention is a production apparatus for obtaining a product different from the raw material by treating a raw material containing metal atoms with plasma, and generating microwaves to be supplied into a reaction chamber And a gas supply means for supplying a reactive gas substantially free of oxygen atoms in the reaction chamber, a raw material supply means for vaporizing the raw material and supplying it into the plasma of the reactive gas, and the generated An adhesion means for depositing the product, and a surface temperature of the surface to which the product of the adhesion means is deposited are kept within a predetermined temperature range suitable for precipitation of the product, which is arranged in a range where plasma exists. Temperature control means.
  • suppression means for suppressing adhesion of the raw material and the product to the surface of the window.
  • the raw material supply means includes at least a cathode part having a surface exposed in the reaction chamber, at least exposed in the reaction chamber, An anode portion having a surface to be disposed; and voltage applying means for applying a voltage between the anode portion and the cathode portion.
  • the manufacturing method of magnesium hydride with sufficient production efficiency without a carbon dioxide, the electric power generation system without a carbon dioxide and radiation using magnesium hydride, and the manufacturing apparatus of magnesium hydride can be provided. .
  • a magnesium compound different from magnesium hydride is reduced with hydrogen plasma, and a phenomenon in which magnesium hydride precipitates on the surface of the low temperature portion by creating a low temperature portion in the hydrogen plasma was discovered. Is based on that.
  • hydrogen plasma is more precisely a high-density microwave surface wave hydrogen plasma having a low electron temperature, and a dielectric material window for introducing microwaves into the reaction chamber 2 (see FIG. 2).
  • the magnesium product deposited on the surface of the window W contains magnesium hydride to the extent that it shoots vigorously and generates hydrogen just by dripping water droplets. Based on having discovered that.
  • the magnesium compound different from magnesium hydride is magnesium chloride
  • the magnesium compound may be a magnesium halide different from magnesium chloride such as fluorinated magnesium. .
  • a magnesium compound other than magnesium halide may be used as a magnesium compound different from magnesium hydride.
  • the magnesium compound different from magnesium hydride is preferably a magnesium compound having no oxygen.
  • the magnesium compound preferably does not contain oxygen-containing impurities.
  • magnesium chloride when magnesium chloride is used as a magnesium compound different from magnesium hydride, there are many advantages. Therefore, it is preferable to use magnesium chloride as a magnesium compound different from magnesium hydride. .
  • Magnesium chloride is contained in bittern, which can be obtained as a by-product when producing salt from seawater, its reserves are inexhaustible, and magnesium chloride is produced inexpensively using it as a raw material Therefore, there is no problem even if magnesium chloride is not regenerated from the by-product after separating hydrogen from magnesium hydride.
  • extraction of hydrogen from magnesium hydride can be performed by adding water to magnesium hydride (see Formula 1).
  • reaction of this Formula 1 becomes exothermic reaction, it is also possible to generate electric power using the heat
  • magnesium chloride hexahydrate crystals are precipitated by evaporating water at a temperature at which the magnesium chloride is not decomposed in the aqueous solution containing magnesium chloride to generate a basic base (Mg (OH) Cl).
  • anhydrous magnesium chloride By dehydrating the magnesium chloride hexahydrate thus obtained, anhydrous magnesium chloride can be obtained again.
  • dehydration is performed by heat treatment at a molar ratio of magnesium chloride hexahydrate to ammonium chloride of about 1: 8 (see Formula 3).
  • the dehydration reaction shown in Formula 3 may be performed at a temperature of about 340 ° C. or higher, which is the decomposition temperature of ammonium chloride.
  • a temperature of this heat treatment is too high, magnesium oxide is generated. Therefore, it is preferable to perform the heat treatment at a temperature not exceeding 400 ° C.
  • magnesium chloride when magnesium chloride is used as a magnesium compound different from magnesium hydride, magnesium chloride can be regenerated from the by-product after separating hydrogen from magnesium hydride.
  • magnesium hydride can be obtained by reduction with hydrogen plasma, and metal magnesium itself can be used to circulate.
  • hydrochloric acid and chlorine are generated in the reduction treatment using hydrogen plasma that generates magnesium hydride from magnesium chloride, so that this hydrochloric acid can be used in the reaction of Formula 2 shown above.
  • an aqueous hydrochloric acid solution can be prepared by exhaust gas treatment in which the exhaust gas during the reduction reaction is submerged in a water shower. Just use water.
  • Equation 4 the problem is how to change the environment (pressure / temperature) during the reaction so that the right side in Equation 4 becomes stable and the reaction proceeds to the right side.
  • Equation 4 which is stable can be understood by considering Gibbs free energy, but in the case of Equation 4, the pressure in the reactor for performing the plasma reaction is set to a high density and low electron temperature micro plasma. Assuming that 10 Pa is used to generate the wave surface wave hydrogen plasma, the furnace temperature needs to be about 1150 ° C. or higher in order to proceed the reaction to the right side.
  • the magnesium hydride itself is in a gas state, so that it is necessary to lower the temperature in the furnace in order to precipitate as a solid, but in the temperature range lower than about 1150 ° C. Since the reaction to the left side of 4 becomes dominant, the substance that precipitates as a solid becomes magnesium chloride, and magnesium hydride does not precipitate.
  • the magnesium product deposited on the surface of the dielectric material window W (see FIG. 2) for introducing microwaves into the reaction chamber 2 (see FIG. 2) drips water droplets. It was so hard that it contained magnesium hydride enough to generate hydrogen.
  • FIG. 1 shows that the pressure in the reaction chamber 2 (see FIG. 2) is 10 Pa, the horizontal axis represents the hydrogen atom partial pressure (mPa), and the vertical axis represents the temperature (° C.). 5 is a graph showing how many times (° C.) the boundary between the reaction proceeding to the right and the reaction proceeding to the left when the partial pressure (mPa) is changed.
  • MgH 2 is generated by lowering the temperature. At the same temperature, MgH 2 is generated as the partial pressure of hydrogen atoms increases. It has become so.
  • MgH 2 is solution exists to generate MgH 2 even at a temperature range below 100 ° C. does not decompose to Mg and H 2, thereby favorably precipitate the MgH 2 as a solid
  • the dielectric material window W (see FIG. 2) for introducing the microwave into the reaction chamber 2 (see FIG. 2) was in a relatively low temperature state.
  • the atoms in the hydrogen plasma generated on the surface of the dielectric material window W (see FIG. 2) for introducing the microwave into the reaction chamber 2 (see FIG. 2)
  • the plasma density decreases as the distance from the window W decreases.
  • the surface of the window W contains hydrogen plasma having a high density enough to satisfy the assumption of Equation 5, and MgH 2 Is estimated to have precipitated as a solid.
  • the adhering means 80 (see FIG. 2) for adhering magnesium hydride is arranged, and the surface temperature of the adhering means 80 is set to a surface temperature at which magnesium hydride can be precipitated as a solid to obtain magnesium hydride. be able to.
  • the decrease in the density of the hydrogen plasma varies depending on the configuration and conditions of the apparatus, for example, when viewed from a viewing window in which the inside of the reaction chamber 2 (see FIG. 2) can be seen, the high density range is Since the emission color is visible, if the plasma emission is in a range that can be seen visually, the equation assuming the presence of hydrogen atoms or the like as shown in Equation 5 is satisfied, but sufficient hydrogen plasma is present. It is considered that it exists.
  • FIG. 2 is a cross-sectional view for explaining the magnesium hydride production apparatus 1 according to the first embodiment of the present invention.
  • the manufacturing apparatus 1 includes a housing 10 that forms a reaction chamber 2.
  • the manufacturing device 1 includes a partition 11 having an opening 11 ⁇ / b> A at the center in the housing 10.
  • the reaction chamber 2 has the 1st space F and the 2nd space S, this partition part 11 may be abbreviate
  • the manufacturing apparatus 1 includes a window W of a dielectric material (for example, quartz or ceramics) provided in a portion where microwaves are incident in the reaction chamber 2, and the first in the reaction chamber 2 through the window W.
  • a microwave generation unit 20 (for example, a magnetron) that generates a microwave supplied to the space F; and a waveguide 21 that guides the microwave generated by the microwave generation unit 20 to the window W.
  • the frequency of the generated microwave is 2.45 GHz.
  • 5 GHz, 24.1 GHz, 915 MHz of the ISM band that can be used for purposes other than communication It may be 40.6 MHz, 27.1 MHz, 13.56 MHz, or the like.
  • the manufacturing apparatus 1 also has a decompression means 30 that exhausts the gas in the reaction chamber 2 and decompresses the reaction chamber 2. Specifically, as the decompression means 30, the manufacturing apparatus 1 enters the first space F via the first exhaust pipe 31 provided with a first exhaust valve 31 ⁇ / b> A that determines the presence or absence of exhaust by an opening / closing operation or opening / closing control.
  • a first vacuum pump 32 connected to the second space S is connected to the second space S via a second exhaust pipe 33 provided with a second exhaust valve 33A that determines whether or not to exhaust by an opening / closing operation or opening / closing control.
  • a vacuum pump 34 a vacuum pump 34.
  • the pressure in the reaction chamber 2 is low, and at least the pressure in the reaction chamber 2 is 1/10 atm or less.
  • the pressure is preferably 1/100 atm or less, more preferably 1/1000 atm or less, and in this embodiment, about 10 Pa, which is about 1 / 10,000 atm.
  • At least one of 34 is a mechanical booster pump having a high gas suction force.
  • the manufacturing apparatus 1 includes a first pressure gauge 32A for measuring the pressure in the first space F of the reaction chamber 2 and a second pressure for measuring the pressure in the second space S of the reaction chamber 2.
  • the first vacuum pump 32 is configured so that the pressure in the first space F becomes a predetermined pressure (for example, about 10 Pa).
  • the operation of the first exhaust valve 31A may be controlled.
  • the first vacuum pump 32 may be operated, and the operation of the first exhaust valve 31A may be controlled based on the pressure measured by the first pressure gauge 32A.
  • the second vacuum pump 34 and the second exhaust valve are set so that the pressure in the second space S becomes a predetermined pressure (for example, about 10 Pa).
  • the operation of 33A may be controlled.
  • the second vacuum pump 34 may be operated and the operation of the second exhaust valve 33A may be controlled based on the pressure measured by the second pressure gauge 34A.
  • the first vacuum pump 32 and the second vacuum pump 34 are operated, and the pressure in the reaction chamber 2 is set to a predetermined pressure.
  • the first exhaust valve 31A is closed to stop the operation of the first vacuum pump 32, and thereafter the reaction is performed based on the pressure measured by the first pressure gauge 32A or the second pressure gauge 34A. You may make it control operation
  • the pressures measured by the first pressure gauge 32A and the second pressure gauge 34A were averaged. You may make it use a thing.
  • the production apparatus 1 also includes a hydrogen supply means (not shown) for supplying hydrogen as a reducing gas into the reaction chamber 2.
  • the hydrogen supply means includes a hydrogen storage unit (hydrogen cylinder or hydrogen storage tank) (not shown) that serves as a hydrogen supply source, and a flow rate such as a mass flow meter that controls the amount of hydrogen supplied from the hydrogen storage unit to the reaction chamber 2. Controllers (first flow rate controller MFC1 and second flow rate controller MFC2).
  • the hydrogen storage unit is connected so that hydrogen can be supplied to the first space F via the first supply pipe 41, and hydrogen is supplied to the second space S via the second supply pipe 42.
  • a first flow rate controller MFC1 is provided on the hydrogen storage section side of the first supply pipe 41, and a first supply valve 41A for determining whether to supply or not by opening / closing operation or opening / closing control is provided downstream thereof. ing.
  • a second flow rate controller MFC2 is provided on the hydrogen storage unit side of the second supply pipe 42, and a second supply valve 42A for determining whether to supply or not by an opening / closing operation or opening / closing control is provided on the downstream side thereof.
  • the production apparatus 1 includes a raw material supply means 50 for supplying magnesium chloride, which is a magnesium compound different from magnesium hydride, into the reaction chamber 2 (more specifically, in the first space F of the reaction chamber 2). Yes.
  • the raw material supply means 50 includes a raw material storage unit 51 for storing magnesium chloride, which is a magnesium compound different from magnesium hydride as a raw material for generating magnesium hydride, and magnesium chloride in the raw material storage unit 51.
  • a raw material storage unit 51 for storing magnesium chloride which is a magnesium compound different from magnesium hydride as a raw material for generating magnesium hydride
  • magnesium chloride in the raw material storage unit 51. Is supplied to the first space F of the reaction chamber 2 and the first heating unit 53 that generates heat by supplying power from the first power source 53A and heats the raw material supply tube 52 and the raw material storage unit 51. And a first thermometer 54 that measures the temperature of the first heating unit 53.
  • the amount of power supplied from the first power supply 53A to the first heating unit 53 is controlled so that the temperature measurement result by the first thermometer 54 becomes a predetermined temperature that is set, and the raw material supply pipe 52 and the raw material storage 51 are heated to a predetermined temperature.
  • the first heating unit 53 heats the raw material supply pipe 52 and the raw material storage unit 51 to a temperature of about 700 ° C. so that the magnesium chloride is in a gaseous state. Then, the vaporized magnesium chloride flows toward the first space F in the reaction chamber 2 and is supplied into the first space F.
  • the manufacturing apparatus 1 is provided in the first space F of the reaction chamber 2 as the heating means 60 for heating the inside of the reaction chamber 2, and generates heat due to the supply of electric power from the second power source 61 ⁇ / b> A.
  • the 2nd heating part 61 which heats the inside of the space F is provided.
  • the production apparatus 1 includes a second thermometer 62 that measures the temperature in the first space F of the reaction chamber 2, and the measurement result of the temperature by the second thermometer 62 is a predetermined temperature that is set.
  • the supply amount of power supplied from the second power source 61A to the second heating unit 61 is controlled, and the temperature in the first space F of the reaction chamber 2 is maintained at a predetermined temperature.
  • the temperature in the first space F is maintained at a temperature at which magnesium chloride can exist as a gas by the second heating unit 61.
  • a reflector 70 that reflects radiant heat is provided outside the second heating unit 61 in order to prevent the casing 10 from becoming high temperature due to radiant heat from the second heating unit 61.
  • a cooling pipe 71 for water cooling is provided on the outer surface.
  • the reflector 70 is provided with an insertion pipe 72 that is inserted into the second space S from the first space F through the opening 11A of the partitioning portion 11 at a position closer to the center on the upper side.
  • a gas containing hydrogen plasma and magnesium is emitted from the insertion tube 72 to the second space S.
  • the manufacturing apparatus 1 is provided with the adhesion means 80 which makes the magnesium product containing magnesium hydride adhere to the position facing the insertion pipe 72, and after stopping the manufacturing apparatus 1,
  • the attaching means 80 is detachably attached to the housing 10 so that the attaching means 80 can be taken out.
  • the adhering means 80 has a refrigerant supply port IN that supplies a refrigerant (for example, outside air) and a refrigerant outlet OUT that discharges the refrigerant, and a sealed container that prevents the refrigerant from leaking into the second space S of the reaction chamber 2. It has a structure.
  • the attachment means 80 has a surface 81 on which a magnesium product containing magnesium hydride on the side facing the insertion tube 72 is attached, and a high-density hydrogen plasma from which the emission state emitted from the insertion tube 72 can be visually confirmed. By being arranged at a position in direct contact, it is arranged within the range where the generated hydrogen plasma exists.
  • the manufacturing apparatus 1 includes, for example, a cooling means (not shown) (for example, a fan or a compressor) for supplying outside air serving as a refrigerant into the adhering means 80 from the refrigerant supply port IN.
  • a cooling means for example, a fan or a compressor
  • the surface temperature of the surface 81 on which the magnesium product containing magnesium hydride is adhered is kept below a predetermined temperature at which magnesium hydride precipitates.
  • a pipe may be connected to the refrigerant outlet OUT so as to be open to the atmosphere.
  • the alternative chlorofluorocarbon discharged from the refrigerant discharge port OUT is compressed by the compressor, and the compressed alternative chlorofluorocarbon is introduced again from the refrigerant supply port IN (so-called The same as for a refrigerator etc.).
  • the predetermined temperature at which magnesium hydride precipitates is preferably 200 ° C. or lower, more preferably 150 ° C. or lower, and even more preferably 100 ° C. or lower because the amount of precipitation is greatly reduced when it exceeds 200 ° C.
  • the predetermined temperature at which magnesium hydride precipitates is most preferably 100 ° C. or lower.
  • the precipitation amount per unit time of the magnesium product containing magnesium hydride is larger at about 70 ° C. than when the surface temperature is about 80 ° C., and the precipitation per unit time is further about 50 ° C. The result is a large amount.
  • the manufacturing apparatus 1 includes an atmosphere opening pipe 90 provided with a leak valve 91 in the middle, and one end (not shown) of the atmosphere opening pipe 90 is in an atmosphere opening state outside the building where the manufacturing apparatus 1 is installed. ing.
  • the atmosphere release pipe 90 is used to open the reaction chamber 2 to the atmosphere open as an emergency measure when the pressure in the reaction chamber 2 becomes an abnormal pressure. Normally, the leak valve 91 is closed. Thus, the atmosphere is not mixed into the reaction chamber 2.
  • the microwave can be supplied with the reaction chamber 2 in a high vacuum state. Therefore, the hydrogen plasma (microwave surface wave hydrogen plasma) has a high density (for example, a plasma density of 10 ⁇ A microwave surface wave hydrogen plasma having a low electron temperature (for example, 1 eV or less) at 12 / cm 3 or more and 10 ⁇ 14 / cm 3 or less can be stably generated. Moreover, hydrogen plasma having a wide range can be obtained by resonance between the surface wave plasma generated on the surface of the window W and the microwave.
  • microwave surface wave hydrogen plasma has an advantage of low energy loss unlike plasma that consumes energy in order to achieve high electron temperature (for example, 10 eV or more) like high-frequency plasma and DC discharge plasma.
  • the temperature of the plasma disclosed in Patent Document 1 is about 2000 K (about 1700 ° C.), for example, even if the adhering means 80 is made of a metal such as stainless steel or aluminum and cooled with a coolant, If the adhesion means 80 is disposed in the plasma, it is difficult to keep the temperature below the heat resistant temperature of the material, and even if the temperature can be kept below the heat resistant temperature of the material, the surface temperature of the adhesion means 80 is hydrogenated. It is virtually impossible to achieve a surface temperature at which magnesium can precipitate as a solid.
  • the microwave surface wave hydrogen plasma of the present embodiment is a low-temperature plasma in which the temperature of the plasma itself in Celsius (not the electron temperature but the temperature as the atmosphere) is the same as the normal temperature.
  • An adhering means 80 for adhering magnesium hydride is arranged in a range where a fresh hydrogen plasma exists, and the surface temperature of the adhering means 80 (the temperature of the surface 81) is set to a surface temperature at which magnesium hydride can precipitate as a solid. Is possible.
  • some inert gas may be mixed with hydrogen gas. Since the plasma is easily lit by mixing some of the inert gas in this way, the lighting state of the microwave surface wave hydrogen plasma can be stabilized.
  • the decompression means 30 (the first vacuum pump 32 and the second vacuum pump 34) is driven, and the pressure is reduced so that the pressure in the reaction chamber 2 becomes a predetermined pressure (for example, about 10 Pa). To implement.
  • the heating means 60 for heating the inside of the reaction chamber 2 is also driven to raise the temperature in the first space F of the reaction chamber 2 to a predetermined temperature (for example, about 700 ° C.).
  • a predetermined temperature for example, about 700 ° C.
  • the temperature increase in the first space F by the heating means 60 can be performed in a relatively short time, it may be performed at a timing when the pressure in the reaction chamber 2 approaches a predetermined pressure.
  • hydrogen is supplied into the reaction chamber 2 by the hydrogen supply means.
  • the procedure is started, and for example, generation (light emission) of hydrogen plasma is confirmed from a viewing window (not shown). Note that whether hydrogen plasma is generated may be confirmed by a measuring instrument that measures the emission spectrum intensity.
  • the gas containing magnesium means a composite gas containing magnesium atoms, magnesium chloride, magnesium hydride and the like because it is in hydrogen plasma.
  • the driving of the manufacturing apparatus 1 is stopped, the pressure in the reaction chamber 2 is returned to atmospheric pressure, and the temperature at which the adhering means 80 can be taken out (for example, magnesium hydride). After the temperature reaches a temperature that does not react violently with moisture in the air, the adhering means 80 is removed, and the magnesium product containing magnesium hydride adhering to the surface 81 of the adhering means 80 is recovered. .
  • the temperature at which the adhering means 80 can be taken out for example, magnesium hydride.
  • reaction chamber 2 is purged with nitrogen gas or inert gas having a low dew point until the driving of the manufacturing apparatus 1 is stopped and the adhering means 80 is removed.
  • the magnesium product containing magnesium hydride thus produced can be suitably used for a power generation system using magnesium hydride.
  • the power generation system using magnesium hydride generates a magnesium product containing magnesium hydride from a magnesium compound different from magnesium hydride, and generates hydrogen from the magnesium product. It is preferable to include a procedure for generating, a procedure for supplying the generated hydrogen to the power generation unit to generate power, and a procedure for generating a magnesium compound from the by-product containing magnesium after generating hydrogen.
  • the reaction in the procedure for generating hydrogen from the magnesium product is an exothermic reaction, the heat generated in the procedure for generating hydrogen from the magnesium product is further used for power generation. It is possible to further improve the efficiency of power generation by including the procedure to perform.
  • the magnesium compound is magnesium chloride
  • a by-product containing magnesium hydroxide or magnesium oxide is reacted with hydrochloric acid to obtain a magnesium chloride hydrate, and By performing the procedure for dehydrating this hydrate, it is possible to regenerate magnesium chloride as a magnesium compound different from magnesium hydride, and to circulate magnesium while suppressing the generation of carbon. Power generation system.
  • FIG. 3 is a cross-sectional view for explaining the magnesium hydride production apparatus 1 according to the second embodiment of the present invention.
  • the manufacturing apparatus 1 of 2nd Embodiment also has many parts similar to the manufacturing apparatus 1 of 1st Embodiment, below, mainly a different point is demonstrated and description about the same part is abbreviate
  • the portion in which the housing 10 forms the second space S is more lateral (the right side in FIG. 3) than the portion in which the housing 10 forms the first space F. It is formed to extend.
  • a lower third space T provided so as to be able to be cut off from the second space S is formed by the edge cutting door 3. It can be accessed from the outside by opening the door 4.
  • the third space T as described below, magnesium products containing magnesium hydride are accumulated, and the third space T can be opened by opening the extraction door 4 with the edge door 3 closed. And, it does not affect the atmosphere in the second space S, and functions as a take-out chamber capable of taking out the accumulated magnesium product.
  • the magnesium product containing magnesium hydride is attached to the surface 81 of the sealed container structure of the attaching means 80.
  • the attaching means 80 is sealed.
  • a surface 81 of the belt 83 facing the insertion tube 72 is a surface 81 to which a magnesium product containing magnesium hydride is attached.
  • the belt 83 itself in contact with the container 82
  • the surface temperature of the surface 81 is kept below a predetermined temperature at which magnesium hydride precipitates.
  • the driven pulley R2 is installed at a position above the third space T serving as the take-out chamber, and the peeling means 5 for peeling the magnesium product comes into contact with the belt 83 along the driven pulley R2. Is provided.
  • the peeling means 5 when the peeling means 5 is in a state where the edge door 3 is opened, when the magnesium product is peeled from the adhesion means 80 (more specifically, the belt 83), the peeled magnesium product becomes the take-out chamber. It is provided at a position accommodated in the third space T.
  • the peeling means 5 may be a spatula-like member having a leading end width corresponding to the width of the belt 83 and decreasing in thickness toward the leading end side, and is set so that the leading end portion abuts the belt 83 firmly. Has been.
  • the first vacuum pump 32 is connected via a branch exhaust pipe 35 branched from the first exhaust pipe 31 provided with an exhaust valve 31B that determines whether or not exhaust is performed by an opening / closing operation or opening / closing control.
  • a branch exhaust pipe 35 branched from the first exhaust pipe 31 provided with an exhaust valve 31B that determines whether or not exhaust is performed by an opening / closing operation or opening / closing control.
  • the inside of the third space T can be evacuated, and a purge gas supply port PIN for supplying a purge gas into the third space T is provided.
  • a gas such as nitrogen or inert gas having a low dew point is introduced from the purge gas supply port PIN to make the third space T serving as an extraction chamber large.
  • the accumulated magnesium product can be taken out by opening the take-out door 4 under atmospheric pressure, so that the magnesium product can be taken out without affecting the first space F and the second space S.
  • the take-out door 4 is closed and the gas in the third space T is sucked with the first vacuum pump 32 to be in a vacuum state.
  • the magnesium product can be accumulated again in the third space T serving as the extraction chamber without affecting the first space F and the second space S.
  • the manufacturing apparatus 1 does not stop the irradiation of the hydrogen plasma to the peeling means 5 which peels a magnesium product from the adhesion means 80 (more specifically, the belt 83), and a magnesium compound. And a third space T serving as a take-out chamber from which the magnesium product can be taken out.
  • the peeling means 5 is provided at a position where the peeled magnesium product is accommodated in the third space T serving as a take-out chamber when the magnesium product is peeled off from the attaching means 80 (more specifically, the belt 83).
  • the attachment means 80 includes a belt 83, and the magnesium product attached to the position where the magnesium product is peeled by the peeling means 5 can be moved. It is a very different part.
  • the procedure for recovering the magnesium product in the manufacturing method of magnesium hydride starts from the manufacturing apparatus 1 that irradiates the hydrogen plasma without stopping the irradiation of the hydrogen plasma to the magnesium compound.
  • the magnesium product adhering to the adhering means 80 (more specifically, the belt 83) is moved to a position where the separated magnesium product can be accommodated in the third space T serving as a take-out chamber from which the magnesium product can be taken out.
  • hydrogen plasma on the magnesium compound including a procedure for removing the magnesium product from the adhering means 80 (more specifically, the belt 83) so as to be accommodated in the third space T serving as an extraction chamber.
  • the manufacturing cost can be greatly reduced by enabling continuous production as in the manufacturing apparatus 1 of the second embodiment.
  • the peeling means 5 is preferably brought into contact with a position where bending stress is applied to the adhered magnesium product.
  • the structure is not necessarily limited to such a structure.
  • titanium is made by reacting metallic chloride with titanium chloride at a temperature of 800 to 850 ° C. to form magnesium chloride and titanium (see Formula 6), and after crushing and pressing the formed porous sponge titanium, Heated in a vacuum arc furnace and manufactured as titanium ingot.
  • a titanium ingot is manufactured according to a manufacturing method similar to the above-described manufacturing method of a magnesium product containing magnesium hydride, that is, a raw material containing a metal atom (in this example, titanium) (for example, If the production method is such that titanium chloride) is treated with plasma to obtain a product (titanium) different from the raw material, the reaction formula is as shown in the following formula 7. TiCl 4 + 2H 2 ⁇ Ti + 4HCl (7) However, in the case of this example, in the raw material storage part 51, titanium chloride as a raw material containing a metal atom (titanium) is stored.
  • titanium chloride Since titanium chloride has a low vapor pressure, it is vaporized as the reaction chamber 2 (first space F) is depressurized by the depressurization means 30 only by storing it in the raw material storage unit 51. For this reason, as described above, in the case where the pressure is sufficiently reduced, it is not necessary to heat, but it is preferable to be able to heat like the raw material supply means 50 described above. It can be vaporized efficiently. Since some raw materials (for example, titanium chloride) containing metal atoms (for example, titanium chloride) can be vaporized without being heated, the raw material supply means 50 and the reaction chamber 2 (first space) F) may not necessarily have heating means.
  • titanium chloride as a raw material is vaporized and hydrogen substantially free of oxygen atoms is supplied as a reactive gas into the reactive gas plasma (microwave surface wave hydrogen plasma), titanium is formed. It has been confirmed by experiments that titanium can be produced more efficiently than by irradiating microwave surface wave hydrogen plasma to titanium chloride that has not been vaporized by being vaporized and supplied in this way. it can.
  • the required amount of metallic magnesium and the required amount of hydrogen used to turn titanium chloride into titanium are the same at 2 mol, but hydrogen is 1 mol.
  • the material cost can be greatly reduced because the price is about 1/3 to 1/4 of metal magnesium.
  • the surface temperature of the surface of the attaching means 80 disposed in the range where the plasma exists is kept within a predetermined temperature range where the product (titanium) is deposited.
  • titanium adheres and grows directly on the attachment means 80, and the attached titanium is not in the form of a sponge. Therefore, there is no need to treat the porous sponge titanium as a titanium metal.
  • the titanium ingot can be removed simply by removing the thin plate. Can be recovered.
  • the gas supply means for supplying the reactive gas is replaced by the nitrogen supply means instead of the hydrogen supply means described above.
  • a hydrogen storage unit hydrogen cylinder or hydrogen storage tank (not shown) that serves as the hydrogen supply source of the hydrogen supply means described above is changed to a nitrogen supply source (nitrogen cylinder or nitrogen storage tank).
  • the flow rate controller (first flow rate controller MFC1 and second flow rate controller MFC2) such as the mass flow meter described above may be changed from that for hydrogen to that for nitrogen.
  • magnesium nitride has obtained experimental results that tend to precipitate in relatively low temperature locations, but in the case of this method, as described above, adhesion that is arranged within the range where plasma exists Since the surface temperature of the surface of the means 80 can be kept within a predetermined temperature range in which magnesium nitride (target product) is likely to precipitate, the product in the state of magnesium nitride is efficiently attached onto the attaching means 80. It is possible to make it.
  • magnesium nitride is produced by treating metal magnesium in a high-temperature nitrogen atmosphere. For this reason, in a general production method, in order to produce magnesium nitride, first, a step of producing metallic magnesium using magnesium chloride as a raw material is necessary, but in the method of the present invention, a step of producing metallic magnesium. It is possible to directly produce magnesium nitride using magnesium chloride as a raw material.
  • Magnesium nitride contains magnesium chloride vaporized using magnesium chloride as a raw material, in addition to reactive gas plasma (microwave surface wave nitrogen plasma) using nitrogen that does not substantially contain oxygen atoms as a reactive gas.
  • reactive gas plasma microwave surface wave nitrogen plasma
  • the reactive plasma may be a plasma in which a plurality of reactive gases are mixed.
  • nitrogen supply means may be provided in addition to the hydrogen supply means described above as the gas supply means for supplying the reactive gas.
  • the surface temperature of the surface of the adhesion means 80 disposed within the range where the plasma exists is maintained within a predetermined temperature range suitable for the precipitation of the product, a product containing metal atoms can be obtained satisfactorily.
  • metal atoms combine with oxygen atoms to form stable oxides, and if oxygen atoms are included, oxides are formed in plasma. Is preferably substantially free of oxygen atoms.
  • a reactive gas that does not substantially contain oxygen atoms means that there is little oxygen contamination in the reactive gas to the extent that it does not hinder the reaction with plasma, and the reactive gas to the extent that it does not hinder the reaction with plasma. It means a highly reactive gas with a sufficiently low moisture content and a low dew point.
  • some of the raw materials containing metal atoms have a heating temperature required for vaporization exceeding 1000 ° C., and the raw material supply means 50 of the manufacturing apparatus 1 described above is set to such a high temperature.
  • a carbon material is used for a portion that becomes high temperature, and the inside of a metal such as SUS (stainless steel) that can withstand a relatively high temperature so that the carbon material does not touch air (oxygen).
  • the carbon material may be energized and heated while energizing and heating, while a portion such as SUS (stainless steel) may be cooled by water so as not to cause thermal deterioration or melting.
  • the manufacturing apparatus 1 that can handle a case where a high temperature is necessary for the vaporization of the raw material, and obtain a product different from the raw material by treating the raw material containing metal atoms with plasma, Next, a description will be given.
  • FIG. 4 shows a process for obtaining a product different from a raw material by treating a raw material containing metal atoms with plasma, which can cope with a case where a high temperature is required for vaporization of the raw material with the simple configuration of the third embodiment according to the present invention.
  • FIG. 3 is a diagram for explaining the device 1.
  • the manufacturing apparatus 1 shown in FIG. 4 has many parts in common with the manufacturing apparatus 1 shown in FIG. 2 described above, mainly different parts will be described, and description of similar parts will be omitted. There is.
  • the manufacturing apparatus 1 of the third embodiment includes at least a cathode portion 55 having a surface 55 ⁇ / b> A exposed to the first space F in the reaction chamber 2 and at least the first space F in the reaction chamber 2.
  • the anode part 56 is a plate that can withstand high temperatures, functions as an electrode, and is formed of a material (for example, tungsten) that can generate heat as will be described later.
  • the described reflector 70 can be used so as to be formed of a conductive material such as SUS (stainless steel).
  • the voltage application means 57 applies a voltage between the anode portion 56 and the cathode portion 55 so that the anode portion 56 functions as an anode and the cathode portion 55 functions as a cathode.
  • the raw material containing a metal atom is arrange
  • the anode portion 56 needs to be exposed so that electrons can collide.
  • the back surface opposite to the surface 56A on which the raw material of the anode portion 56 is arranged is exposed.
  • the raw material is disposed on the surface 56A so that a part of the anode portion 56 is exposed and can collide with electrons.
  • means for feeding the raw material onto the anode portion 56 may be provided in accordance with the reduction of the raw material.
  • positive ions for example, positive hydrogen ions
  • the positive ions are attracted and receive electrons, so that the balance between electrons and positive ions is maintained.
  • the anode portion 56 has a surface area size, thickness, etc. that generate heat to a temperature necessary for vaporizing the raw material.
  • the cathode portion 55 does not need to generate heat, and preferably has a sufficiently large surface area with which positive ions can contact so as to efficiently maintain a balance between electrons and positive ions.
  • the reflector 70 is used for the cathode part 55.
  • the reflector 70 is omitted and the inner surface of the housing 10 exposed to the first space F of the reaction chamber 2 becomes the cathode part 55. May be.
  • the plate that becomes the anode portion 56 is arranged in the first space F of the reaction chamber 2, but the anode portion 56 is partly in the first space of the reaction chamber 2. Even if it is not located in F, the surface 56 ⁇ / b> A on which the raw material is disposed only needs to be exposed in the first space F of the reaction chamber 2.
  • the raw material or product adheres to the window W, and plasma may not be generated or may not be generated. Therefore, a reactive gas is blown toward the window W.
  • the suppression means which suppresses adhesion to the surface of the window W of a raw material and a product.
  • a pure quartz window W or the like can withstand temperatures exceeding 1500 ° C., so the window W is formed of pure quartz and a reactive gas is blown onto the window W.
  • the temperature of the window W may be a suppressing means that makes the temperature at which the raw materials and products do not adhere.
  • the reactive gas may be a gas other than a rare gas that does not contain an oxygen atom, such as methane or fluoride gas.
  • the reactive gas which does not substantially contain oxygen atoms does not contain oxygen gas.
  • a reactive gas may be mixed.
  • attachment means 80 which is arrange
  • a cooling means In order to keep it within a predetermined temperature range, it is cooled by a cooling means.
  • the adhering means 80 often has a temperature higher than a predetermined temperature range, and therefore, the means for keeping the predetermined temperature range is considered to be a cooling means.
  • the attaching means 80 may be at a temperature lower than a predetermined temperature range.
  • the surface temperature of the surface to which the product of the attaching means 80 is attached is a predetermined temperature range.
  • a heating means is provided. Therefore, the manufacturing apparatus 1 includes temperature control means for keeping the surface temperature of the surface on which the product of the attaching means 80 is attached within a predetermined temperature range suitable for precipitation of the product.

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Abstract

Le but de la présente invention est de fournir : une méthode sans dioxyde de carbone pour produire de l'hydrure de magnésium avec une bonne efficacité de production ; un système de génération d'énergie sans dioxyde de carbone ou sans rayonnement utilisant de l'hydrure de magnésium ; et un appareil pour produire de l'hydrure de magnésium. A cet effet, cette méthode de production d'hydrure de magnésium comprend : une étape d'irradiation d'un composé de magnésium, qui n'est pas un hydrure de magnésium, avec un plasma d'hydrogène ; et une étape de dépôt d'un produit de magnésium contenant de l'hydrure de magnésium sur un moyen de dépôt (80) qui est destiné à déposer de l'hydrure de magnésium et est disposé dans une plage dans laquelle le plasma d'hydrogène est présent, la température de surface du moyen de dépôt (80) étant maintenue à une température inférieure ou égale à une température prédéterminée à laquelle l'hydrure de magnésium est précipité.
PCT/JP2018/015418 2017-06-02 2018-04-12 Méthode de production d'hydrure de magnésium, système de production d'énergie utilisant de l'hydrure de magnésium, et appareil de production d'hydrure de magnésium WO2018221036A1 (fr)

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KR1020197035694A KR102111622B1 (ko) 2017-06-02 2018-04-12 수소화 마그네슘 등의 제조 방법, 수소화 마그네슘을 이용한 발전 방법 및 수소화 마그네슘 등의 제조 장치
MYPI2020002269A MY176543A (en) 2017-06-02 2018-04-12 Method for producing magnesium hydride,power generation system using magnesium hydride, and apparatus for producing magnesium hydride
EP18810561.3A EP3632842A4 (fr) 2017-06-02 2018-04-12 Méthode de production d'hydrure de magnésium, système de production d'énergie utilisant de l'hydrure de magnésium, et appareil de production d'hydrure de magnésium
US16/617,436 US11643704B2 (en) 2017-06-02 2018-04-12 Producing method for producing magnesium hydride, power generation system using magnesium hydride, and producing apparatus for producing magnesium hydride
MA47828A MA47828B1 (fr) 2017-06-02 2018-04-12 Méthode de production d'hydrure de magnésium, système de production d'énergie utilisant de l'hydrure de magnésium, et appareil de production d'hydrure de magnésium

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