TW201238901A - Globular magnesium hydroxide particles, globular magnesium oxide particles and method for manufacturing the same - Google Patents

Abstract

Provided are globular magnesium hydroxide particles and globular magnesium oxide particles with excellent dispersibility, and a method for manufacturing the same. The magnesium hydroxide particles and magnesium oxide particles have globular shapes resulted from the aggregation of the original, flaked particles, and have a mode volume of 1.4 ml/mg or more and a mode diameter of 0.4 μ m or more in a fine pore distribution.

Description

201238901 VI. Description of the Invention: [Technical Field] The present invention relates to spherical argon oxide particles, spherical magnesium oxide particles, and a method for producing the particles. [Prior Art] Magnesium hydroxide particles and magnesium oxide particles are used in various fields. Examples of the use of the magnesium arsenide particles include coating materials for inkjet paper, flame retardants, heat storage materials, catalysts, and electronic materials, and the use of magnesium oxide particles, for example, coating of optical materials and inkjet paper. Layering agents, catalysts, and electronic materials. If the magnesium hydroxide particles are used as a coating agent for an inkjet paper, a flame retardant, a heat storage material, a catalyst, and an electronic material, it is desirable to meet the following requirements. For the coating agent, it is required to have a 0H group having a high affinity with a majority of the 0H group of the dye ink, and a positive charge which is easily adsorbed to a pigment ink having a large negative charge, and the dye is easily dyed. Magnesium hydroxide particles of aggregate structure between particles. Further, among the flame retardant, the heat storage material, and the catalyst, it is required to have excellent dispersibility and to hold magnesium hydroxide particles having an aggregate structure exhibiting high reactivity. Further, for electronic materials, magnesium hydroxide particles having excellent dispersibility are required. When magnesium oxide particles are used as an optical material, a coating agent for inkjet paper, a catalyst, and an electronic material, it is desirable to meet the following requirements. The optical material is excellent in dispersibility and holds magnesium oxide particles having an aggregate structure which easily diffuses light. Further, in the case of a catalyst, it is excellent in dispersibility and holds a magnesium oxide particle having a highly reactive aggregate structure 323914 3 201238901. Further, for electronic materials, oxidized town particles having excellent dispersibility are required. Patent Document 1 describes that an ion concentration ratio of a sulfate ion [(s〇4) 2 -] / magnesium ion [(Mg) 2+] is obtained as a range of 至. 3 to 2. 〇, which has a difference of 2 or more. The directional leaflet-like sheets are bonded and/or cross-linked spherical magnesium hydroxide particles. However, according to the method described in Patent Document 1, spherical magnesium hydroxide cannot be stably formed, so that plate-like and columnar hydroquinone magnesium are mixed, and such magnesium hydroxide particles are used for resins and the like. The problem of insufficient dispersion. [Prior Art] [Patent Document 1] [Patent Document 1] JP-A-2003-261796 SUMMARY OF INVENTION [Problem to be Solved by the Invention] An object of the present invention is to solve the above problems and to provide (4) dispersion of fat or the like. A spherical A-oxidation coke and an age-independent seed, and a method for producing the same. The inventors of the present invention have found that, in the dispersion containing at least one or more compounds selected from the group consisting of Zn (de), & (error), Hf (giving), and Ti (titanium), the addition is selected from the two-valent And a compound of a trivalent metal element and a nitrate of a divalent or trivalent metal-based metal nitrate (except for a compound of Zn Zr Hf and Τι), and an organic acid is further added thereto. The anti-ship, mixed with the oxidation record, and under the high shear stress, the hydration reaction is carried out to produce the spherical gas with excellent dispersibility and oxidizes the fact of 323914 201238901 magnesium particles. Further, the inventors of the present invention have found that the fact that spherical magnesium oxide particles can be obtained by firing the magnesium hydroxide particles of the present invention at 500 ° C to 1,400 ° C in an atmospheric mist. I. The volume of the mode is 1. 4ml/mg or more. The mode volume of the pore volume distribution is 1. 4ml/mg or more. The mode diameter is 0.4 jtzm or more. The present invention relates to a magnesium oxide particle as described above, wherein the cumulative volume (accumu 1 at i ve volume) measured by a laser diffraction scattering particle size distribution is 50 ° /. The particle size (D5〇) is from 0.5 to 20 μm. The present invention relates to the magnesium hydroxide particles as described above, wherein the oil absorption amount is 30 ml/l or more. 01质量质量质量质量质量质量质量质量质量质量质量质量质量质量质量质量质量质量质量质量。 %, in terms of metal element, 'containing one or more metal elements selected from the group consisting of divalent and trivalent metal elements (except for Zn, Zr, Hf, and Ti) 〇. 〇1 to 5 . 0 mass%. The present invention relates to a magnesium oxide particle which is characterized in that it has a spherical shape of agglomerated scaly particles, and has a mode volume of 1.4 ml/mg or more in a pore distribution and a modal diameter of 〇 4 μm or more. The present invention relates to the magnesium oxide particles as described above, wherein the 5Q% particle diameter (5) of the cumulative volume measured by the laser diffraction scattering particle size distribution is 323914 5 201238901 0. 5 to 20 // m. The present invention relates to the magnesium oxide particles as described above, wherein the oil absorption amount is 30 ml/100 g or more. 01质量质量质量质量质量质量质量质量质量质量质量质量质量质量质量质量质量质量质量质量质量质量质量质量质量质量质量质量质量质量质量质量质量质量质量质量质量质量质量质量质量质量质量质量质量质量质量质量质量质量质量质量质量质量质量质量质量质量质量质量质量质量质量质量质量质量质量质量质量质量质量质量质量质量质量质量质量质量质量质量质量质量质量质量质量质量质量质量质量重量01至5. 0。 0. 01至5. 0。 0. 01至5. 0。 0. 01至5. 0。 0. 01至5. 0。 The metal element of the metal element of the group of the metal element (including Zn, Zr, Hf, and Ti). quality%. The present invention relates to a method for producing magnesium hydroxide particles, which comprises: (a) adding a dispersion of a compound containing one or more compounds selected from the group consisting of Zn, Zr, Hf, and Ti; One or more compounds in groups of chlorides of divalent and trivalent metal elements and nitrates of divalent and trivalent metal elements (except for compounds of Zn, Zr, Hf, and Ti), a step of adding an organic acid to prepare a reaction liquid, and (b) mixing the reaction liquid of the step (a) with magnesium oxide particles having an average particle diameter of 0.1 to 30/zm to prepare a mixed liquid (in the step of至质量质量质量为2的2,1% by mass, from 2 to 5. 0% by mass, selected from 2 One or more compounds of a valence and a vapor of a trivalent metal element and a nitrate of a divalent or trivalent metal element, in terms of a metal element 323914 6 201238901, a magnesia particle of g. 丨 to 5 The organic acid system is relative to the oxidized town particle mass, (6) the mixture of step (8) is 50 To =: to 3 phase), with a peripheral speed of 7 to 0; under the temperature, take the step, (meter) / S (8) machine to mix (d) at a temperature of 30 to 丨〇〇 ° C hydrogen (4) of the oxygen slick (s), and (4) the step of preparing the magnesium oxide particles of the hydrogen slurry of the step (4). Dry λ ^ Invented in (4)) find the rush, the oxygen tilt (four) degree is the manufacturing method of the other to the yam, which is characterized by the packaged t-de-de- Γ 化 化 镇 或 或 或 或 或 或 或 或 或 或 或 或 或 或 或 或 或 或 或Magnesium oxide particles, in the atmosphere of the fog,

The step of firing is performed. * 500 to 1400 C. Magnesium hydroxide particles and magnesium oxide particles are highly soluble in various fields. Further, according to the production method of the present invention, oxidized age and magnesium oxide particles can be easily produced. [Embodiment] The magnesium hydroxide particles of the present invention are obtained by concentrating scaly original particles, and the pore volume distribution has a mode volume of 14 mi/? or more, and the mode 牷 is 0.4 μm or more. In the present invention, the shape of the original particles is the thickness (short axis) of the scale-like scales, which is, for example, 比例1 to 〇.丨"m, the ratio of the maximum length to the thickness of the scale 323914 201238901 (aspect ratio, The ct rati0) is, for example, 10 to 1 00. The shape of the spherical shape of the aggregated primary particles is due to the presence of uniform pores on the surface of the particles, and the liquid and gas molecules are higher than the hexagonal plate-shaped magnesium hydroxide particles obtained by the conventional manufacturing method. It is spherical and has high dispersibility to resins and the like. If the magnesium hydroxide particles having such a mode diameter are used as a coating for paper, the ink is excellent in fixability and absorbability. Further, the magnesium hydroxide particles having such a modal volume have excellent adsorptivity to the ink due to the fact that the spherical scaly iron oxide is too dense. The modal volume of the pore distribution of the nitrogen oxynitride of the present invention is preferably from 4 to 1 〇ml/mg, and the diameter of _ is preferably from 0.4 to 3. Ο/zm, more preferably 〇. 5 to 2. "-the modal volume and modal diameter of the present invention" is determined by the mercury intrusion method, where the 'modal volume system' means the maximum value of the 1 〇g (logarithmic) differential pore volume distribution curve, and The modal diameter refers to the pore diameter corresponding to the maximum value of the log differential fine product distribution curve. For example, the pores of the oxidized town particles of the present invention or the aggregates of the oxidized town particles are distributed according to the mercury calendar. When the measurement is carried out, the mode corresponds to the magnesium hydroxide particles constituting the spherical particles or the voids between the magnesium oxide particles. The magnesium hydride particles of the present invention are irradiated by laser diffraction. The cumulative 5% by volume of the volume basis (5) determined by the particle size distribution measurement method is 至. 5 to 20/zm. If it is within this range, the viscosity at the time of compounding the resin or the like is not too high' Suppresses the aggregation of particles, so the dispersibility is good, and if the hydroxide of this size is used as a coating agent for money, since the particles do not protrude from the ink receiving layer, and the particle size is not After 323914 Λ 201238901 big 'as an optical material And the electronic material is useful. The Dso of the oxidized particles of the present invention is preferably from 1 〇 to 2 〇 。. The oil absorption of the magnesium hydroxide particles of the present invention is at least 3 〇 mi / i 〇〇 g. The oil absorption in the invention is the oil absorption of dioctyl dibenzoate. The oil absorption is pure to the end of the ride, and this method can be used as the evaluation of filling (Journal, Industrial Materials, Vol. 39) Μ, p. 116 to 帛 117 (10) D). Specifically, the oil absorption amount is obtained by kneading under the dropping of dioctyl phthalate (D0P) into the sample powder, and measuring the amount of 〇p required for the whole 胄b to become one hard block. It can be expressed as the amount of DOP per 100g of the ancient material powder (ml/lOOg). When the oil absorption amount is 30 ml/l or more, the dispersibility to the resin or the like is good, and when used as a coating agent for paper, the ink has good fixability and absorbability. The oil absorption amount of the magnesium hydroxide particles of the present invention is preferably 5 Å to 3 〇〇 ml / 1 〇〇 g. The magnesium hydroxide particles of the present invention may further contain a metal element of a compound used in the production step. The magnesium hydroxide particles of the present invention contain at least one metal element selected from the group consisting of Zn Zr, Hf, and Ti in an amount of 〇〇1 to 4. 〇% by mass in terms of an oxide. One or more other metal elements (excluding Zn, yttrium, Hf, and Ti) selected from the group consisting of divalent and trivalent metal elements are 〇〇1 to 5% by mass. When the content of such a halogen is used, when magnesium hydroxide particles are used as a coating agent, whiteness, ultraviolet absorbability, and refractive index are sufficient. Depending on the vapor compound, one or more metal elements selected from the group consisting of Zn, Zr, Hf, and Ti, that is, Zn, Zr 'Hf, Ti, or a mixture of such 323914 201238901 is preferably ' 0% by mass, more preferably 0.2 to 4.0% by mass, still more preferably 〇. 4 to 4. 〇% by mass. In the present invention, one or more metal elements selected from the group consisting of divalent and trivalent metal elements (except for Zn, Zr, Hf, and Ti) are not particularly limited, and examples thereof include Ag ( Silver), A1 (aluminum), B (boron), Ba (钡),

Bi (铋), Cd (镐), Co (cobalt), Cr (chromium), Cu (copper), Fe (鐡), Ga (gallium), In (indium), Mn (manganese), Mo (molybdenum), Ni (nickel), Pb (lead), Sr (stroke), T1 (铊), and V (vanadium), among which Α1 and Fe are preferable. The content of one or more other metal elements (except Zn, Zr, Hf, and Ti) in a group of two or more metal elements, preferably in the range of 0. 05. 0质量质量的。 0 to 0% by mass, more preferably 〇. 1 to 5. 0% by mass, and even more preferably 〇·3 to 4. 0 mass 0 / 〇. The singularity of the smear is 0. 4 / zm or more. The modal volume of the pores of the present invention is 1. 4 ml / mg or more. Such magnesium oxide particles are excellent in dispersibility to resins and the like. Specifically, when the magnesium oxide particles having such a modal diameter are used as a coating agent for paper, the fixing property and the absorbability of the ink are good, and the magnesium oxide particles having such a mode volume are formed. The scaly oxidized town of the shape is not too dense, and the ink adsorption property is good. The modal volume of the pores is preferably from 14 to 1 〇 ml/mg, and the modal diameter ′ is preferably from 0.4 to 3. 0/z m ′ is more preferably from 〇 5 to 2. O/zm. The magnesium oxide particles of the present invention have a cumulative 5 〇% particle diameter (〇5.) based on a volume basis measured by a laser ray scattering particle size distribution measurement method of 〇. 5 to 2 。. If it is within this range, the viscosity at the time of blending the resin or the like is not too high, and the dispersibility is good because the aggregation of the particles can be suppressed. Further, when used as a coating agent for paper, it is used as an optical material and an electronic material because the particles do not protrude from the ink receiving layer and the particle diameter is not excessive. The volume-based cumulative 50% particle diameter ' of the magnesium oxide particles of the present invention is preferably from 1 to 2 Å//ln. The oil absorption amount of the magnesium oxide particles of the present invention is 3 〇 ml / 1 〇〇 g or more. When it is in such a range, the dispersibility of the resin or the like is good, and when it is used as a coating agent for use, the ink is excellent in fixability and absorbability. The oil absorption amount of the magnesium oxide particles of the present invention is preferably 5 Å to 3 〇〇 ml / 1 〇〇 g. The magnesium oxide particles of the present invention may further contain a metal element of a compound used in the production step. The magnesium oxide particles of the present invention are selected from the group consisting of oxides

One or more metal elements of the group consisting of Zn Zr, Hf, and Ti 0. 01 to 4. The enamel is contained in a group of U or more selected from the group consisting of two or more metal elements. Other metal elements (except Zn, Hf, and Τι) 〇. 〇1 to 5· 〇 mass%. When the content of such a gold element is used, when the magnesium oxide particles are used as a coating agent, whiteness, ultraviolet absorbing property, and refractive index are sufficient. In the oxide conversion, one or more metal elements selected from the group consisting of Zn, Zr, Hf, and Ti, that is, the content of Zn Ti or such agglomerates is preferably 〇. 〇5 To 4. 〇 mass%, more preferably 〇. 2 to 4·〇 mass%' is more preferably 〇.4 to 4 () mass%. One or more other halogens selected from the group consisting of 2/f shells and trivalent metal elements (except for Zn, Zr, Hf, and Ti) are not limited by 323914 11 201238901. For example: Ag, A1, B, Ba, B i, Cd, Co, Cu, Fe, Ga, In, Mn, Mo, Ni, Pb, Sr, T1, and V, of which A1 and Fe are preferred. . The content of one or more other metal elements (excluding Zn, Zr, Hf, #KTi) selected from the group consisting of a metal element of a divalent or a trivalent value is preferably 0.1. It is 5.0% by mass, more preferably 0.3 to 4.0% by mass, still more preferably 0.4 to 4.0% by mass. The method for producing the oxidized granules of the present invention comprises: (a) adding a valence selected from the group consisting of a compound containing one or more compounds selected from the group consisting of Zn, Zr, Hf, and Ti; One or more compounds of a vapor of a trivalent metal element and a nitrate of a divalent or trivalent metal element (except for compounds of Zn, Zr, Hf, and Ti), and an organic acid is added thereto. a step of obtaining a reaction liquid, (b) a step of preparing a mixed liquid by mixing the reaction liquid of the step (a) with magnesium oxide particles having an average particle diameter of 0.1 to 30/zm (here, selected from Zn) And the oxidized town is 0.1 to 5.0% by mass, selected from the group consisting of divalent and trivalent metal elements. The organic compound, relative to oxidation, is oxidized to 1 to 5.0% by mass of the metal oxide in terms of metal element, in terms of metal element, in terms of metal element, relative to oxidation. Magnesium 100g, from 0.01 to 3. Omol), (c) The mixture of step (b) is taken at a temperature of 50 to 100 ° C. 323914 12 201238901 With a peripheral speed of 7 to 2 _ machine into (four) combined (4) at 30 to (10). At the temperature of C, the step of preparing the slurry of magnesium hydroxide is carried out, and the step of preparing the magnesium hydroxide slurry by the step (4) is carried out to prepare the magnesium hydroxide particles. w water hydrazine, dry step (4) is a step of preparing water for magnesium oxide. The reaction to be used is a compound selected from the group consisting of Zn, Zr, Hf, and Ti, and is a composite hydroxide of the present invention and a complex oxygen: Wo: and magnesium oxide particles k liter The whiteness, the outer absorption of the i-ray, the refractive index, etc., may be the coating agent of the material or the paper of the ink, and the gas-oxygen of the invention: -::Hf, the compound of the broad and Ti' as long as it has such a metal = The a substance is not particularly limited, and examples thereof include oxides, cerium oxides, hydrides, halides (fluoride, chloride, bromide, and iodination), phosphates, and carbonates. And nitrates, etc., and preferably zinc oxide, zinc hydroxide, zinc vapor, zinc nitrate, oxidized, wrong acid, cerium oxide, cerium hydroxide, gasification, helium, cerium oxide, hydrogen peroxide Titanium, vaporized titanium, and niobium nitrate.

5度。 The Zn, Zr, Hf, and Ti, preferably having a purity of 99. 〇0 / 〇 or more, more preferably at 99. 5 ° /. the above. In the present invention, purity refers to the measurement of impurities in the particles of the object (Ag, Al, B, Ba, Bi, Cd, C1, 323914 13 201238901

After content of Co, Cr, Cu, Fe, Ga, In, yttrium, Li, Μη, Mo, Na, Ni, P, Pb, S, Si, Sr, ΤΙ, V, Zn, Ti, and Zr), and The sum of these totals is subtracted from the value of 100% by mass. The method for measuring the content of such an impurity element may, for example, be a measurement method using an ICP (Inductively Coupled Plasma) luminescence analyzer.

The compound of Zn, Zr, Hf, and Ti preferably has an average particle diameter of from 0.1 to 100 / / m, more preferably from 0.5 to 50 # 111.至至至至至至至至至至至至至至至至至至至至至至至至至至至至至至至至至至至至至至至至至至至至至至至至至至至至至至至至至至至至至至至至至至至至至至至至至至至至至至至至至至至至至至至至至至至至至至至至至至至至至至至5. 0% by mass. When the amount of the compound in which the compound selected from the group consisting of Zn, Zr, Hf, and Ti is 0.1% by mass or less, when used as a coating agent, whiteness, ultraviolet absorbing property, refractive index, and the like may be insufficient. Further, the particle shape does not become a hexagonal plate-like particle which is a spherical particle of the original particle which aggregates scales. Further, when the amount of the compound of the compound selected from the group consisting of Zn, Zr, Hf, and Ti is 5.0% by mass or more, it does not become the spherical particles of the aggregated scaly original particles of the present invention. It becomes a hexagonal columnar particle. The amount of the compound of the compound selected from the group consisting of Zn, Zr, Hf, and Ti is preferably from 0.4 to 4.0% by mass based on the weight of the magnesium oxide particles. A dispersion of one or more kinds of compounds containing a group of compounds containing Zn, Zr, Hf, and Ti, for example, a compound selected from the group consisting of Zn, Zr, Hf, and Ti added to ion exchange water One or more compounds of the group can be obtained. The chloride of the divalent and trivalent metal elements, and the nitrates of the divalent and trivalent 323914 14 201238901 metal elements are used to control the solubility of the hydroxide particles of the present invention, and the solubility and precipitation rate of the hydroxides. Used to add. As the vapor of the 2 mussel and the trivalent metal element, and the nitrate of the divalent and trivalent metal elements, aluminum chloride, iron chloride, aluminum nitrate, and iron nitrate are preferable. The 5% or more, more preferably 99.5% or more, of the chloride of the metal element of the 2 and 3 mussels, and the nitrate of the metal element of the divalent and trivalent. Further, the chloride of the metal element of the divalent and 3 mussels, and the nitrate of the metal element of the divalent and trivalent, preferably have an average particle diameter of from 〇·丨 to 1〇〇, more preferably 〇. 5 to 50// m. The amount of one or more compounds selected from the group consisting of a chloride of a divalent or trivalent metal element and a nitrate of a divalent or trivalent metal element, in terms of gold (element), relative to step (b) The magnesium oxide particles used in the invention are from 0.1 to 5.0% by mass. When the amount of addition is 0.1% by mass or less, the precipitation rate of the crystal is slow, so that it is a monodisperse hexagonal columnar particle. If the amount is more than 5% by mass, the precipitation rate of the crystal is too fast. ^ For coarse aggregated particles. The amount of a compound selected from the group consisting of a vapor of a divalent or trivalent metal element and a nitrate of a divalent or trivalent metal element, or more than one or more kinds of compounds, in terms of metal elements, relative to the magnesium particles It is preferably from 0.4 to 4.0% by mass. Emulsification In the present invention, the organic acid is added to suppress the solubility of the gas as a raw material. The organic acid may, for example, be a ketone group or an aromatic organic acid, and among them, formic acid, acetic acid/fat 323914 201238901 acid, and benzoic acid are preferred. The amount of the organic I added is 〇·G1 to 3_ with respect to 100 g of the oxidized money particles used in the step (6). For example, the amount of the organic acid added is relative to the magnesium oxide particles 1QGg^Q.Qlm. When the 丨 is below, the precipitation rate of the crystal is sluggish, so that it is a monodisperse hexa-particle-like particle. If the amount is more than or more than Omol, the precipitation rate of the crystal is too fast to become coarse aggregated particles. The amount of the organic acid added is preferably 0.01 to 2. 〇mo, the step (b) is the reaction liquid for the hydration reaction obtained in the step (a), with respect to 100 g of the magnesium oxide used in the step (8). The step of mixing the magnesium oxide particles as a raw material. The magnesium oxide particles used as the raw material have an average particle diameter of from 01 to 30. If the average particle diameter is below Q1_, the hydration rate is too fast, and the aggregated particles are coarse. X, such as an average particle diameter of the above, such as 1 water. The reaction does not proceed sufficiently so that the average particle diameter of the oxidized particles containing the particulate iron oxide remains, preferably 0.5 Sl 5 /zm. In the step (6), the magnesium oxide intensity of the mixed liquid is preferably 20 S 200 g/L, and is 50 to 180 g/L. That is, with respect to the reaction liquid obtained in the step (a), the amount of the product is preferably adjusted to 2 〇 to · g / L, more preferably 5 () to 15 〇 g / L. The reaction liquid towel has a concentration of oxygen storage, and the hemp reaction is fully carried out. In the step (b), the temperature of the reaction liquid is preferably from 5 Torr to 1 Torr, more preferably from 50 to 95 Torr, and still more preferably from 7 Torr to Torr. If this temperature is reached, the 7 σ reaction will proceed sufficiently. Step (c) 'Steps of mixing at a temperature of rc of 50 to 10 using a lion machine with a peripheral speed of 7 _/s. The number of rotations of the stirring is adjusted to 323914 201238901 to control the dispersion state during the reaction. In the present invention, if the peripheral speed is 7 m/s or less, the magnesium hydroxide of the spherical particles of the scaly-like original particles cannot be obtained. X, if the peripheral velocity is 2 Gm/s or more, the gas-oxidized town particles When the nucleus is generated, it is sufficiently dispersed to become a monodisperse hexagonal columnar hydroxide residue, so that spherical gas-like oxidized particles can not be obtained as in the case of the device. For example, a homodisperser (hQmo-disper) (Brymex, τ κ. homodisperser, etc.) peripheral speed, preferably 8 to 18 in/s, more preferably 9 to test. The reaction temperature in the step (c) is preferably π to, more preferably 60 to 95 ° C. In the step (6), the towel 'mixing _ can be changed according to the degree of hydration anti-redness, for example, from 10 minutes to 36 minutes. 〇 minutes, minutes to 200 minutes. Step (4), at 30 to 10 (rc temperature, long time to stir The step of obtaining a magnesium hydroxide material is obtained, thereby promoting the hydration reaction of the unreacted oxidized town to form magnesium hydroxide. The temperature is preferably from 5 to 95 C, more preferably from 70 to 9 ° C. The stirring speed is not particularly limited as long as it can sufficiently agitate the magnesium hydroxide slurry, and for example, it can be used in the range of (10) to 500 rpra of the three pieces of the carcass. (4) Time is sufficient The hydration reaction can be carried out to obtain the desired time for the magnesium hydroxide material to be aggregated, and is not particularly limited. For example, it can be 0.5 to 6 hours. (4) (6) 'The filtration of the gas oxidation polymerization of the step (4) is carried out. , washing and drying to obtain the magnesium hydroxide particles. Thus, the magnesium hydroxide particles of the invention of 323914 17 201238901 can be obtained. The magnesium oxide particles of the present invention will be subjected to the step (a) comprising the present invention. The magnesium hydroxide particles obtained by the production method of the step (e) are prepared by the steps of 500 to 14 Å in the atmospheric mist, preferably in the lower firing step. Method of firing at 1300 〇C For example, the magnesium hydroxide particles are heated in a temperature range of 1 to 2 (TC/min (preferably 3 to i〇t:/min) to (5)^^ to 14〇〇°C in the atmosphere. Preferably, it is 60 (rc to 1300, and after raising the temperature, at 5 〇〇. (: to 14 ° C, preferably 600. (: to 130 (rc to 〇 1 to 5 hours, then The magnesium oxide particles of the present invention are obtained. When the firing temperature is 5 Torr or less, the amount of heat is insufficient to cause magnesium hydroxide. In other respects, if the firing temperature is 140 (TC or more, magnesium oxide) That is, the particles are grown so as not to become spherical magnesium oxide of the aggregated scaly original particles. Thus, spherical magnesium hydroxide particles and magnesium hydroxide particles excellent in dispersibility can be obtained. [Examples] Hereinafter, the contents of the present invention will be specifically described by way of Examples and Comparative Examples, but the present invention is not limited thereto. [Analytical method] (1) Laser diffraction scattering type particle size distribution measurement Using a laser diffraction scattering type particle size distribution measuring apparatus (trade name: MT3300, manufactured by Hiroshi Seisakusho Co., Ltd.), the volumetric reference cumulative 5 〇MMf (D5) .). (2) Element mass measurement method as a measurement target element in particles (Al, Fe, Ζπ, Zi*, Hf, Ti > 323914 18 201238901 Using an ICP luminescence analyzer (trade name: SPS-5100, manufactured by Seiko Instruments Co., Ltd.) After the sample was dissolved, the mass was measured. (3) Measurement of pore distribution (modal volume and mode diameter) The mercury-indented pore size distribution measuring apparatus was measured using Autopore 9410 manufactured by Micrometrix Co., Ltd. Mercury is a mercury-based reagent with a purity of 99.5 mass% or more and a density of 13.5335 x 103 kg/m3. The maximum value (modal volume) of the differential pore volume distribution curve of 1 〇g is obtained by measuring the pore size distribution of mercury. 'and the pore diameter (modal diameter) corresponding to the modal volume. (4) Measurement of oil absorption The sample powder is mixed with dioctyl phthalate (D0P) while being mixed with 2·5x1 Og. The point at which the whole becomes a hard block is used as the end point, and the amount of D0P at this time is taken as the oil absorption amount. [Example 1] The zinc oxide and ion-exchanged water containing 4% by mass of magnesium oxide relative to the reaction are used. 1 liter In the solution of the sub-exchanged water, 0.5% by mass of aluminum chloride 6 hydrate in terms of metal ruthenium, and 0.5 g of propionic acid in an amount of 0.1 g of oxidized town were added to prepare a reaction liquid. After the temperature of the reaction liquid was raised to 6 Torr, 100 g of magnesium oxide having a plate diameter of 8.8/ζη was placed to prepare a mixed liquid. After the magnesium oxide was placed, the temperature of the reaction liquid was raised to 95 Torr, and (4) The mixing machine (the τ·κ·distribution machine made by Bramico Co., Ltd.) adjusts the peripheral speed to 9m/s, and the degree of rotation of the fan is made. Then the hydrogen produced is then at 90 ° C. The slurry was stirred for 1 hour to prepare a magnesium hydroxide slurry 323914 201238901. The magnesium oxide slurry was filtered, washed with water, and dried to obtain the magnesium hydroxide particles of the present invention. [Example 2] Except for zinc oxide The addition was carried out in the same manner as in Example 1 except that the amount of addition was 3.0% by mass. [Example 3] The same procedure as in Example 1 was carried out except that the amount of zinc oxide added was 0.1% by mass. [Example 4] Except that zinc oxide was changed to 0.5% by mass of titanium oxide The remainder was carried out in the same manner as in Example 1. [Example 5] The same procedure as in Example 1 was carried out except that the amount of the gasification of the hydrated hydrate was determined to be 3.0% by mass in terms of metal element. [Example 6] The same procedure as in Example 1 was carried out except that the amount of the gasification of the gas hydrate was determined to be 0.1% by mass in terms of the metal element. [Example 7] The same procedure as in Example 1 was carried out except that the vaporized aluminum 6 hydrate was changed to 0.5% by mass of ferric chloride. [Example 8] The same procedure as in Example 1 was carried out except that the aluminum chloride 6 hydrate was changed to 0.5% by mass of aluminum nitrate. [Example 9] 323914 20 201238901 Except that the amount of propionic acid added was changed to 0.5 mol, the rest was carried out in the same manner as in Example i. [Example 10] Except that acetic acid was changed to 0.02 «1〇1 acetic acid, the rest of the examples were given! The same way is implemented. [Example 11] Except that the propionic acid was changed to 0.02 Π1Ο1 of butyric acid, the rest of the examples were given! The same way is implemented. [Example 12] The same procedure as in Example 1 was carried out except that the peripheral speed of the mixer at the time of the hydration reaction was set to 14 m/s. [Example 13] The same procedure as in Example 1 was carried out except that the peripheral speed of the mixer at the time of the hydration reaction was changed to 7 in/s. [Example 14] The oxidized hydroxide produced in Example 7 was fired in an atmospheric mist at 8 〇〇 π for 1 hour to obtain magnesium oxide particles. [Example 15] The rest was carried out in the same manner as in Example 14 except that the firing temperature was set to "(10).

[Example 16 J; 13⁄4 2 The winding temperature was set to 1200 ° C, and the rest was carried out in the same manner as in Example 14. [Comparative Example 1] 323914 21 201238901 The same procedure as in Example 1 was carried out except that the amount of the oxidation was added to 6.0% by mass. [Comparative Example 2] The same procedure as in Example 1 was carried out except that zinc oxide was not added. [Comparative Example 3] The spears were changed to the same as in Example 1 except that the gasified hexahydrate was changed to 5% by mass of sulfuric acid. [Comparative Example 4] The same procedure as in Example 1 was carried out except that propionic acid was not added. [Comparative Example 5] The same procedure as in Example 1 was carried out except that the spear and the hexahydrate were not added. [Comparative Example 6] The same procedure as in Example 1 was carried out except that the gasified hexahydrate was changed to the aluminum acetate. [Comparative Example 7] The procedure was carried out in the same manner as in Example 1 except that the speed of the kiln at the time of the hydration reaction was changed to 21 m/s. [Comparative Example 8] The same procedure was carried out except that the firing temperature was set to 1503⁄4. Except the rest of the embodiment 14

The results of the oxygenation obtained in the comparative example are shown in Table 2. Measurement results of magnesium particles and magnesium oxide particles, 323914 22 201238901 [Table 1] Example 16 S 3 1 j 0.03 | in es φ s 1200 I MgO 1 spherical 1 5 CD 2.18 1 0J9 I 1 0.49 1 0.07 This S 1 tn 1 1 0.03 U) <n ο s 1000 MgO 1 Sphere 1 C0 ιό 1.94 2.84 S 0.38 1 o 0.08 Example | t4 1 2 1 S 1 1 0.03 in o A s ♦ § 〇MgO 1 Sphere 1 CD S 2^4 junction a4i 1 0.48 aos Example 13 in 1 1 1 0.03 1 1 in a> r- s 1 1 M^OH), 1 1 spherical 1 17.4 op 1.69 s 0.26 1 0.32 0.06 Example 12 — S 1 1 1 a〇3 1 1 tn O) s 1 1 MgiOH), | 1 globular 1 β» (Ο 9.68 to tn 0.26 1 0.34 0.05 Example 11 2 to 1 1 1 1 1 0.02 tn 〇α» s 1 Mg(0H)2 | I Sphere | , · 0.76 CM us 0.28 幽0.33 a〇7 Example 10 3 (A 1 1 1 1 0.02 1 40 A β> s Like 1 | Mg(0H)21 | 3 0.93 2.52 s 0.26 1 0.34 a〇6 本嫦" 4« 5 ΙΟ 1 1 1 in 1 1 <n c> α» 芑1 Μ*(0Η), | 1 Sphere 1 <D OB S so 0.27 1 0.33 0.06 Example 8 5 Sun 1 u> 1 0.03 1 1 m at ο» s 1 Mg(0H)a | 1 Sphere | 11.2 ry 2.48 s 0.26 1 CM σ> a〇7 Example 7 S 1 n 1 1 0.03 1 1 in o β» s 1 | Mg(0H)2 | I Sphere | 10.2 1.32 2.64 ϊο 0.28 1 0.07 a36 Example 6 5 5 1 1 1 0.03 \ 1 ui o <Β s 1 MgCOH), | 1 spheroid | to iri 1.24 ZJ5 芑1 0.068 0.36 0.06 this 2 s 1 1 1 0.03 1 1 tn β» ο s 1! Mg(0H), I ball Shape | l〇1.35 2.86 s 0.24 1 2.12 0.04 Example 4 tn η 幽 1 1 a〇3 1 1 <A a» 4» s \ | MeiOH): 1 1 globular I CO o 2.86 s 1 0.34 0.34 0.0 S Example 3 5 S 1 1 1 0.03 1 1 m a> m 3 Like 1 1 MeiOH), 1 globular | 卜' 0.66 1.49 s 0.074 1 0.38 0.06 5 S ΙΟ 1 1 1 0.03 1 1 in o φ s 1 Mg(0H)a II Sphere | eq 0.62 1.48 s Z28 1 0.34 aoe Example 1 S wl 1 1 0.03 Coffee 1 tA β» ο s 1 ! Mg(〇H)a 1 Sphere .1 r> ΐ 0.75 s 0.26 t 0.3S 0.07 Sample name I mass% | 1 mass XI 1 mass X| 1 mass 43⁄4 1 mass X mass X 1 mo! o EP 1 m/s 1 P £. P substance t particle shape 10, m 1〇 -*m I ml/g | Iml/IOOgJ 1 mass x 1 1 mass x II mass% II mass x I ZnO ΤΪΟ AI(AICba6H2〇) Fe(FeCI3) A1 (AI(N〇3)3-9H2〇) AI(AI2(S〇4)3-16H2〇) Propionic acid butyric acid|temperature at reaction 1 peripheral speed I ripening temperature ripening time firing temperature mode diameter modal volume oil absorption ZnO TiO ιΣ manufacturing conditions 23 323914 201238901 [ Table 2] Comparative Example 8 | 1 1 1 1 0.03 | 1 1 in β» Oi s 1500 | MgO | Six-sided S 0.28 | s 0.38 | 1 0.34 | 0.03 | Comparative Example 7 Domain a 1 tn 1 1 1 0.03 1 1 ΙΑ 〇> s 1 Mg(0H), hexagonal plate οΐ 0,3758 1.19 s 0.26 1 0.34 0.09 Comparative example 6 2 1 1 1 \ 2 0.03 1 1 ιο α> A § inch 1 MgiOH), spherical fs Csj o' 1.23 CO CM 0.26 1 0.36 0.076 Comparative Example 5 cS 1 1 1 \ 1 0.03 1 1 to α>σ> 1 Mg(0H)a 1 Hexagonal column 1 (Ο CJ 0.22 1.67 s 0.26 1 1 0.07 Comparative Example 4 Rr G> 1 (η 1 1 * 1 1 1 ιο 〇>σ> s 1 Μ«(0Η), 1 hexagonal column I ΙΟ 0.87 t.86 s 0.24 1 0.36 0.07 Comparative example 3 Curved Ο 1 1 1 in o 1 0.03 1 1 ιο α>α> s 1 Mg(0H), hexagonal column 09 uS 0.28 1.35 s 0.28 1 0.34 0.02 Comparative Example 2 1 1 in 1 1 1 0.03 1 1 ιη σ>σ> s 1 Mg(0H) 2 1 hexagon plate | Ρ- 0.47 0.65 s 1 1 0.36 0.06 Comparative Example 1 ο <d 1 in 1 1 1 0.03 1 1 α» σ> s 1 Mg(0H)2 1 Hexagonal column 1 <q cn 1.43 4.12 1 0.34 0.02 1 Sample name 1 mass 蛩χ i 1 mass X 1 1 'mass X 1 1 f amount X 1 mass % mass X 1 mol 1 Ρ m/s PXP substance particle shape ' »〇-*m ΙΟΛη ml/g ml/100g 1 mass》 1 I mass XI | mass % I Mass % ZnO ΤιΟ AI(AICI3.6H20) o Φ u. d CO 5 S ooo 5! Temperature at the reaction of propionic acid butyric acid, circumferential speed, ripening temperature, ripening time, firing temperature, mode diameter, mode volume, oil absorption, ZnO o 5 Manufacture condition 24 323914 201238901 [Industrial use possibility] The magnesium hydroxide particles and the magnesium oxide particles of the present invention are spherical, have a small particle size and are uniform, and are useful in various fields because of good dispersibility. High sex. Further, according to the production method of the present invention, it is easy to prepare particles as described above, and the convenience is high. The use of the argon magnesium oxide particles of the present invention may, for example, be a coating agent for an inkjet paper, a flame retardant, a heat storage material, a catalyst, an electronic material, or the like, and the use of the magnesium oxide particles may, for example, be an optical material. Coating agents, catalysts, and electronic materials for inkjet paper. BRIEF DESCRIPTION OF THE DRAWINGS Fig. 1 is an electron micrograph of the magnesium hydroxide particles of the present invention. [Main component symbol description] None 323914 25

Claims (1)

201238901 VII. Patent application scope: 1. A magnesium hydroxide particle which is formed into a spherical shape by collecting scaly original particles. The mode volume in the pore distribution is 14 inl/mg or more, and the mode diameter is 〇. . 4 vm or more. 2. The magnesium hydroxide particles according to the invention of claim 2, wherein the cumulative volume of the 5 〇% particle diameter (D5Q) determined by the laser diffraction scattering particle size distribution is 〇. 5 to 20/zm . 3. The magnesium hydroxide particles according to the second or second aspect of the patent application, wherein the oil absorption is 30 ml/100 g or more. 4. The magnesium hydroxide particles according to any one of claims 1 to 3, further comprising a group selected from the group consisting of ruthenium, osmium, iridium, and Ti in terms of an oxide. The metal element is 〇〇1 to 4% by mass. 5. The magnesium hydroxide particles according to any one of the above-mentioned claims, wherein the 'metal element' is further selected to contain other metal elements selected from the group consisting of divalent and trivalent metals. (However, except for Zn, Zr, Hf, and Ti) 〇·〇ι to 5·〇% by mass. 6·: A kind of magnesium oxide particles, which are formed into a spherical shape by collecting the original particles of a sheet of money, and have a mode volume of 1.4 ml/mg or more in a pore distribution, and a mode diameter of 〇. 4 em or more. 7. The magnesium oxide particle according to claim 6, wherein the cumulative volume of the coffee particle diameter (Dsd) determined by the laser diffraction scattering particle size distribution is 〇. 5 to 20 #m. 8. The oxidized town particles described in claim 6 or 7, wherein the oil absorption amount is 30 ml/l 〇〇 g or more. 323914 1 201238901 9. The magnesium oxide particles as described in any of claims 6 to 8 of the patent application 'in which the food is selected from the group consisting of Zn, Zr, Hf, and Ti. The metal element of the group 〇. 〇1爻4·0 mass%. 1. The magnesium oxide particles as described in any one of claims 6 to 9 wherein, in terms of metal elements, other metal elements selected from the group consisting of divalent and trivalent metals are further included. (except for Zn, Zr, Hf, and Τι) 0. 01 to 5· 〇 mass%. A method for producing a seed magnesium oxide particle, comprising the steps of: (4) adding, in a dispersion liquid of a compound containing one or more compounds selected from the group consisting of Zn, Zr, Hf, and Ti; "The gasification of benzalkonium and the divalent and trivalent gold salts are grouped together! Compounds of the above species (except for the compounds of Ζη, ΖΓ, ^, s:h)" The reaction liquid J (8) is mixed with the magnesium oxide particles having an average particle diameter of q by the reverse reaction of the step (4) to obtain a mixture of 3 〇^m (here, the above compounds of rzn, zr, and ^ are grouped) The compound, in terms of oxide, is relative to, the meal. 1 to 5. 〇 mass%, the vaporized money is the chloride of the divalent and trivalent metal elements, and the nitric acid of the 9 bismuth metal 7G The salt is a group of two kinds of bonds and three elements, which are based on magnesium oxide. Therefore, the gold organic acid is 〇〇1 with respect to magnesium oxide. 〇1 〇 323914 3. 〇 1Q〇J) 201238901 (c) The mixture of step (b) is at a temperature of 50 to 100 ° C, using a peripheral speed of 7 to a mixing step of a 20 m/s mixer, (d) a step of stirring at a temperature of 30 to 100 ° C for a long time to obtain a magnesium hydroxide slurry, and (e) a hydroxide of the step (d) The method for producing the magnesium hydroxide particles according to the invention of claim 11, wherein the mixture of the mixture is in the step (b) The magnesium oxide has a concentration of 20 to 200 g/L. 13. A method for producing a magnesium oxide particle, comprising: the magnesium hydroxide particle according to any one of claims 1 to 5 Or the magnesium hydroxide particles obtained by the method according to any one of claims 11 to 12, which are subjected to a calcination step at 500 to 1400 ° C in an atmospheric mist. 323914 3