Method for producing beryllium solution, method for producing beryllium, method for producing beryllium hydroxide, method for producing beryllium oxide, apparatus for producing solution, system for producing beryllium, and beryllium

Abstract

To provide a novel method for producing a beryllium solution, which has high energy efficiency.SOLUTION: A method (M10) for producing a beryllium liquid includes a main-heating step (S12) for producing the beryllium liquid by using beryllium and a material containing the beryllium as starting materials and dielectrically heating an acid liquid containing the starting materials.SELECTED DRAWING: Figure 1

Description

[Technical Field]

[0001] The present invention relates to a method for producing a beryllium solution. The present invention also relates to a method for producing beryllium, a method for producing beryllium hydroxide, a method for producing beryllium oxide, an apparatus for producing a solution, a system for producing beryllium, and beryllium. [Background technology]

[0002] Beryllium is known to be contained in Be-Si-O ores and Be-Si-Al-O ores. Examples of Be-Si-O ores include bertrandite and phenacite, and examples of Be-Si-Al-O ores include beryl and chrysoberyl. Hereinafter, ores containing beryllium such as these will be referred to as beryllium ores. Beryllium ores are an example of beryllium oxides.

[0003] When producing beryllium, a compound containing beryllium, or an alloy containing beryllium, beryllium is extracted from beryllium ore by dissolving the ore in a solvent. However, dissolving beryllium ore in a solvent is not easy. Acidic solutions such as sulfuric acid are known as solvents that easily dissolve beryllium ore, but beryllium ore is difficult to dissolve even in acidic solutions.

[0004] Therefore, Non-Patent Document 1 describes that beryllium ore can be dissolved in a solvent by subjecting the ore to a pretreatment such as a sintering treatment or a melting treatment. [Prior art documents] [Non-patent literature]

[0005] [Non-Patent Document 1] "Beryllium", [online], Wikipedia, [Retrieved June 25, 2019], Internet〈URL:https: / / en.wikipedia.org / siki / Beryllium〉 Summary of the Invention [Problem to be solved by the invention]

[0006] However, the pretreatment of dissolving beryllium ore in a solvent requires a large amount of energy. According to the "Production" section of Non-Patent Document 1, the temperature for sintering is, for example, 770°C, and the temperature for melting is, for example, 1650°C.

[0007] One aspect of the present invention has been made in view of the above-mentioned problems, and its object is to provide a novel method for producing a beryllium solution that is highly energy efficient. [Means for solving the problem]

[0008] A method for producing a beryllium solution according to one embodiment of the present invention includes a main heating step of producing a beryllium solution by dielectrically heating an acidic solution containing starting materials selected from the group consisting of beryllium, an intermetallic compound containing beryllium, beryllium having an oxide layer formed on its surface, and an intermetallic compound containing beryllium having an oxide layer formed on its surface.

[0009] A method for producing beryllium according to one aspect of the present invention includes the steps included in the method for producing a beryllium solution according to one aspect of the present invention, as well as a dehydration step for producing a beryllium salt by dehydrating the beryllium solution, and an electrolysis step for producing beryllium by molten salt electrolysis of the beryllium salt.

[0010] A method for producing beryllium hydroxide according to one embodiment of the present invention includes the steps included in the method for producing a beryllium solution according to one embodiment of the present invention, and a neutralization step of producing beryllium hydroxide by neutralizing the beryllium solution with a base.

[0011] A method for producing beryllium oxide according to one embodiment of the present invention includes the steps included in the method for producing a beryllium solution according to one embodiment of the present invention, and a third heating step of heating the beryllium solution to produce beryllium oxide.

[0012] A solution manufacturing apparatus according to one embodiment of the present invention comprises a main heating container, an acidic solution supply unit that supplies an acidic solution to the main heating container, and a main heating device that dielectrically heats the acidic solution contained in the main heating container.

[0013] A beryllium production system according to one embodiment of the present invention includes a solution production apparatus according to one embodiment of the present invention, a dehydration device that produces beryllium chloride by dehydrating the beryllium chloride solution, and an electrolysis device that produces beryllium by molten salt electrolysis of the beryllium chloride.

[0014] Beryllium according to one embodiment of the present invention has a uranium concentration of less than 0.7 ppm. [Effects of the Invention]

[0015] According to one aspect of the present invention, a novel method for producing a beryllium solution can be provided that is highly energy efficient. [Brief explanation of the drawings]

[0016] [Figure 1] 1 is a flowchart showing a method for producing a beryllium chloride solution according to a first embodiment of the present invention. [Figure 2]1(a) to 1(c) are flowcharts showing methods for producing beryllium, a method for producing beryllium hydroxide, and a method for producing beryllium oxide according to second to fourth embodiments of the present invention, respectively. [Figure 3] 10 is a flowchart showing a method for separating titanium and lithium according to a fifth embodiment of the present invention. [Figure 4] 10 is a flowchart showing a method for producing a lithium chloride solution according to a sixth embodiment of the present invention. [Figure 5] FIG. 10 is a schematic view of an apparatus for producing a beryllium solution according to a seventh embodiment of the present invention. [Figure 6] 6 is a graph showing the temperature change of the container when a main heating step is carried out using the beryllium solution manufacturing apparatus shown in FIG. 5. [Figure 7] FIG. 13 is a schematic view of a beryllium solution manufacturing device provided in a beryllium manufacturing system according to an eighth embodiment of the present invention. [Figure 8] (a) is a schematic diagram of a crystallizer, a dehydration device, and an electrolysis device provided in a beryllium production system according to an eighth embodiment of the present invention. (b) is a schematic diagram of a modified crystallization treatment tank provided in the crystallizer shown in (a). (c) is a schematic diagram of a modified dryer provided in the dehydration device shown in (a). [Figure 9] 10(a) shows a flowchart of a method for producing lithium hydroxide according to a ninth embodiment of the present invention, and FIG. 10(b) shows a flowchart of a method for producing lithium carbonate according to a tenth embodiment of the present invention. DETAILED DESCRIPTION OF THE INVENTION

[0017] [First embodiment] (Beryllium solution manufacturing method M10) A method M10 for producing a beryllium solution according to a first embodiment of the present invention will be described with reference to FIG. 1. FIG. 1 is a flowchart of the method M10 for producing a beryllium solution. Hereinafter, the method M10 for producing a beryllium solution will also be referred to simply as the method M10. In this embodiment, a method for producing a BeCl solution, which is an aqueous solution of beryllium chloride (BeCl), which is the hydrochloride salt of beryllium, will be described. However, the beryllium solution produced using the method M10 is not limited to a BeCl solution. It may be a BeSO solution, which is an aqueous solution of beryllium sulfate (BeSO), which is the sulfate salt of beryllium; a Be(NO) solution, which is an aqueous solution of beryllium nitrate (Be(NO)), which is the nitrate salt of beryllium; a BeF solution, which is an aqueous solution of beryllium fluoride (BeF), which is the hydrofluoride salt of beryllium; a BeBr solution, which is an aqueous solution of beryllium bromide (BeBr), which is the hydrobromide salt of beryllium; or a BeI solution, which is an aqueous solution of beryllium iodide (BeI), which is the hydroiodide salt of beryllium.

[0018] As shown in FIG. 1, the manufacturing method M10 includes a removal step S11, a main heating step S12, a first filtration step S13, a sodium hydroxide addition step S14, a second filtration step S15, a hydrochloric acid addition step S16, a first impurity removal step S17, and a second impurity removal step S18.

[0019] (Removal step S11) The removal step S11 is a step of removing spent tritium breeder materials and neutron multiplier materials, which are filled inside the blanket of a fusion reactor, from the blanket. In the manufacturing method M10, the spent tritium breeder materials and neutron multiplier materials are used as starting materials.

[0020] Examples of tritium breeding materials include lithium oxides. Specifically, lithium titanate (Li2TiO3), lithium oxide (Li2O), lithium aluminate (LiAlO2), and lithium silicate (Li2SiO3 and / or Li4SiO4) are listed. Examples of neutron multiplier materials include beryllium (Be) and beryllium-containing intermetallic compounds (Be 12 Ti and / or Be 12 Examples of the tritium breeder material include tritium breeder material (also called tritium V or beryllium) and neutron multiplier material (also called beryllium V or beryllide). Each of the tritium breeder material and the neutron multiplier material is formed into a minute sphere having a diameter of about 1 mm. The interior of the blanket is then filled with tritium breeder material and neutron multiplier material that are mixed as uniformly as possible. Therefore, the starting material removed from the blanket in the removal step S11 is a mixture of tritium breeder material and neutron multiplier material. In this embodiment, manufacturing method M10 will be described using lithium titanate as an example of the tritium breeder material and beryllium with an oxide layer formed on its surface as an example of the neutron multiplier material. Note that the tritium breeder material and the neutron multiplier material used as starting materials in manufacturing method M10 are not limited to lithium titanate and beryllium, and can be appropriately selected from the examples described above.

[0021] Even when beryllium is used as a neutron multiplier, the majority of it (for example, about 98%) remains as beryllium. Therefore, in order to reduce the operating costs of fusion reactors, there is a strong demand for the establishment of technology to convert beryllium, an expensive element, into a beryllium solution and reuse it. In addition, a layer of beryllium oxide (BeO) forms on the surface of used beryllium. Therefore, simply immersing used beryllium in an acidic solution will hardly dissolve the beryllium contained in the used beryllium.

[0022] As described above, the starting material used in manufacturing method M10 functions as a neutron multiplier and includes at least one of (1) beryllium, (2) an intermetallic compound containing beryllium, (3) beryllium having an oxide layer formed on its surface, and (4) an intermetallic compound having an oxide layer formed on its surface and containing beryllium. The starting material used in manufacturing method M10 may further include lithium oxide, which functions as a tritium breeding material.

[0023] Furthermore, the starting materials used in Manufacturing Method M10 are not limited to spent neutron multipliers and tritium breeders from fusion reactors. The starting materials may also be spent beryllium and its alloys from nuclear energy and accelerator fields other than fusion, or beryllium and its alloys generated as industrial waste in general industry. Manufacturing Method M10 can process (1) spent neutron multipliers and tritium breeders generated in fusion reactors, (2) spent beryllium and its alloys contained in neutron reflectors, neutron moderators, and target materials as neutron sources generated in nuclear energy and accelerator fields other than fusion, and (3) beryllium and its alloys generated as industrial waste in general industry without distinguishing between them to produce new beryllium. Manufacturing Method M10 also allows for the removal of uranium and other elements contained as impurities in these starting materials.

[0024] (Crushing process) Furthermore, a pulverization step of pulverizing the starting material may be carried out between the removal step S11 and the main heating step S12. The pulverization step is a step in which the particle size of the starting material is reduced by pulverizing the starting material, and even if an oxide layer is formed on the surface of the neutron multiplier material, the oxide layer is mechanically destroyed to expose the beryllium that was covered by the oxide layer. The technique used to pulverize the starting material is not limited and can be appropriately selected from existing techniques, and examples thereof include a ball mill.

[0025] (Main heating process S12) The main heating step S12 is a step of dielectrically heating an acidic solution containing the starting materials after the unloading step S11. By carrying out the main heating step S12, the beryllium, which is a neutron multiplier, is dissolved, and an acidic solution is produced in which most of the lithium contained in the lithium titanate, which is a tritium breeder, is dissolved. Hereinafter, this acidic solution will also be referred to as a lithium-containing beryllium solution. Note that even when the main heating step S12 is carried out, some of the lithium titanate and titanium oxide do not dissolve and remain as a solid phase in the acidic solution.

[0026] The acidic solution is not particularly limited, but may be an aqueous solution of any of the acidic solutes hydrogen chloride (HCl), sulfuric acid (H2SO4), nitric acid (HNO3), hydrogen fluoride (HF), hydrogen bromide (HBr), and hydrogen iodide (HI). In this embodiment, an HCl solution is used as the acidic solution. The concentration of HCl in the HCl solution can be adjusted as appropriate, but it is preferable that the pH be adjusted to 1 or less.

[0027] Dielectric heating is a general term for a technique for heating an object by applying electromagnetic waves of a predetermined frequency to the object. Depending on the frequency band of the applied electromagnetic waves, it is also called high-frequency heating or microwave heating. For example, high-frequency heating applies electromagnetic waves in the frequency band of 3 MHz or more but less than 300 MHz (so-called short waves or ultra-short waves) to the object, while microwave heating applies electromagnetic waves in the frequency band of 300 MHz or more but less than 30 GHz (so-called microwaves) to the object. Microwave ovens, which are widely used in homes, are an example of a device capable of microwave heating.

[0028] In this embodiment, in the main heating step S12, electromagnetic waves having a frequency of 2.45 GHz are applied to the beryllium solution containing lithium. The configuration of an apparatus for applying electromagnetic waves to the beryllium solution containing lithium will be described later with reference to FIG. 5 or FIG. 7.

[0029] By using dielectric heating to heat an acidic solution containing starting materials, the starting materials can be dissolved in the acidic solution with higher energy efficiency than conventional methods. Specifically, a hydrochloric acid solution containing beryllium chloride hydrate (BeCl2·xH2O) and lithium chloride (LiCl) can be obtained. Therefore, manufacturing method M10 can provide a new, highly energy-efficient manufacturing method.

[0030] The heating temperature in the main heating step S12 can be set as appropriate. However, the heating temperature in the main heating step S12 is preferably equal to or lower than the heat-resistant temperature of a container (e.g., the main heating container 14 described in the seventh embodiment) that accommodates the acidic solution containing the starting materials. For example, if the container is made of polytetrafluoroethylene, like the main heating container 14, the heating temperature in the main heating step S12 is preferably equal to or lower than 250°C. If the material constituting the container is corrosion-resistant to the acidic solution and has a heat-resistant temperature exceeding 250°C, the heating temperature in the main heating step S12 may exceed 250°C. Increasing the heating temperature in the main heating step S12 is likely to shorten the time required for the main heating step S12. Furthermore, the heating temperature in the main heating step S12 is preferably equal to or higher than 180°C. A heating temperature of 180°C or higher allows much of the beryllium and lithium contained in the starting materials to be dissolved in the solution as beryllium chloride hydrate and lithium chloride. The heating time in the main heating step S12 can also be set appropriately, but is preferably, for example, 60 minutes or more.

[0031] (Preheating process) If the rate at which beryllium dissolves in the acidic solution is slow when the main heating step S12 is performed alone, in other words, if the solubility of beryllium is not sufficient when the main heating step S12 is performed at a predetermined heating temperature for a predetermined heating time, the manufacturing method M10 may include a pre-heating step performed prior to the main heating step S12.

[0032] Among the above-mentioned examples of neutron multiplier materials, in the case of beryllium having an oxide layer formed on its surface and in the case of an intermetallic compound having an oxide layer formed on its surface and containing beryllium, if the oxide layer is thick, the rate at which the beryllium dissolves in the acidic solution may be slowed down by simply performing the main heating step S12. In such cases, it is preferable to perform a pre-heating step before the main heating step S12.

[0033] The preheating step is a step of dielectrically heating a basic solution containing starting materials. The basic solution is not particularly limited, but may be an aqueous solution of sodium hydroxide (NaOH) or potassium hydroxide (KOH), which are basic solutes. In this embodiment, an NaOH solution is used as the basic solution. The concentration of NaOH in the NaOH solution can be adjusted as appropriate, but it is preferable that the pH be adjusted to 14 or higher.

[0034] The dielectric heating performed in the preheating step is the same as the dielectric heating performed in the main heating step S12. That is, in this embodiment, an electromagnetic wave with a frequency of 2.45 GHz is applied to the NaOH solution containing the starting material.

[0035] By carrying out the pre-heating step before carrying out the main heating step S12, a plurality of reaction portions are formed on the surface of the starting material by corrosion, dissolution, collapse, etc. of the surface structure. The shape of the reaction zone is not limited, but may be, for example, a recess. Thus, the surface of the starting material on which the multiple reaction zones are formed becomes more fragile than the surface of the starting material before the pre-heating step. As a result, the starting material after the pre-heating step is easily dissolved in the acidic solution by performing the main heating step S12. Thus, by including the pre-heating step in manufacturing method M10, starting materials that are difficult to dissolve by performing the main heating step S12 alone can be easily dissolved. Therefore, even when starting materials that are relatively difficult to dissolve in acidic solutions are used, a lithium-containing beryllium solution can be produced by performing the pre-heating step and the main heating step S12.

[0036] (First filtration step S13) The first filtration step S13 is a step carried out after the main heating step S12. The first filtration step S13 is a step of separating a solid phase and a liquid phase contained in the lithium-containing beryllium solution using a filter. The solid phase contains some lithium titanate and titanium oxide. The liquid phase, which is an acidic solution, mainly contains beryllium chloride hydrate and lithium chloride.

[0037] By carrying out the first filtration step S13, it is possible to easily separate the titanium oxide contained in the solid phase from the beryllium chloride hydrate and lithium chloride contained in the liquid phase.

[0038] (Sodium hydroxide addition step S14) The sodium hydroxide addition step S14 is a step carried out after the first filtration step S13. The sodium hydroxide addition step S14 is a step of adjusting the polarity of the acidic solution separated in the first filtration step S13, which contains beryllium chloride hydrate and lithium chloride in a liquid phase but does not contain titanium oxide in a solid phase, from acidic to basic via neutral.

[0039] In this embodiment, the sodium hydroxide addition step S14 is defined as adding an aqueous solution of sodium hydroxide to the acidic solution separated in the first filtration step S13. As a result, the polarity of the solution separated in the first filtration step S13 changes from acidic to neutral (pH 7) and then to basic, and the beryllium chloride hydrate contained in the solution becomes beryllium hydroxide (Be(OH)2) and precipitates as a solid phase in the basic solution. Note that lithium chloride is dissolved in the basic solution and does not precipitate. That is, lithium chloride remains present in the liquid phase as lithium hydroxide even after the sodium hydroxide addition step S14 is performed.

[0040] (Second filtration step S15) The second filtration step S15 is a step carried out after the sodium hydroxide addition step S14. The second filtration step S15 is a step of separating, using a filter, the solid phase and the liquid phase contained in the basic solution obtained in the sodium hydroxide addition step S14. The solid phase contains beryllium hydroxide, and the liquid phase contains lithium hydroxide.

[0041] By carrying out the second filtration step S15, it is possible to easily separate the beryllium hydroxide contained in the solid phase from the lithium hydroxide contained in the liquid phase.

[0042] (Hydrochloric acid addition step S16) The hydrochloric acid addition step S16 is a step carried out after the second filtration step S15. In the hydrochloric acid addition step S16, an HCl solution is added to the beryllium hydroxide obtained in the second filtration step S15, thereby dissolving the beryllium again in the form of beryllium chloride hydrate in the acidic solution. The concentration of HCl in the HCl solution can be adjusted as appropriate, but it is preferably adjusted so that the pH is 1 or less.

[0043] By carrying out the hydrochloric acid adding step S16, a hydrochloric acid solution (also referred to as a beryllium solution or a BeCl2 solution) in which beryllium chloride hydrate is dissolved can be obtained.

[0044] (First impurity removal step S17) The first impurity removal step S17 is a step carried out after the hydrochloric acid addition step S16. The first impurity removal step S17 is a step of removing the first element from the beryllium solution obtained in the hydrochloric acid addition step S16 using an organic compound that adsorbs the first element.

[0045] The first element to be removed in the first impurity removal step S17 is determined by the organic compound used. Examples of organic compounds that can be used in the first impurity removal step S17 include tri-n-octylphosphine oxide (TOPO), di-(2-ethylhexyl) phosphoric acid (DEHPA), tri-n-butyl phosphate (TBP), and ethylenediaminetetraacetic acid (EDTA). A commercially available organic compound that can be used in the first impurity removal step S17 is UTEVA® resin from Eichrom Technologies.

[0046] TOPO is Al, Au, Co, Cr, Fe, Hf, Re, Ti, UO2 2+ , V, Zr, rare earth elements, and actinide elements. D2EHPA can adsorb U, Co, Ni, Mn, etc. TBP can adsorb U, Th, etc. EDTA and the like can adsorb Mg, Ca, Ba, Cu, Zn, Al, Mn, Fe, etc. UTEVA® Resin can adsorb U, Th, Pu, Am, etc. These elements are examples of the first element.

[0047] These organic compounds dissolve in organic solvents (e.g., kerosene, cyclohexane, benzene, etc.). By mixing the solution in which these organic compounds are dissolved (hereinafter also referred to as organic compound solution) with the HCl solution obtained after the hydrochloric acid addition step S16 has been performed and stirring the mixture, the organic compounds adsorb the first element.

[0048] In the first impurity removal step S17, the HCl solution mixed with the organic compound solution is preferably acidic, and more preferably has a pH of 2 or less. This configuration increases the efficiency with which the organic compound adsorbs the first element without adsorbing beryllium. Note that the closer the HCl solution is to neutral, the higher the efficiency with which the organic compound adsorbs beryllium and the lower the efficiency with which the organic compound adsorbs the first element.

[0049] In this embodiment, TOPO and kerosene are used as the organic compound and organic solvent used in the first impurity removal step S17. However, the organic compound and organic solvent are not limited to TOPO and kerosene, and can be appropriately selected from the combinations exemplified above.

[0050] The aqueous beryllium solution and the organic compound solution obtained in the hydrochloric acid addition step S16 are separated into two layers by leaving them for a while. Therefore, the beryllium solution in which the content of the first element has been reduced by performing the first impurity removal step S17 can be easily separated from the organic compound solution containing the first element.

[0051] By performing the first impurity removal step S17, the concentration of the first element contained in the beryllium solution can be reduced. As a result, when a beryllium solution is produced by dissolving a starting material in an acidic solution, even if the starting material contains a first element other than beryllium as described above, the concentration of the first element contained when producing beryllium, beryllium hydroxide, or beryllium oxide from the beryllium solution can be reduced. Examples of the first element include uranium, thorium, plutonium, and americium.

[0052] As a specific example, when beryllium is produced using beryllium chloride produced using the production method M10 including the first impurity removal step S17, the uranium concentration in the beryllium can be suppressed to less than 0.7 ppm. Even when beryllium with a uranium concentration of less than 0.7 ppm is used as a neutron multiplier in a fusion reactor, the uranium concentration after use falls below the threshold value that determines whether shallow disposal is possible. Therefore, beryllium included in one embodiment of the present invention can be directly disposed of at shallow land even when used as a neutron multiplier in a fusion reactor.

[0053] (Second impurity removal step S18) The second impurity removal step S18 is a step performed after the first impurity removal step S17, and is a step of removing a second element from the beryllium solution by adjusting the polarity of the beryllium solution obtained in the hydrochloric acid addition step S16 from acidic to neutral and then to basic. Note that, in this embodiment, the first impurity removal step S17 and the second impurity removal step S18 are described as being performed in this order after the hydrochloric acid addition step S16, but the order of the first impurity removal step S17 and the second impurity removal step S18 can be reversed.

[0054] In this embodiment, the second impurity removal step S18 involves adding sodium bicarbonate (NaHCO3) to the beryllium solution after the hydrochloric acid addition step S16 has been performed until the solution is saturated. As a result, after the beryllium solution reaches neutrality (pH 7), elements other than beryllium (e.g., Al, Fe, etc.) become hydroxides (e.g., Al(OH)3, Fe(OH)3, etc.) and precipitate in the beryllium solution. Note that even when the sodium bicarbonate solution is saturated, Be(OH)2 remains dissolved in the beryllium solution and does not precipitate. Thus, aluminum (Al) and iron (Fe) are examples of the second element.

[0055] The hydroxides of elements other than beryllium that have precipitated in the beryllium solution by carrying out the second impurity removal step S18 can be easily removed from the beryllium solution by filtering the beryllium solution.

[0056] It is preferable to add HCl to the beryllium solution from which the second element has been removed by performing the second impurity removal step S18. By adding HCl to the beryllium solution in this manner, the polarity of the Be(OH)2 solution is adjusted from neutral to acidic, and highly pure beryllium chloride hydrate (BeCl2·xH2O) is produced in the solution.

[0057] In this way, by performing the second impurity removal step S18, the concentration of the second element contained in the beryllium solution can be reduced. As a result, when a beryllium solution is produced by dissolving a starting material in an acidic solution, even if the starting material contains a second element other than beryllium as described above, the concentration of the second element contained when beryllium, beryllium hydroxide, or beryllium oxide is produced using the beryllium solution can be reduced.

[0058] As described above, in manufacturing method M10, the main heating step S12 preferably involves dielectrically heating the acidic solution containing beryllium oxide by applying microwaves.

[0059] Furthermore, when manufacturing method M10 includes a preheating step, the preheating step preferably involves dielectrically heating the basic solution containing beryllium oxide by applying microwaves, similar to main heating step S12.

[0060] The technology of dielectric heating using microwaves (i.e., microwave dielectric heating) is a technology used in so-called microwave ovens and is widely used. Therefore, manufacturing method M10 can reduce the cost required for implementation compared to conventional manufacturing methods.

[0061] As mentioned above, in manufacturing method M10, the beryllium solution is preferably a beryllium chloride solution.

[0062] According to the manufacturing method M10, a beryllium chloride solution can be easily produced without going through beryllium hydroxide. As will be described later, beryllium, beryllium hydroxide, and beryllium oxide can be easily produced from the beryllium chloride solution. Therefore, a beryllium chloride solution is preferable as the beryllium solution.

[0063] [Second to Fourth Embodiments] A method M20 for producing beryllium (Be), a method M30 for producing beryllium hydroxide (Be(OH)2), and a method M40 for producing beryllium oxide (BeO) according to second to fourth embodiments of the present invention will be described with reference to (a) to (c) of FIG. 2. (a) to (c) of FIG. 2 are flowcharts showing the main parts of the method M20 for producing beryllium, the method M30 for producing beryllium hydroxide, and the method M40 for producing beryllium oxide, respectively. Note that hereinafter, the method M20 for producing beryllium, the method M30 for producing beryllium hydroxide, and the method M40 for producing beryllium oxide will also be simply referred to as the method M20, the method M30, and the method M40, respectively.

[0064] (Beryllium manufacturing method M20) As shown in Fig. 2, manufacturing method M20 includes the steps of removing S11, main heating S12, first filtration S13, sodium hydroxide adding S14, second filtration S15, first impurity removing S17, and second impurity removing S18 included in manufacturing method M10 shown in Fig. 1, as well as a dehydration step S21 and an electrolysis step S22. Hereinafter, the removing S11, main heating S12, first filtration S13, sodium hydroxide adding S14, second filtration S15, first impurity removing S17, and second impurity removing S18 will also be simply referred to as each step S11 to S18.

[0065] The steps S11 to S18 of the manufacturing method M10 included in the manufacturing method M20 are the same as the steps S11 to S18 described in the first embodiment. Therefore, the description of the steps S11 to S18 will be omitted here. That is, assuming that a BeCl2 solution in which BeCl2 is dissolved in an HCl solution has been obtained, only the dehydration step S21 and the electrolysis step S22 of the manufacturing method M20 will be described.

[0066] The dehydration step S21 is a step of producing BeCl2, an example of a beryllium salt, by dehydrating beryllium chloride hydrate (BeCl2·xH2O) contained in the BeCl2 solution obtained in each of steps S11 to S15 of manufacturing method M10.

[0067] In the dehydration step S21, ammonium chloride is added to the beryllium chloride hydrate, and the beryllium chloride hydrate is heated in a vacuum at 90°C for 24 hours, thereby reducing the water content as close to zero as possible. In other words, the beryllium chloride hydrate can be dehydrated.

[0068] Ammonium chloride reacts with the water in the beryllium chloride hydrate to form ammonium hydroxide and hydrochloric acid. The resulting ammonium hydroxide and hydrochloric acid then react again to return to ammonium chloride, releasing water. In this process, anhydrous beryllium chloride can be obtained from the beryllium chloride hydrate.

[0069] The heating temperature in the dehydration step S21 is not limited to 90°C, but can be appropriately selected from the temperature range of 80°C to 110°C. However, if the heating temperature is too high, the dehydration of the beryllium chloride hydrate tends to be insufficient. Therefore, the heating temperature is preferably 80°C to 90°C, and more preferably 90°C.

[0070] The time period for carrying out the dehydration treatment in the dehydration step S21 is not limited to 24 hours, but can be determined as appropriate.

[0071] The electrolysis step S22 is a step of producing metallic beryllium by subjecting the BeCl2 obtained in the dehydration step S21 to molten salt electrolysis.

[0072] As described above, by carrying out manufacturing method M20, metallic beryllium can be produced from the starting material.

[0073] (Beryllium hydroxide manufacturing method M30) 2, production method M30 includes steps S11 to S15 of production method M10 and a neutralization step S31. As in production method M20, only the neutralization step S31 will be described here.

[0074] The neutralization step S31 is a step in which BeCl2·xH2O contained in the BeCl2 solution obtained in each of steps S11 to S15 of the production method M10 is neutralized with a base to produce Be(OH)2.

[0075] As described above, by carrying out production method M30, Be(OH)2 can be produced from the starting material.

[0076] (Beryllium oxide manufacturing method M40) 2, manufacturing method M40 includes steps S11 to S15 of manufacturing method M10 and a heating step S41. As in manufacturing method M20, only the heating step S41 will be described here.

[0077] Heating step S41 is a third heating step in which BeO is produced by heating the BeCl2 solution obtained by steps S11 to S15 of manufacturing method M10. In this step, BeCl2·xH2O dissolved in the BeCl2 solution is hydrolyzed to produce BeO.

[0078] As described above, by carrying out production method M40, BeO can be produced from starting materials.

[0079] (Small summary) According to these manufacturing methods M20, M30, and M40, beryllium, beryllium hydroxide, and beryllium oxide can be produced using novel, highly energy-efficient manufacturing methods. Note that the dehydration step S21, electrolysis step S22, neutralization step S31, and heating step S41 can all be carried out using existing technologies.

[0080] Fifth Embodiment (Titanium and lithium separation method M50) A titanium and lithium separation method M50 according to a fifth embodiment of the present invention will be described with reference to Fig. 3. Fig. 3 is a flowchart of the titanium and lithium separation method M50. Note that, hereinafter, the titanium and lithium separation method M50 will also be simply referred to as the separation method M50.

[0081] As shown in Fig. 3, separation method M50 includes the removal step S11, main heating step S12, and first filtration step S13 included in production method M10 shown in Fig. 1, as well as a crushing step S51, a hydrochloric acid soaking step S52, and a third filtration step S53. Hereinafter, the removal step S11, main heating step S12, and first filtration step S13 will also be simply referred to as each of steps S11 to S13.

[0082] Steps S11 to S13 of manufacturing method M10, which are included in separation method M50, are the same as steps S11 to S13 described in the first embodiment. Therefore, a description of steps S11 to S13 will be omitted here. That is, assuming that lithium titanate contained in the solid phase and beryllium chloride hydrate and lithium chloride contained in the liquid phase are separated, only the pulverization step S51, the hydrochloric acid immersion step S52, and the third filtration step S53 of separation method M50 will be described. Note that the solid phase obtained after step S13 may contain titanium oxide in addition to lithium titanate.

[0083] The pulverization step S51 is a step of reducing the particle size of the lithium titanate by pulverizing the lithium titanate contained in the solid phase after the first filtration step S13. The technique used to pulverize the lithium titanate is not limited and can be appropriately selected from existing techniques, such as a ball mill.

[0084] If lithium titanate can be pulverized more finely, the ratio of the surface area to the total volume of the lithium titanate can be increased, which is expected to shorten the time required to dissolve the lithium contained in the lithium titanate in the solution in the hydrochloric acid immersion step S52 described below. On the other hand, if lithium titanate is pulverized too finely, the time and cost required for the pulverization step S51 will increase. Therefore, it is preferable to determine the particle size of the lithium titanate obtained after performing the pulverization step S51 in consideration of the time required for the hydrochloric acid immersion step S52, the time required for the pulverization step S51, the cost required for the pulverization step S51, etc.

[0085] The particle size of lithium titanate may be any of the average size, mode size, and median size. When the particle size distribution of lithium titanate is measured, the average size is the particle size that is the average value of the obtained particle size distribution, the mode size is the most frequent particle size in the particle size distribution, and the median size is the particle size where the cumulative frequency in the particle size distribution is 50%.

[0086] In this embodiment, the pulverization step S51 is carried out so that the average particle size of the lithium titanate becomes 100 μm.

[0087] The hydrochloric acid immersion step S52 is a step carried out after the pulverization step S51. The hydrochloric acid immersion step S52 is a step of immersing the lithium titanate pulverized in the pulverization step S51 in a hydrochloric acid solution. By carrying out the hydrochloric acid immersion step S52, the lithium contained in the lithium titanate dissolves in the hydrochloric acid solution in the form of lithium chloride, and the titanium contained in the lithium titanate remains in the hydrochloric acid solution in the form of titanium oxide (e.g., TiO2). Therefore, the hydrochloric acid solution after carrying out the hydrochloric acid immersion step S52 contains titanium oxide contained in a solid phase and lithium chloride contained in a liquid phase.

[0088] If it is desired to dissolve the lithium contained in the lithium titanate in the hydrochloric acid solution more quickly, the hydrochloric acid solution containing the lithium titanate may be dielectrically heated by applying a method similar to that in the main heating step S12.

[0089] The third filtration step S53 is a step carried out after the hydrochloric acid immersion step S52. The third filtration step S53 is a step of separating titanium oxide contained in the solid phase from lithium chloride contained in the liquid phase using a filter.

[0090] By carrying out the third filtration step S53, it is possible to easily separate the titanium oxide contained in the solid phase from the lithium chloride contained in the liquid phase.

[0091] The acidic solution containing lithium chloride separated in the third filtration step S53 is preferably returned to the sodium hydroxide addition step S14, similar to the acidic solution separated in the first filtration step S13. By separating the lithium contained in the solid phase separated in the first filtration step S13 as lithium chloride and returning it to the sodium hydroxide addition step S14, the lithium compound can be recovered more efficiently. In other words, the crushing step S51, the hydrochloric acid soaking step S52, and the third filtration step S53 of the separation method M50 can be included as part of the production method M10.

[0092] As described above, by carrying out separation method M50, titanium and lithium contained in lithium titanate can be separated into titanium oxide and lithium chloride, respectively. Therefore, lithium, which is a valuable resource, can be recovered and reused together with titanium.

[0093] Sixth Embodiment (Lithium solution manufacturing method M60) A lithium solution manufacturing method M60 according to a sixth embodiment of the present invention will be described with reference to FIG. 4. FIG. 4 is a flowchart of the lithium solution manufacturing method M60. Note that, hereinafter, the lithium solution manufacturing method M60 will also be simply referred to as manufacturing method M60. In this embodiment, a method for manufacturing a LiCl solution, which is an aqueous solution of lithium chloride (LiCl), which is the hydrochloride salt of lithium, will be described. However, the lithium solution manufactured using manufacturing method M60 is not limited to a LiCl solution, and may be a Li2SO4 solution, which is an aqueous solution of lithium sulfate (Li2SO4), which is the sulfate salt of lithium, a LiNO3 solution, which is an aqueous solution of lithium nitrate (LiNO3), which is the nitrate salt of lithium, lithium fluoride (LiF), which is the hydrofluoride salt of lithium, lithium bromide (LiBr), which is the hydrobromide salt of lithium, or lithium iodide (LiI), which is the hydroiodide salt of lithium.

[0094] As shown in FIG. 4, the manufacturing method M60 includes a crushing step S61, a preheating step S62, a main heating step S63, a first impurity removal step S64, and a second impurity removal step S65. In the manufacturing method M60, lithium ore is used as a starting material for producing the lithium solution. Lithium ore is a general term for ores containing lithium, and is also an example of lithium oxide. Lithium ore has crystallinity. Examples of lithium ores include lepidolite (K(Al,Li)2(Si,Al)4O 10 (OH,F)2), Petalite (LiAlSi4O 10), and Elbaite (Na(Li,Al)3Al6(BO3)3Si6O 18 (OH)4). In this embodiment, a manufacturing method M60 will be described using lepidolite as an example of a starting material.

[0095] The pulverization step S61 is a step in which lumps of lepidolite are pulverized into granules. The technique used to pulverize lepidolite is not limited and can be appropriately selected from existing techniques, such as a hammer or a ball mill. Furthermore, a combination of techniques (e.g., a hammer and a ball mill) may be used to pulverize lepidolite. In this case, a hammer may be used in the first stage of the pulverization step S61, and a ball mill may be used in the second stage.

[0096] If spodumene can be pulverized more finely, the ratio of the surface area to the total volume of the spodumene can be increased, which is expected to shorten the time required to dissolve the lithium contained in the spodumene in the solution in the pre-heating step S62 and the main heating step S63 described below. On the other hand, if spodumene is pulverized too finely, the time and cost required for the pulverization step S61 will increase. Therefore, it is preferable to determine the particle size of the spodumene obtained after the pulverization step S61 in consideration of the time required for the pre-heating step S62 and the main heating step S63, the time required for the pulverization step S61, the cost required for the pulverization step S61, and the like.

[0097] The particle size of lepidolite may be any of the average size, mode size, and median size. When the particle size distribution of lepidolite is measured, the average size is the particle size that is the average value of the obtained particle size distribution, the mode size is the most frequent particle size in the particle size distribution, and the median size is the particle size where the cumulative frequency in the particle size distribution is 50%.

[0098] In this embodiment, the pulverization step S61 is carried out so that the average particle size of the lepidolite becomes 100 μm.

[0099] (Preheating step S62) The preheating step S62 is a step performed before the main heating step S63 described below, and is a step of dielectrically heating a basic solution containing lepidolite. The basic solution is not particularly limited, but may be an aqueous solution of sodium hydroxide (NaOH) or potassium hydroxide (KOH), which are basic solutes. In this embodiment, an NaOH solution is used as the basic solution. The concentration of NaOH in the NaOH solution can be adjusted as appropriate, but it is preferably adjusted so that the pH is 14 or higher.

[0100] Dielectric heating is a general term for a technique for heating an object by applying electromagnetic waves of a predetermined frequency to the object. Depending on the frequency band of the applied electromagnetic waves, it is also called high-frequency heating or microwave heating. For example, high-frequency heating applies electromagnetic waves in the frequency band of 3 MHz or more but less than 300 MHz (so-called short waves or ultra-short waves) to the object, while microwave heating applies electromagnetic waves in the frequency band of 300 MHz or more but less than 30 GHz (so-called microwaves) to the object. Microwave ovens, which are widely used in homes, are an example of a device capable of microwave heating.

[0101] In this embodiment, in the preheating step S62, electromagnetic waves having a frequency of 2.45 GHz are applied to the NaOH solution containing lepidolite. The configuration of an apparatus for applying electromagnetic waves to the NaOH solution containing lepidolite will be described later with reference to FIGS. 5 and 7.

[0102] By performing the preheating step S62 before performing the main heating step S63, multiple reaction sites are formed on the surface of the spodumene mica due to corrosion, dissolution, collapse, or the like of surface structures. The shape of these reaction sites is not limited, and may be, for example, recesses. The surface of the spodumene mica on which multiple reaction sites have been formed is weakened compared to the surface of the spodumene mica before performing the main heating step S63. As a result, the spodumene mica after performing the preheating step S62 dissolves in an acidic solution when the main heating step S63 described below is performed. In this way, by including the preheating step S62 in the manufacturing method M60, it is possible to dissolve lithium ores that are difficult to dissolve by performing the main heating step S63 alone. Therefore, by including the preheating step S62 in the manufacturing method M60, it is possible to produce a lithium chloride solution using not only lithium ores that are relatively soluble in acidic solutions, but also lithium ores that are difficult to dissolve in acidic solutions as starting materials.

[0103] Whether or not to omit the preheating step S62 in the manufacturing method M60 can be determined appropriately depending on the ease with which the lithium ore serving as the starting material dissolves in the acidic solution.

[0104] (Main heating process S63) The main heating step S63 is a step that follows the pre-heating step S62 and involves dielectrically heating an acidic solution containing lepidolite to produce a lithium solution, which is an acidic solution in which lithium is dissolved.

[0105] The acidic solution is not particularly limited, but may be an aqueous solution of any of the acidic solutes hydrogen chloride (HCl), sulfuric acid (H2SO4), nitric acid (HNO3), hydrogen fluoride (HF), hydrogen bromide (HBr), and hydrogen iodide (HI). In this embodiment, an HCl solution is used as the acidic solution. The concentration of HCl in the HCl solution can be adjusted as appropriate, but it is preferable that the pH be adjusted to 1 or less.

[0106] By adding an appropriate amount of HCl solution to the NaOH solution after the preheating step S62, the basic solution containing lithium becomes neutral and then an acidic solution containing lithium.

[0107] The dielectric heating performed in the main heating step S63 is the same as the dielectric heating performed in the preheating step S62. That is, in this embodiment, an electromagnetic wave with a frequency of 2.45 GHz is applied to the HCl solution containing lithium ore.

[0108] By using dielectric heating to heat an acidic solution containing lithium oxide, it is possible to dissolve lithium oxide in the acidic solution with higher energy efficiency than conventional methods. Specifically, a hydrochloric acid solution containing dissolved lithium chloride (LiCl) can be obtained. Therefore, manufacturing method M60 can provide a new manufacturing method with high energy efficiency.

[0109] The heating temperature in the main heating step S63 can be set appropriately, similar to the heating temperature in the main heating step S12. That is, when the container (for example, the main heating container 14 described in the seventh embodiment) that contains the acidic solution containing lithium oxide is made of polytetrafluoroethylene, the heating temperature in the main heating step S63 is preferably 250°C or less. Furthermore, the heating temperature in the main heating step S63 is preferably 180°C or more. Furthermore, the heating time in the main heating step S63 can also be set appropriately, but is preferably, for example, 60 minutes or more.

[0110] (First impurity removal step S64) The first impurity removal step S64 is a step performed after the main heating step S63. The first impurity removal step S64 is a step of removing the first element from the LiCl solution obtained in the main heating step S63 using an organic compound that adsorbs the first element.

[0111] The first element to be removed in the first impurity removal step S64 is determined by the organic compound used. Examples of organic compounds that can be used in the first impurity removal step S64 include tri-n-octylphosphine oxide (TOPO), di-(2-ethylhexyl) phosphoric acid (DEHPA), tri-n-butyl phosphate (TBP), and ethylenediaminetetraacetic acid (EDTA). Another commercially available organic compound that can be used in the first impurity removal step S64 is UTEVA® resin from Eichrom Technologies®.

[0112] TOPO is Al, Au, Co, Cr, Fe, Hf, Re, Ti, UO2 2+ , V, Zr, rare earth elements, and actinide elements. D2EHPA can adsorb U, Co, Ni, Mn, etc. TBP can adsorb U, Th, etc. EDTA and the like can adsorb Mg, Ca, Ba, Cu, Zn, Al, Mn, Fe, etc. UTEVA® Resin can adsorb U, Th, Pu, Am, etc. These elements are examples of the first element.

[0113] These organic compounds are dissolved in an organic solvent (e.g., kerosene). The solution in which these organic compounds are dissolved (hereinafter also referred to as an organic compound solution) is mixed with the HCl solution obtained after the main heating step S63 and stirred, whereby the organic compounds adsorb the first element.

[0114] The aqueous LiCl solution and the organic compound solution obtained in the main heating step S63 are separated into two layers by leaving them for a while. Therefore, the LiCl solution in which the content of the first element has been reduced by performing the first impurity removal step S64 can be easily separated from the organic compound solution containing the first element.

[0115] By performing the first impurity removal step S64, the concentration of the first element contained in the lithium solution can be reduced. As a result, when producing a lithium solution by dissolving lithium ore in an acidic solution, even if the lithium ore contains a first element other than lithium as described above, the concentration of the first element contained when producing any of lithium, lithium hydroxide, lithium oxide, and lithium carbonate from the lithium solution can be reduced. Examples of the first element include uranium, thorium, plutonium, and americium.

[0116] (Second impurity removal step S65) The second impurity removal step S65 is a step performed after the main heating step S63, and further includes a step of removing a second element from the LiCl solution by adjusting the polarity of the LiCl solution obtained by the main heating step S63 from acidic, via neutral, to basic. Note that, in the present embodiment, the first impurity removal step S64 and the second impurity removal step S65 are described as being performed in this order after the main heating step S63, but the order of the first impurity removal step S64 and the second impurity removal step S65 can be reversed.

[0117] In this embodiment, the second impurity removal step S65 involves adding a basic compound or a basic aqueous solution in which a basic compound is dissolved to the lithium solution (HCl solution containing lithium) after the main heating step S63 has been performed. An example of the basic compound is sodium bicarbonate (NaHCO), and an example of the basic aqueous solution is a sodium hydroxide (NaOH) aqueous solution. In this embodiment, a sodium hydroxide aqueous solution is used as the basic aqueous solution.

[0118] By carrying out the second impurity removal step S65, the polarity of the lithium solution changes from acidic to neutral (pH 7) and then to basic. Elements other than lithium (e.g., Al, Fe, etc.) contained in the lithium solution become hydroxides (e.g., Al(OH)3, Fe(OH)3, etc.) and precipitate in the lithium solution. Even if an excess of sodium hydroxide is added or the solution is saturated with sodium bicarbonate, LiOH remains dissolved in the lithium solution and does not precipitate. Thus, aluminum (Al) and iron (Fe) are examples of second elements.

[0119] The hydroxides of elements other than lithium that have precipitated in the lithium solution by carrying out the second impurity removal step S65 can be easily removed from the lithium solution by filtering the lithium solution.

[0120] It is preferable to add HCl again to the lithium solution from which the second element has been removed by performing the second impurity removal step S65. By adding HCl again to the lithium solution in this manner, the polarity of the LiOH solution is adjusted from neutral to acidic, and highly pure lithium chloride (LiCl) is produced in the solution.

[0121] In this way, by performing the second impurity removal step S65, the concentration of the second element contained in the lithium solution can be reduced. As a result, when a lithium solution is produced by dissolving lithium ore in an acidic solution, even if the lithium ore contains the second element other than lithium as described above, the concentration of the second element contained when lithium, lithium hydroxide, lithium oxide, or lithium carbonate is produced using the lithium solution can be reduced.

[0122] As described above, in manufacturing method M60, it is preferable that the preliminary heating step S62 dielectrically heats the basic solution containing lithium oxide by applying microwaves, and the main heating step S63 dielectrically heats the acidic solution containing lithium oxide by applying microwaves.

[0123] The technology of dielectric heating using microwaves (i.e., microwave dielectric heating) is a technology used in so-called microwave ovens and is widely used. Therefore, manufacturing method M60 can reduce the cost required for implementation compared to conventional manufacturing methods.

[0124] As mentioned above, in manufacturing method M60, the lithium solution is preferably a lithium chloride solution.

[0125] According to Production Method M60, a lithium chloride solution can be easily produced. As will be described later, lithium, lithium hydroxide, lithium oxide, and lithium carbonate can be easily produced from the lithium chloride solution. Therefore, a lithium chloride solution is preferable as the lithium solution.

[0126] (Variations of starting materials) In this embodiment, the lithium solution manufacturing method M60 has been described using lithium ore (more specifically, lepidolite) as the starting material. However, the starting material in manufacturing method M60 is not limited to lithium ore, and may be beryllium ore, or ore or mud containing one or more types of metals.

[0127] Beryllium ores are ores containing beryllium and are known to be classified into Be-Si-O ores and Be-Si-Al-O ores. Examples of Be-Si-O ores include bertrandite and phenacite, and examples of Be-Si-Al-O ores include beryl and chrysoberyl. In the case of Be-Si-O ores, beryllium can be easily dissolved in an acidic solution by omitting the preheating step S62 and simply performing the main heating step S63. On the other hand, in the case of Be-Si-Al-O ores, beryllium can be easily dissolved in an acidic solution by performing both the preheating step S62 and the main heating step S63.

[0128] Ores containing one or more types of metals are also called polymetallic nodules, and known examples include seafloor hydrothermal deposits, cobalt-rich crusts, and manganese nodules.

[0129] Seafloor hydrothermal deposits contain base metals such as copper, lead, and zinc, as well as precious metals such as gold and silver, and rare metals. Cobalt-rich crusts contain rare metals such as nickel, cobalt, and platinum. Manganese nodules contain base metals such as copper, and rare metals such as nickel and cobalt.

[0130] Furthermore, as mud containing one or more types of metals, rare earth mud containing rare earth elements is known.

[0131] By carrying out production method M60 using these starting materials, it is possible to produce a solution in which each metal is dissolved from starting materials containing various metals.

[0132] Seventh Embodiment A dielectric heating device 10 according to a seventh embodiment of the present invention will be described with reference to Fig. 5. The dielectric heating device 10 is an example of an apparatus for producing a beryllium solution according to one aspect of the present invention. Fig. 5 is a schematic diagram of the dielectric heating device 10. The dielectric heating device 10 is a heating device that performs each of the main heating step S12 included in the production method M10 shown in Fig. 1, the main heating step S12 included in the separation method M50 shown in Fig. 3, the preheating step S62 included in the production method M60 shown in Fig. 4, and the main heating step S63 included in the production method M60 shown in Fig. 4.

[0133] As explained in the first embodiment, dielectric heating is classified as either high-frequency heating or microwave heating depending on the frequency band of the applied electromagnetic waves. The dielectric heating device 10 is a device that performs microwave heating, out of high-frequency heating and microwave heating, on an object.

[0134] As shown in Fig. 5, the dielectric heating device 10 includes a microwave oscillator 11, a waveguide 12, a microwave applicator 13, a main heating vessel 14, a rotary table 15, a stirrer 16, and a thermometer 17. The dielectric heating device 10 also includes a control unit not shown in Fig. 5.

[0135] The microwave oscillator 11 is configured to oscillate electromagnetic waves having a predetermined frequency. The predetermined frequency can be selected appropriately within the microwave band, for example, but in this embodiment, the predetermined frequency is set to 2.45 GHz. The frequency of 2.45 GHz is the same frequency as the electromagnetic waves used in home microwave ovens.

[0136] Waveguide 12 is a cylindrical member made of metal, one end of which is connected to microwave oscillator 11 and the other end of which is connected to microwave application unit 13. Waveguide 12 guides the electromagnetic waves generated by microwave oscillator 11 from one end to the other end, and radiates the electromagnetic waves from the other end into the internal space of microwave application unit 13.

[0137] The microwave application unit 13 is a metal box-shaped member with a hollow interior space, and is configured so that the interior space can accommodate the main heating vessel 14. The microwave application unit 13 applies electromagnetic waves irradiated from the other end of the waveguide 12 to the main heating vessel 14 and the object to be heated accommodated in the main heating vessel 14. The microwave application unit 13 is configured to confine the electromagnetic waves within the interior space and prevent them from leaking to the outside.

[0138] Although not shown in Fig. 5, the main heating container 14 is a container made up of a main body and a lid. The main body is made up of a cylindrical side wall and a bottom that seals one end of the side wall. The main heating container 14 is configured so that the internal space formed by the main body and the lid can be sealed by joining the main body and the lid.

[0139] The main heating vessel 14 is preferably made of a material that has high transmittance to the electromagnetic waves (2.45 GHz in this embodiment) oscillated by the microwave oscillator 11. In this embodiment, the main heating vessel 14 is made of a fluorine-based resin such as polytetrafluoroethylene.

[0140] Furthermore, it is preferable that the main heating vessel 14 has pressure resistance that can withstand even when the pressure in the internal space becomes higher than atmospheric pressure. By being able to seal the internal space and having pressure resistance that can withstand a predetermined pressure, the main heating vessel 14 can keep the object to be heated contained in the internal space even when electromagnetic waves are applied and the temperature of the object to be heated contained in the internal space rises.

[0141] The turntable 15 is a sample stage provided on the bottom surface of the internal space of the microwave application unit 13, and is configured so that the main heating container 14 can be placed on its upper surface. The turntable 15 is circular in plan view and is configured to rotate at a predetermined speed around its central axis. With this configuration, the main heating container 14 placed on the upper surface of the turntable 15 rotates periodically, allowing the target object to be heated more uniformly.

[0142] The stirrer 16 is a metallic vane-shaped member provided on the ceiling surface of the internal space of the microwave application unit 13. It is fixed in a freely rotatable state relative to the ceiling surface by a support rod connected to the center of the vane-shaped member. The stirrer 16 rotates at a predetermined speed around the support rod as the rotation axis, thereby reflecting the electromagnetic waves generated by the microwave oscillator 11 and scattering them in the internal space of the microwave application unit 13. With this configuration, the stirrer 16 scatters the electromagnetic waves, allowing the target object to be heated more uniformly.

[0143] The thermometer 17 is a radiation thermometer that measures the temperature of the main heating container 14 by detecting infrared rays emitted by the main heating container 14. The temperature of the main heating container 14 becomes approximately the same as the temperature of the object contained in the internal space of the main heating container 14 after a predetermined temperature relaxation time has elapsed. This temperature relaxation time depends on the material (fluororesin in this embodiment) constituting the main heating container 14 and its thickness (e.g., 1 mm). For a main heating container 14 made of fluororesin and 1 mm thick, as in this embodiment, the temperature relaxation time is expected to be approximately 3 minutes. Therefore, if the heating time is sufficiently long compared to the temperature relaxation time and / or if the temperature change of the object contained in the internal space of the main heating container 14 is sufficiently gradual, the temperature of the object contained in the internal space of the main heating container 14 and the temperature of the main heating container 14 can be considered to be the same. Therefore, in such cases, the thermometer 17 can be considered to be capable of measuring the temperature of the object. The thermometer 17 outputs a temperature signal indicating the measured temperature of the main heating vessel 14 or the object to the control unit.

[0144] The control unit may control the output of microwave oscillator 11 so that the output becomes a predetermined value, or may control the output of microwave oscillator 11 so that the temperature of the temperature signal received from thermometer 17 becomes a predetermined temperature. Note that this predetermined temperature may be constant over time, or may change over time. In this embodiment, the control unit controls the output of microwave oscillator 11 so that the output value changes over time. An example of the output value that changes over time is a pattern in which the output is changed from 0 W to 600 W over 30 minutes, and then maintained at 600 W for 60 minutes.

[0145] Taking manufacturing method M10 as an example, the dielectric heating device 10 configured in this manner can be used to carry out the main heating step S12 by storing the starting material removed from the blanket in the starting material removal step S11 and an acidic solution in the internal space of the main heating vessel 14.

[0146] Taking manufacturing method M60 as an example, the dielectric heating device 10 configured as described above can be used to carry out the preheating step S62 by storing the lepidolite pulverized in the crushing step S61 and a basic solution in the internal space of the main heating vessel 14. Similarly, the dielectric heating device 10 can be used to carry out the main heating step S63 by storing the lepidolite after the preheating step S62 and an acidic solution in the internal space of the main heating vessel 14.

[0147] 6 is a graph showing the temperature change of the container in an example of the above-mentioned main heating step S12. In this example, the output value of the dielectric heating device 10 was changed over time. Specifically, the output value was increased from 0 W to 600 W over 30 minutes, then maintained at 600 W for 60 minutes, and then the output value was quickly reduced to 0 W.

[0148] When the output value of the microwave oscillator 11 was changed according to the above-described pattern, as shown in FIG. 6, the temperature of the main heating vessel 14 continued to rise even after the output value reached 600 W, and the maximum temperature reached was approximately 220°C.

[0149] Eighth Embodiment (Beryllium production system) A beryllium production system 20 according to an eighth embodiment of the present invention will be described with reference to FIGS. 7 and 8. FIG. 7 is a schematic diagram of a beryllium solution (BeCl solution) production apparatus 20A constituting part of the beryllium production system 20. FIG. 8(a) is a schematic diagram of a crystallization apparatus 20B, a dehydration apparatus 20C, and an electrolysis apparatus 20D. FIG. 8(b) is a schematic diagram of a modified crystallization treatment tank 31 provided in the crystallization apparatus 20B shown in FIG. 8(a). FIG. 8(c) is a schematic diagram of a modified dryer 33 provided in the dehydration apparatus 20C shown in FIG. 8(a). Each of the crystallization apparatus 20B, the dehydration apparatus 20C, and the electrolysis apparatus 20D constitutes part of the beryllium production system 20. Note that, hereinafter, the beryllium production system 20 will also be simply referred to as the production system 20, and the beryllium solution production apparatus 20A will also be simply referred to as the production apparatus 20A.

[0150] 7 and 8, the production system 20 includes a production apparatus 20A, a crystallizer 20B, a dehydration apparatus 20C, and an electrolysis apparatus 20D, and is an apparatus for carrying out the production method M20 shown in Fig. 2. More specifically, the production apparatus 20A is an apparatus for carrying out each step of the production method M10 shown in Fig. 1 except for the removal step S11, the crystallizer 20B and the dehydration apparatus 20C are apparatus for carrying out the dehydration step S21 shown in Fig. 2, and the electrolysis apparatus 20D is an apparatus for carrying out the electrolysis step S22 shown in Fig. 2.

[0151] In this embodiment, as in the first embodiment, lithium titanate (Li2TiO3), an example of a tritium breeder, and beryllium (Be), an example of a neutron multiplier, with an oxide layer of beryllium oxide (BeO) formed on the surface are used as starting materials. However, the starting materials in the manufacturing apparatus 20A are not limited to those exemplified in the first embodiment. The starting material in the manufacturing apparatus 20A may be, for example, beryllium ore. Beryllium ore is a general term for ores containing beryllium. Known beryllium ores include Be-Si-O ores and Be-Si-Al-O ores. Examples of Be-Si-O ores include bertrandite and phenacite, and examples of Be-Si-Al-O ores include beryl and chrysoberyl.

[0152] <Beryllium solution manufacturing equipment 20A> 7, the manufacturing apparatus 20A includes a pulverizer 21, a feeder F1, valves V1 to V15, a dielectric heating device 22, filters 23 and 29, containers 24, 26, 27, 28, and 30, and a centrifuge 25. The manufacturing apparatus 20A also includes a control unit not shown in FIG. 7. The control unit controls each of the feeder F1, the valves V1 to V15, and the dielectric heating device 22.

[0153] The pulverizer 21 pulverizes the input starting materials, lithium titanate and beryllium with an oxide layer formed on their surfaces, and supplies them to the feeder F1. The pulverizer 21 can be appropriately selected from existing pulverizers according to the desired specifications. Therefore, a detailed description of the pulverizer 21 is omitted here. By pulverizing the starting materials using the pulverizer 21, even if an oxide layer has formed on the surface of beryllium, an example of a neutron multiplier material, the oxide layer can be mechanically destroyed, exposing the beryllium that was covered by the oxide layer. This increases the rate at which beryllium dissolves in the HCl solution in the main heating step S12. Note that the pulverizer 21 can be omitted if the oxide layer formed on the surface of the beryllium is thin and easily dissolved by the dielectric heating device 22 (described later).

[0154] The feeder F1 is controlled by the control unit and supplies the starting material supplied from the pulverizer 21 to a main heating vessel 22c of the dielectric heating device 22, which will be described later. The feeder F1 is an example of a raw material supply unit that supplies the starting material to the main heating vessel 22c.

[0155] The dielectric heating device 22 includes a microwave oscillator 22a, a waveguide 22b, a main heating vessel 22c, a stirring mechanism, and a thermometer. The dielectric heating device 22 performs the main heating step S12 of the manufacturing method M10 shown in FIG.

[0156] The microwave oscillator 22a, which is an example of a main heating device, is controlled by the controller and configured to oscillate electromagnetic waves having a predetermined frequency. The predetermined frequency can be selected appropriately within the microwave band, for example, but in this embodiment, the predetermined frequency is set to 2.45 GHz. The frequency of 2.45 GHz is the same frequency as the electromagnetic waves used in home microwave ovens.

[0157] Waveguide 22b is a cylindrical metal member, one end of which is connected to microwave oscillator 22a and the other end of which is connected to main heating vessel 22c. Waveguide 22b guides the electromagnetic waves generated by microwave oscillator 22a from one end to the other end, and radiates the electromagnetic waves from the other end into the internal space of main heating vessel 22c.

[0158] The main heating vessel 22c is an acid-resistant box-shaped member with a hollow, sealed interior. The starting materials are supplied from the mill 21 via a feeder F1 to the main heating vessel 22c, and an HCl solution is supplied via a valve V1. The mechanism that supplies the HCl solution to the main heating vessel 22c via the valve V1 functions as an acid solution supply unit that supplies the acid solution to the starting materials. The starting materials and the HCl solution supplied to the main heating vessel 22c are mixed in the interior space of the main heating vessel 22c.

[0159] The main heating vessel 22c preferably has a pressure resistance that can withstand high pressures even when the pressure in the internal space becomes higher than atmospheric pressure due to a rise in temperature of the HCl solution containing the starting materials contained in the internal space caused by dielectric heating. By being able to seal the internal space and having a pressure resistance that can withstand a predetermined pressure, the main heating vessel 22c can keep the object to be heated contained in the internal space even when electromagnetic waves are applied and the temperature of the object to be heated contained in the internal space rises.

[0160] The stirring mechanism, not shown in FIG. 7, stirs the starting materials and the HCl solution so that the starting materials are dispersed as uniformly as possible in the HCl solution in the internal space of the main heating vessel 22c.

[0161] A thermometer (not shown in FIG. 7) detects the temperature of the HCl solution containing the starting materials contained in the internal space of the main heating vessel 22c and outputs a temperature signal representing that temperature to the control unit. The thermometer may be a non-contact thermometer such as a radiation thermometer, or a contact thermometer such as a thermocouple. Regardless of the type of thermometer used, it is preferable that the thermometer be provided in the internal space of the main heating vessel 22c and configured to be able to directly detect the temperature of the HCl solution containing the starting materials.

[0162] The control unit may control the output of microwave oscillator 22a so that the output reaches a predetermined value, or may control the output of microwave oscillator 22a so that the temperature indicated by the temperature signal received from the thermometer reaches a predetermined temperature. This predetermined temperature may be constant over time, or may vary over time. In this embodiment, the control unit controls the output of microwave oscillator 22a so that the temperature indicated by the temperature signal varies over time according to a predetermined profile. An example of the predetermined temperature profile is a pattern in which the temperature is changed from room temperature to 250°C over 30 minutes, and then maintained at 250°C for 60 minutes.

[0163] The dielectric heating device 22 configured in this manner performs the main heating step S12 of the manufacturing method M10 shown in FIG. 1 to produce a beryllium solution (BeCl solution) containing titanium oxide in a solid phase and lithium in a liquid phase.

[0164] In this embodiment, the preheating step that can be performed between the removal step S11 and the main heating step S12 of manufacturing method M10 is omitted. Therefore, manufacturing apparatus 20A is equipped only with dielectric heating device 22 that performs the main heating step S12, and does not have a dielectric heating device that performs the preheating step. When the preheating step is performed in manufacturing method M10, a dielectric heating device that is configured similarly to dielectric heating device 22 and performs the preheating step may be further disposed between feeder F1 and dielectric heating device 22.

[0165] The dielectric heating device that performs the preheating step may include a preheating container, a basic solution supply unit (a valve corresponding to valve V1) that supplies a basic solution (e.g., an NaOH solution) to the preheating container, a raw material supply unit that supplies starting materials to at least one of the preheating container and the basic solution supply unit (in this embodiment, the preheating container), a preheating device that dielectrically heats the basic solution contained in the preheating container, and a discharge unit that discharges the basic solution containing the starting materials from the preheating container to the main heating container.

[0166] Whether or not the manufacturing apparatus 20A is provided with a dielectric heating device for performing the preheating step can be determined appropriately depending on the ease of dissolution of the starting materials in an acidic solution. For example, in the case of beryllium ore, phenacite and bertrandite are easily soluble in an acidic solution, while beryl and chrysoberyl are difficult to dissolve in an acidic solution. Therefore, when phenacite and bertrandite are used as the starting materials, the dielectric heating device for performing the preheating step may be omitted from the manufacturing apparatus 20A. On the other hand, when beryl and chrysoberyl are used as the starting materials, it is preferable that the manufacturing apparatus 20A be provided with a dielectric heating device for performing the preheating step.

[0167] Valve V2 opens and closes a path between the internal space of the main heating vessel 22c and a filter 23 (described later). The control unit closes valve V2 while the main heating step S12 is being performed, and opens valve V2 after the main heating step S12 is completed. As a result, the beryllium solution containing lithium obtained in the main heating step S12 is supplied from the main heating vessel 22c to the filter 23.

[0168] The filter 23 is configured to pass the liquid phase (i.e., the BeCl2 solution containing LiCl) of the lithium-containing beryllium solution and filter out the solid phase (i.e., titanium oxide). That is, the filter 23 performs the first filtration step S13 of the manufacturing method M10. The filter 23 can be appropriately selected from existing filters according to the desired specifications. Therefore, a detailed description of the filter 23 will be omitted here.

[0169] Valve V3 opens and closes a path between filter 23 and container 24, which will be described later. The control unit opens valve V3 at least during the period in which the lithium-containing beryllium solution is being supplied to filter 23. As a result, the LiCl-containing BeCl solution obtained in the first filtration step S13 is supplied from filter 23 to container 24.

[0170] Container 24 is a box-shaped member with a hollow interior that is acid-resistant and base-resistant. Each of containers 26, 27, 28, and 30, the configuration of which will be described later, is an acid-resistant box-shaped member. NaOH solution is supplied to container 24 via valve V4. The mechanism that supplies NaOH solution to the beryllium solution in container 24 via valve V4 functions as a NaOH solution supply unit that supplies NaOH solution to the beryllium solution.

[0171] The BeCl2 solution containing LiCl and the NaOH solution supplied to the container 24 are mixed in the internal space of the container 24. That is, the sodium hydroxide adding step S14 of the manufacturing method M10 is carried out in the internal space of the container 24. As a result, solid beryllium hydroxide (Be(OH)2) is produced inside the container 24, and liquid LiOH dissolves in the NaOH solution.

[0172] 7, a stirring mechanism for stirring the BeCl2 solution containing LiCl and the NaOH solution may be provided in the internal space of the container 24. Similarly, stirring mechanisms may be provided in the internal spaces of the containers 26, 27, 28, and 30 described below.

[0173] Valve V5 opens and closes a path between the internal space of container 24 and centrifuge 25, which will be described later. The control unit closes valve V5 while sodium hydroxide addition step S14 is being performed, and opens valve V5 after sodium hydroxide addition step S14 is completed. As a result, the NaOH solution containing Be(OH)2 and LiOH obtained in sodium hydroxide addition step S14 is supplied from container 24 to centrifuge 25.

[0174] The centrifuge 25 separates the NaOH solution containing Be(OH)2 and LiOH into a liquid phase (i.e., the NaOH solution containing LiOH) and a solid phase (i.e., Be(OH)2). That is, the centrifuge 25 performs the second filtration step S15 of the manufacturing method M10. The centrifuge 25 can be appropriately selected from existing centrifuges according to the desired specifications. Therefore, a detailed description of the centrifuge 25 will be omitted here. The Be(OH)2 obtained in the second filtration step S15 is introduced into the internal space of a container 26 described below, and the NaOH aqueous solution containing LiOH obtained in the second filtration step S15 is recovered in a recovery line (not shown).

[0175] Also, a filter such as filter 23 may be used instead of centrifuge 25 to separate the liquid phase and the solid phase in the NaOH solution containing Be(OH)2 and LiOH.

[0176] An HCl solution is supplied to the container 26 via a valve V6. The Be(OH)2 and HCl solution supplied to the container 26 are mixed in the internal space of the container 26. That is, the hydrochloric acid adding step S16 of the manufacturing method M10 is carried out in the internal space of the container 26. As a result, a beryllium solution (BeCl2 solution) is produced inside the container 26, in which the produced BeCl2 is dissolved in the HCl solution.

[0177] Valve V7 opens and closes the path between the internal space of container 26 and the internal space of container 27, which will be described later. The control unit closes valve V7 while hydrochloric acid addition step S16 is being performed, and opens valve V7 after hydrochloric acid addition step S16 is completed. As a result, the beryllium solution obtained in hydrochloric acid addition step S16 is supplied from container 26 to container 27.

[0178] An organic compound solution is supplied to the container 27 via a valve V8. The mechanism for supplying the organic compound solution to the container 27 via the valve V8 functions as an organic compound solution supply unit that supplies the organic compound solution to the beryllium chloride solution. This organic compound solution is the organic compound solution described in the first impurity removal step S17 of the manufacturing method M10. Therefore, a description of the organic compound solution will be omitted here.

[0179] The beryllium solution and the organic compound solution supplied to the container 27 are mixed in the internal space of the container 27. That is, the first impurity removal step S17 is carried out in the internal space of the container 27. As a result, the beryllium solution in which the content of the first element is suppressed and the organic compound solution containing the first element are separated into two layers inside the container 27. Because the specific gravity of the beryllium solution exceeds the specific gravity of the organic compound solution, the beryllium solution is located below the organic compound solution.

[0180] Valve V9 opens and closes the path between the internal space of container 27 and a recovery line (not shown). Valve V10 opens and closes the path between the internal space of container 27 and the internal space of container 28 (described later).

[0181] The control unit keeps both valves V9 and V10 closed while the first impurity removal step S17 is being performed. After the first impurity removal step S17 is performed, the control unit first opens only valve V10. As a result, the beryllium solution with a reduced content of the first element obtained by the first impurity removal step S17 is supplied from container 27 to container 28. Thereafter, the control unit closes valve V10 and opens valve V9. As a result, the organic compound solution containing the first element obtained by the first impurity removal step S17 is recovered in the recovery line.

[0182] Sodium bicarbonate is supplied to the container 28 via a valve V11. The mechanism for supplying sodium bicarbonate to the container 28 via the valve V11 functions as a sodium bicarbonate supply unit that supplies sodium bicarbonate to the beryllium chloride solution. This sodium bicarbonate is the same as that described in the second impurity removal step S18 of the manufacturing method M10. Therefore, a description of the sodium bicarbonate will be omitted here.

[0183] The beryllium solution and sodium bicarbonate supplied to the container 28 are mixed in the internal space of the container 28. That is, the second impurity removal step S18 is carried out in the internal space of the container 28. As a result, the hydroxide of the second element precipitates inside the container 28, and the content of the second element in the beryllium hydroxide (Be(OH)2) solution is suppressed.

[0184] Valve V12 opens and closes a path between the internal space of container 28 and a filter, which will be described later. The control unit closes valve V12 while the second impurity removal step S18 is being performed, and opens valve V12 after the second impurity removal step S18 is completed. As a result, the beryllium hydroxide solution obtained in the second impurity removal step S18, which contains the hydroxide of the second element, is supplied from container 28 to filter 29.

[0185] Filter 29 is configured to pass the liquid phase (i.e., the beryllium hydroxide solution) of the beryllium hydroxide solution containing the hydroxide of the second element and to filter the solid phase (i.e., the hydroxide of the second element). Filter 29 can be appropriately selected from existing filters according to the desired specifications. Therefore, a detailed description of filter 29 will be omitted here.

[0186] Valve V13 opens and closes the path between filter 29 and container 30, which will be described later. The control unit opens valve V13 at least during the period in which the beryllium hydroxide solution containing the hydroxide of the second element is being supplied to filter 29. As a result, the beryllium hydroxide solution obtained in the second impurity removal step S18, in which the content of the second element is reduced, is supplied from filter 29 to container 30.

[0187] A beryllium hydroxide solution is supplied to the container 30 via a valve V13, and an HCl solution is supplied via a valve V14. The Be(OH)2 solution and the HCl solution supplied to the container 30 are mixed in the internal space of the container 30. As a result, a beryllium solution (BeCl2 solution) is produced inside the container 30, in which the produced BeCl2 is dissolved in the HCl solution.

[0188] Valve V15 opens and closes the path between the container 30 and a crystallization treatment tank 31 of a crystallizer 20B, which will be described later. The control unit closes valve V15 at least while the HCl solution is being supplied to the container 30, and opens valve V15 after the Be(OH)2 solution and the HCl solution supplied to the container 30 are sufficiently mixed. As a result, the beryllium solution (BeCl2 solution) is supplied from the container 30 to the crystallization treatment tank 31.

[0189] <Crystallizer 20B> As shown in Fig. 8, the crystallizer 20B includes a crystallization treatment tank 31, a chiller C, a pump P, a condensate tank, and valves V16 and V17. The crystallizer 20B also includes a control unit not shown in Fig. 8. The control unit controls each of the crystallization treatment tank 31, the chiller C, the pump P, and the valves V16 and V17.

[0190] The crystallization treatment tank 31 comprises an inner tank and an outer tank. Warm water is supplied to the inner space of the outer tank via a valve V16. A beryllium solution (BeCl solution) produced by the manufacturing apparatus 20A is supplied to the inner space of the inner tank. The above-mentioned warm water heats the beryllium solution and HCl solution contained in the inner tank. The use of warm water is an example of a heating means employing an external heating method.

[0191] The chiller C, condensate tank, and pump P make up the reduced pressure dehydration system. The pump P evacuates the internal space of the inner tank. The chiller C cools the gas exhausted from the internal space of the inner tank. The condensate tank stores the condensate that has been liquefied by being cooled by the chiller C.

[0192] The crystallizer 20B configured in this manner is capable of crystallizing beryllium chloride. The crystallized beryllium chloride is supplied from the crystallization treatment tank 31 via the valve V17 to the centrifugal separator 32, which will be described later.

[0193] As shown in Fig. 8(b), the crystallization treatment tank 31 may be provided with a microwave oscillator 31a and a waveguide 31b instead of the valve V16 for supplying hot water. The microwave oscillator 31a and the waveguide 31b are configured similarly to the microwave oscillator 22a and the waveguide 22b shown in Fig. 7, respectively, and are an example of an induction heating device.

[0194] As described above, the heating means for heating the beryllium solution and the HCl solution in the crystallizer 20B may be an external heating system as shown in Fig. 8(a) or an induction heating system as shown in Fig. 8(b). From the viewpoint of energy efficiency, it is preferable to employ an induction heating system.

[0195] <Dehydration equipment 20C> As shown in Fig. 8, the dehydration apparatus 20C includes a centrifuge 32 and a dryer 33. The dehydration apparatus 20C also includes a control unit not shown in Fig. 8. The control unit controls each of the centrifuge 32 and the dryer 33.

[0196] The beryllium chloride crystallized by the crystallizer 20B is dehydrated using a centrifuge 32. The dehydrated beryllium chloride is then dehydrated using a dryer 33. An example of the dryer 33 is a hot air generating mechanism that generates hot air, and the hot air generated by the hot air generating mechanism is used to heat and dehydrate the beryllium chloride. In other words, the crystallizer 20B and the dehydration device 20C are examples of the dehydration device described in the claims, and are capable of carrying out the dehydration step S21 of the production method M20 shown in FIG. 2. The hot air is an example of a heating means that employs an external heating method.

[0197] The dryer 33 may include a microwave oscillator 33a and a waveguide 33b instead of the hot air generating mechanism that generates hot air. The microwave oscillator 33a and the waveguide 33b are configured similarly to the microwave oscillator 22a and the waveguide 22b shown in Fig. 7, respectively, and are an example of an induction heating device.

[0198] As described above, the heating means for heating beryllium chloride in the dehydration apparatus 20C may be an external heating method as shown in Fig. 8(a) or an induction heating method as shown in Fig. 8(c). From the viewpoint of energy efficiency, it is preferable to employ an induction heating method.

[0199] <Electrolyzer 20D> As shown in Fig. 8, the electrolysis device 20D includes an electrolysis furnace 34a, a power supply 34b, an anode 34c, a cathode 34d, and a feeder F2. The electrolysis furnace 34a also includes a heater (not shown in Fig. 8). The electrolysis device 20D also includes a control unit (not shown in Fig. 8). The control unit controls each of the power supply 34b, the heater, and the feeder F2.

[0200] Anhydrous beryllium chloride produced by the dehydration device 20C is supplied into the electrolytic furnace 34a. Sodium chloride (NaCl) is also supplied into the electrolytic furnace 34a via a feeder F2.

[0201] The electrolytic furnace 34a, which contains beryllium chloride and sodium chloride, is heated using a heater. As a result, the beryllium chloride and sodium chloride melt. The melting point of the electrolytic bath can be lowered by using a binary bath containing beryllium chloride and sodium chloride. The temperature of the electrolytic furnace 34a when heated can be appropriately set within a range exceeding the melting point of the binary bath. An example of the temperature of the electrolytic furnace 34a is 350°C.

[0202] The anode 34c is an electrode made of, for example, carbon, and the cathode 34d is an electrode made of, for example, nickel.

[0203] While the binary bath is in a molten state, the control unit uses power supply 34b to apply a current between anode 34c and cathode 34d, causing electrolysis of the binary bath and producing metallic beryllium on the surface of cathode 34d.

[0204] As described above, the electrolysis device 20D can perform the electrolysis step S22 of the manufacturing method M20 shown in FIG.

[0205] Other Embodiments In the above-described eighth embodiment, a beryllium production system 20 using the production apparatus 20A, the crystallization apparatus 20B, and the dehydration apparatus 20C, which performs the production method M20, has been described.

[0206] However, the scope of the present invention includes not only the beryllium production system 20, but also a beryllium hydroxide production system that implements the beryllium hydroxide production method M30, and a beryllium oxide production system that implements the beryllium oxide production method M40.

[0207] The beryllium hydroxide manufacturing system includes manufacturing apparatus 20A shown in Fig. 7 and a neutralization device that produces beryllium hydroxide by neutralizing the beryllium chloride solution produced by manufacturing apparatus 20A with a base. The neutralization device can be composed of components corresponding to vessel 24, valves V4 and V5, and centrifuge 25 shown in Fig. 7, for example. Furthermore, ammonia may be used as the base used for neutralization instead of sodium hydroxide.

[0208] The beryllium oxide production system includes the production apparatus 20A shown in Figure 7 and a third heating device that produces beryllium oxide by heating the beryllium chloride solution produced by the production apparatus 20A. The third heating device is not limited to, but may be, for example, an electric furnace.

[0209] [Ninth and Tenth Embodiments] A method M70 for producing lithium hydroxide (LiOH) according to a ninth embodiment of the present invention and a method M80 for producing lithium carbonate (LiCO) according to a tenth embodiment of the present invention will be described with reference to Fig. 9. (a) and (b) of Fig. 9 are flowcharts of the method M70 for producing lithium hydroxide and the method M80 for producing lithium carbonate, respectively.

[0210] Both the lithium hydroxide production method M70 and the lithium carbonate production method M80 use a solution containing lithium hydroxide, which is separated as a liquid phase in the second filtration step S15. Moreover, which of the lithium hydroxide production method M70 and the lithium carbonate production method M80 to carry out can be determined appropriately according to the priority at that time.

[0211] (Lithium hydroxide manufacturing method M70) 9(a), lithium hydroxide production method M70 includes a drying step S71. Drying step S71 is a step of evaporating the solution separated in the second filtration step S15 and drying the precipitated lithium hydroxide. By performing lithium hydroxide production method M70, solid lithium hydroxide can be obtained.

[0212] (Lithium carbonate manufacturing method M80) As shown in FIG. 9(b), a lithium carbonate manufacturing method M80 includes a carbon dioxide gas introducing step S81, a fourth filtration step S82, and a drying step S83.

[0213] The carbon dioxide gas introducing step S81 is a step of introducing carbon dioxide gas into the solution separated in the second filtration step S15, thereby precipitating lithium carbonate in the solution.

[0214] The fourth filtration step S82 is a step carried out after the carbon dioxide gas introduction step S81. The fourth filtration step S82 is a step of separating lithium carbonate precipitated in the solution from the solution using a filter.

[0215] The drying step S83 is a step carried out after the fourth filtration step S82. The drying step S83 is a step of drying the lithium carbonate separated in the fourth filtration step S82.

[0216] By carrying out the lithium carbonate production method M80, solid lithium carbonate can be obtained.

[0217] (Small summary) As described above, solid lithium hydroxide or solid lithium carbonate can be produced by carrying out lithium hydroxide production method M70 or lithium carbonate production method M80 using the solution containing lithium hydroxide separated as a liquid phase in second filtration step S15. Therefore, the lithium hydroxide separated as a liquid phase in second filtration step S15 can be recovered without being wasted as a resource.

[0218] It should be noted that each of the lithium hydroxide production method M70 and the lithium carbonate production method M80 can be included as part of the production method M10, similar to the separation method M50.

[0219] 〔summary〕 In order to solve the above problems, a method for producing a beryllium solution according to a first aspect of the present invention includes a main heating step in which at least one of beryllium, an intermetallic compound containing beryllium, beryllium having an oxide layer formed on its surface, and an intermetallic compound containing beryllium having an oxide layer formed on its surface is used as a starting material, and an acidic solution containing the starting material is dielectrically heated to produce a beryllium solution.

[0220] By utilizing dielectric heating to heat an acidic solution containing at least one of beryllium, an intermetallic compound containing beryllium, beryllium having an oxide layer formed on its surface, and an intermetallic compound containing beryllium having an oxide layer formed on its surface, the starting materials can be dissolved in the acidic solution with high energy efficiency. Therefore, this production method can provide a novel, highly energy-efficient method for producing a beryllium solution.

[0221] A second aspect of the present invention relates to a method for producing a beryllium solution according to the first aspect, and further includes a preheating step carried out before the main heating step, in which the basic solution containing the starting material is dielectrically heated.

[0222] By carrying out the pre-heating step before carrying out the main heating step, it is possible to dissolve starting materials that are difficult to dissolve by carrying out the main heating step alone, and therefore it is possible to produce a solution using a wider range of substances as starting materials.

[0223] A third aspect of the present invention relates to a method for producing a beryllium solution, and is the same as the first or second aspect, and further includes a first impurity removal step carried out after the main heating step, in which the first element is removed from the beryllium solution obtained by the main heating step using an organic compound that adsorbs the first element.

[0224] By carrying out the first impurity removal step, the concentration of the first element contained in the beryllium solution can be reduced. As a result, the concentration of the first element contained in the beryllium solution when producing beryllium, beryllium hydroxide, or beryllium oxide using the beryllium solution can be reduced. Examples of the first element include uranium, thorium, plutonium, and americium.

[0225] A fourth aspect of the present invention relates to a method for producing a beryllium solution according to the third aspect, wherein in the first impurity removal step, the organic compound is dissolved in an organic solvent and the beryllium solution is acidic.

[0226] This configuration can increase the efficiency with which the organic compound adsorbs the first element.

[0227] A fifth aspect of the present invention relates to a method for producing a beryllium solution, and is any one of the first to fourth aspects. The method further includes a second impurity removal step carried out after the main heating step, in which the polarity of the beryllium solution obtained by the main heating step is adjusted from acidic to basic, thereby removing a second element from the beryllium solution.

[0228] By carrying out the second impurity removal step, the concentration of the second element contained in the beryllium solution can be reduced. As a result, when beryllium, beryllium hydroxide, or beryllium oxide is produced using the beryllium solution, the concentration of the second element contained can be reduced. Examples of the second element include aluminum and iron.

[0229] A sixth aspect of the present invention is a method for producing a beryllium solution according to any one of the first to fifth aspects, wherein the main heating step comprises applying microwaves to dielectrically heat the acidic solution containing the starting material.

[0230] The technology of dielectric heating using microwaves (i.e., microwave dielectric heating) is a technology used in so-called microwave ovens and is widely used. Therefore, the production method of the present invention can reduce the cost required for implementation compared to conventional production methods.

[0231] A seventh aspect of the present invention is directed to a method for producing a beryllium solution according to any one of the first to sixth aspects, wherein the beryllium solution is a beryllium chloride solution.

[0232] According to this production method, a beryllium chloride solution can be easily produced without going through beryllium hydroxide. As will be described later, beryllium, beryllium hydroxide, and beryllium oxide can be easily produced from the beryllium chloride solution. Therefore, a beryllium chloride solution is preferred as the solution.

[0233] A method for producing beryllium according to an eighth aspect of the present invention includes the steps included in the method for producing a beryllium solution according to any one of the first to sixth aspects, as well as a dehydration step of producing a beryllium salt by dehydrating the beryllium solution, and an electrolysis step of producing beryllium by molten salt electrolysis of the beryllium salt.

[0234] A tenth aspect of the present invention relates to a method for producing beryllium hydroxide, which includes the steps included in the method for producing a beryllium solution according to any one of the first to sixth aspects, and a neutralization step of producing beryllium hydroxide by neutralizing the beryllium solution with a base.

[0235] A method for producing beryllium oxide according to an eleventh aspect of the present invention includes the steps included in the method for producing a beryllium solution according to any one of the first to sixth aspects, and a third heating step of producing beryllium oxide by heating the beryllium solution.

[0236] These manufacturing methods allow for the production of beryllium, beryllium hydroxide, and beryllium oxide using novel, energy-efficient manufacturing methods.

[0237] A ninth aspect of the present invention relates to a method for producing beryllium according to the eighth aspect, wherein the beryllium solution is a beryllium chloride solution, and the dehydration step involves heating the beryllium chloride hydrate contained in the beryllium chloride solution in a vacuum at a temperature of 80°C or higher and 110°C or lower.

[0238] According to this configuration, when the beryllium solution is a beryllium chloride solution, the beryllium chloride hydrate can be reliably subjected to the dehydration treatment.

[0239] A solution manufacturing apparatus according to a twelfth aspect of the present invention comprises a main heating vessel, an acidic solution supply unit that supplies an acidic solution to the main heating vessel, and a main heating device that dielectrically heats the acidic solution contained in the main heating vessel.

[0240] By using dielectric heating to heat the acidic solution contained in the main heating vessel, when the acidic solution contains a solute that is a starting material, the starting material can be dissolved in the acidic solution with high energy efficiency. Therefore, this manufacturing apparatus can provide a new solution manufacturing apparatus with high energy efficiency.

[0241] A thirteenth aspect of the present invention is the solution manufacturing apparatus of the twelfth aspect, further comprising a raw material supply unit that supplies at least one of beryllium, an intermetallic compound containing beryllium, beryllium having an oxide layer formed on its surface, and an intermetallic compound containing beryllium having an oxide layer formed on its surface as a starting raw material to at least one of the main heating vessel and the acidic solution supply unit.

[0242] By utilizing dielectric heating to heat an acidic solution containing at least one of beryllium, an intermetallic compound containing beryllium, beryllium having an oxide layer formed on its surface, and an intermetallic compound containing beryllium having an oxide layer formed on its surface, the starting materials can be dissolved in the acidic solution with high energy efficiency. Therefore, this manufacturing apparatus can provide a novel, highly energy-efficient manufacturing apparatus for a beryllium solution.

[0243] A solution manufacturing apparatus according to a fourteenth aspect of the present invention is the same as that of the twelfth aspect, further comprising a preheating container, a basic solution supply unit that supplies a basic solution to the preheating container, a raw material supply unit that supplies starting materials to at least one of the preheating container and the basic solution supply unit, a preheating device that dielectrically heats the basic solution contained in the preheating container, and a discharge unit that discharges the basic solution containing the starting materials from the preheating container to the main heating container.

[0244] Some beryllium oxides are difficult to dissolve by dielectric heating alone in an acidic solution, but by first dielectrically heating them in a basic solution before dielectrically heating them in an acidic solution, even difficult-to-dissolve beryllium oxides can be dissolved by dielectric heating in the acidic solution.

[0245] According to the above configuration, the basic solution containing beryllium oxide contained in the preheating vessel is dielectrically heated, and the dielectrically heated basic solution containing beryllium oxide is then discharged into the main heating vessel. Therefore, even when beryllium oxide is used as the starting material, which is difficult to dissolve in an acidic solution by dielectric heating alone, the starting material can be dissolved in the acidic solution.

[0246] A solution manufacturing apparatus according to a 15th aspect of the present invention is any one of the 12th to 14th aspects, wherein the main heating device is configured to dielectrically heat the acidic solution contained in the main heating container by applying microwaves.

[0247] According to the above arrangement, the same effects as those of the method for producing a beryllium solution according to the fifth aspect can be achieved.

[0248] The solution producing apparatus according to a sixteenth aspect of the present invention is configured in any one of the twelfth to fifteenth aspects, wherein the solution is a beryllium chloride solution.

[0249] According to the above arrangement, the same effects as those of the method for producing a beryllium solution according to the sixth aspect can be achieved.

[0250] A beryllium production system according to a seventeenth aspect of the present invention comprises the solution production apparatus according to the sixteenth aspect, a dehydration device that produces beryllium chloride by dehydrating the beryllium chloride solution, and an electrolysis device that produces beryllium by molten salt electrolysis of the beryllium chloride.

[0251] A beryllium hydroxide manufacturing system according to an eighteenth aspect of the present invention includes the solution manufacturing apparatus according to the sixteenth aspect, and a neutralization apparatus that produces beryllium hydroxide by neutralizing the beryllium chloride solution with a base.

[0252] A beryllium oxide manufacturing system according to a nineteenth aspect of the present invention includes the solution manufacturing apparatus according to the sixteenth aspect, and a third heating device that generates beryllium oxide by heating the beryllium chloride solution.

[0253] According to the above configuration, the same effects as those of the seventh to ninth aspects of the invention are achieved.

[0254] Beryllium according to a twentieth aspect of the present invention has a uranium concentration of less than 0.7 ppm.

[0255] Beryllium with a uranium concentration of less than 0.7 ppm can be disposed of at shallow depths after use, even if it is used as a neutron multiplier in a fusion reactor. Therefore, even if this beryllium is used as a neutron multiplier in a fusion reactor, it can be disposed of at shallow depths as is.

[0256] [Additional Notes] The present invention is not limited to the above-described embodiments, and various modifications are possible within the scope of the claims. Embodiments obtained by appropriately combining the technical means disclosed in different embodiments are also included in the technical scope of the present invention. [Explanation of symbols]

[0257] M10 Manufacturing method (method for manufacturing beryllium solution, method for manufacturing BeCl2 solution) S12 Main heating process S17, S18 First and second impurity removal processes M20, M30, M40 Methods for producing beryllium, beryllium hydroxide, and beryllium oxide S21 Anhydrous process S22 Electrolysis process S31 Neutralization process S41 Heating process M60 Manufacturing method (method for manufacturing lithium solution, method for manufacturing LiCl solution) S62 Preheating process S63 Main heating process S64, S65 First and second impurity removal processes 20A Manufacturing Equipment (Beryllium Solution Manufacturing Equipment, BeCl2 Solution Manufacturing Equipment) 22a Microwave oscillator (main heating device) 22c Main heating container F1 Feeder (raw material supply section) V1 valve (part of the acid solution supply section) 20B Crystallizer 20C dehydration equipment 20D electrolyzer

Claims

[Claim 1] The invention described in the specification.

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