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WO2019044121A1 - Poudre de carbonate de magnésium basique hautement dispersée, et sa méthode de production - Google Patents

Poudre de carbonate de magnésium basique hautement dispersée, et sa méthode de production Download PDF

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Publication number
WO2019044121A1
WO2019044121A1 PCT/JP2018/022917 JP2018022917W WO2019044121A1 WO 2019044121 A1 WO2019044121 A1 WO 2019044121A1 JP 2018022917 W JP2018022917 W JP 2018022917W WO 2019044121 A1 WO2019044121 A1 WO 2019044121A1
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basic magnesium
powder
highly dispersed
magnesium carbonate
carbonate powder
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Japanese (ja)
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将志 中村
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Konoshima Chemical Co Ltd
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Konoshima Chemical Co Ltd
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    • A—HUMAN NECESSITIES
    • A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23L—FOODS, FOODSTUFFS OR NON-ALCOHOLIC BEVERAGES, NOT OTHERWISE PROVIDED FOR; PREPARATION OR TREATMENT THEREOF
    • A23L29/00—Foods or foodstuffs containing additives; Preparation or treatment thereof
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00—Cosmetics or similar toiletry preparations
    • A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/19—Cosmetics or similar toiletry preparations characterised by the composition containing inorganic ingredients
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61Q—SPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
    • A61Q1/00—Make-up preparations; Body powders; Preparations for removing make-up
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61Q—SPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
    • A61Q19/00—Preparations for care of the skin
    • 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
    • C01F5/24—Magnesium carbonates
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00—Use of inorganic substances as compounding ingredients
    • C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
    • C08K3/24—Acids; Salts thereof
    • C08K3/26—Carbonates; Bicarbonates
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L101/00—Compositions of unspecified macromolecular compounds
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D201/00—Coating compositions based on unspecified macromolecular compounds
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
    • C09D7/40—Additives
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
    • C09D7/40—Additives
    • C09D7/60—Additives non-macromolecular
    • C09D7/61—Additives non-macromolecular inorganic

Definitions

  • the present invention relates to highly dispersed basic magnesium carbonate and a method of producing the same.
  • Basic magnesium carbonate has properties such as poor water solubility, oil absorption, and thickening properties, and is used in various fields as additives for paints, foods, medicines, cosmetics, rubber, paper, and the like.
  • basic magnesium carbonate powder is in the form of aggregates or aggregates of flaky primary particles, and the form of aggregation or aggregation is controlled depending on the use (eg, Patent Documents 1 and 2).
  • Patent Documents 1 and 2 With regard to natural basic magnesium carbonate, the size of primary particles is relatively large, and the variation in size is large, making it difficult to develop applications.
  • the basic magnesium carbonate powder has a form in which primary particles are aggregated, a decrease in properties due to the form may be observed when applied to each use.
  • the heat resistance and color of the paint deteriorate as the amount added increases, and when added to cosmetics, the smoothness decreases, and it is used for food, paint, medicine, etc.
  • the particles settle with time in water to cause phase separation, which affects the handling and the uniformity of quality during production and use.
  • An object of the present invention is to provide a highly dispersed basic magnesium carbonate powder which can suppress the aggregation of primary particles and can be developed for various uses, and a method for producing the same.
  • the present invention relates to a highly dispersed basic magnesium carbonate powder having a sedimentation volume of 60 mL or more obtained by measurement under the following measurement conditions.
  • Measurement conditions of sedimentation volume 5 g of the basic magnesium carbonate powder is put into a 100 mL measuring cylinder with a lid, and then the pure water is weighed to 100 mL, mixed, and allowed to stand for 2 hours at 20 ° C. The volume occupied by the powder dispersed phase in the phase is measured as settling volume (mL).
  • the present inventors have found that the sedimentation volume of a basic magnesium carbonate powder correlates well with the cohesion of primary particles, and completed the present invention.
  • the highly dispersed basic magnesium carbonate powder hereinafter, also referred to as "highly dispersed powder”
  • the sedimentation volume is in the above range, the aggregation of the primary particles is suppressed, in other words, the dispersion at the primary particle level is achieved.
  • a highly dispersed powder suitable for various application development can be obtained. If the sedimentation volume is less than the above range, the degree of aggregation of primary particles may be increased, which may cause the problems observed in conventional low-dispersion basic magnesium carbonate powders.
  • the degree of dispersion represented by the following formula is preferably 6 or more.
  • Degree of dispersion (d L / d 50 ) ⁇ 100 (Wherein, d L is the average major axis ( ⁇ m) of primary particles obtained using a SEM photograph, and d 50 is the cumulative 50% diameter ( ⁇ m on a volume basis) in the particle size distribution obtained by a laser diffraction particle size distribution analyzer )))
  • the average particle size (average major axis d L ) of the primary particles can be determined regardless of the presence or absence of aggregation of the primary particles.
  • a value (d 50 ) including the particle diameter of any of primary particles and secondary particles which are aggregates of primary particles can be obtained, and generally d L 50 is a larger value.
  • d 50 can be treated as an index of secondary particle diameter. Therefore, if the primary particles are dispersed as they are without aggregation, d L and d 50 approximate each other, and the degree of dispersion represented by the above equation also increases.
  • the dispersion degree represented by the said Formula is made into the said range, aggregation (formation of secondary particle) of a primary particle is suppressed, and a primary particle can exhibit the state with high dispersibility.
  • the highly dispersed powder preferably has a cumulative 50% diameter (d 50 ) on a volume basis of 7 ⁇ m or less in a particle size distribution obtained by a laser diffraction type particle size distribution analyzer.
  • d 50 cumulative 50% diameter
  • the high dispersion powder despite the smaller the cumulative 50% diameter (d 50), since aggregation of the primary particles is suppressed, can be performed widely efficiently expansion into various applications .
  • the highly dispersed powder preferably has a BET specific surface area of 50 m 2 / g or less.
  • the BET specific surface area of the aggregates tends to be high.
  • the present invention provides, in a further embodiment, a method of producing the highly dispersed basic magnesium carbonate powder, wherein A preparation step of preparing a raw material dispersion in which a raw material basic magnesium carbonate powder having a sedimentation volume of less than 60 mL is dispersed in a dispersion medium, and hydrothermal treatment of the raw material dispersion at a temperature of 150 ° C. or less to obtain a treated dispersion.
  • the present invention relates to a method for producing a highly dispersed basic magnesium carbonate powder including the steps.
  • the said manufacturing method it is relatively low temperature of 150 degrees C or less with respect to the dispersion liquid of the raw material basic magnesium carbonate powder (Hereafter, it is also called “raw material powder”) with relatively large abundance of the aggregate of primary particles.
  • a highly dispersed powder can be efficiently produced only by subjecting it to hydrothermal treatment. Although the reason for this is not clear, it is presumed as follows. By performing predetermined hydrothermal treatment, aggregation of primary particles in the raw material powder is gradually loosened while suppressing undesired decomposition reaction (described later) of the raw material powder, and a state in which the primary particles are dispersed individually is obtained.
  • a high dispersion state at the primary particle level which can not be obtained merely by pulverizing the dry powder, will be achieved by the destruction or separation of aggregates of primary particles that have undergone a predetermined hydrothermal treatment.
  • the hydrothermal treatment is carried out at a temperature exceeding 150 ° C., the decomposition reaction of the raw material powder proceeds and it becomes a mixed phase in which anhydrous magnesium carbonate and magnesium hydroxide coexist, and the target basic magnesium carbonate powder is obtained. It will not be possible.
  • the said hydrothermal treatment it is preferable to perform the said hydrothermal treatment at the temperature of 100 degreeC or more and 150 degrees C or less.
  • the manufacturing method may further include a drying step of filtering the treated dispersion after the hydrothermal step and drying the filtered powder. Thereby, the dried highly dispersed powder can be suitably manufactured.
  • the present invention relates, in one embodiment, to a powder suspension composition containing 0.1 to 100 parts by mass of the highly dispersed basic magnesium powder with respect to 100 parts by mass of a solvent.
  • the powder suspension composition is suitably used as a cosmetic, a food or a paint.
  • the present invention relates, in one embodiment, to a powdery cosmetic comprising the highly dispersed basic magnesium powder in a blending amount of 0.5% by weight or more and 80% by weight or less.
  • the present invention relates, in another embodiment, to a polymer composition in which 1 to 500 parts by mass of the highly dispersed basic magnesium powder is blended with 100 parts by mass of the polymer material.
  • the said polymeric material is resin, rubber
  • Example 3 is a SEM photograph of the basic magnesium carbonate of Example 1.
  • 5 is a SEM photograph of the basic magnesium carbonate of Comparative Example 1;
  • the sedimentation volume obtained by measurement under the following measurement conditions is 60 mL or more.
  • Measurement conditions of sedimentation volume Charge 5 g of basic magnesium carbonate powder into a 100 mL measuring cylinder with a lid, measure up to 100 mL of pure water, mix, and separate from the powder dispersed phase and the pure water phase after standing for 2 hours at 20 ° C. Measure the volume occupied by the powder dispersed phase in as the sedimentation volume (mL).
  • the highly dispersed powder since the highly dispersed powder has a sedimentation volume in the above range, aggregation of primary particles can be suppressed to achieve a dispersed state at the primary particle level. Thereby, a highly dispersed powder suitable for various application development can be obtained.
  • the sedimentation volume may be 60 mL or more, 70 mL or more is preferable, 80 mL or more is more preferable, and 85 mL or more is particularly preferable.
  • the sedimentation volume may be approximately 100 mL or less when the powder dispersed phase is in the form of a colloid, or may be 98 mL or less in consideration of handling properties and the like.
  • the degree of aggregation of primary particles may be increased, which may cause the problems observed in conventional low-dispersion basic magnesium carbonate powders.
  • the pure water phase after mixing and leaving the powder and pure water contains substantially no basic magnesium carbonate powder, it contains a small amount of powder which is difficult to distinguish by ordinary visual inspection. It is also good. Even in this case, the distinction between the powder dispersed phase and the pure water phase can be easily made visually.
  • the degree of dispersion represented by the following formula is preferably 6 or more, more preferably 8 or more, further preferably 10 or more, and particularly preferably 15 or more.
  • Degree of dispersion (d L / d 50 ) ⁇ 100 (Wherein, d L is the average major axis ( ⁇ m) of primary particles obtained using a SEM photograph, and d 50 is the cumulative 50% diameter ( ⁇ m on a volume basis) in the particle size distribution obtained by a laser diffraction particle size distribution analyzer ))))
  • the degree of dispersion of the highly dispersed powder is in the above range, the aggregation of primary particles (formation of secondary particles) is suppressed, and the primary particles can exhibit a highly dispersed state.
  • the higher the degree of dispersion the better, but from the viewpoint of simplification of the process of cohesive failure of primary particles and physical limitations, 90 or less is preferable, and 80 or less is more preferable.
  • the highly dispersed powder preferably has a cumulative 50% diameter (d 50 ) on a volume basis of 7 ⁇ m or less, more preferably 5 ⁇ m or less, still more preferably 4 ⁇ m or less, in the particle size distribution obtained by a laser diffraction particle size distribution analyzer. Particularly preferred is 3.5 ⁇ m or less.
  • the cumulative 50% diameter (d 50 ) is preferably 0.1 ⁇ m or more, more preferably 0.3 ⁇ m or more, and still more preferably 0.5 ⁇ m or more from the viewpoint of handling properties and the like.
  • the standard deviation in the particle size distribution obtained by the laser diffraction particle size distribution analyzer is not particularly limited, but is preferably 9 ⁇ m or less, more preferably 8 ⁇ m or less, and 5 ⁇ m or less More preferably, 3 ⁇ m or less is particularly preferred.
  • the standard deviation is obtained by the following equation.
  • Standard deviation (d 84- d 16 ) / 2 (Wherein, d 84 is the cumulative 84% diameter on a volume basis in the particle size distribution obtained by a laser diffraction particle size distribution analyzer, and d 16 is the accumulation on a volume basis in the particle size distribution obtained by a laser diffraction particle size distribution analyzer 16% diameter)
  • BET specific surface area of the highly dispersed powder is preferably not more than 50 m 2 / g, more preferably not more than 40m 2 / g, 30m 2 / g more preferably less, and particularly preferably less 20 m 2 / g .
  • the smaller the BET specific surface area the larger the size of the plate-like primary particles, and the firmer the structure of the primary particles along with that, the water is easily held or fixed between the plate-like primary particles, and the high dispersion is achieved. The state can be achieved.
  • 10 m 2 / g or more is preferable, and 15 m 2 / g or more of the BET specific surface area is more preferable.
  • the BET specific surface area of anhydrous magnesium carbonate is low, and when anhydrous magnesium carbonate is produced as a by-product in the production of a highly dispersed powder, the BET specific surface area is lowered.
  • Magnesite is a cubic particle, and since there is no void between primary particles such as basic magnesium carbonate, water can not be held or fixed between primary particles, and as a result, high dispersibility is achieved. It can not be done. Therefore, the BET specific surface area is preferably in the above range from the viewpoint of suppressing the formation of anhydrous magnesium carbonate.
  • the apparent specific gravity of the high dispersion powder is preferably 0.28 g / mL or less, more preferably 0.25 g / mL or less, still more preferably 0.22 g / mL or less, particularly 0.2 g / mL or less preferable. 0.15 g / mL or more is preferable and, as for the apparent specific gravity of highly dispersed powder, 0.16 g / mL or more is more preferable.
  • the apparent specific gravity can be measured according to JIS K 6220-1: 2001.
  • the average major axis of the primary particles obtained in the SEM photograph is preferably 0.1 ⁇ m or more, more preferably 0.2 ⁇ m or more, and 0.3 ⁇ m or more. Is more preferable, and 0.4 ⁇ m or more is particularly preferable.
  • the average major axis of the primary particles is preferably 2 ⁇ m or less, more preferably 2.5 ⁇ m or less, and still more preferably 2 ⁇ m or less.
  • the average thickness of the primary particles obtained in the SEM photograph is preferably 0.001 ⁇ m or more, more preferably 0.005 ⁇ m or more, and 0.01 ⁇ m or more. Is more preferable, and particularly preferably 0.015 ⁇ m or more.
  • the average thickness of the primary particles is preferably 0.5 ⁇ m or less, more preferably 0.3 ⁇ m or less, and still more preferably 0.2 ⁇ m or less.
  • the aspect ratio of primary particles represented by the following formula is preferably 5 or more, more preferably 6 or more, still more preferably 7 or more, and particularly preferably 8 or more.
  • the aspect ratio is preferably 30 or less, more preferably 25 or less, and still more preferably 20 or less.
  • Ask ratio average major diameter of primary particles ( ⁇ m) / average thickness of primary particles ( ⁇ m)
  • the average crystallite diameter of the primary particles obtained by X-ray diffraction is not particularly limited, but is preferably 110 ⁇ to 200 ⁇ , more preferably 120 ⁇ to 190 ⁇ , and more preferably 130 ⁇ to 180 ⁇ . More preferably, 140 ⁇ or more and 180 ⁇ or less are particularly preferable.
  • the average crystallite diameter of the primary particles is in the above range, the heat resistance of the highly dispersed powder can be improved.
  • Basic magnesium carbonate is a compound represented by the following chemical formula. x MgCO 3 ⁇ Mg (OH) 2 ⁇ yH 2 O (Wherein, x is an integer of 3 to 5 and y is an integer of 3 to 8)
  • the highly dispersed powder of the present embodiment contains basic magnesium carbonate as a main component. 95% or more is preferable, as for the ratio of basic magnesium carbonate, 98% or more is more preferable, and 99% or more is more preferable.
  • highly dispersed powder may contain the unavoidable impurity component originating in a raw material, a manufacturing method, etc.
  • the impurity component is, for example, Ca, S, Si or the like.
  • the content of these impurities is preferably 0.3% by mass or less in the highly dispersed powder in terms of each element.
  • the shape of the primary particles of the highly dispersed powder of the present embodiment is mainly plate-like, but may be cubic, indeterminate, needle-like or the like in part.
  • the application of the highly dispersed powder of the present embodiment is not particularly limited.
  • a powder suspension in which 0.1 to 100 parts by mass, preferably 1 to 50 parts by mass of the highly dispersed basic magnesium powder of the present embodiment is blended with 100 parts by mass of a solvent A turbid composition can be suitably employed.
  • a solvent it can select suitably according to the use of a powder suspension composition, For example, organic solvents, such as water and alcohol (for example, ethanol etc.), acetone, toluene, etc. are mentioned.
  • organic solvents such as water and alcohol (for example, ethanol etc.), acetone, toluene, etc. are mentioned.
  • the use of this powder suspension composition is not particularly limited, but it is suitable as a cosmetic, food or paint because the highly dispersed powder is plate-like and has hiding power, oil absorption, thickening properties and high smoothness. Used.
  • the highly dispersed powder of the present embodiment has excellent smoothness, it can also be used as a base material for powdery cosmetics.
  • 0.5 weight%-80 weight% are preferable, and, as for the compounding quantity of highly dispersed powder, 1 weight%-50 weight% is more preferable.
  • a polymer composition in which 1 to 500 parts by mass, preferably 5 to 300 parts by mass of the highly dispersed basic magnesium powder of the present embodiment is blended with 100 parts by mass of the polymer material is preferably listed.
  • the polymeric material may be either a natural polymeric material or a synthetic polymeric material, and is preferably a resin, rubber or paper (pulp).
  • the highly dispersed powder is in the form of a plate, and has heat resistance and smoothness, so it can be suitably used as a reinforcing filler for products using these polymer materials.
  • the gas method will be described as a representative example.
  • the magnesium hydroxide powder is dispersed in water to prepare a slurry.
  • the slurry concentration may be set in consideration of the reaction efficiency with the carbon dioxide gas in the next step, etc., and is about 10 to 80 g / L, preferably about 20 to 60 g / L as the MgO concentration.
  • This slurry is heated to about 50 to 100 ° C., preferably about 60 to 80 ° C., carbon dioxide gas is blown into the slurry, and basic magnesium carbonate is obtained by carbonation reaction of magnesium hydroxide and carbon dioxide gas. it can.
  • the flow rate of carbon dioxide gas may be appropriately set in consideration of reaction efficiency and the like, and is generally 10 to 50 L / min, preferably about 20 to 40 L / min.
  • the raw material powder After completion of the carbonation reaction, the raw material powder can be obtained by dehydration and drying.
  • the raw material powder is dispersed in a dispersion medium to prepare a raw material dispersion.
  • Water is preferred as the dispersion medium.
  • the concentration of the raw material powder can be set according to the efficiency, yield, etc. of the hydrothermal reaction in the next step, and is preferably 15 to 70 g / L, more preferably 20 to 60 g / L, and more preferably 25 to 50 g in terms of MgO concentration. / L is more preferable.
  • a known mixer equipped with a stirring blade can be used for dispersing the raw material powder.
  • a raw material dispersion is obtained by sufficiently stirring and mixing water and raw material powder in a mixer.
  • the temperature during dispersion may be room temperature or may be heated at a temperature of 100 ° C.
  • the slurry after carbonation reaction of magnesium hydroxide can be used as a raw material dispersion liquid as it is.
  • the concentration of the raw material powder may be adjusted to a predetermined range by increasing or decreasing the water content.
  • the raw material dispersion is hydrothermally treated at a temperature of 150 ° C. or less to obtain a treated dispersion.
  • the aggregation of the primary particles in the raw material powder is gradually loosened while the undesirable decomposition reaction (decomposition to anhydrous magnesium carbonate and magnesium hydroxide) of the raw material powder is suppressed, and the primary particles are dispersed individually Can be obtained.
  • crystal growth in primary particles can be promoted, and the crystallite diameter can be increased.
  • the hydrothermal treatment can be carried out by stirring the raw material dispersion under heating conditions in a known pressure resistant heating vessel such as an autoclave.
  • the heating temperature is 150 ° C. or less.
  • the heating temperature is 100 ° C. to 150 ° C., more preferably 120 ° C. to 150 ° C., still more preferably 130 ° C. to 150 ° C., particularly preferably 140 ° C. to 150 ° C. is there.
  • the temperature of the hydrothermal treatment exceeds 150 ° C., the decomposition reaction of the raw material powder proceeds to become a mixed phase in which anhydrous magnesium carbonate and magnesium hydroxide co-exist, and the target basic magnesium carbonate powder can not be obtained.
  • the time of the hydrothermal treatment is set in a range to sufficiently advance the cohesive failure of the primary particles and to suppress the decomposition reaction of the raw material powder due to the long time treatment, and is about 1 to 12 hours, preferably about 2 to 8 hours, Preferably, it is about 2.5 to 6 hours.
  • the treatment dispersion containing the highly dispersed powder may be filtered, and the dried powder may be dried.
  • filtration and dehydration may be performed while pressurizing with a known filter press.
  • the pressure at the time of dehydration can be set appropriately, and is generally about 0.5 to 10 MPa, preferably 1 to 6 MPa, and more preferably 1.5 to 4 MPa.
  • the filtered powder is then dried in a dryer.
  • a well-known thing can be used for a dryer, for example, a hot-air dryer, an infrared dryer, a vacuum dryer etc. are mentioned.
  • the drying temperature is preferably 50 to 150 ° C., more preferably 70 to 140 ° C., still more preferably 80 to 130 ° C., and particularly preferably 90 to 120 ° C.
  • the drying time is about 1 to 20 hours, preferably 3 to 18 hours, more preferably 6 to 15 hours.
  • Example 1 In a reaction container equipped with a stirring blade, 80 L of magnesium hydroxide slurry with an MgO concentration of 40 g / L was heated to 70 ° C., and carbon dioxide gas was blown at a gas flow rate of 30 L / min while stirring to carry out a carbonation reaction. Phenolphthalein was added to the slurry, and the reaction was terminated when the color changed from pink to colorless. When the end was reached, the carbon dioxide gas blowing was stopped. Thereby, a slurry of raw material basic magnesium carbonate powder was obtained. Thereafter, water was added to adjust the concentration of basic magnesium carbonate to 35 g / L in terms of MgO concentration to obtain a raw material dispersion.
  • 70 L of the raw material dispersion liquid with an MgO concentration of 35 g / L was placed in a stirrer-equipped autoclave with a capacity of 100 L, and subjected to hydrothermal treatment at a temperature of 150 ° C. for 4 hours while stirring to obtain a treated dispersion.
  • the treated dispersion was then transferred to a filter press and dewatered by applying a pressure of 2.5 MPa for 3 minutes.
  • the dewatered powder was allowed to stand and dried for 12 hours in a dryer set at 105 ° C. to obtain a highly dispersed basic magnesium carbonate powder.
  • Example 2 A highly dispersed basic magnesium carbonate powder was produced in the same manner as in Example 1 except that the temperature of the hydrothermal treatment was 140 ° C.
  • Example 3 A highly dispersed basic magnesium carbonate powder was produced in the same manner as in Example 1 except that the temperature of the hydrothermal treatment was set to 120 ° C.
  • Example 4 A highly dispersed basic magnesium carbonate powder was produced in the same manner as in Example 1 except that the temperature of the hydrothermal treatment was set to 100 ° C.
  • Example 1 A basic magnesium carbonate powder was produced in the same manner as in Example 1 except that the raw material dispersion was dewatered and dried, and the hydrothermal treatment was not performed.
  • Example 2 A basic magnesium carbonate powder was produced in the same manner as in Example 1 except that the temperature of the hydrothermal treatment was set to 80 ° C.
  • Sedimentation Volume 5 g of basic magnesium carbonate powder was charged into a 100 mL measuring cylinder with a lid, and pure water was poured in to make up 100 mL.
  • the lid of the measuring cylinder was closed and shaken for about 1 minute with a swing width of about 20 cm for uniform mixing, to prepare a dispersion. Thereafter, it was allowed to stand at 20 ° C. for 2 hours.
  • the volume occupied by the powder dispersed phase in the separated phase of the powder dispersed phase and the pure water phase was read, and this was measured as a settling volume (mL).
  • Image analysis software (Image J) was used to randomly select 50 particles in the photograph, and the average major diameter ( ⁇ m) and the average thickness ( ⁇ m) of primary particles were determined.
  • the major axis of the primary particle is the size (that is, the longest diameter) of the particle in the direction in which the size of the particle becomes the largest by measuring the size of the measurement object particle from each direction.
  • BET specific surface area A sample powder pretreated at about 130 ° C. for about 30 minutes in a nitrogen gas atmosphere using an 8-station preheating unit (manufactured by MOUNTECH) was used as a BET specific surface area measuring device Macsorb HM Model-1208 The BET specific surface area (m 2 / g) was measured by a nitrogen gas adsorption method using (manufactured by MOUNTECH).
  • Weight loss (%) ⁇ (initial weight-weight at each temperature) / initial weight ⁇ x 100
  • the highly dispersed basic magnesium carbonate powder of the present invention is a cosmetic (liquid cosmetic or powdery cosmetic), a food and a paint, and a resin, a rubber, and a rubber, which are required to have heat resistance and reinforcement.
  • a cosmetic liquid cosmetic or powdery cosmetic
  • a food and a paint a paint
  • a resin a rubber, and a rubber, which are required to have heat resistance and reinforcement.
  • development to various applications can be suitably achieved.

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Abstract

L'invention concerne : une poudre de carbonate de magnésium basique hautement dispersée dans laquelle l'agrégation de particules primaires est supprimée et qui peut être développée pour diverses applications ; et sa méthode de production. La poudre de carbonate de magnésium basique hautement dispersée a un volume de sédimentation de 60 mL ou plus obtenu par mesure dans les conditions de mesure suivantes. (Conditions de mesure du volume de sédimentation) 5 g de la poudre de carbonate de magnésium basique sont introduites dans un cylindre de mesure de 100 mL avec un couvercle, puis de l'eau pure est pesée jusqu'à atteindre 100 mL et mélangée, le mélange résultant est laissé reposer à 20 °C pendant 2 heures, puis, dans une phase de séparation d'une phase dispersée de poudre et d'une phase aqueuse pure, le volume occupé par la phase dispersée de poudre est mesuré en tant que volume de sédimentation (mL).
PCT/JP2018/022917 2017-08-28 2018-06-15 Poudre de carbonate de magnésium basique hautement dispersée, et sa méthode de production Ceased WO2019044121A1 (fr)

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JP2017163098A JP6976773B2 (ja) 2017-08-28 2017-08-28 高分散塩基性炭酸マグネシウム粉末及びその製造方法
JP2017-163098 2017-08-28

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Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2003306325A (ja) * 2002-02-13 2003-10-28 Nittetsu Mining Co Ltd 塩基性炭酸マグネシウム及びその製造方法、並びに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
JP2005154158A (ja) * 2003-11-20 2005-06-16 Ube Material Industries Ltd 多孔質粒状塩基性炭酸マグネシウム及びその製造方法
JP2005220082A (ja) * 2004-02-06 2005-08-18 Nippon Shikizai Inc 粉末状クレンジング化粧料
JP2017088424A (ja) * 2015-11-04 2017-05-25 ナイカイ塩業株式会社 塩基性炭酸マグネシウムの製造方法

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2003306325A (ja) * 2002-02-13 2003-10-28 Nittetsu Mining Co Ltd 塩基性炭酸マグネシウム及びその製造方法、並びに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
JP2005154158A (ja) * 2003-11-20 2005-06-16 Ube Material Industries Ltd 多孔質粒状塩基性炭酸マグネシウム及びその製造方法
JP2005220082A (ja) * 2004-02-06 2005-08-18 Nippon Shikizai Inc 粉末状クレンジング化粧料
JP2017088424A (ja) * 2015-11-04 2017-05-25 ナイカイ塩業株式会社 塩基性炭酸マグネシウムの製造方法

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