TW201219307A - Magnesium hydroxide microparticle and magnesium oxide microparticle, and method for producing the same - Google Patents

Abstract

Provided are a highly-pure magnesium hydroxide microparticle and a highly-pure magnesium oxide microparticle having small diameters and good uniformity. The magnesium hydroxide microparticle has a BET specific surface area of 5m<SP>2</SP>/g or more, a cumulative 50% particle diameter (D50) in volume reference obtained by laser diffraction scattering particle-distribution measurement with a value of 0.1 to 0.5 μ m, a D90/D10 ratio of the cumulative 10% particle diameter (D10) in volume reference to the cumulative 90% particle diameter (D90) in volume reference obtained by laser diffraction scattering particle-distribution measurement with a value of 10 or less, and a purity of 99.5% by mass or more. The magnesium oxide microparticle has a BET specific surface area of 5m<SP>2</SP>/g or more, a cumulative 50% particle diameter (D50) in volume reference obtained by laser diffraction scattering particle-distribution measurement with a value of 0.1 to 0.5 μ m, a D90/D10 ratio of the cumulative 10% particle diameter (D10) in volume reference to the cumulative 90% particle diameter (D90) in volume reference obtained by laser diffraction scattering particle-distribution measurement with a value of 10 or less, and a purity of 99.5% by mass or more.

Description

201219307 VI. Description of the Invention: [Technical Field of the Invention] The invention relates to a high-purity oxidized town of a small particle size and a uniform sentence, and a magnesium oxide fine particle of purity, and the like [the prior art] and a method for producing a smear microparticle . Magnesium hydroxide and magnesium oxide are helmets that are used in various fields. For the purposes of the former, additives, resin fillers, energy materials, and catalysts may be used, and the latter may be used for fire resistance. =, resin filler, high functional materials, electromagnetic steel sheet materials, and touch materials. Including these applications, the requirements for magnesium hydroxide and oxygen tilting are high, the particle size is small, and the fine particle form is uniform. In the method of producing magnesium hydroxide having a small particle size and uniformity, it is proposed to: add an analyte f in an aqueous solution containing magnesium hydroxide, and then add a surfactant; thereby modulating (10) to hydrogen of the coffee (10) Method of magnesium oxide fine particles j (refer to Patent Document 1). However, in the specific case, the amount of addition is large, and the high-pressure dad container dissolves the impurities, and there is a problem that the impurities are mixed. Also 'is also proposed to make the gasification μ and the test substance hydrothermal reaction in the aqueous medium aydmhemal reaetiQn) $ method of making barium hydroxide 'adding thief, material or scale (4), and arbitrary control The method of the aspect ratio of the oxidized town (refer to Patent Wire 2). However, in this method, there is a problem that it is difficult to control the particle diameter, and it is impossible to obtain a fine particle having a uniform particle diameter. (Prior Art Document) (Patent Document) 323520 4 201219307 (Patent Document No. JP-A-2009-62214 (Patent Document 2) JP-A-2005-200300 SUMMARY OF THE INVENTION (Problems to be Solved by the Invention) (4) The purpose of the invention is to provide a method for producing small particle size and uniform granules, oxidized particles and high-purity magnesium oxide particles, and fine particles such as shai. Magnesium oxide microparticles, the specific surface area of the 纟 其 r r ^ 雷 雷 雷 绕 绕 绕 绕 绕 绕 绕 绕 雷 雷 雷 雷 雷 雷 雷 雷 雷 雷 体 体 体 体 体 体 体 体 体 体 体 体 体 体 体 体 体 = = = Under the cumulative_path, the purity is 99.5 mass ^1^() ratio WD'. It is 10 to accumulate in the oxidized town microparticles, and its nautical surface surface is Zhaojiji 5 (; (4) shot (four) type city distribution failure method Early accumulation of 5_path (four) is

The cumulative 10% particle size of the n-product of the volume of Am obtained by the scattering particle size distribution method (.0.5 diffraction diffraction) (the cumulative_particle size of D)

Next, the purity is above 99.5 mass%. The present invention relates to a step (^) for preparing an aqueous magnesium chloride solution containing oxidized granules of the following steps; and a chlorination aqueous solution and an alkaline aqueous solution of 1 to 10, at a reaction rate of 323520 5 201219307 m to 21 〇 % molar reaction, and obtain the step (8) of oxidizing the town mud; maintaining the gas oxidizing slurry - surface mixing - surface to m to ·. The temperature of c, the step of obtaining the hydrothermally treated magnesium hydroxide (IV) (〇; and the hydrothermally treated magnesium hydroxide m, washing with water and drying to obtain the oxidized granules (D). The present invention relates to a method for producing oxidized granules comprising the steps of: calcining the above-mentioned hydroxide particles or the oxidized particles obtained by the above-mentioned production method in a domain environment Step (E). (Effects of the Invention) The magnesium hydroxide fine particles and the oxidized granules of the present invention have high purity, a small particle size, and are uniform in various fields, and have high usefulness in various fields. The manufacturing method of the present invention can easily prepare the above-mentioned high-precision property. [Embodiment] The hydroxide-based particles of the present invention have a β-ΕΤ specific surface area of 5 仏 or more: a volume-based accumulation of a laser diffraction scattering particle size distribution measurement_ (5) is (U to Q 5 (10)' f-ray diffraction scattering particle size distribution measurement = volume-based cumulative cryptoparticle _... cumulative volume with volume basis 9 〇 % particle size 9 °, orbit D9 ° / Dl ° below 10 . Such magnesium hydroxide microparticles The particles are small in shape and have excellent reaction properties, so they are suitable for additives, resin fillers, catalysts, etc., and the particle size is small, the particle size variation is small, and there is excellent: politicality, so for highly functional materials. The BET specific surface area of the magnesium oxychloride fine particles of the present invention is preferably i 〇 mVg or more, Ds. 323520 6 201219307 is preferably 0.2 to 〇. 5叩' Dm/Di. The purity of the magnesium hydroxide fine particles of the present invention is 99.5% by mass or more. If it is within this range, the elution of impurities can be suppressed extremely, and it can be suitably used for a highly functional material. The purity of the magnesium hydroxide fine particles of the present invention. Preferably, the purity is 99.9% by mass or more. In the present specification, the purity is an impurity element (Ag ' Al ' B ' , βί ' Cd ' Cl, Co, C r, Cu, Fe, Ga) in the microparticle to be measured. ,

The contents of In ' K , Li , Mn , Mo ' Na , Ni ' p , pb , S , S i , S r , T1 , V ' Zn ' Ti and Zr ) and the total content of these are determined by i値 Quality deducted 値. In the present specification, 'high purity' means a purity of 99.5% by mass or more as calculated as described above. As an impurity element (Ag, A, B, Ba, Bi, Cd,

Co , Cr ′ Cu , Fe , Ga , In , K , Li , Μη , Mo , Na , N i , p ,

Pb ' S, Si ' Sr, ΤΙ, V, Zn ' Ti and Zr) are obtained by dissolving a sample in an acid using an ICP luminescence analyzer, and measuring the mass. The amount of C1 is obtained by dissolving the sample in an acid using a spectrophotometer. Determine the value of the mass. The magnesium hydroxide fine particles of the present invention are a combination of Fe, Ti, Ni, Cr, Mo and Μη, and the content thereof is preferably 5 〇〇 or less. When the total content is 500 mass% or less, the elution electrode of the metal impurities is suppressed. It can be suitably used for additives, resin fillers, and highly functional materials. The total content is preferably 450 mass 卯m or less. It is preferable that the magnesium hydroxide fine particles of the present month have a chlorine content of 5 or less in a mass of 5 (10) or less. When the content of the chlorine is less than or equal to the mass, the particle is extremely subjected to calcination (4) when the oxygen field is micro (four), the particle filament is extremely affected (four), and can be = 323520 7 201219307 A fine magnesium oxide powder is obtained. The content is more preferably 450 mass ppnl or less. The oxidized fine particles of the present invention preferably have a ratio Dv/Dn of a volume-based average particle diameter (Dv) to a number-based average particle diameter (Dn) of from 1 to 1 Torr. When the Dv/Dn is from 1 to 10, it has excellent ink fixing property when used for an ink fixing agent, and is excellent in heat resistance, flame retardancy, bending property, and catalytic function when added to a resin or the like. It is also resistant to acid and has good moisture resistance. Dv/Dn is preferably in the range of 1 to 8. The BET specific surface area of the magnesium oxide fine particles of the present invention is 5 mVg, and the volume-based 50% grain edge obtained by laser diffraction scattering particle size distribution measurement (DM is 〇.1 to 〇.5um, laser diffraction scattering type) The particle size distribution is determined by the volume ratio of the cumulative 10% particle size (Difl) to the volume-based 90% particle size (f) ratio D4. Below 1 。. Such oxidized town particles = shape: small, and excellent reaction It is suitable for use as a refractory additive, a resin filler, an electromagnetic steel sheet material, and a catalyst. Moreover, the shape of the 'small particle size variation is small' has excellent dispersibility, so 1 k 5 is used for south functionality. Materials, etc. The oxidized granules of the present invention are 2 〇 mVg or more, more preferably the u 2 T * surface area is preferably 乂η, more preferably 40 m/g or more, and D5G is preferably 杲η 9 3

〇♦, WD,. It is preferably 5 or less. Preferably, the range of the magnesium oxide fine particles of the present invention is 'the elution of the impurities is more than: -&quot; In functional materials. The oxygen day of the present invention: tantalum can be suitably used in a high mass% or more. The purity of the particles is preferably 99. £. The magnesium oxide bismuth of the present invention is preferably Fe'Ti, Ni, Cr, M〇323520 8 201219307 'f, and the content of the gum is 500 mass% or less. . The total amount of these people is right. * When the amount is less than 500 mils in the summer, the metal impurity is dissolved in the blister. It is suitable for use in additives, resin fillers, and highly functional materials. The content is preferably _ or less. Force 4 material section. In general, the magnesium oxide fine particles of the present invention preferably have a chlorine content of 5 liters or less. When the content is 5 〇〇 mass Å or less, the chlorine is extremely suppressed, and it is suitable for use as an additive material. Preferably, the content is less than or equal to the gamma quality. Preferably, the oxidized granules of the hair enthalpy are the volume-based average particle diameter ^" the ratio of the average particle diameter (10) of the solid number reference Dv/Dn is from i to 10. When the =L is at 1 to 1 G, the ink is applied to the fixing agent (4) of the ink. When it is added to the tree, the heat resistance, the flame retardancy, the bending property, the light diffusion effect, and the catalytic effect are good, and the acidity and the moisture resistance are good, and it is more preferably 1 to 8. The magnesium oxide fine particles of the present invention preferably have a citric acid activity (final rate of 40/.20.0 C) of 20 to 2 sec. The citric acid activity is excellent in reactivity to 2_(four)' occupational iron, and it can be suitably used as an insulating material for electromagnetic steel sheets and an insulating coating material for dust cores as an electromagnetic steel sheet. The citric acid activity is preferably from 2 to 5 sec. The magnesium hydroxide fine particles of the present invention are obtained by the following steps: preparing the magnesium carbonate aqueous solution (A); and gasifying the lock 7JC/liquid mixture with the i to 18N aqueous solution at a reaction rate Step 1 (8) to obtain a magnesium hydroxide slurry to 210 ribs; 323520 9 201219307 The hydrogenation is maintained at a concentration of lGi to the test. The severity of c, and the step of obtaining the hydrothermally treated gas-gas-locked mud (6); and the gas-oxidized town of Jiang, which is finely pulverized, washed and dried, obtained in the step of oxidizing the test particles (D) . Preferably m is to prepare the gas phase water soluble (four) (four). The aqueous solution of chlorine is =^0.410mol/L, _0.im, the production efficiency is not good. In addition, the viscosity is higher than the viscosity of the l0moi pulp, and the operation is paid from the 才 贝 虱 虱 虱 虱 05 05 05 05 05 05 05 05 05 05 05 05 05 05 05 05 05 05 05 05 Preferably, the step (A) of the emulsified aqueous solution is such that the step (A) may include the following steps: a step of preparing a crude aqueous magnesium chloride solution (Ay). The ratio is obtained by reacting an alkaline aqueous solution of 1 to UN with a reaction lb. Crude hydrogenation m step (A_2); after adding the aggregating agent to the coarse magnesium hydroxide slurry, the hydrogen and oxygen are used as the mash to obtain the vaporization % / 隼 precipitation, and the two m aggregating agent obtains the gas oxidized condensate to obtain gasification Step of the aqueous solution of the town (A-3). / A]) is a step-by-step magnesium preparation for coarse gasification of magnesium solution (for gasification of magnesium, gas can be used, for example, in chlorine town, bite, seawater μ Γ 6 water and water or anhydrous magnesium chloride or sea water, alkaline water Or bitter juice) added to the fat and refined to the conductivity of the water) and: = crude magnesium chloride solution can be used as two ^ 1 〇:, preferably (1) er, more preferably 2 to yang i / L steps (A - slave pair Pure pour water test, smear / 323520 10 201219307 30mol% way, react with hydrazine to 18N alkaline aqueous solution to obtain the crude magnesium hydroxide slurry. The reaction rate refers to the alkali required for all magnesium chloride to become magnesium hydroxide. The amount is calculated as l〇〇mol%. For example, 2〇〇m〇i% means the equivalent of 2 times the equivalent amount. For the alkaline aqueous solution, an aqueous sodium hydroxide solution can be used, and the concentration can be set. It is 1 to 18 mol/L, preferably 5 to 1 Smol/L, more preferably 10 to 18 mol/L. Step (A-3) is to filter magnesium hydroxide after adding a flocculating agent to the coarse magnesium hydroxide slurry. Obtaining a magnesium chloride solution for the filtrate, or adding a flocculating agent to cause the magnesium hydroxide to aggregate and precipitate, and obtaining the magnesium carbonate aqueous solution as the supernatant liquid. In the case of aggregating agent, the main component is acrylamide/sodium acrylate copolymer, acrylamide, acrylamide-methyl-2-methylpropane sulfonate copolymer, polypropylene decylamine, alkylamine group. A fourth-stage ammonium salt polymer of methacrylic acid, an acrylacrylic acid grade 4 ammonium salt, an acrylamide copolymer, a polyammine hydrochloride or the like, preferably acrylamide. Sodium acrylate copolymer. The amount of the aggregating agent added may be set to 1 〇〇 to 1 〇〇〇 mass ppm of the amount of dry magnesium hydroxide in the coarse magnesium hydroxide slurry. The concentration of the aqueous magnesium chloride solution obtained in this manner is The adjustment can be made to a concentration of 0.1 to 10. 〇mol/L of an aqueous solution of magnesium chloride. Step (B) is to obtain an aqueous solution of magnesium chloride with an aqueous solution of 1 to 18 N at a reaction rate of 101 to 210 mol% to obtain a hydroxide. The step of magnesium mud. When the reaction rate is less than l〇lm〇l%, the crystal growth is excessive in the hydrothermal treatment of magnesium hydroxide mud, and the particle size will become too large. Also, when the anti-deer rate is 323520 11 201219307 than 21 〇111〇1% south, the shell lJ is specified by the high pressure dad container The elements (Fe, Ti, Ni, Cr'Mo and Μη) are eluted and easily mixed with impurities. The reaction rate is better ^ 103 to 200 _ 'more preferably 1 〇 5 to 18 〇 1%. ^ Qualitative, solution Preferably, the aqueous solution of sodium hydroxide has a concentration of 1 to 18 mol/L. When the concentration of hydrogen A axis reading (four) is less than lmQl/L, the production efficiency is not t X, and when the agricultural degree is higher than 18 m〇1/L, the nitrogen is nitrogen. The oxidized money mud is similar in its charm. The operability is not good. The concentration of sodium hydroxide water (4) is preferably 4 to 16 mol/L. (C) 搅拌 stir the magnesium hydroxide slurry and keep it at ιοί A step of obtaining a hydrothermally treated magnesium hydroxide slurry by a degree of separation of 2 〇〇C. . The hydrothermal treatment is carried out by pouring hydrogen and oxygen into a mud, for example, using a high pressure dad, and maintaining it at 101 C to 200 C while stirring. When the hydrothermal treatment temperature is lower than 101 C, the crystal does not grow, and aggregated particles are formed and the dispersion is not good. Further, when the hydrothermal treatment temperature is higher than the case, the occupational crystals are excessively grown, and the particle diameter tends to become excessively large. The hydrothermal treatment temperature is preferably from 1 〇 5 to (10). c. Hydrothermal treatment time u 〇. 5 to 3 hours. When the hydrothermal treatment time is in this range, the crystal growth and particle size can be controlled within a suitable range. The hydrothermal treatment time is preferably from 1 to 2 days. In order to obtain stable fine particles having a uniform particle size, if necessary, pure water may be used to adjust the concentration of the hydrothermal slurry of the hydrothermal treatment to 30 g/L to I50 g/L. Step (D) A step of obtaining the magnesium hydroxide fine particles by subjecting the hydrothermally treated oxidized slurry to excessive care, washing, and drying. The step (D) is a step (D-1) which may contain, for example,: 323520 12 201219307, the hydrothermally treated magnesium arsenate slurry is filtered and washed to obtain the first magnesia cake; a magnesium hydroxide mud cake, which is added to the dry magnesium hydroxide mass standard by 5 to 100 times, is stirred, filtered, and washed with water to obtain the first magnesium oxyapatite cake step (d-2); a magnesium hydroxide mudcake, and the second magnesium hydroxide mudcake' step (D-2) is repeated 1 to 20 times to obtain a high-purity magnesium hydroxide cake (D-3); The high-purity magnesium hydroxide cake is dried to obtain magnesium hydroxide microparticles (D~4). The step (D-1) is a step of filtering and washing the hydrothermally treated magnesium arsenate slurry to obtain the first magnesium sulphate cake. The water washing is carried out by adding dry magnesium hydroxide to the pure water of 5 to 1 times, preferably 20 to 5 times, of the mass basis after the passage of f. Step (D-2) is the first magnesium hydroxide mud cake, adding 5 to 1 times of pure water for the dry magnesium hydroxide mass basis amount, stirring, filtering, washing with water to obtain a second hydrogen The step of the magnesium oxide cake is the step of epulping washing. In this step, for example, the first magnesium hydroxide cake is charged with 5 to 100 times pure water on a dry magnesium hydroxide basis to obtain a second hydrogenation slurry, and the second hydrogen peroxide is obtained. The town gathers the mud, mixes it, filters it, and washes it to obtain the second gas-oxidized lock mud cake. The stirring is, for example, carried out at 10 to 5 (rc, at a rotation of 1 Torr to 8 rpm, G. 5 to 5 (4). After the end of the mixing, it is possible to use crepe paper, and the washing is possible. The person performs the 5,323,520, 2012, 2012,307 to 100 times of pure water on the basis of the quality of the magnesium oxide. The step (D-3) is to replace the first magnesium hydroxide cake, and the second magnesium hydroxide cake, The pulp of the step (D-2) is washed as a pass, and this step is repeated 1 to 20 times to obtain a step of obtaining a high-purity hydroxide cake. The step (EM) is a high-purity magnesium hydroxide cake. The step of obtaining magnesium hydroxide fine particles by drying. Thus, the magnesium hydroxide particles of the present invention can be obtained. The magnesium oxide fine particles of the present invention are the particles of the magnesium oxide particles of the present invention in the step (E). In the environment, it is obtained by calcination of 5 〇〇 to ^. C. In the middle of the process, for example, the magnesium powder in the atmosphere is at a speed of 1 to 2 〇ΐ / min (preferably 3 to 10 ° C). /min, more preferably to 5GQ °C to 112G °C, preferably to 6 () (rc to. (: calciner 〇Γ &quot; after 5〇〇t: to 12 ° ° C, preferably It is in the range of 600 to 800.: 5 hours, thereby obtaining the high-purity magnesium hydroxide mud biscuit obtained by the oxidized town particle drying of the present invention, and gently solving ==3) Microparticles: Oxygen purity and small particle size, and uniform magnesium hydroxide. In the various fields of the hydrogen peroxide of the present invention, there are + and emulsified particles, and in various formulas, arrogant and hexaphoric may be mentioned. (4) For the use of magnesium hydroxide microparticles, etc., as a _fill 1 additive, it can be used as a raw material for inkjet light ink fixing, flame retardant #!, ^, which can be used for the separation heat-resistant layer for secondary batteries, 'The modifier of the film (heat resistance, flexibility) 323520 14 201219307, etc. As a highly functional material, it can be used as a raw material for ceramics for fuel cells, a raw material for phosphors, and a material for superconducting film substrates. The tunnel barrier material used for the magneto-resistance (tmr, tunnel magnet〇resistance) element can be used as a catalyst for drainage treatment, exhaust treatment, etc. Further, the use of magnesium oxide microparticles is ancient. , 讦 高 high functional materials, and catalysts. The magnesium oxide fine particles can be used as a refractory in the case of utilizing their high activity, and can be used as a ceramic sintering aid or the like as an additive, and can be used as an ink filling agent for inkjet paper, and can be used as a resin filler. A raw material for separating a heat-resistant layer for a secondary battery, a modifier (heat resistance, and improved flexibility) of a film sheet, etc., as a highly functional village material, can be used as a refractive index adjuster for LED sealing tree, and light diffusion. Materials for ceramics, fuel cell materials, phosphor materials, materials for superconducting film substrates, tunneling magnetic yoke elements (tunneling materials for tunnel barriers, etc.), as electromagnetic steel sheet materials, can be used as insulation materials for electric steel sheets. The raw material, the insulating coating material for the powdered iron core, etc., can be used as a catalyst for drainage treatment and exhaust treatment. [Examples] &lt;Followingly, the present invention will be described in more detail by way of examples. However, the invention is not limited to these embodiments. The particle diameter, specific surface area, purity and activity of the obtained magnesium hydroxide fine particles and oxidized fine particles were measured by the following methods. (1) Measurement of the laser diffraction scattering type particle size distribution using a laser diffraction scattering type particle size distribution measuring apparatus (trade name: MT33〇〇, manufactured by Nikkiso Co., Ltd.), and measuring the cumulative 10% particle diameter of the volume basis 10), Accumulated 50% particle size of volume basis (D 5〇 and cumulative 90% of volume kite 15 323520 201219307 Particle size (D9.). Volume-based average particle size (Dv) and number-based average particle size (Dn) In the same manner, the BET specific surface area measurement method was used to measure the specific surface area by the bet method of the gas adsorption method using a specific surface area measuring device (trade name: Macsorbl 210, manufactured by Mounteck Co., Ltd.). (3) Magnesium hydroxide And mass spectrometry of magnesium oxide impurity elements to measure the impurity elements of the object (Ag, Al, B, Ba, Bi, Cd, Co,

Cr ′ Cu ′ Fe ′ Ga ′ In, κ, Li, Μη, Mo, Na, Ni, P, Pb, S,

Si ’Sr* ’ΤΙ ’V ’Zn ’Ti and Zr) were measured by dissolving the sample in an acid using an ICP emission spectrometer (trade name: SPS-5100' manufactured by Seiko Instruments Co., Ltd.). The amount of C1 was measured by dissolving the sample in an acid using a spectrophotometer (trade name: uv-2550, manufactured by Shimadzu Corporation). (4) Purity measurement method The purity of the nitrogen oxide town and the magnesium oxide fine particles is the total mass of the impurity substance measured by the above-mentioned "measurement method of magnesium hydroxide and magnesium oxide impurity amount" by 1% by mass. It is calculated as a measurement. (5) The citric acid activity (40%) is determined by weighing 0.4% of the magnesium oxide solution in an amount of 40% of the magnesium oxide solution. The magnesium nitrate microparticles were added to the aqueous solution of the citric acid, and the time during which all of the citric acid reacted with the oxidative lock was measured, that is, the time required to exceed ρΗ7 was measured. (Example 1) 16 323520 201219307 As a crude gasification magnesium solution, water each having a purity (10) mass% or more and a concentration of .5 mol/L was prepared. In the chlorinated aqueous solution, pure water (purified by the exchange resin and refined to a water having the following conductivity) was added to adjust the concentration to obtain a coarse magnesium carbonate aqueous solution having a degree of infiltration of 2. 〇 mol/L. The solution of the crude magnesium chloride solution having a concentration of 〇mQl/L is added with a concentrated aqueous solution of sodium hydroxide in a concentration of .NM/L, and the reaction rate is (4) and the reaction is carried out. Further, as a coagulant, the propylamine is used. The sodium acrylate copolymer adds 5 〇〇 ppm to the hydrogen hydroxide, and the magnesia agglomerates the sulphate, and removes the supernatant liquid, thereby obtaining an aqueous solution of magnesium chloride. Adjusting the concentration of the obtained magnesium hydride solution to a concentration of 2气m〇l/L gasification town aqueous solution. The gasification town aqueous solution is reacted with a sodium hydroxide aqueous solution having a concentration of 17.84mQl/L, and the reaction rate is 200Π1Ο1%, and the hydrogen concentration is adjusted to 1〇〇g/L. Magnesium oxide slurry. The obtained magnesium hydroxide mud was stirred with a high pressure dad for 15 hours while maintaining a temperature of 1 Torr, and subjected to hydrothermal treatment (heating and stirring treatment). The hydrothermally treated first magnesium hydroxide slurry was filtered and washed with water. Thereby, the first magnesium hydroxide cake was obtained. The water washing was carried out by adding pure water which was 40 times by mass based on the dry magnesium hydroxide after filtration. Next, the first magnesium hydroxide obtained was obtained. Mud cake for pulp washing In the pulp washing, first, the dry magnesium hydroxide relative to the first magnesium hydroxide cake is put into 40 times of pure water on a mass basis to obtain a second magnesium hydroxide slurry. Next, the first The magnesium hydroxide slurry of the second is stirred at a normal temperature using a stirring device at a rotational speed of 500 rpm for a few hours, and then the second magnesium hydroxide slurry after the stirring is completed, using a filter paper transition, 323520 17 201219307 will be relative to the dry oxidized hydroxide. Magnesium is 20 times pure water on a mass basis, and after filtration, it is put into water and washed to obtain a second magnesium hydroxide cake. The above-mentioned pulp is washed once, and then the pulp is washed 10 times. Thereby, a high-purity magnesium hydroxide mud cake is obtained. The high-purity magnesium hydroxide mud cake is dried to obtain high-purity magnesium hydroxide fine particles. (Example 2) The reaction rate in the reaction of the chlorinated aqueous solution and the aqueous sodium hydroxide solution is changed. In the same manner as in Example 1 except that the hydrothermal treatment time was changed to 0.5 mol%, the reaction rate in the reaction of the aqueous solution of ruthenium chloride and the aqueous sodium ruthenium oxide solution was changed to 105 m〇r/. The same procedure as in Example 1 was carried out except that the heat treatment time was changed to 3 hours. (Example 4) The hydrothermal treatment temperature was changed to 130 ° C, and the aqueous sodium hydroxide solution was diluted with pure water to 8.92 mol/L, and the same as in Example 1. (Example 5) The hydrothermal treatment temperature was changed to 105 ° C, and the magnesium hydroxide slurry to be hydrothermally treated was changed to 130 g/L, and the same procedure as in Example 1 was carried out. 18 323520 201219307 (Example 6) Hydrogen peroxide The aqueous sodium hydroxide solution was diluted with pure water to 4.96 mol/L, and was carried out in the same manner as in Example 1. (Example 7) The magnesium hydroxide slurry to be hydrothermally treated was diluted with pure water to obtain 50 g/L, and Examples 1 is also implemented. (Comparative Example 1) The same procedure as in Example 1 was carried out except that the reaction rate in the reaction between the chlorinated aqueous solution and the aqueous sodium hydroxide solution was changed to 250 mol%. (Comparative Example 2) The reaction was carried out in the same manner as in Example 1 except that the reaction rate in the reaction between the aqueous magnesium chloride solution and the aqueous sodium hydroxide solution was changed to 90 mol%. (Comparative Example 3) The reaction rate in the reaction between the aqueous magnesium chloride solution and the aqueous sodium hydroxide solution was changed to 105 mol%, and the same as in Example 1 except that the hydrothermal treatment was not carried out. (Comparative Example 4) The same procedure as in Example 1 was carried out except that the aqueous sodium hydroxide solution was changed to 21 mol/L in pure water. 19 323520 201219307 (Example 8) The magnesium hydroxide fine particles prepared in Example 1 were calcined at 1000 ° C for 1 hour in an atmosphere to obtain magnesium oxide fine particles. (Example 9) Magnesium oxide fine particles prepared in Example 3 were calcined at 600 ° C for 1 hour in an atmosphere to obtain magnesium oxide fine particles. (Comparative Example 5) The magnesium hydroxide fine particles prepared in Example 1 were obtained by calcining at 140 (TC) for 1 hour in an atmosphere to obtain magnesium oxide fine particles. The obtained by the above examples and comparative examples were as follows. The measurement results of the magnesium hydroxide fine particles are shown in the first table, and the measurement of the magnesium oxide fine particles is completed, and is shown in the second table. The magnesium hydroxide fine particles and the magnesium oxide fine particles of the examples all have a purity of 99.9 mass%/◦ or more. The particle size is small and uniform. 20 323520 201219307 &lt;1—I hiding (% by mass) 1 &gt;99.9 1 &gt;99.9 | &gt;99.9 &gt;99.9 &gt;99.9 &gt;99.9 &gt;99.9 &gt;99.9 &gt; 99.9 丨&gt;99.9 &gt;99.9 Impurity quantity ^ ^ 5 〇IH cn inch CO CN Ό CS iH cs OO inch Ό »-Η v〇Cl (ppm) Pi inch 00 CO OO CM inch m 荨 OO 荨 S S ON令妨: 4 ! D90/D10 P inch · 〇 \ cn VO inch ' 0 inch · OO — Ο) On 1 can not measure CO US particle size Dv / Dn 00 inch (N CN cn CN «-Η cs P; &lt ;N OO m ro CN j 11.99 1 Cannot measure CN inch oi j D90 (μιη). 1 〇〇\ 00 〇〇\ 00 0 1 0,574 1 l 0.467 1 1 0.759 1 i .855 I 12.105 [24.29 Cannot measure 0.911 D50 (μπι) | 0.473 I | 0.375 I 1 0.383 1 1 0.287 1 I 0.183 I 1 0.438 1 1 0.483 1 0.846 I σ\ cs CN Cannot measure 0.569 Dio (μπι) | 0.178 | 0.224 | ! 0.183 1 ! 0.147 1 0.102 1 0.192 1 OO 0 0.183 0.248" 1 Cannot measure 0.173 BET ratio; Surface area (m2/g) | 10.87 1 inch 〇 \ 1 17.15 1 18.63 22.27 11.87 49.66 16.81 16.71 1 97.16 17.20 Condition Magnesium Hydroxide Mud Concentration Cff/L) 〇〇〇0 〇〇0 CO 〇0 tH Ο 〇1-H 0 r*^ Sodium hydroxide concentration (mol/L) 17.84 | 17.84 I 1 17.84 I cs 〇\ 06 17.84 Ό ON I 17.84 I 17.84 1 17.84 I 丨17.8/4 Se ^ 隹έ rH 〇m TH rH tH iH τ-Η 1 Temperature (°C) 〇ι〇〇m 0 0 cn 0 〇〇»£) 〇Ο 1 〇1-H Reaction rate (mol%) 〇(N 0 CN IH 0 〇CN 0 0 &lt;N 0 CN 〇&lt;N CN S rH 〇CN | Example 11 1 Example 2 I 1 Example 31 1 Example 4 I 1 Example 5 I Example 61 1 Example 7 I 匕 Comparative Example 11 [^ 匕 Comparative Example 2 1 Comparative Example 3 Comparative Example 4 21 323520 201219307 1^1 Ό 2252 Purity (% by mass) &gt;99.9 &gt;99.9 &gt;99.9 Impurity content Total content of Fe, Ti, Ni, Cr, Mo and Μη (PPm) Μ σ σ\ Cl (ppm) CN v〇00 rH Particle size distribution 00 CO S Particle size Q ο v〇CO 00 ra CO σ\ 00 D90 (μιη) 0.855 0.486 1.428 〇5〇(μιη) 0.483 0.193 i 1 0.862 1 Dio (μιη) 〇〇ί-Η d 0.112 0.235 BET specific surface area (m2/g) 49.66 41.63 g Condition of calcination (°C) 1000 〇v〇1400 Magnesium hydroxide slurry concentration (g/L) 0 rH 〇r~H 〇rH “铋〇 17.84 17.84 17.84 Se ^ World 3 r*H 1— H temperature (°C) 〇r*H Reaction rate (mol%) 〇(N s rH 〇cN Example 8 Example 9 Comparative Example 5 22 323520 201219307 (industrial use possibility) The hydroxide particle of the present invention The oxygen-cut microparticles are high-purity and 'uniform' and have good dispersibility (small platelet distribution (fine)), and are highly useful in the field of the sample. χ, according to the hair: two of the above particles, the convenience is high. For example, in the case of use of hydrogen oxygen = sub-, a force can be added, a resin filler, a moon-like material, and a catalyst. η力黑定° can be used as an additive for inkjet inks, etc.; as a raw material for resin filling, a flame retardant, and a modification of film sheets. Heat resistance, etc.; for high functionality (4), there are (four) = heat resistance 'material improvement" treatment. As a catalyst, there are drainage treatment, and exhaust gas addition and tree = use, refractory, addition, etc. 〆Return to this material, electromagnetic steel plate material and catalyst, etc. It can be used for: as a refractory, there is a filler for ceramics sintering aid, two Ray, ink-printing agent for ink paper, etc.; as a resin agent (heat-resistant heat-resistant layer of raw materials, film sheet seal The refractive index of the resin is used as a highly functional material, and is used for LED raw materials, phosphor light diffusing agents, ceramic cells for fuel cells (10), raw materials for superconducting thin film substrates, and magnetic reluctance members. As a material for the electromagnetic barrier steel plate 323520 23 201219307, it is used as a raw material for an insulating material for electromagnetic steel sheets and an insulating coating material for a powdered iron core, and is used as a catalyst for drainage treatment and exhaust treatment. [Simple description of the diagram] None. [Main component symbol description] None. 24 323520

Claims (1)

201219307 VII 1. Patent application scope: - A kind of magnesium hydroxide microparticles with a BET specific surface area of 5 laser diffraction scattering particle size - 'Accumulate the particle size (5) in the volume of 〇1 to 〇5疋Volume 2 obtained from the basis of the cumulative distribution measurement;; cumulative 10% particle size (Dh) of the laser diffraction scattering type particle size reference and cumulative 9°% granular green of the body =. ) than D4. It is 10 or less, and the tonnage is 99.5 mass% or more. Ά 2 · For example, the bismuth magnesium oxide granules described in the scope of the patent scope, Hall 1, Road, +, Λ + nn, j: ton is 99.9 mass% or more. 3. For example, the scope of the patent application is 哎篦9ή, where Fe, Ti, NrCrT, ^500 are below the quality. M. And the total content of the oxidized granules as described in any one of the above-mentioned claims, wherein the chlorine content is below _mass. 6. 5. The gas-oxidized granule fine particles according to any one of the items 4 to 4, wherein the ratio of the volume-based average particle diameter (f) to the virtual number-based average particle diameter (Dn) is /. - Oxidized town microparticles, the BET specific surface area of 5 mVg or more of the diffraction diffraction filament fraction _ method obtained from the _ product basis 50% particle size (five) is 〇.! to 〇. 5 (10), laser diffraction scattering particle size distribution determination The volume-based g-product (10) particle diameter obtained by the method (D ^ disk volume basis of the cumulative 90% particle diameter (D9fl) ratio WDi. 1 〇 to 99.5 mass% or more. The magnesium oxide fine particles according to the sixth aspect, wherein the purity is 323520 1 201219307, which is 99.9% by mass or more. 8. The magnesium oxide fine particles according to claim 6 or 7, wherein 卩6, The oxidized town granules of any one of the above-mentioned items of the ninth aspect of the present invention, wherein The magnesium oxide microparticles according to any one of claims 6 to 9 have a citric acid activity (40%) of 20 to 2000 seconds. The magnesium oxide fine particles according to any one of claims 6 to 10, wherein the volume-based average particles The ratio Dv/Dn of the average particle diameter (Dn) of (Dv) to the number standard is 1 to 10. 12. A method for producing an argon magnesium oxide fine particle, comprising the steps of: preparing a magnesium carbonate aqueous solution (A): a step (B) of obtaining a magnesium hydroxide slurry by reacting a chlorinated aqueous solution with an aqueous solution of 1 to 18 N at a reaction rate of 101 to 210 mol%; maintaining the magnesium hydroxide slurry while maintaining 101 a step (C) of obtaining a hydrothermally treated magnesium hydroxide slurry at a temperature of 200 ° C; and a step (D) of collecting the water-treated magnesium hydroxide slurry by filtration, washing with water and drying to obtain oxidized granules 13. The method for producing magnesium hydroxide particles according to claim 12, wherein the step (D) comprises the steps of: filtering the hydrothermally treated magnesium hydroxide slurry and washing with water to obtain 2 323520 201219307 The step of obtaining the first magnesium hydroxide cake; adding the pure water of 5 to 100 times the mass basis of the dry magnesium hydroxide in the first magnesium hydroxide cake, stirring, filtering, washing with water Obtaining the second hydroxide Magnesium cake step (D_2); instead of the first magnesium hydroxide cake, and for the second magnesium hydroxide cake, step (D-2) is repeated 1 to 2 times to obtain high-purity magnesium hydroxide a step (D-3) of the mud cake; and a step (D-4) of drying the high-purity magnesium hydroxide cake to obtain the hydroxide particles. 14. As described in claim 12 or item 13 The method for producing an argon magnesium oxide fine particle, wherein the step (A) comprises the following steps: a step of preparing a crude magnesium chloride aqueous solution (A-I); and a crude magnesium chloride aqueous solution and an aqueous solution of 1 to 18 N at a reaction rate 1 to 30 mol% of the reaction, to obtain the crude argon magnesium oxide slurry step (A-2); and after adding the aggregating agent to the coarse magnesium hydroxide slurry, the magnesium hydroxide is used as a filtrate to obtain a magnesium chloride solution, or to add agglomeration And a step (A-3) of obtaining an aqueous solution of magnesium chloride as a supernatant liquid by agglomerating the magnesium oxynitride. A method for producing a magnesium oxide fine particle, comprising: the magnesium hydroxide fine particles according to any one of claims 1 to 5, or the items 12 to 14 of the scope of the patent application The magnesium hydroxide fine particles obtained by the method according to any one of the steps (E) calcined at 5 Torr to 1500 ° C in an atmosphere. 3 323520 201219307 IV. Designated representative map: There is no schema in this case. (1) The representative representative of the case is: No.驷 (2) The symbol of the symbol of this representative figure is simple: None. 5. If there is a chemical formula in this case, please disclose the chemical formula that best shows the characteristics of the invention: There is no chemical formula in this case. 323520