Method for producing magnesium compound

Abstract

A method for producing a magnesium compound, wherein at least one of magnesium metal, an alcohol, and iodine is mixed with a fluorinated alcohol represented by formula (1) and a solvent to thereby form a magnesium precursor represented by formula (2), and a solvent containing the magnesium precursor is mixed with borane and a fluorinated alcohol to thereby form a magnesium compound represented by formula (3).　Formula (1): (R1)3COH (Each of the three R1 is one of hydrogen, fluorine, an alkyl group, and a fluorinated alkyl group. However, at least one of the three R1 is one of fluorine and a fluorinated alkyl group.)　Formula (2): Mg[OC(R2)3]2 (Each of the six R2 is one of hydrogen, fluorine, an alkyl group, and a fluorinated alkyl group. However, at least one of the six R2 is one of fluorine and a fluorinated alkyl group.　Formula (3): Mg[B(OC(R3)3)4]2 (Each of the 24 R3 is one of hydrogen, fluorine, an alkyl group, and a fluorinated alkyl group. However, at least one of the 24 R3 is one of fluorine and a fluorinated alkyl group.)

Description

Method for producing magnesium compounds

[0001] This technology is a method for producing magnesium compounds.

[0002] The development of magnesium compounds has been progressing, and various studies have been conducted on methods for producing such magnesium compounds. Specifically, magnesium borohydride (Mg(BH)) is used as a starting material. 4 ) 2 ) or dibutylmagnesium (Mg(C 4 H 9 ) 2 A method for producing a magnesium compound using magnesium stearate has been proposed (see, for example, Non-Patent Document 1). The magnesium compound produced by this method is used as an electrolyte salt in an electrolytic solution (see, for example, Patent Document 1).

[0003] International Publication No. 2020 / 235314

[0004] Critical Issues of Fluorinated Alkoxyborate-Based Electrolytes in Magnesium Battery Applications, ACS Appl. Mater. Interfaces 2020, 12, 39135-39144

[0005] Various studies have been conducted on methods for producing magnesium compounds, but the ease and stability of the methods for producing magnesium compounds are still insufficient, and there is room for improvement.

[0006] There is a demand for a method for producing a magnesium compound that can easily and stably obtain the magnesium compound.

[0007] In one embodiment of the present technology, a method for producing a magnesium compound includes mixing metallic magnesium, at least one of alcohol and iodine, a fluorinated alcohol represented by formula (1), and a solvent to form a magnesium precursor represented by formula (2), and then mixing the solvent containing the magnesium precursor, borane, and the fluorinated alcohol to form a magnesium compound represented by formula (3).

[0008] (R1) 3 COH (1) (Each of the three R1s is either hydrogen, fluorine, an alkyl group, or a fluorinated alkyl group, provided that at least one of the three R1s is either fluorine or a fluorinated alkyl group.)

[0009] Mg[OC(R2) 3 ] 2 ...(2) (Each of the six R2s is either hydrogen, fluorine, an alkyl group, or a fluorinated alkyl group, provided that at least one of the six R2s is either fluorine or a fluorinated alkyl group.)

[0010] Mg[B(OC(R3) 3 ) 4 ] 2 ... (3) (Each of the 24 R3's is any one of hydrogen, fluorine, an alkyl group, and a fluorinated alkyl group, provided that at least one of the 24 R3's is any one of fluorine and a fluorinated alkyl group.)

[0011] Here, "metallic magnesium" refers to so-called elemental magnesium. However, since the purity of metallic magnesium is not particularly limited, the metallic magnesium may contain any amount of impurities.

[0012] According to the method for producing a magnesium compound of one embodiment of the present technology, metallic magnesium, at least one of alcohol and iodine, a fluorinated alcohol, and a solvent are mixed together to form a magnesium precursor, and then the solvent containing the magnesium precursor, borane, and the fluorinated alcohol are mixed together to form the magnesium compound, thereby making it possible to easily and stably produce the magnesium compound.

[0013] Note that the effects of the present technology are not necessarily limited to the effects described here, but may be any of a series of effects related to the present technology described below.

[0014] 1 is a flowchart illustrating a method for producing a magnesium compound according to a first embodiment of the present technology; 2 is a flowchart illustrating a method for producing a magnesium compound according to a second embodiment of the present technology;

[0015] Hereinafter, one embodiment of the present technology will be described in detail with reference to the drawings. The description will be made in the following order: 1. Method for producing magnesium compound (first embodiment) 1-1. Overview 1-2. Production procedure 1-3. Actions and effects 2. Method for producing magnesium compound (second embodiment) 2-1. Overview 2-2. Production procedure 2-3. Actions and effects 3. Modification 4. Uses of magnesium battery

[0016] 1. Method for Producing Magnesium Compound (First Embodiment) First, a method for producing a magnesium compound according to a first embodiment of the present technology will be described.

[0017] <1-1. Overview> The method for producing a magnesium compound described here is a method for producing a magnesium compound represented by formula (3) described below, and more specifically, a method for producing a magnesium compound using metallic magnesium as a starting material.

[0018] As is clear from formula (3), this magnesium compound contains magnesium ions (Mg 2+ ) and a boron-containing ion ([B(OC(R3) 3 ) 4 ] - ) is a magnesium salt containing

[0019] The use of the magnesium compound is not particularly limited, but specifically, it is used as an electrolyte solution for a magnesium battery, etc. In this case, the magnesium compound is used as an electrolyte salt.

[0020] <1-2. Production Procedure> Fig. 1 shows the flow of the production procedure to explain the method for producing a magnesium compound in the first embodiment. The production procedure of the magnesium compound will be described below with reference to Fig. 1.

[0021] [Preparation of Raw Materials] When producing a magnesium compound, first, raw materials for synthesizing the magnesium compound are prepared (step S101).

[0022] In this case, elemental magnesium (metallic magnesium) is used as the supply source of magnesium contained in the magnesium compound, rather than magnesium compounds such as magnesium borohydride and dibutylmagnesium.

[0023] Specifically, metallic magnesium, alcohol, fluorinated alcohol, borane, and a solvent are prepared as raw materials.

[0024] (Metallic magnesium) As described above, metallic magnesium is magnesium alone and may contain any amount of impurities. The content of these impurities is preferably as small as possible, because this makes it easier to form magnesium compounds.

[0025] (Alcohol) Alcohol is a catalyst for promoting the dissolution reaction of metallic magnesium. Unlike fluorinated alcohol, this alcohol is a compound that does not contain fluorine as a constituent element. The type of alcohol is not particularly limited as long as it is one or more of any alcohol. Specific examples of alcohol include methanol, ethanol, and propanol. Note that alcohols with three or more carbon atoms, such as propanol, may be linear or branched.

[0026] Among these, it is preferable that the alcohol contains methanol, because this facilitates the dissolution reaction of metallic magnesium and makes it easier to form magnesium compounds.

[0027] (Fluorinated Alcohol) Fluorinated alcohol is a fluorine-containing group (—OC(R3)) contained in a magnesium compound. 3 ) is a material that serves as a supply source. Unlike alcohols, fluorinated alcohols are compounds that contain fluorine as a constituent element. That is, fluorinated alcohols are compounds in which one or more hydrogen atoms in alcohols have been substituted with fluorine, and more specifically, they contain one or more types of compounds represented by formula (1).

[0028] (R1) 3 COH (1) (Each of the three R1s is either hydrogen, fluorine, an alkyl group, or a fluorinated alkyl group, provided that at least one of the three R1s is either fluorine or a fluorinated alkyl group.)

[0029] As is clear from formula (1), this fluorinated alcohol is a compound in which one or more hydrogen atoms in an alcohol are substituted with fluorine atoms. Therefore, a compound in which all three R1s are either hydrogen atoms or alkyl groups does not fall under the category of fluorinated alcohols described here.

[0030] The number of carbon atoms in the alkyl group is not particularly limited. The type of alkyl group may be linear or branched. Specific examples of the alkyl group include a methyl group and an ethyl group. Of these, the alkyl group is preferably a methyl group, as this improves the compatibility of the fluorinated alcohol.

[0031] A fluorinated alkyl group is an alkyl group in which one or more hydrogen atoms have been substituted with fluorine atoms. The number of fluorine atoms contained in the fluorinated alkyl group is not particularly limited.

[0032] Specific examples of fluorinated alcohols include (CF), as described below in relation to specific examples of magnesium compounds. 3 ) 2 HCOH, (CF 3 ) 3 COH, (CH 3 ) (CF 3 ) HCOH, (CH 3 ) (CF 3 ) 2 COH, (CH 3 )2 (CF 3 ) COH, (CH 3 ) 2 FCOH and (CF 3 ) 2 FCOH, etc.

[0033] Among the fluorinated alcohols is hexafluoroisopropanol (hexafluoro-2-propanol) (CF 3 ) 2 It is preferable that HCOH is contained, since this facilitates the formation of magnesium compounds.

[0034] (Borane) Borane is a material that serves as a supply source of boron (B) contained in the magnesium compound. As described above, boron is the central element of the anion (boron-containing ion) contained in the magnesium compound.

[0035] (Solvent) The solvent contains one or more organic solvents capable of dissolving metallic magnesium.

[0036] Among these, it is preferable that the solvent contains an ether compound, because this allows metallic magnesium to be stably dissolved. The ether compound is a compound having an ether bond (—O—), and may be a chain compound, a cyclic compound, or both.

[0037] Specific examples of ether compounds include dimethoxyethane, diethylene glycol dimethyl ether, tetraethylene glycol dimethyl ether, and tetrahydrofuran, because they dissolve metallic magnesium sufficiently. The specific examples of the series of ether compounds described here are mainly so-called glyme-based ethers.

[0038] Among these, the ether compound preferably contains one or both of dimethoxyethane and tetrahydrofuran, because metallic magnesium is more easily dissolved in these compounds.

[0039] [Formation of Magnesium Precursor] Subsequently, the magnesium precursor represented by formula (2) is formed using the raw materials.

[0040] (Formation Procedure) Specifically, metallic magnesium, alcohol, fluorinated alcohol, and a solvent are mixed together (step S102). In this case, the solvent may be stirred using a stirring device or the like.

[0041] As a result, metallic magnesium reacts with the fluorinated alcohol in the solvent, and the magnesium precursor shown in formula (2) is synthesized (step S103).

[0042] Mg[OC(R2) 3 ] 2 ...(2) (Each of the six R2s is either hydrogen, fluorine, an alkyl group, or a fluorinated alkyl group, provided that at least one of the six R2s is either fluorine or a fluorinated alkyl group.)

[0043] This magnesium precursor is an intermediate product used to synthesize a magnesium compound, and as is clear from formula (2), the magnesium atom is bonded to two fluorine-containing groups (—OC(R2) 3 ) is bonded to the compound. Therefore, a compound in which all six R2 are either hydrogen or an alkyl group does not fall under the category of magnesium precursors described here.

[0044] (Chemical Reactions) In the magnesium precursor synthesis process, the chemical reactions represented by the following formulas (A) to (C) proceed, thereby synthesizing the magnesium precursor. Hereinafter, the chemical reaction shown in formula (A) will be referred to as "chemical reaction A," the chemical reaction shown in formula (B) as "chemical reaction B," and the chemical reaction shown in formula (C) as "chemical reaction C."

[0045] Chemical reactions A to C described here involve using methanol (CH 3 OH) was used as a fluorinated alcohol, and hexafluoroisopropanol ((CF 3 ) 2 HClOH) as the magnesium precursor, Mg[OCH(CF 3 ) 2 ] 2 This is the chemical reaction in which

[0046] Mg + 2CH 3 OH → Mg(CH 3 O) 2 +H 2 ...(A)

[0047] Mg(CH 3 O) 2 +2 (CF 3 ) 2 HOH→Mg[OCH(CF 3 ) 2 ] 2 +2CH 3 OH... (B)

[0048] Mg+2(CF 3 ) 2 CHOH→Mg[OCH(CF 3 ) 2 ] 2 +H 2 ...(C)

[0049] Details regarding chemical reactions A to C are described below.

[0050] Chemical reaction A proceeds at room temperature and produces magnesium methoxide (Mg(CH 3 O) 2 However, alcohol (CH 3 Since magnesium methoxide has low solubility in magnesium methoxide (OH), the reaction rate of chemical reaction A decreases as the chemical reaction A progresses. This is because the presence of magnesium methoxide, which has low solubility, coats the surface of metallic magnesium (Mg) and reduces the stirring efficiency of the solvent containing magnesium methoxide.

[0051] Therefore, a fluorinated alcohol (CF) was added to a solvent containing magnesium methoxide. 3 ) 2 By adding the magnesium precursor (Mg[OCH(CF)], chemical reaction B proceeds. 3 ) 2 ] 2 ) is synthesized. Since the solubility of the magnesium precursor in alcohol is significantly higher than that of magnesium methoxide in that alcohol, converting the magnesium methoxide to the magnesium precursor makes the magnesium precursor soluble in the alcohol. This prevents the aforementioned decrease in reaction rate caused by the presence of magnesium methoxide.

[0052] The alcohol produced in chemical reaction B is reused in chemical reaction A. This reduces the amount of alcohol consumed in chemical reaction A.

[0053] In this case, the use of an ether compound as the solvent promotes dissolution of the magnesium precursor, thereby further suppressing a decrease in the reaction rate.

[0054] In the magnesium precursor synthesis process, not only do chemical reactions A and B proceed, but also chemical reaction C. Unlike chemical reactions A and B, chemical reaction C synthesizes the magnesium precursor directly from metallic magnesium without passing through magnesium methoxide.

[0055] The reaction rate of chemical reaction C at room temperature is lower than the reaction rates of chemical reactions A and B. In this case, the reaction rate becomes lower due to the formation of an oxide film on the surface of the metallic magnesium, and therefore the progress of chemical reaction C is hindered.

[0056] However, in chemical reaction A, the oxide film formed on the surface of the metallic magnesium is dissolved, making the surface (active surface) of the metallic magnesium more likely to be exposed. This promotes the progress of chemical reaction C, and a magnesium precursor is also synthesized in chemical reaction C.

[0057] From these facts, in the magnesium precursor synthesis process, the magnesium precursor is indirectly synthesized using metallic magnesium as a starting material in chemical reactions A and B, and the magnesium precursor is directly synthesized using metallic magnesium as a starting material in chemical reaction C.

[0058] [Formation of Magnesium Compound] Finally, the magnesium compound represented by formula (3) is formed using the magnesium precursor.

[0059] (Formation Procedure) Specifically, a solvent containing a magnesium precursor, borane, and a fluorinated alcohol are mixed together (step S104). In this case, the solvent may be stirred using a stirring device or the like.

[0060] As a result, the magnesium precursor reacts with the borane and the fluorinated alcohol in the solvent, and the magnesium compound shown in formula (3) is synthesized (step S105).

[0061] Mg[B(OC(R3) 3 ) 4 ] 2 ... (3) (Each of the 24 R3's is any one of hydrogen, fluorine, an alkyl group, and a fluorinated alkyl group, provided that at least one of the 24 R3's is any one of fluorine and a fluorinated alkyl group.)

[0062] As is clear from formula (3), this magnesium compound has two magnesium atoms in a boron-containing group (-B(OC(R3) 3 ) 4 Therefore, a compound in which all 24 R3 are either hydrogen or an alkyl group does not fall under the magnesium compound described here.

[0063] As a result, a magnesium compound is obtained. As described above, this magnesium compound contains magnesium ions (Mg 2+ ) and a boron-containing ion ([B(OC(R3) 3 ) 4 ] - ) is a magnesium salt containing

[0064] (Chemical Reaction) In the synthesis process of the magnesium compound, the chemical reaction represented by the following formula (D) proceeds, thereby synthesizing a magnesium precursor. Hereinafter, the chemical reaction represented by formula (D) is referred to as "chemical reaction D."

[0065] Chemical reaction D described here uses hexafluoroisopropanol (CF) as the fluorinated alcohol. 3 ) 2 By using Mg[B(OCH(CF)] as the magnesium compound, 3 ) 2 ) 4 ] 2 This is the chemical reaction in which

[0066] Mg[OCH(CF 3 ) 2 ] 2 +2BH 3 +6 (CF 3 ) 2 HCOH→Mg[B(OCH(CF 3 ) 2 ) 4 ] 2 +6H 2 ... (D)

[0067] In chemical reaction D, the magnesium precursor (Mg[OCH(CF) 3 ) 2 ] 2 ) is Boran (BH 3 ) and fluorinated alcohols ((CF 3 ) 2 HClOH), which produces magnesium compounds (Mg[B(OCH(CF 3 ) 2 ) 4 ] 2 ) is synthesized.

[0068] (Specific Example) The structure of the magnesium compound produced by the above-described production procedure is determined depending on the structure of the fluorinated alcohol used in the production procedure.

[0069] For example, the relationship between the structure of the fluorinated alcohol, the structure of the magnesium precursor, and the structure of the magnesium compound is as follows:

[0070] Fluorinated alcohols (CF 3 ) 2 When HClOH was used, Mg[OCH(CF)] was used as the magnesium precursor. 3 )2 ] 2 is formed, and the magnesium compound Mg[B(OCH(CF 3 ) 2 ) 4 ] 2 is manufactured.

[0071] Fluorinated alcohols (CF 3 ) 3 When COH was used, Mg[OC(CF 3 ) 3 ] 2 is formed, and the magnesium compound Mg[B(OC(CF 3 ) 3 ) 4 ] 2 is manufactured.

[0072] Fluorinated alcohols (CH 3 ) (CF 3 When HCl was used, Mg[OCH(CF)] was used as the magnesium precursor. 3 ) (CH 3 )] 2 is formed, and the magnesium compound Mg[B(OCH(CF 3 ) (CH 3 )) 4 ] 2 is manufactured.

[0073] Fluorinated alcohols (CH 3 ) (CF 3 ) 2 When COH was used, Mg[OC(CF 3 ) 2 (CH 3 )] 2 is formed, and the magnesium compound Mg[B(OC(CF 3 ) 2 (CH 3 )) 4 ] 2 is manufactured.

[0074] Fluorinated alcohols (CH 3 ) 2 (CF 3 When )COH was used, Mg[OC(CF 3 ) (CH 3 ) 2 ] 2 is formed, and the magnesium compound Mg[B(OC(CF 3 ) (CH 3 ) 2 ) 4 ] 2 is manufactured.

[0075] Fluorinated alcohols (CH 3 ) 2 When FCOH was used, Mg[OCF(CH 3 ) 2 ] 2 is formed, and Mg[B(OCF(CH 3 ) 2 ) 4 ] 2 is manufactured.

[0076] Fluorinated alcohols (CF 3 ) 2 When FCOH was used, Mg[OCF(CF 3 ) 2 ] 2 is formed, and the magnesium compound Mg[B(OCF(CF 3 ) 2 ) 4 ] 2 is manufactured.

[0077] <1-3. Actions and Effects> According to the method for producing a magnesium compound in the first embodiment, metallic magnesium, alcohol, a fluorinated alcohol, and a solvent are mixed together to form a magnesium precursor, and then the solvent containing the magnesium precursor, borane, and the fluorinated alcohol are mixed together to form a magnesium compound.

[0078] In this case, the magnesium compound is synthesized using chemically stable elemental magnesium (metallic magnesium) as the starting material, rather than using a chemically unstable magnesium compound as the starting material. Specific examples of the chemically unstable magnesium compound include the above-mentioned magnesium borohydride and dibutylmagnesium.

[0079] Moreover, to synthesize a magnesium compound using metallic magnesium as a starting material, only a simple process of reacting metallic magnesium with a fluorinated alcohol and a borane is used.

[0080] Therefore, the magnesium compound can be easily and stably synthesized, and thus the magnesium compound can be easily and stably obtained. In this case, in particular, since there is no need to use an expensive magnesium compound as a starting material, the magnesium compound can be obtained in large quantities at low cost.

[0081] In particular, if the fluorinated alcohol contains hexafluoroisopropanol, a magnesium compound is more likely to be formed, and therefore a higher effect can be obtained.

[0082] Furthermore, if the alcohol contains methanol, magnesium compounds are more likely to be formed, resulting in a higher effect.

[0083] Furthermore, if the solvent contains an ether compound having an ether bond, the magnesium compound can be stably dissolved, thereby achieving a higher effect. In this case, if the ether compound contains one or both of dimethoxyethane and tetrahydrofuran, the magnesium compound can be sufficiently dissolved, thereby achieving an even higher effect.

[0084] 2. Method for Producing Magnesium Compound (Second Embodiment) Next, a method for producing a magnesium compound according to a second embodiment of the present technology will be described.

[0085] <2-1. Overview> The method for producing a magnesium compound in the second embodiment is to use iodine (I) instead of alcohol. 2 The method for producing a magnesium compound is the same as that of the first embodiment, except that iodine is used. This iodine, like alcohol, is a catalyst for promoting the dissolution reaction of metallic magnesium.

[0086] <2-2. Production Procedure> Fig. 2 shows the flow of the production procedure for explaining the method for producing a magnesium compound in the second embodiment, and corresponds to Fig. 1. The production procedure of the magnesium compound will be described below with reference to Fig. 2.

[0087] [Preparation of Raw Materials] When producing a magnesium compound, first, raw materials for synthesizing the magnesium compound are prepared (step S201).

[0088] In this case, similarly to the first embodiment, metallic magnesium is used as the supply source of magnesium contained in the magnesium compound, instead of the magnesium compound.

[0089] Specifically, metallic magnesium, iodine, a fluorinated alcohol, borane, and a solvent are prepared as raw materials. Details of the metallic magnesium, the fluorinated alcohol, and the solvent are as described above.

[0090] [Formation of Magnesium Precursor] Subsequently, the magnesium precursor represented by formula (2) is formed using the raw materials.

[0091] (Formation Procedure) Specifically, metallic magnesium, iodine, a fluorinated alcohol, and a solvent are mixed together (step S202). In this case, the solvent may be stirred using a stirring device or the like. This synthesizes a magnesium precursor (step S203). Details regarding the magnesium precursor are as described above.

[0092] (Chemical Reaction) In the magnesium precursor synthesis step, the chemical reaction represented by the following formula (E) proceeds, thereby synthesizing the magnesium precursor. Hereinafter, the chemical reaction represented by formula (E) will be referred to as "chemical reaction E."

[0093] Chemical reaction E described here uses hexafluoroisopropanol (CF) as the fluorinated alcohol. 3 ) 2 HClOH) as the magnesium precursor, Mg[OCH(CF 3 ) 2 ] 2 This is the chemical reaction in which

[0094] Mg+I 2 →MgI 2 ...(E)

[0095] Chemical reaction E proceeds at room temperature and produces magnesium iodide (MgI 2 ) is synthesized. Furthermore, the above-mentioned chemical reaction C proceeds.

[0096] At room temperature, an oxide film is formed on the surface of metallic magnesium (Mg), slowing down the reaction rate of the metallic magnesium. However, in chemical reaction E, the oxide film formed on the surface of the metallic magnesium is dissolved, making the surface (active surface) of the metallic magnesium more likely to be exposed. This promotes chemical reaction C, which in turn accelerates the reaction of the magnesium precursor (Mg[OCH(CF 3 ) 2 ] 2 ) is synthesized.

[0097] Formation of the Magnesium Compound Finally, the magnesium precursor is used to form the magnesium compound shown in formula (3).

[0098] (Formation Procedure) Specifically, as in the first embodiment, a solvent containing a magnesium precursor, borane, and a fluorinated alcohol are mixed together (step S204). In this case, the solvent may be stirred using a stirring device or the like.

[0099] As a result, the magnesium precursor reacts with the borane and the fluorinated alcohol in the solvent, and a magnesium compound is synthesized (step S205).

[0100] (Chemical Reaction) In the synthesis process of the magnesium compound, chemical reaction D proceeds, and the magnesium compound (Mg[B(OCH(CF 3 ) 2 ) 4 ] 2 ) is synthesized.

[0101] (Specific Example) The structure of the magnesium compound produced by the above-described production procedure is determined depending on the structure of the fluorinated alcohol used in the production procedure. The relationship between the structure of the fluorinated alcohol, the structure of the magnesium precursor, and the structure of the magnesium compound is as described in the first embodiment.

[0102] <2-3. Actions and Effects> According to the method for producing a magnesium compound in the second embodiment, metallic magnesium, iodine, a fluorinated alcohol, and a solvent are mixed together to form a magnesium precursor, and then the solvent containing the magnesium precursor, borane, and a fluorinated alcohol are mixed together to form a magnesium compound.

[0103] In this case, for the same reasons as those explained in the first embodiment, chemically stable metallic magnesium is used as a starting material, and a magnesium compound is synthesized simply by using a simple process in which iodine is used to react the metallic magnesium with a fluorinated alcohol and borane.

[0104] Therefore, the magnesium compound can be produced easily and stably, and therefore the magnesium compound can be obtained easily and stably.

[0105] Other actions and effects of the method for producing a magnesium compound in the second embodiment are similar to other actions and effects of the method for producing a magnesium compound in the first embodiment, except for actions and effects based on alcohol.

[0106] 3. Modifications The above-described method for producing a magnesium compound can be modified as appropriate.

[0107] Specifically, in the first embodiment, alcohol was used as a catalyst for promoting the dissolution reaction of metallic magnesium, and in the second embodiment, iodine was used as a catalyst for promoting the dissolution reaction of metallic magnesium.

[0108] However, instead of using only one of the alcohol and iodine, both the alcohol and iodine may be used, and in this case, the magnesium compound can be produced easily and stably, and the same effect can be obtained.

[0109] 4. Uses of Magnesium Batteries There are no particular limitations on the uses (application examples) of magnesium batteries. Secondary batteries used as power sources may be the main power source or auxiliary power source in electronic devices, electric vehicles, and the like. The main power source is a power source that is used preferentially regardless of the presence or absence of other power sources. The auxiliary power source may be a power source used in place of the main power source or a power source that can be switched from the main power source.

[0110] Specific examples of uses for magnesium batteries are as follows: Electronic devices such as video cameras, digital still cameras, mobile phones, laptop computers, headphone stereos, portable radios, and portable information terminals. Storage devices such as backup power supplies and memory cards. Power tools such as power drills and power saws. Battery packs installed in electronic devices. Medical electronic devices such as pacemakers and hearing aids. Electric vehicles such as electric cars (including hybrid cars). Power storage systems such as home or industrial battery systems that store power in preparation for emergencies. In these uses, one or more magnesium batteries may be used.

[0111] The battery pack may use a single cell or a battery pack. The electric vehicle is a vehicle that runs using a magnesium battery as a driving power source, and may be a hybrid vehicle that also has a driving source other than the magnesium battery. In a home power storage system, the power stored in the magnesium battery, which is a power storage source, can be used to power home electrical appliances, etc.

[0112] An embodiment of the present technology will be described.

[0113] After the magnesium compound was produced, the magnesium compound was evaluated.

[0114] [Production of Magnesium Compound] A magnesium compound was produced according to the procedure described below.

[0115] Example 1 A magnesium compound was produced using the method for producing a magnesium compound in the first embodiment.

[0116] First, the alcohol (methanol (CH 3 OH)) 1 cm 3 100 mg (4 mmol) of metallic magnesium (Mg) was added to 25 mmol of alcohol, and the alcohol was stirred to prepare Solution W. In this case, Solution W foamed due to the generation of hydrogen.

[0117] Subsequently, the solution W was mixed with a fluorinated alcohol (hexafluoroisopropanol (CF 3 ) 2 HCOH)) 1 cm 3 (10 mmol) was added to the solution W, and the solution W was stirred. Then, 1.5 cm of a solvent (tetrahydrofuran, an ether compound) was added to the solution W. 3 (18 mmol) was added to the solution W, and the solution W was further stirred. This resulted in the formation of a magnesium precursor (Mg[OCH(CF 3 ) 2 ] 2 ) was synthesized, and a solution X containing its magnesium precursor was prepared.

[0118] Subsequently, the solution X was dried under reduced pressure to recover the magnesium precursor.

[0119] Next, 20 cm of solvent (dimethoxyethane, an ether compound) 3 A magnesium precursor (0.01 mol) was added to the solvent, and the solvent was stirred to prepare a solution Y in which the magnesium precursor was dissolved.

[0120] Next, borane was added to a solvent (tetrahydrofuran, an ether compound), and the solvent was stirred to prepare a tetrahydrofuran solution of borane. 3 (borane 0.022 mol) and 12 cm of fluorinated alcohol (hexafluoroisopropanol) 3 (0.11 mol) was added to solution Y, and then solution Z was prepared by stirring.

[0121] Finally, Solution Z was stirred (stirring time = 1 day) in a room temperature environment (temperature = 23 °C), and then reduced pressure in a high temperature environment (temperature = 50 °C) (reduced pressure time = 1 day) to volatilize and remove the solvent. As a result, the magnesium compound (Mg[B(OCH(CF 3 ) 2 ) 4 ] 2 ) was synthesized, resulting in its magnesium compound.

[0122] Example 2 A magnesium compound was produced using the method for producing a magnesium compound according to the second embodiment.

[0123] First, iodine (I) was added to a solvent (tetrahydrofuran, an ether compound). 2 ) was added, and the solvent was stirred to prepare a solution of iodine in tetrahydrofuran.

[0124] Next, a solution of iodine in tetrahydrofuran (4 mmol / dm 3 ) and 100 mg (4 mmol) of metallic magnesium (Mg) and 1 cm of fluorinated alcohol (hexafluoroisopropanol). 3 (10 mmol) was added, and the iodine tetrahydrofuran solution was stirred. This resulted in the formation of a magnesium precursor (Mg(OCH(CF) 3 ) 2 ) 2 ) was synthesized, and a solution P containing its magnesium precursor was prepared.

[0125] Subsequently, the solution P was dried under reduced pressure to recover the magnesium precursor.

[0126] Finally, a magnesium compound (Mg[B(OCH(CF)]) was prepared using a magnesium precursor in the same manner as in Example 1. 3 ) 2 ) 4 ] 2 ) was synthesized.

[0127] [Evaluation of Magnesium Compounds] The magnesium compounds were evaluated using nuclear magnetic resonance (NMR) spectroscopy according to the following procedure, along with the magnesium precursors used to synthesize the magnesium compounds, for confirmation.

[0128] When evaluating a magnesium precursor, the magnesium precursor was placed in a solvent and the solvent was stirred. This dissolved the magnesium precursor in the solvent, and a sample for analysis was obtained. The solvent used was lithium bis(trifluoromethanesulfonyl)imide (LiN(CF 3 SO 2 ) 2 ) dimethyl sulfoxide-d 6 Solution (LiTFSI DMSO-d 6 ) was used. After that, proton nuclear magnetic resonance ( 1 The samples were analyzed using 1 H NMR.

[0129] When evaluating magnesium compounds, the samples were analyzed using proton nuclear magnetic resonance spectroscopy using a procedure similar to that for evaluating the magnesium precursor, except that the magnesium compound was used instead of the magnesium precursor.

[0130] [Evaluation Results] When the magnesium compounds were evaluated, the following results were obtained.

[0131] Example 1 The analysis of the magnesium precursor using proton nuclear magnetic resonance spectroscopy revealed that the fluorine-containing group (—OCH(CF 3 ) 2 A peak due to the magnesium precursor (Mg(OCH(CF)) was detected at 8.0 ppm (reference material: tetramethylsilane). 3 ) 2 ) 2 It was confirmed that the alcohol (methanol) and solvent (dimethoxyethane and tetrahydrofuran) were present as crystallization or coordination solvents in this case.

[0132] In addition, the analysis of the magnesium compound using proton nuclear magnetic resonance spectroscopy revealed that the fluorine-containing group (—OCH(CF 3 ) 2 ) and a peak due to dimethoxyethane were detected. This indicated that the magnesium compound (Mg[B(OCH(CF) 3 ) 2 ) 4 ] 2 ) was confirmed to have been synthesized.

[0133] In this case, the fluorine-containing group (—OCH(CF 3 ) 2 Since the molar ratio of the magnesium compound (Mg[B(OCH(CF)]) to the solvent (dimethoxyethane) was 8:3, the target magnesium compound (Mg[B(OCH(CF)]) was obtained. 3 ) 2 ) 4 ] 2 ) is [Mg(CH 3 O.C. 2 H 4 CH 3 ) 3 ][B(OCH(CF 3 ) 2 ) 4 ] 2 It was confirmed that it exists in this state.

[0134] Example 2 The same evaluation results as those of Example 1 were obtained. As a result, the magnesium precursor (Mg(OCH(CF) 3 ) 2 ) 2 ) was synthesized, and a magnesium compound (Mg[B(OCH(CF) 3 ) 2 ) 4 ] 2 ) was confirmed to have been synthesized.

[0135] Normally, hydrogen should not be generated in the reaction between metallic magnesium and iodine. However, in Example 2, as described above, hydrogen was generated due to the reaction of metallic magnesium, and it was confirmed that the metallic magnesium reacted with the fluorinated alcohol (hexafluoroisopropanol). This result also confirmed that a magnesium compound was synthesized via a magnesium precursor.

[0136] [Summary] From the above evaluation results, it was found that a magnesium compound was formed using metallic magnesium as a starting material, and therefore, the magnesium compound could be obtained easily and stably.

[0137] The present technology has been described above using examples along with several embodiments, but the configuration of the present technology is not limited to the configurations described in those embodiments and examples, and can be modified in various ways.

[0138] Specifically, although the magnesium compound has been described as being used in a magnesium battery, the use of the magnesium compound is not particularly limited, and the magnesium compound can be widely used in applications other than magnesium batteries.

[0139] The effects described in this specification are merely examples, and the effects of the present technology are not limited to the effects described in this specification. Therefore, other effects may be obtained with respect to the present technology.

[0140] The present technology can also be configured as follows: <1> A method for producing a magnesium compound, comprising mixing metallic magnesium, at least one of alcohol and iodine, a fluorinated alcohol represented by formula (1), and a solvent to form a magnesium precursor represented by formula (2), and mixing the solvent containing the magnesium precursor, borane, and the fluorinated alcohol to form a magnesium compound represented by formula (3). (R1) 3 COH (1) (Each of the three R1s is either hydrogen, fluorine, an alkyl group, or a fluorinated alkyl group, provided that at least one of the three R1s is either fluorine or a fluorinated alkyl group.) Mg[OC(R2) 3 ] 2 ... (2) (Each of the six R2 is either hydrogen, fluorine, an alkyl group, or a fluorinated alkyl group, provided that at least one of the six R2 is either fluorine or a fluorinated alkyl group.) Mg[B(OC(R3) 3 ) 4 ] 2 ... (3) (Each of the 24 R3's is either hydrogen, fluorine, an alkyl group, or a fluorinated alkyl group, with the proviso that at least one of the 24 R3's is either fluorine or a fluorinated alkyl group.) <2> The method for producing a magnesium compound according to <1>, wherein the fluorinated alcohol includes hexafluoroisopropanol. <3> The method for producing a magnesium compound according to <1> or <2>, wherein the alcohol includes methanol. <4> The method for producing a magnesium compound according to any one of <1> to <3>, wherein the solvent includes an ether compound having an ether bond (—O—). <5> The method for producing a magnesium compound according to <4>, wherein the ether compound includes at least one of dimethoxyethane and tetrahydrofuran.

Claims

1. forming a magnesium precursor represented by formula (2) by mixing metallic magnesium, at least one of an alcohol and iodine, a fluorinated alcohol represented by formula (1), and a solvent; mixing the solvent containing the magnesium precursor, borane, and the fluorinated alcohol together to form a magnesium compound represented by formula (3); A method for producing magnesium compounds. (R1) 3 COH ・・・(1) (Each of the three R1s is any one of hydrogen, fluorine, an alkyl group, and a fluorinated alkyl group, provided that at least one of the three R1s is any one of fluorine and a fluorinated alkyl group.) Mg[OC(R2) 3 ] 2 ・・・(2) (Each of the six R2's is any one of hydrogen, fluorine, an alkyl group, and a fluorinated alkyl group, provided that at least one of the six R2's is any one of fluorine and a fluorinated alkyl group.) Mg[B(OC(R3) 3 ) 4 ] 2 ・・・(3) (Each of the 24 R3 is any one of hydrogen, fluorine, an alkyl group, and a fluorinated alkyl group, provided that at least one of the 24 R3 is any one of fluorine and a fluorinated alkyl group.)

2. The fluorinated alcohol includes hexafluoroisopropanol; A method for producing the magnesium compound according to claim 1.

3. The alcohol includes methanol. A method for producing the magnesium compound according to claim 1.

4. The alcohol includes methanol. The method for producing the magnesium compound according to claim 2.

5. The solvent contains an ether compound having an ether bond (—O—). A method for producing the magnesium compound according to any one of claims 1 to 4.

6. The ether compound includes at least one of dimethoxyethane and tetrahydrofuran. The method for producing the magnesium compound according to claim 5.