WO2024101158A1 - Méthode de production d'oxyde de magnésium - Google Patents
Méthode de production d'oxyde de magnésium Download PDFInfo
- Publication number
- WO2024101158A1 WO2024101158A1 PCT/JP2023/038523 JP2023038523W WO2024101158A1 WO 2024101158 A1 WO2024101158 A1 WO 2024101158A1 JP 2023038523 W JP2023038523 W JP 2023038523W WO 2024101158 A1 WO2024101158 A1 WO 2024101158A1
- Authority
- WO
- WIPO (PCT)
- Prior art keywords
- magnesium
- suspension
- carbonation
- magnesium oxide
- magnesium carbonate
- Prior art date
Links
- 239000000395 magnesium oxide Substances 0.000 title claims abstract description 61
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 title claims abstract description 61
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 title claims abstract description 59
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 41
- 239000000725 suspension Substances 0.000 claims abstract description 78
- ZLNQQNXFFQJAID-UHFFFAOYSA-L magnesium carbonate Chemical compound [Mg+2].[O-]C([O-])=O ZLNQQNXFFQJAID-UHFFFAOYSA-L 0.000 claims abstract description 71
- 239000001095 magnesium carbonate Substances 0.000 claims abstract description 67
- 229910000021 magnesium carbonate Inorganic materials 0.000 claims abstract description 67
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 claims abstract description 66
- 238000000926 separation method Methods 0.000 claims abstract description 49
- 239000001569 carbon dioxide Substances 0.000 claims abstract description 33
- 229910002092 carbon dioxide Inorganic materials 0.000 claims abstract description 33
- 238000002425 crystallisation Methods 0.000 claims abstract description 26
- 230000008025 crystallization Effects 0.000 claims abstract description 26
- VTHJTEIRLNZDEV-UHFFFAOYSA-L magnesium dihydroxide Chemical compound [OH-].[OH-].[Mg+2] VTHJTEIRLNZDEV-UHFFFAOYSA-L 0.000 claims abstract description 24
- 239000000347 magnesium hydroxide Substances 0.000 claims abstract description 24
- 229910001862 magnesium hydroxide Inorganic materials 0.000 claims abstract description 24
- QWDJLDTYWNBUKE-UHFFFAOYSA-L magnesium bicarbonate Chemical compound [Mg+2].OC([O-])=O.OC([O-])=O QWDJLDTYWNBUKE-UHFFFAOYSA-L 0.000 claims abstract description 23
- 229910000022 magnesium bicarbonate Inorganic materials 0.000 claims abstract description 23
- 239000002370 magnesium bicarbonate Substances 0.000 claims abstract description 23
- 235000014824 magnesium bicarbonate Nutrition 0.000 claims abstract description 23
- 239000000243 solution Substances 0.000 claims abstract description 22
- 239000007788 liquid Substances 0.000 claims abstract description 17
- 239000007864 aqueous solution Substances 0.000 claims abstract description 14
- AXCZMVOFGPJBDE-UHFFFAOYSA-L calcium dihydroxide Chemical compound [OH-].[OH-].[Ca+2] AXCZMVOFGPJBDE-UHFFFAOYSA-L 0.000 claims abstract description 13
- 239000000920 calcium hydroxide Substances 0.000 claims abstract description 13
- 229910001861 calcium hydroxide Inorganic materials 0.000 claims abstract description 13
- 238000007664 blowing Methods 0.000 claims abstract description 9
- 238000000034 method Methods 0.000 claims description 55
- 238000010438 heat treatment Methods 0.000 claims description 38
- 239000007789 gas Substances 0.000 claims description 32
- 238000001354 calcination Methods 0.000 claims description 22
- 239000000463 material Substances 0.000 claims description 5
- 238000010304 firing Methods 0.000 abstract description 15
- 239000012535 impurity Substances 0.000 description 33
- 239000007787 solid Substances 0.000 description 14
- 239000013078 crystal Substances 0.000 description 8
- 239000011777 magnesium Substances 0.000 description 8
- 229910052749 magnesium Inorganic materials 0.000 description 7
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 description 6
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 6
- 229910000514 dolomite Inorganic materials 0.000 description 4
- 239000010459 dolomite Substances 0.000 description 4
- 239000002244 precipitate Substances 0.000 description 4
- 229910000019 calcium carbonate Inorganic materials 0.000 description 3
- 239000000292 calcium oxide Substances 0.000 description 3
- ODINCKMPIJJUCX-UHFFFAOYSA-N calcium oxide Inorganic materials [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 description 3
- 230000007423 decrease Effects 0.000 description 3
- 239000013067 intermediate product Substances 0.000 description 3
- 239000000843 powder Substances 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- 239000003082 abrasive agent Substances 0.000 description 2
- 239000003463 adsorbent Substances 0.000 description 2
- 239000011575 calcium Substances 0.000 description 2
- 239000003054 catalyst Substances 0.000 description 2
- 229910010293 ceramic material Inorganic materials 0.000 description 2
- 239000003814 drug Substances 0.000 description 2
- 238000000605 extraction Methods 0.000 description 2
- 239000000706 filtrate Substances 0.000 description 2
- 235000013305 food Nutrition 0.000 description 2
- 238000005338 heat storage Methods 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 239000000049 pigment Substances 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 238000011084 recovery Methods 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- 239000011232 storage material Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000004073 vulcanization Methods 0.000 description 2
- 238000004876 x-ray fluorescence Methods 0.000 description 2
- 229910019440 Mg(OH) Inorganic materials 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 229910052791 calcium Inorganic materials 0.000 description 1
- BRPQOXSCLDDYGP-UHFFFAOYSA-N calcium oxide Chemical compound [O-2].[Ca+2] BRPQOXSCLDDYGP-UHFFFAOYSA-N 0.000 description 1
- 238000005119 centrifugation Methods 0.000 description 1
- 239000012295 chemical reaction liquid Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- 238000004445 quantitative analysis Methods 0.000 description 1
- 239000013535 sea water Substances 0.000 description 1
- 239000002002 slurry Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000004381 surface treatment Methods 0.000 description 1
- 239000012756 surface treatment agent Substances 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F5/00—Compounds of magnesium
- C01F5/02—Magnesia
- C01F5/06—Magnesia by thermal decomposition of magnesium compounds
Definitions
- the present invention relates to a new method for producing magnesium oxide.
- Magnesium oxide is used in a variety of industrial fields as an industrial and pharmaceutical raw material.
- magnesium oxide is known to have excellent effects in a variety of applications, including pharmaceuticals, food, vulcanization accelerators, pigments, chemical heat storage materials, battery materials, ceramic materials, adsorbents, abrasives, and catalysts.
- Magnesium oxide is industrially produced by various methods using seawater or ores as naturally occurring raw materials. Among these methods, a method is known in which magnesium oxide is finally obtained by converting mineral resources, dolimes (CaO.MgO) or dolomides (CaMg(CO 3 ) 2 ), into the intermediate product magnesium carbonate.
- Patent Document 1 proposes a method for extracting magnesium oxide from semi-burned dolomite, which includes a slaking/carbonation step, a separation step, and a recovery/calcination step.
- the slaking/carbonation step is a step in which semi-burned dolomite containing 11% or less free calcium oxide and 10% or more free magnesium oxide is added to a solution in which carbon dioxide-containing gas is blown in and stirred, and the semi-burned dolomite is slaking and carbonated.
- the separation step is a step in which the eluted residue, the main component of which is calcium carbonate, is filtered to obtain a filtrate containing the magnesium component of the semi-burned dolomite.
- the recovery/calcination step is a step in which an additive that precipitates magnesium carbonate salt is added to the filtrate to recover the magnesium component as magnesium carbonate salt, and the recovered magnesium carbonate salt is calcined at a temperature above the decomposition temperature to obtain magnesium oxide with a purity of 99% or more by mass. It is said that the magnesium oxide extraction method of Patent Document 1 can obtain high-purity magnesium oxide with a purity of 99% or more by mass.
- Patent Document 2 also proposes a method for removing impurities in a method for producing magnesium carbonate by reacting magnesium hydroxide slurry with carbon dioxide gas.
- the proposed method for removing impurities involves maintaining the pH, which decreases during the carbonation process, at a pH value of 7.6 to 8.0 at which magnesium carbonate does not dissolve 100%, and using the undissolved magnesium produced at the end of carbonation as a precoat agent to filter the reaction liquid after carbonation.
- JP 2014-80347 A Japanese Patent Application Laid-Open No. 63-40722
- magnesium oxide may require extremely high purity with as many impurities removed as possible.
- impurities may still remain, and further improvements in the removal of impurities from magnesium oxide are required.
- the method of Patent Document 2 is diverted as part of a magnesium oxide production method, it remains unclear whether impurities from magnesium oxide can be sufficiently removed.
- the present invention aims to provide a new manufacturing method that can produce magnesium oxide with higher purity.
- This disclosure includes the following aspects:
- the first disclosure relates to a method for producing magnesium oxide.
- the method for producing magnesium oxide of the first disclosure includes the following carbonation step, separation step, crystallization step, and calcination step.
- the carbonation step is a step in which carbon dioxide gas is blown into a suspension of magnesium hydroxide and calcium hydroxide to obtain an aqueous solution of magnesium hydrogen carbonate.
- the separation step is a step of subjecting the aqueous magnesium hydrogen carbonate solution to solid-liquid separation.
- the crystallization step is a step of crystallizing magnesium carbonate from the aqueous solution obtained in the separation step.
- the calcination step is a step of calcining the magnesium carbonate to obtain magnesium oxide.
- the carbonation step is characterized in that the pH of the suspension is adjusted.
- the second disclosure is the manufacturing method of the first disclosure, characterized in that in the carbonation step, the pH of the suspension is adjusted to within a range of 6.0 or more and less than 8.0.
- a third disclosure is the manufacturing method according to the first or second disclosure, characterized in that in the carbonation step, the suspension is heated to a temperature of 0°C or higher and 50°C or lower, and carbon dioxide gas is blown in.
- a fourth disclosure is the manufacturing method according to any one of the first to third disclosures, characterized in that in the carbonation step, the suspension is pressurized.
- a fifth disclosure is the manufacturing method according to any one of the first to fourth disclosures, characterized in that in the carbonation step, the suspension is made of at least one material selected from dolimes and dolomides.
- a sixth disclosure is the manufacturing method according to any one of the first to fifth disclosures, characterized in that in the carbonation step, the concentration of the suspension is 1 to 30 g/L.
- a seventh disclosure is the manufacturing method according to any one of the first to sixth disclosures, characterized in that the crystallization step further includes a heating step in which the crystallized magnesium carbonate is heated.
- An eighth disclosure is the manufacturing method according to the seventh disclosure, characterized in that in the heating step, the magnesium carbonate is heated at a temperature of 50° C. or more and 250° C. or less.
- a ninth disclosure is the manufacturing method according to the seventh or eighth disclosure, characterized in that in the heating step, the magnesium carbonate is heated for a heating time of 1 hour or more and 72 hours or less.
- the present invention provides a new manufacturing method that can produce magnesium oxide with higher purity.
- One embodiment of the present invention is a method for producing magnesium oxide, which includes the following carbonation step, separation step, crystallization step, and calcination step.
- carbonation step carbon dioxide gas is blown into a suspension of magnesium hydroxide and calcium hydroxide to obtain an aqueous magnesium hydrogen carbonate solution.
- separation step the aqueous magnesium hydrogen carbonate solution is subjected to solid-liquid separation.
- crystallization step magnesium carbonate is crystallized from the aqueous solution obtained in the separation step.
- magnesium oxide is obtained by calcining the magnesium carbonate.
- the pH of the suspension is adjusted in the carbonation process.
- the pH of the suspension By adjusting the pH of the suspension in the carbonation process, it is possible to cause impurities contained in the suspension to precipitate as a solid while leaving the magnesium bicarbonate, which is a magnesium component, dissolved.
- the degree of dissolution of the impurities can be determined by the pH of the suspension.
- impurities include Fe, Al, Si, As, and Pb.
- the pH of the suspension can be adjusted according to the types of impurities contained in the suspension or the types of impurities that are to be preferentially removed, so that impurity components with a relatively low tendency to ionize precipitate as a solid.
- the impurities that precipitate as a solid by adjusting the pH of the suspension can be removed by solid-liquid separation in the next separation process.
- the impurities contained in the magnesium bicarbonate after the carbonation process can be sufficiently reduced.
- the magnesium oxide obtained through the subsequent crystallization and firing processes has an extremely low impurity content, resulting in magnesium oxide of higher purity.
- the impurity components can be precipitated as a solid by adjusting the pH according to the type of impurity to be removed.
- the carbonation process and separation process are considered as one set, and these processes may be repeated in multiple sets.
- the pH of the magnesium hydroxide suspension may be adjusted so that it is different for each set.
- the pH of the magnesium hydroxide suspension may be adjusted so that it is the same for each set.
- the manufacturing method of this embodiment has an extremely low impurity content and produces magnesium oxide of higher purity, which has the advantage of contributing to the achievement of the SDGs (Sustainable Development Goals) adopted at the United Nations Summit.
- the magnesium hydroxide and calcium hydroxide suspension that can be used in the manufacturing method of this embodiment is not particularly limited.
- the magnesium hydroxide and calcium hydroxide suspension may be made from at least one material selected from dolimes and dolomides.
- the manufacturing method of this embodiment may include a step of producing a magnesium hydroxide and calcium hydroxide suspension as follows before the carbonation step.
- the process for producing a suspension of magnesium hydroxide and calcium hydroxide may be a process of adding water to at least one selected from dolimes and dolomides to suspend them.
- the water used in this case may be, for example, ion-exchanged water.
- the suspension of magnesium hydroxide and calcium hydroxide obtained by the above production process is then subjected to the carbonation process.
- the carbonation step is a step of blowing carbon dioxide gas into a suspension of magnesium hydroxide and calcium hydroxide to obtain an aqueous magnesium hydrogen carbonate solution.
- the carbon dioxide gas that can be used in the carbonation step may contain other gases within a range that does not inhibit the carbonation of magnesium hydroxide.
- the pH of the suspension is adjusted as described above.
- the pH of the suspension may be adjusted appropriately depending on the type and content of impurities contained in the suspension.
- the pH of the suspension in the carbonation process can be adjusted to less than 8.0, less than 7.6, less than 7.5, or less than 7.4.
- the pH of the suspension in the carbonation process can be adjusted to 6.0 or more, 6.5 or more, 7.0 or more, or 7.1 or more.
- the pH of the suspension it is preferable to adjust the pH of the suspension to within the range of 6.0 or more and less than 8.0.
- the various types of impurities contained in the suspension can be more reliably precipitated.
- magnesium oxide of even higher purity can be obtained.
- both Mg and Ca will dissolve, and there is a risk that calcium carbonate will be incorporated into the magnesium carbonate intermediate product described below. In other words, there is a risk that impurities contained in calcium carbonate will also be incorporated into the magnesium carbonate.
- the pH of the suspension is 8.0 or higher, the amount of magnesium component dissolved will be reduced, and there is a risk that the yield will deteriorate.
- a more preferred upper limit of the pH of the suspension is pH 7.5.
- a more preferred lower limit of the pH of the suspension is 6.5.
- the pH of the suspension can be adjusted by blowing in carbon dioxide gas. Therefore, in the carbonation process, it is preferable to blow in carbon dioxide gas while continuously or intermittently measuring the pH of the suspension.
- the amount of carbon dioxide gas supplied when blowing the carbon dioxide gas into the suspension is not particularly limited.
- the amount of carbon dioxide gas supplied is 5.0 L/min or less.
- the amount of carbon dioxide gas supplied is 0.1 L/min or more.
- a preferred upper limit of the amount of carbon dioxide gas supplied is 3.0 L/min.
- a preferred lower limit of the amount of carbon dioxide gas supplied is 0.2 L/min.
- the amount of carbon dioxide gas supplied is more than 5.0 L/min per 1 L of magnesium hydroxide suspension, the supplied carbon dioxide gas will not dissolve completely in the magnesium hydroxide suspension. If the amount of carbon dioxide gas supplied is less than 0.1 L/min per 1 L of magnesium hydroxide suspension, productivity will decrease.
- the concentration of the suspension is not particularly limited.
- the concentration of the suspension is 30 g/L or less.
- the concentration of the suspension is 1 g/L or more.
- the concentration of the suspension is preferably 28 g/L or less.
- the concentration of the suspension is preferably 3 g/L or more.
- the concentration of the magnesium hydroxide suspension is higher than 30 g/L, the magnesium hydroxide will not dissolve completely, resulting in a reduced yield. If the concentration of the magnesium hydroxide suspension is lower than 1 g/L, productivity will decrease.
- the temperature of the suspension when carbon dioxide gas is blown in is not particularly limited, but it is preferable to blow in carbon dioxide gas at a temperature of 0°C or higher and 50°C or lower during the carbonation process. If the temperature of the suspension is within this range, the multiple types of impurities contained in the suspension can be more reliably precipitated. As a result, magnesium oxide of even higher purity can be obtained.
- the more preferred upper limit of the temperature of the suspension in the carbonation process is 40°C.
- the even more preferred upper limit of the temperature of the suspension in the carbonation process is 30°C.
- the even more preferred lower limit of the temperature of the suspension in the carbonation process is 20°C.
- the carbonation step when blowing carbon dioxide gas into the suspension, it is preferable to pressurize the suspension. Pressurizing the suspension makes it easier for Mg to dissolve, and makes it easier to separate MgO and CaO.
- the pressure of the carbon dioxide gas when pressurizing the suspension can be, for example, 0.01 MPa or more, 0.05 MPa or more, or 0.1 MPa or more.
- the pressure of the carbon dioxide gas when pressurizing the suspension can be, for example, 10 MPa or less, 5 MPa or less, or 1 MPa or less.
- the aqueous magnesium bicarbonate solution after the carbon dioxide gas has been blown in contains undissolved magnesium carbonate. If the aqueous magnesium bicarbonate solution after the carbon dioxide gas has been blown in contains such undissolved magnesium carbonate, solid-liquid separation after the carbonation process becomes easier. As a result, magnesium oxide of higher purity can be obtained.
- carbon dioxide gas may be blown into the suspension, followed by air.
- carbon dioxide gas By first blowing carbon dioxide gas into the suspension, the magnesium components are dissolved while the impurity Fe is precipitated. Next, by blowing air into the suspension, the still dissolved Fe can be precipitated as FeO. This makes it possible to obtain magnesium oxide of even higher purity, with Fe as an impurity further reduced.
- the impurities that precipitate as solids during the carbonation process described above can be removed by solid-liquid separation in the next separation process.
- the aqueous magnesium hydrogen carbonate solution obtained by the carbonation process is subjected to the next separation process.
- the separation step is a step of performing solid-liquid separation of the aqueous magnesium hydrogen carbonate solution after the carbonation step. More specifically, the separation step is a step of separating the aqueous magnesium hydrogen carbonate solution, which is a liquid component, from impurities, which are solid components. This step removes the impurities from the aqueous magnesium hydrogen carbonate solution, thereby obtaining an aqueous magnesium hydrogen carbonate solution with high purity.
- separation includes cases where the solid and liquid components are completely separated, as well as cases where the solid components contain a small amount of unavoidable moisture.
- separation means there are no particular limitations on the separation means that can be used in the separation process, and examples include filtration means, membrane separation means, centrifugation means, solid-liquid separation means, and natural settling means.
- the separation step may use the aqueous magnesium bicarbonate solution after the carbonation step as is, but is not limited to this form.
- the separation step may be performed in advance by adding water to the aqueous magnesium bicarbonate solution to adjust the concentration.
- the water used in this case may be, for example, ion-exchanged water.
- the separation step may be performed only once, or may be performed in multiple steps, two or more.
- the magnesium bicarbonate solution from which impurities have been removed by the above separation process is then sent to the next crystallization process.
- the crystallization step is a step of crystallizing magnesium carbonate from the aqueous solution obtained in the separation step.
- the means for crystallizing magnesium carbonate from the aqueous solution after the separation step is not particularly limited, and may be, for example, a heating means. That is, in the crystallization step, magnesium carbonate can be crystallized by heating the aqueous solution after the separation step.
- the heating temperature when crystallizing magnesium carbonate is not particularly limited, and may be, for example, a temperature of 30°C or higher.
- the preferred lower limit of the heating temperature is 50°C.
- the preferred upper limit of the heating temperature when crystallizing magnesium carbonate is not particularly limited, and may be, for example, 100°C.
- the preferred upper limit of the heating temperature is 95°C.
- the "heating temperature when crystallizing magnesium carbonate” may be referred to as the "crystallization temperature" to distinguish it from the heating temperature in the heating step described below.
- the shape of magnesium carbonate crystals is inherited by the shape of magnesium oxide crystals produced by calcining it. In other words, by improving the handling properties of magnesium carbonate, the handling properties of the final magnesium oxide can be improved.
- the heating time for crystallizing magnesium carbonate is not particularly limited, and may be, for example, 1 minute or more.
- the preferable lower limit of the heating time for crystallizing magnesium carbonate is 15 minutes.
- the upper limit of the heating time for crystallizing magnesium carbonate is not particularly limited, but from the viewpoint of productivity, it is, for example, 600 minutes, and more preferably 180 minutes.
- the "heating time for crystallizing magnesium carbonate” may be referred to as the "crystallization time" to distinguish it from the heating time of the heating step described later.
- this crystallization time means the time from the point at which the aqueous solution after the separation step is heated to the crystallization temperature and the temperature is maintained.
- the crystallization step may further include a heating step of heating the crystallized magnesium carbonate.
- a heating step of heating the crystallized magnesium carbonate By heating the crystallized magnesium carbonate, the needle-like crystals of magnesium carbonate become plate-like crystals. This reduces the bulk of magnesium carbonate, improving the handleability of magnesium carbonate.
- the heating temperature of magnesium carbonate is not particularly limited, and may be, for example, a temperature of 50° C. or more and 250° C. or less. From the viewpoint of the handleability of magnesium carbonate, the preferable lower limit of the heating temperature is 60° C. From the viewpoint of the handleability or productivity of magnesium carbonate, the preferable upper limit of the heating temperature is 150° C.
- the heating time of magnesium carbonate is not particularly limited, but may be, for example, 1 hour or more and 72 hours or less. From the viewpoint of handling of magnesium carbonate, the preferable lower limit of the heating time is 3 hours. From the viewpoint of handling or productivity of magnesium carbonate, the preferable upper limit of the heating time is 48 hours.
- the aqueous solution containing the crystallized magnesium carbonate can be subjected to solid-liquid separation to obtain magnesium carbonate as a solid.
- the crystallization process may further include a step of performing solid-liquid separation of the aqueous solution containing the crystallized magnesium carbonate to obtain magnesium carbonate as a solid.
- the means for performing solid-liquid separation of the aqueous solution containing crystallized magnesium carbonate is not particularly limited, and for example, the same separation means as those used in the separation process described above can be used.
- a washing process for the crystallized magnesium carbonate may be carried out if necessary.
- the magnesium carbonate obtained through the above crystallization process is then subjected to the next firing process.
- the calcination step is a step in which the magnesium carbonate obtained in the crystallization step is calcined to obtain magnesium oxide.
- the calcination method for calcining magnesium carbonate is not particularly limited as long as it can produce magnesium oxide.
- Examples of such calcination methods include those using a calcination furnace or microwaves.
- the calcination temperature when calcining magnesium carbonate is not particularly limited as long as it is a temperature at which magnesium oxide can be produced.
- Examples of such a calcination temperature include temperatures of 500°C or higher.
- the upper limit of the calcination temperature is not particularly limited, but is, for example, 1500°C from the viewpoint of the quality or productivity of magnesium oxide.
- the calcination temperature is preferably 700°C or higher. Also, the calcination temperature is preferably 1200°C or lower.
- the firing time when firing magnesium carbonate is not particularly limited as long as it is a time that can produce magnesium oxide.
- An example of such a firing time is 1 minute or more.
- the magnesium oxide obtained by the above firing process may be subjected to additional treatment processes as necessary.
- additional treatment processes include a surface treatment process in which the surface of magnesium oxide particles is treated with various surface treatment agents, a crushing process in which magnesium oxide is crushed into powder, a classification process in which magnesium oxide is classified by particle size, and a molding process in which magnesium oxide is molded into a predetermined shape.
- the manufacturing method of this embodiment described above allows for the production of magnesium oxide with extremely low impurity content and higher purity.
- Example 1 A pressure vessel having a volume of 0.98 L was prepared and a suspension of magnesium hydroxide and calcium hydroxide was placed in the pressure vessel. Carbon dioxide gas was blown into the pressure vessel at a partial pressure of 0.20 MPa for 70 minutes while stirring the suspension of magnesium hydroxide and calcium hydroxide, to obtain an aqueous magnesium hydrogen carbonate solution.
- the resulting magnesium bicarbonate aqueous solution was subjected to solid-liquid separation using a Nutsche separator to remove solid impurities. The solution was then heated to 90°C and held at that temperature for 60 minutes to precipitate magnesium carbonate. The solution was then filtered to obtain a solid magnesium carbonate. The resulting solid was heated at 105°C for 24 hours to obtain magnesium carbonate powder.
- a crucible for firing was prepared and magnesium carbonate was placed in it. This crucible was then placed in a firing furnace that had been preheated to 900°C. After placement, the crucible was fired at 900°C for 2 hours under atmospheric pressure to obtain a fired magnesium oxide product. The resulting fired product was sieved through a 150 micron filter to obtain the magnesium oxide powder of Example 1.
- the magnesium oxide manufacturing method of Example 1 was found to produce magnesium oxide with fewer impurities.
- the magnesium oxide manufacturing method of the present invention can be suitably used to manufacture magnesium oxide that can be used for various applications, such as pharmaceuticals, foods, vulcanization accelerators, pigments, chemical heat storage materials, battery materials, ceramic materials, adsorbents, abrasives, and catalysts.
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Physics & Mathematics (AREA)
- Thermal Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Geology (AREA)
- Inorganic Chemistry (AREA)
- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
Abstract
La présente invention concerne une nouvelle méthode de production avec laquelle de l'oxyde de magnésium ayant une pureté plus élevée peut être obtenu. La présente invention concerne une méthode de production d'oxyde de magnésium. Une méthode de production d'oxyde de magnésium selon la présente invention comprend : une étape de carbonatation ; une étape de séparation ; une étape de cristallisation ; et une étape de cuisson. L'étape de carbonatation est destinée à souffler du dioxyde de carbone gazeux dans un liquide de suspension d'hydroxyde de magnésium et d'hydroxyde de calcium pour obtenir une solution aqueuse d'hydrogénocarbonate de magnésium. L'étape de séparation consiste à soumettre la solution aqueuse d'hydrogénocarbonate de magnésium à une séparation solide-liquide. L'étape de cristallisation est destinée à cristalliser du carbonate de magnésium à partir de la solution aqueuse obtenue dans l'étape de séparation. L'étape de cuisson consiste à cuire le carbonate de magnésium pour obtenir de l'oxyde de magnésium. De plus, la présente invention est caractérisée en ce que le pH du liquide de suspension est ajusté dans l'étape de carbonatation.
Applications Claiming Priority (2)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
JP2022178400 | 2022-11-07 | ||
JP2022-178400 | 2022-11-07 |
Publications (1)
Publication Number | Publication Date |
---|---|
WO2024101158A1 true WO2024101158A1 (fr) | 2024-05-16 |
Family
ID=91032664
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
PCT/JP2023/038523 WO2024101158A1 (fr) | 2022-11-07 | 2023-10-25 | Méthode de production d'oxyde de magnésium |
Country Status (1)
Country | Link |
---|---|
WO (1) | WO2024101158A1 (fr) |
Citations (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JPS5860616A (ja) * | 1981-10-07 | 1983-04-11 | Toyo Denka Kogyo Kk | 高純度酸化マグネシウムの製造方法 |
JP2004059378A (ja) * | 2002-07-30 | 2004-02-26 | Nittetsu Mining Co Ltd | 塩基性炭酸マグネシウムの製造方法及び該塩基性炭酸マグネシウムを含有する組成物又は構造体 |
CN101648721A (zh) * | 2009-08-31 | 2010-02-17 | 吉林大学 | 制备纳米氧化镁和活性轻质碳酸钙的方法 |
CN108529653A (zh) * | 2018-05-24 | 2018-09-14 | 中南大学 | 以白云石为原料制备高纯氧化镁的装置及其方法和应用 |
CN113149042A (zh) * | 2021-04-02 | 2021-07-23 | 河北化工医药职业技术学院 | 高活性氧化镁的制备方法 |
-
2023
- 2023-10-25 WO PCT/JP2023/038523 patent/WO2024101158A1/fr unknown
Patent Citations (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JPS5860616A (ja) * | 1981-10-07 | 1983-04-11 | Toyo Denka Kogyo Kk | 高純度酸化マグネシウムの製造方法 |
JP2004059378A (ja) * | 2002-07-30 | 2004-02-26 | Nittetsu Mining Co Ltd | 塩基性炭酸マグネシウムの製造方法及び該塩基性炭酸マグネシウムを含有する組成物又は構造体 |
CN101648721A (zh) * | 2009-08-31 | 2010-02-17 | 吉林大学 | 制备纳米氧化镁和活性轻质碳酸钙的方法 |
CN108529653A (zh) * | 2018-05-24 | 2018-09-14 | 中南大学 | 以白云石为原料制备高纯氧化镁的装置及其方法和应用 |
CN113149042A (zh) * | 2021-04-02 | 2021-07-23 | 河北化工医药职业技术学院 | 高活性氧化镁的制备方法 |
Similar Documents
Publication | Publication Date | Title |
---|---|---|
EP1097247B1 (fr) | Procede d'isolation et de production de produits a base de magnesium | |
US4298379A (en) | Production of high purity and high surface area magnesium oxide | |
US8603428B2 (en) | Method of producing calcium carbonate from waste and by-products | |
KR101502592B1 (ko) | 실리카 및 마그네시아 추출을 위한 슬래그의 처리방법 | |
US20220185689A1 (en) | Process for preparing alumina | |
JP5044925B2 (ja) | 純度の高い炭酸カルシウムの製造方法 | |
JPH0260606B2 (fr) | ||
US4871519A (en) | Method of making magnesium oxide and hydrates thereof | |
AU2022230558A1 (en) | Method of preparing alumina | |
JP5389491B2 (ja) | 高純度炭酸カルシウムの製造方法 | |
EA010106B1 (ru) | Способ комплексного использования составляющих оливина | |
WO2024101158A1 (fr) | Méthode de production d'oxyde de magnésium | |
CA1079932A (fr) | Methode de recuperation de la magnesie contenue dans les briques mises au rebut | |
WO2024101157A1 (fr) | Méthode de production d'oxyde de magnésium | |
CN112520777A (zh) | 一种利用钛白副产盐酸渣水制取氯化钙的工艺 | |
US4179490A (en) | Preparation of pure magnesian values | |
JP2011051835A (ja) | 高純度炭酸カルシウムの製造方法 | |
KR101120106B1 (ko) | 슬래그를 이용한 염화칼슘의 제조방법 | |
KR20010083819A (ko) | 탄산칼슘의 제조 방법 | |
JP2024162738A (ja) | 酸化マグネシウムの製造方法 | |
WO1983000142A1 (fr) | Production d'oxyde de magnesium | |
KR102738320B1 (ko) | 백운석으로부터 고순도 산화마그네슘을 제조하는 방법 | |
RU2513652C2 (ru) | Способ получения оксида магния | |
KR100600806B1 (ko) | 회수율 및 순도가 우수한 마그네시아 제조방법 | |
CA1072297A (fr) | Recuperation du magnesium en solution aqueuse |
Legal Events
Date | Code | Title | Description |
---|---|---|---|
121 | Ep: the epo has been informed by wipo that ep was designated in this application |
Ref document number: 23888506 Country of ref document: EP Kind code of ref document: A1 |