WO2016163562A1 - Particules d'hydroxyde de magnésium et leur procédé de production - Google Patents

Particules d'hydroxyde de magnésium et leur procédé de production Download PDF

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WO2016163562A1
WO2016163562A1 PCT/JP2016/061957 JP2016061957W WO2016163562A1 WO 2016163562 A1 WO2016163562 A1 WO 2016163562A1 JP 2016061957 W JP2016061957 W JP 2016061957W WO 2016163562 A1 WO2016163562 A1 WO 2016163562A1
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magnesium hydroxide
hydroxide particles
magnesium
particles
weight
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PCT/JP2016/061957
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Japanese (ja)
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興東 王
康平 大堀
純子 武藤
浩一 根立
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協和化学工業株式会社
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    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
    • C01F5/00—Compounds of magnesium
    • C01F5/02—Magnesia
    • C01F5/06—Magnesia by thermal decomposition of magnesium compounds
    • C01F5/08—Magnesia by thermal decomposition of magnesium compounds by calcining magnesium hydroxide
    • 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
    • C01F5/14—Magnesium hydroxide
    • C01F5/22—Magnesium hydroxide from magnesium compounds with alkali hydroxides or alkaline- earth oxides or hydroxides
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK  ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
    • C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
    • C09C1/02—Compounds of alkaline earth metals or magnesium
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK  ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
    • C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
    • C09C3/08—Treatment with low-molecular-weight non-polymer organic compounds
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
    • C09K21/00—Fireproofing materials
    • C09K21/02—Inorganic materials

Definitions

  • the present invention relates to magnesium hydroxide particles having a fine and uniform particle size, high purity and excellent dispersibility, and a method for producing the same.
  • Magnesium hydroxide is widely used as a flame retardant for polymer materials, highly functional materials, catalysts and the like. Magnesium oxide is used as a fiber acid acceptor, electromagnetic steel material, resin filler, catalyst, catalyst carrier, and the like. In order to exhibit excellent performance in these applications, the magnesium hydroxide particles and the magnesium oxide particles are required to have fine and uniform particle diameters, high purity, and excellent dispersibility.
  • a method for producing fine magnesium hydroxide particles there is disclosed a method of producing magnesium hydroxide particles of 5 to 80 nm by vapor phase oxidation method, and further contacting these magnesium oxide particles with water vapor to produce magnesium hydroxide. (Patent Document 1). This method is expensive to manufacture and difficult to produce in large quantities.
  • Patent Document 2 describes a method of producing magnesium hydroxide particles by reacting an aqueous magnesium chloride solution and an aqueous alkaline solution to produce a magnesium hydroxide slurry, and maintaining the temperature at 101 to 200 ° C. In this manufacturing method, since the time for growing the crystal is short, the aggregate formed immediately after the synthesis grows while maintaining the aggregation.
  • the finally obtained magnesium hydroxide particles contain a large amount of agglomerates, so that it is difficult to obtain those having excellent dispersibility.
  • this manufacturing method when there are many alkali raw materials, since impurities elute from an autoclave and an impurity mixes, it is necessary to limit a reaction rate. JP 2007-137694 A JP 2012-72004 A
  • An object of the present invention is to provide magnesium hydroxide particles having a fine and uniform particle diameter, high purity and excellent dispersibility, and a method for producing the same.
  • Another object of the present invention is to provide magnesium oxide particles having a fine and uniform particle diameter, high purity and excellent dispersibility.
  • aqueous alkaline solution is an aqueous solution of sodium hydroxide. 4).
  • the resulting magnesium hydroxide particles are (A) The average secondary particle size (MV) is 50 to 800 nm, (B) D 50 / MV is 0.70 to 0.99, where D 50 is a volume-based cumulative 50% particle diameter by laser diffraction scattering particle size distribution measurement, (C) The OH desorption temperature in thermogravimetric analysis when heated at 10 ° C./min in an air atmosphere is 360 to 388 ° C., The manufacturing method of the preceding clause 1. 6).
  • the average secondary particle size (MV) is 50 to 800 nm
  • D 50 / MV is 0.70 to 0.99
  • D 50 is a volume-based cumulative 50% particle diameter by laser diffraction scattering particle size distribution measurement
  • C The OH desorption temperature in thermogravimetric analysis when heated at 10 ° C./min in an air atmosphere is 360 to 388 ° C., Magnesium hydroxide particles characterized by the above. 7). 7. Magnesium hydroxide particles according to item 6 above, wherein the Cl ion content is 50 to 300 ppm. 8). 7. Magnesium hydroxide particles according to item 6 above, wherein the content of SO 4 ions is 50 to 300 ppm. 9. 7.
  • FIG. 1 shows an X-ray diffraction spectrum (top) and library search results (bottom) of magnesium hydroxide particles (Example 1) that were heat-treated at 45 ° C. for 140 hours and then dried at 120 ° C. for 20 hours.
  • FIG. 2 is an SEM photograph of magnesium hydroxide particles (Example 3) taken at 50,000 times.
  • FIG. 3 is an SEM photograph of the surface-treated magnesium hydroxide particles (Example 7) taken at 50,000 times.
  • FIG. 4 shows the particle size distribution of magnesium hydroxide particles (Example 1) that were heat-treated at 45 ° C. for 140 hours and then dried at 120 ° C. for 20 hours.
  • FIG. 5 is a particle size distribution of magnesium hydroxide particles (Example 3).
  • FIG. 6 is a particle size distribution of the surface-treated magnesium hydroxide particles (Example 7).
  • FIG. 7 is an SEM photograph of a cross section of a resin composition in which 130 parts by weight of magnesium hydroxide particles (Example 3) are blended with 100 parts by weight of LLDPE resin at a magnification of 10,000 times.
  • FIG. 8 is an SEM photograph of a cross section of a resin composition obtained by mixing 130 parts by weight of magnesium hydroxide particles (Comparative Example D) with 100 parts by weight of LLDPE resin at a magnification of 10,000 times.
  • FIG. 9 shows a TG-DTA curve and OH desorption temperature of magnesium hydroxide particles (Example 1) that were heat-treated at 45 ° C. for 140 hours and then dried at 120 ° C.
  • FIG. 10 shows a TG-DTA curve and OH desorption temperature of magnesium hydroxide particles (Example 3). The desorption temperature of OH was 378.5 ° C.
  • FIG. 11 shows a TG-DTA curve and OH desorption temperature of magnesium hydroxide particles (Comparative Example A). The desorption temperature of OH was 389.3 ° C.
  • FIG. 12 shows a TG-DTA curve and OH desorption temperature of magnesium hydroxide particles (Comparative Example D). The desorption temperature of OH was 402.5 ° C.
  • FIG. 13 shows the X-ray diffraction spectrum (upper) and library search result (lower) of the magnesium oxide particles (Example 11).
  • FIG. 14 is a SEM photograph of magnesium oxide particles (Example 11) taken at 35,000 times.
  • FIG. 15 is a particle size distribution of magnesium oxide particles (Example 11).
  • FIG. 16 is a particle size distribution of magnesium oxide particles (Example 9).
  • the method for producing magnesium hydroxide particles of the present invention includes each step of a reaction step (i), a heat treatment step (ii), a separation and purification step (iii), and a drying step (iv).
  • the reaction step (i) is a step of producing a slurry containing magnesium hydroxide particles by reacting an aqueous solution of a soluble magnesium salt with an aqueous alkaline solution.
  • Soluble magnesium salt A soluble magnesium salt can be used as the magnesium raw material.
  • the soluble magnesium salt examples include magnesium chloride, magnesium chloride dihydrate, magnesium chloride hexahydrate, magnesium nitrate, magnesium acetate, magnesium sulfate, and bitter juice.
  • magnesium chloride or magnesium sulfate is preferred.
  • the concentration of the soluble magnesium salt is preferably 0.1 to 5.7 mol / L, more preferably 0.5 to 5.5 mol / L, and still more preferably 1.0 to 5.0 mol / L.
  • a magnesium chloride aqueous solution it is preferably 0.1 to 5.7 mol / L, more preferably 0.5 to 5.5 mol / L, and still more preferably 1.0 to 5.0 mol / L.
  • a magnesium sulfate aqueous solution When a magnesium sulfate aqueous solution is used, it is preferably 0.1 to 4.6 mol / L, more preferably 0.5 to 4.4 mol / L, and still more preferably 1.0 to 4.2 mol / L. .
  • alkali alkali
  • the alkaline aqueous solution include aqueous solutions of sodium hydroxide, potassium hydroxide, ammonia and the like.
  • the aqueous alkaline solution is preferably an aqueous solution of sodium hydroxide.
  • the concentration of the alkaline aqueous solution is preferably 1.0 to 18.0 N, more preferably 2.0 to 15.0 N, and still more preferably 3.0 to 12.0 N.
  • reaction rate The reaction rate between the aqueous solution of the soluble magnesium salt and the alkaline aqueous solution is 50 to 400 mol%, preferably 60 to 350 mol%, more preferably 80 to 300 mol%, as magnesium.
  • the heat treatment step is a step of heat treating the obtained slurry at 0 to 100 ° C. for 5 to 500 hours under atmospheric pressure.
  • the heat treatment is performed under atmospheric pressure.
  • the obtained magnesium hydroxide particles have both a primary particle size and a secondary particle size that are increased if the heat treatment time is lengthened, and aggregates are contained if the heat treatment time is shortened. And dispersibility will deteriorate. Therefore, the heat treatment temperature is 0 to 100 ° C., preferably 0 to 95 ° C., more preferably 20 to 90 ° C., and further preferably 35 to 85 ° C. Within this range, the crystal growth of the primary particles of magnesium hydroxide is difficult to promote, and the heat treatment time can be extended.
  • the heat treatment time is 5 to 500 hours, preferably 8 to 400 hours, more preferably 10 to 300 hours.
  • the magnesium hydroxide agglomerates generated in the reaction step are sufficiently separated, and hydrogen bonding and capillary action between the fine particles after drying are suppressed, so that the dispersibility having a uniform particle size is achieved. Excellent magnesium hydroxide particles can be obtained.
  • the separation and purification step is a step of separating and purifying the cake containing magnesium hydroxide particles from the heat-treated slurry.
  • the magnesium hydroxide cake can be separated by filtration. You may filter, washing with water. Purification can be performed by washing with water.
  • the water washing it is preferable to resuspend the magnesium hydroxide cake while stirring the magnesium hydroxide cake and water, and then filter this to obtain the magnesium hydroxide cake again.
  • the water is preferably washed in 1 to 4 portions, and more preferably in 1 to 3 portions.
  • the amount of water is preferably 5 to 100 times that of magnesium hydroxide particles on a weight basis.
  • the conductivity (purity) of water is preferably 100 ⁇ S / cm or less, more preferably 10 ⁇ S / cm or less, and even more preferably 0.5 ⁇ S / cm or less.
  • the temperature of water and the water bath at the time of stirring can be 10 to 80 ° C.
  • the stirring speed can be 100 to 800 rpm
  • the stirring time can be 0.5 to 5 hours.
  • impurities in the magnesium hydroxide can be removed by washing with water, the magnesium hydroxide particles obtained after drying aggregate and deteriorate dispersibility. Therefore, in order to obtain magnesium hydroxide particles with few impurities and excellent dispersibility, it is required to reduce impurities contained in magnesium hydroxide after heat treatment and reduce the amount of water used for washing.
  • the heat treatment temperature is 0 to 100 ° C.
  • the crystal structure has a thermodynamically unstable characteristic as compared with magnesium hydroxide produced at a higher heat treatment temperature.
  • the drying step is a step of drying the magnesium hydroxide cake. Drying can be performed by a known method.
  • the magnesium hydroxide particles of the present invention have a chemical composition represented by Mg (OH) 2 .
  • the magnesium hydroxide particles of the present invention have an average secondary particle size (MV) of 50 to 800 nm, preferably 80 to 600 nm, more preferably 100 to 500 nm after the drying step.
  • the D 50 of the magnesium hydroxide particles of the present invention is preferably 35 to 792 nm, more preferably 57.6 to 594 nm, and even more preferably 75 to 495 nm.
  • the D 50 / MV of the magnesium hydroxide particles of the present invention is 0.70 to 0.99, preferably 0.72 to 0.99, more preferably 0.75 to 0.99.
  • D 50 is a cumulative 50% particle diameter on a volume basis by a laser diffraction scattering particle size distribution measurement.
  • the D 90 / D 10 of the magnesium hydroxide particles of the present invention is preferably 4 or less, more preferably 3.8 or less, and even more preferably 3.5 or less.
  • the magnesium hydroxide particles of the present invention have an OH desorption temperature of 360 to 388 ° C., preferably 365 to 386 ° C., more preferably 370 to 385 ° C.
  • the magnesium hydroxide particles of the present invention are heat-treated at a low temperature of 0 to 100 ° C., the crystal structure is characterized by thermodynamically unstable as compared with magnesium hydroxide heat-treated at a higher temperature. Therefore, the magnesium hydroxide particles of the present invention have a lower OH desorption temperature in thermogravimetric analysis than magnesium hydroxide produced by heat treatment at a temperature higher than 100 ° C. As a result, the flame retardancy is excellent.
  • the BET specific surface area of the magnesium hydroxide particles of the present invention is preferably 8.0 to 280 m 2 / g, more preferably 10.0 to 250 m 2 / g, still more preferably 15.0 to 200 m 2 / g.
  • the content of Cl ions in the magnesium hydroxide particles is preferably 50 to 300 ppm, more preferably 50 to 270 ppm, and still more preferably 50 to 250 ppm.
  • the crystal structure of the magnesium hydroxide particles of the present invention is thermodynamically unstable, can easily remove Cl ions by purification, and has a low Cl ion content.
  • the content of SO 4 ions in the magnesium hydroxide particles of the present invention is preferably 50 to 300 ppm, more preferably 50 to 270 ppm, and still more preferably 50 to 250 ppm.
  • the crystal structure of the magnesium hydroxide particles of the present invention is thermodynamically unstable, and SO 4 ions can be easily removed by purification, and the content of SO 4 ions is small.
  • the purity of the magnesium hydroxide particles of the present invention is preferably 99.5% or more, more preferably 99.6% or more, and further preferably 99.7% or more.
  • the total content of Cr, Ni, Ti, Mn, Mo, Fe, Zn, Al, Cd, Co, Pb and Zr in the magnesium hydroxide particles of the present invention is preferably 10 to 150 ppm, more preferably 15 to 100 ppm. Yes, more preferably 20 to 80 ppm.
  • the crystal structure of the magnesium hydroxide particles of the present invention is thermodynamically unstable, metal impurities can be easily removed by purification, and the content of metal impurities is small.
  • the magnesium oxide particles of the present invention have a chemical composition represented by MgO.
  • the magnesium oxide particles of the present invention can be obtained by firing the magnesium hydroxide particles of the present invention, preferably at 350 to 1200 ° C.
  • the firing temperature is more preferably 400 to 1100 ° C, still more preferably 500 to 1000 ° C.
  • the magnesium oxide particles of the present invention have an average secondary particle size (MV) of preferably 50 to 800 nm, more preferably 80 to 600 nm, and still more preferably 100 to 500 nm.
  • the D 50 of the magnesium oxide particles of the present invention is preferably 35 to 792 nm, more preferably 57.6 to 594 nm, and further preferably 75 to 495 nm.
  • D 50 / MV The D 50 / MV of the magnesium oxide particles of the present invention is preferably 0.70 to 0.99, more preferably 0.72 to 0.99, and even more preferably 0.75 to 0.99.
  • D 50 is a volume-based cumulative 50% particle diameter measured by laser diffraction scattering type particle size distribution measurement.
  • the D 90 / D 10 of the magnesium oxide particles of the present invention is preferably 4 or less, more preferably 3.8 or less, and even more preferably 3.5 or less.
  • the BET specific surface area of the magnesium oxide particles of the present invention is preferably 1.0 to 280 m 2 / g, more preferably 5.0 to 250 m 2 / g, still more preferably 10.0 to 200 m 2 / g.
  • purity The purity of the magnesium oxide particles of the present invention is preferably 99.5% or more, more preferably 99.6% or more, and further preferably 99.7% or more.
  • the total content of Cr, Ni, Ti, Mn, Mo, Fe, Zn, Al, Cd, Co, Pb and Zr in the magnesium oxide particles of the present invention is preferably 10 to 150 ppm, more preferably 15 to 100 ppm, Preferably it is 20 to 80 ppm.
  • the magnesium hydroxide particles and magnesium oxide particles of the present invention are preferably surface-treated depending on the application.
  • a known compound can be used as the surface treatment agent.
  • the surface treatment agent is preferably at least one selected from the group consisting of higher fatty acids, anionic surfactants, higher fatty acid alkaline earth metal salts, coupling agents, phosphoric esters comprising phosphoric acid and higher alcohols, and silicone oils. .
  • higher fatty acids include stearic acid, erucic acid, palmitic acid, lauric acid, and behenic acid.
  • Anionic surfactants include polyethylene glycol ether sulfate, amide bond sulfate, ester bond sulfate, ester bond sulfonate, amide bond sulfonate, ether bond sulfonate, ether bond alkylaryl sulfonic acid. Examples thereof include salts, ester-bonded alkyl aryl sulfonates, and amide-bonded alkyl aryl sulfonates.
  • Examples of the higher fatty acid alkaline earth metal salt include alkaline earth metal salts such as magnesium, beryllium, calcium, and barium.
  • Examples of coupling agents include r- (2-aminoethyl) aminopropyltrimethoxysilane, r- (2-aminoethyl) aminopropylmethyldimethoxysilane, r-methacryloxypropyltrimethoxysilane, N- ⁇ - ( N-vinylbenzylaminoethyl) -r-aminopropyltrimethoxysilane / hydrochloride, r-glycidoxypropyltrimethoxysilane, r-mercaptopropyltrimethoxysilane, methyltrimethoxysilane, methyltriethoxysilane, vinyltriacetoxy Silane, r-chloropropyltrimethoxysilane, hexamethyldisilazane, r-anil
  • Examples of phosphoric acid esters composed of phosphoric acid and higher alcohols include phosphoric acid esters composed of orthophosphoric acid and oleyl alcohol, lauryl alcohol, myristyl alcohol, palmityl alcohol or stearyl alcohol.
  • Examples of the silicone oil include dimethyl silicone oil, methyl hydrogen silicone oil, methyl phenyl silicone oil, and cyclic dimethyl silicone oil.
  • the surface treatment can be performed by a known wet method and dry method. In the wet method, the amount of the surface treatment agent added is preferably 0.5 to 15 parts by weight, more preferably 1.0 to 12 parts by weight, and still more preferably 100 parts by weight of magnesium hydroxide particles and magnesium oxide particles. 2.0 to 10 parts by weight.
  • the surface treatment temperature is preferably 0 to 100 ° C., more preferably 20 to 90 ° C., and further preferably 40 to 80 ° C.
  • the resin composition of the present invention contains 100 parts by weight of a synthetic resin and 0.01 to 350 parts by weight of the magnesium hydroxide particles.
  • synthetic resins polymers or copolymers of C2 to C8 olefins ( ⁇ -olefins) such as polyethylene, polypropylene, ethylene / propylene copolymers, polybutene, poly-4-methylpentene-1, etc., these olefins and dienes These copolymers are mentioned.
  • ethylene-acrylate copolymer polystyrene, ABS resin, AAS resin, AS resin, MBS resin, ethylene / vinyl chloride copolymer resin, ethylene vinyl acetate copolymer resin, ethylene-vinyl chloride-vinyl acetate graft polymer resin, vinylidene chloride, polychlorinated Vinyl, chlorinated polyethylene, chlorinated polypropylene, vinyl chloride copolymer, vinyl acetate resin, phenoxy resin, polyacetal, polyamide, polyimide, polycarbonate, polysulfone, polyphenylene oxide, polyphenylene sulfide, polyethylene terephthalate, polybutylene terephthalate, methacrylic resin, etc.
  • thermoplastic resin can be illustrated.
  • thermosetting resins such as epoxy resins, phenol resins, melamine resins, unsaturated polyester resins, alkyd resins, and urea resins
  • synthetic rubbers such as EPDM, butyl rubber, isoprene rubber, SBR, NBR, chlorosulfonated polyethylene, NIR, urethane rubber, butadiene rubber, acrylic rubber, silicone rubber, and fluorine rubber can be exemplified.
  • the compounding amount of the magnesium hydroxide particles is 0.01 to 350 parts by weight, preferably 0.1 to 320 parts by weight, more preferably 0.5 to 300 parts by weight with respect to 100 parts by weight of the synthetic resin.
  • the resin composition of the present invention contains 100 parts by weight of a synthetic resin and 0.01 to 350 parts by weight of the magnesium oxide particles.
  • the synthetic resin is preferably at least one selected from the group consisting of thermoplastic resins, thermosetting resins and rubbers.
  • thermoplastic resin polyethylene, copolymer of ethylene and ⁇ -olefin, ethylene and vinyl acetate, copolymer of ethylene and ethyl acrylate, copolymer of ethylene and methyl acrylate, polypropylene, propylene and others ⁇ -olefin copolymer, polybutene-1, poly-4-methylpentene-1, polystyrene, copolymer of styrene and acrylonitrile, copolymer of ethylene and propylene diene rubber or butadiene, polyvinyl acetate, polyvinyl Examples include alcohol, polyacrylate, polymethacrylate, polyurethane, polyester, polyether, polyamide, ABS, polycarbonate, and polyphenylene sulfide.
  • thermosetting resin examples include phenol resin, melamine resin, epoxy resin, unsaturated polyester resin, alkyd resin, and the like.
  • EPDM, SBR, NBR copolymerized rubber of ethylene and other ⁇ -olefins such as propylene, octene, butyl rubber, chloroprene rubber, isoprene rubber, chlorosulfonated rubber, silicone rubber, fluorine rubber, chlorinated butyl rubber.
  • examples include brominated butyl rubber, epichlorohydrin rubber, and chlorinated polyethylene rubber.
  • the content of magnesium oxide particles is 0.01 to 350 parts by weight, preferably 0.1 to 320 parts by weight, and more preferably 0.5 to 300 parts by weight with respect to 100 parts by weight of the synthetic resin.
  • Thermogravimetric analysis of the obtained magnesium hydroxide particles and magnesium oxide particles was performed using a thermal analyzer (TG-DTA 2000SA, manufactured by Bruker AXS). The sample weight was 10 mg, the air flow rate was 100 ml / min, and the heating rate was 10 ° C./min. (7) Flame Retardancy Evaluation and Appearance Evaluation of Resin Composition
  • the test specimen is composed of 100 parts by weight of LLDPE resin (linear low density polyethylene, Novatec LLUF-240, Nippon Polyethylene Co., Ltd.) and magnesium hydroxide particles as a flame retardant. 130 parts by weight were mixed and kneaded at 160 ° C.
  • press vulcanization treatment was performed at 153 ° C. for 30 minutes to prepare a sample.
  • the molded article for measuring compression set was subjected to a press vulcanization treatment for 40 minutes.
  • 200% modulus (M200), 400% modulus (M400), 600% modulus (M600) of vulcanized rubber, strength at break (TB), elongation at break (EB) and hardness (Shore A hardness) were measured.
  • vulcanized rubber was aged in an air atmosphere at 100 ° C. for 168 hours based on JIS K6257, and then the change in Shore A hardness was measured.
  • Example 1 At normal pressure and 20 ° C., put 6.5 L of 4.2 mol / L magnesium chloride aqueous solution into a 20 L stainless steel container, slowly add 6.5 L of 8.4 N aqueous sodium hydroxide solution while stirring, and let it react. The total volume of the solution was adjusted to 16 L with ionic water, and the slurry concentration was adjusted to 100 g / L. Next, the temperature of the water bath was set to 45 ° C., and heat treatment was performed under a stirring condition of 350 rpm.
  • Table 3 shows the distribution of the particles of the slurry after 1, 5, 24, 43, 48, 52, 69, 91, 115, 120, 123 and 140 hours after the start of the heat treatment. Further, the slurry after the heat treatment for 140 hours was filtered while adding 20 times the pure water (deionized water, 0.5 ⁇ S / cm) on a weight basis to the magnesium hydroxide particles to obtain magnesium hydroxide particles. On the other hand, it was washed twice with 25 times pure water on a weight basis and dried at 120 ° C. for 20 hours. As a result of analysis by an X-ray diffraction method, the obtained particles were magnesium hydroxide (Mg (OH) 2 ) particles (FIG. 1).
  • Example 2 At normal pressure and 20 ° C., put 6.5 L of 4.2 mol / L magnesium chloride aqueous solution into a 20 L stainless steel container, slowly add 9.1 L of 12.0 N sodium hydroxide aqueous solution with stirring, and let it react. The total volume of the solution was adjusted to 16 L with ionic water, and the slurry concentration was adjusted to 100 g / L. Thereafter, the temperature of the water bath was set to 60 ° C., and heat treatment was performed for 15 hours under a stirring condition of 350 rpm. Thereafter, in the same manner as in Example 1, filtration, washing with water and drying were performed to obtain magnesium hydroxide particles.
  • Example 3 Magnesium hydroxide particles were obtained in the same manner as in Example 1 except that the heat treatment temperature was changed to 70 ° C. and the heat treatment time was changed to 15 hours. Comparative Example A 800 ml of the same slurry as the slurry before heat treatment in Example 3 was taken and reacted in a 0.98 L autoclave (manufactured by Nitto Koatsu Co., Ltd.). Thereafter, the temperature was set to 150 ° C., and heat treatment was performed for 1 hour under a stirring condition of 500 rpm. Thereafter, filtration, washing with water and drying were performed in the same manner as in Example 1 to obtain magnesium hydroxide particles.
  • Example 4 Magnesium hydroxide particles were obtained in the same manner as in Example 3 except that the heat treatment temperature was changed to 90 ° C. Comparative Example B Magnesium hydroxide particles were obtained in the same manner as in Comparative Example A except that the heat treatment time was changed to 3 hours.
  • Example 5 At normal pressure and 20 ° C., put 6.5 L of 4.2 mol / L magnesium chloride aqueous solution into a 20 L stainless steel container, slowly add 3.9 L of 8.4 N sodium hydroxide aqueous solution with stirring, and react to remove. The total volume of the solution was adjusted to 10.6 L with ionic water, and the concentration of the slurry was 90 g / L.
  • Example C The temperature of the water bath was set to 70 ° C., and heat treatment was performed for 15 hours under a stirring condition of 350 rpm. Thereafter, filtration, washing with water and drying were performed in the same manner as in Example 1 to obtain magnesium hydroxide particles.
  • Comparative Example C 800 ml of the same slurry as the slurry before heat treatment of Example 5 was taken and reacted in a 0.98 L autoclave (manufactured by Nitto Koatsu Co., Ltd.), set at 150 ° C., and heat treated for 1 hour under stirring conditions of 500 rpm. Thereafter, in the same manner as in Example 1, filtration, washing and drying were performed to obtain magnesium hydroxide particles.
  • Example 6 At normal pressure and 20 ° C., 4.0 L of a 5.5 mol / L magnesium chloride aqueous solution is placed in a 20 L stainless steel container, and 8.25 L of 16.0 N sodium hydroxide aqueous solution is slowly added with stirring to react. The total volume of the solution was adjusted to 12.83 L with ionic water, and the concentration of the slurry was 100 g / L. The temperature of the water bath was set to 70 ° C., and heat treatment was performed for 15 hours under a stirring condition of 350 rpm.
  • Example 7 After processing in the same manner as in Example 3, surface treatment was performed with 3.0% by weight of stearic acid based on the solid content to obtain magnesium hydroxide particles.
  • Example 8 Magnesium hydroxide particles were obtained in the same manner as in Example 3 except that the magnesium raw material was changed to 4.2 mol / L MgSO 4 .
  • Example 9 Magnesium hydroxide particles were obtained in the same manner as in Example 1 except that the heat treatment temperature was changed to 20 ° C. and the heat treatment time was changed to 165 hours.
  • Example 10 Magnesium hydroxide particles were obtained in the same manner as in Example 1 except that the heat treatment temperature was changed to 99 ° C. and the heat treatment time was changed to 10 hours. (Relationship between heat treatment conditions and particle size distribution) In the method for producing magnesium hydroxide particles of the present invention, as is apparent from the distribution state of the slurry particles after the start of heat treatment (Table 3 (Example 1)), the aggregates produced during the reaction are separated as the heat treatment time becomes longer. It can be confirmed that the particles are fine and uniform. (About particle size distribution) The magnesium hydroxide particles of the present invention have a fine and uniform particle diameter regardless of the presence or absence of surface treatment. As can be seen from the SEM photograph (FIG.
  • the desorption temperatures of OH in the thermogravimetric analysis of the magnesium hydroxide particles of the present invention are 382.4 ° C. (FIG. 9 (Example 1)) and 378.5 ° C. (FIG. 10 (Example 3)). These OH desorption temperatures were 389.3 ° C. (FIG. 11 (Comparative Example A)) and 402.5 ° C. (FIG. 12 (Comparative Example D)). Compared with low characteristics. This is considered to be because the magnesium hydroxide particles of the present invention have a thermodynamically weak crystal structure. Therefore, there is a feature that it can be easily removed by washing with impurities such as Cl incorporated in the magnesium hydroxide particles.
  • Examples 1 to 8 and Comparative Examples A to D the chemical composition of magnesium hydroxide particles (magnesium hydroxide purity, impurities (Cl, SO 4 , Cr, Ni, Ti, Mn, Mo, Fe, Zn, Al, Table 2 shows the contents of Cd, Co, Pb, and Zr)), presence / absence of surface treatment, evaluation of the combustibility of the resin composition, and evaluation of the dispersion state in the molded product.
  • Examples 11 to 17 and Comparative Examples E to H (magnesium oxide particles) Example 11 100 g of the dried magnesium hydroxide particles obtained in Example 3 was put into a 300 ml alumina crucible, and particles fired at 500 ° C. for 2 hours using an electric furnace were obtained.
  • Example 12 Magnesium oxide particles were obtained in the same manner as in Example 11 except that the firing temperature was changed to 650 ° C.
  • Example 13 Magnesium oxide particles were obtained in the same manner as in Example 11 except that the firing temperature was changed to 700 ° C.
  • Example 14 100 g of the dried magnesium hydroxide particles obtained in Example 4 was put into a 300 ml alumina crucible and baked at 500 ° C. for 2 hours using an electric furnace to obtain magnesium oxide particles.
  • Example 15 Magnesium oxide particles were obtained in the same manner as in Example 14 except that the firing temperature was changed to 650 ° C., and then surface treatment was performed with 3.0 wt% stearic acid.
  • Example 16 Magnesium oxide particles were obtained in the same manner as in Example 14 except that the firing temperature was changed to 700 ° C.
  • Example 17 100 g of the dried magnesium hydroxide particles obtained in Example 8 was put in a 300 ml alumina crucible and baked at 650 ° C. for 2 hours using an electric furnace to obtain magnesium oxide particles.
  • Comparative Example E 100 g of the dried magnesium hydroxide particles obtained in Comparative Example A was put into a 300 ml alumina crucible and baked at 650 ° C.
  • the magnesium oxide particles of the present invention have a fine and uniform particle size.
  • Example 11 As can be seen from the SEM photograph (FIG. 14) and the particle size distribution (FIG. 15) of the magnesium oxide particles of the present invention (Example 11), it can be confirmed that there are no noticeable aggregates and that the particles have a fine and uniform particle size.
  • treatment conditions raw material concentration, raw material usage, reaction rate, heat treatment temperature, heat treatment time, slurry concentration, firing temperature, firing time
  • characteristics of the obtained magnesium oxide particles BET specific surface area, particle size, presence / absence of surface treatment
  • vulcanized physical properties M200, M400, M600, TB, EB, Shore A, compression set, scorch time
  • heat aging resistance evaluation of dispersion state of molded product Is shown in Table 4.
  • Example 18 The magnesium hydroxide particles of Example 4 were surface-treated with 2% by weight of stearic acid, dried at 105 ° C. for 16 hours and further dried at 120 ° C. for 2 hours.
  • EVA Evaflex V421 Mitsui DuPont Polychemical Co., Ltd.
  • Magnesium hydroxide particles 150 parts by weight with respect to 90 parts by weight, modifier ⁇ -olefin copolymer (Tuffmer MH7020) 10 parts by weight, phenolic antioxidant (IRGANOX 1010) 0.5 parts by weight And 0.5 part by weight of a sulfur-based antioxidant (DLTDP) are melt-mixed at 160 to 200 ° C. with a continuous kneading extruder (Cay Engineering Co., Ltd. KCK80 ⁇ 2-35VEX), and the extruded resin composition strand is pelletized. After cutting with a vacuum dryer (LCV-242 manufactured by Tabai Espec Co., Ltd.
  • Example J Preparation of magnesium hydroxide particles having an MV of 4.31 ⁇ m, a D 50 / MV of 0.86, and a BET specific surface area of 30 m 2 / g in advance, except that the magnesium hydroxide particles used are changed to the magnesium hydroxide particles described above.
  • Example 18 Were the same as in Example 18 to obtain pellets and sheets of the resin composition.
  • Example 19 The magnesium hydroxide particles of Example 4 were surface-treated with 2% by weight of stearic acid, dried at 105 ° C. for 16 hours and further dried at 120 ° C. for 2 hours.
  • EVA Evaflex V421 Mitsui DuPont Polychemical Co., Ltd.
  • Magnesium hydroxide particles 150 parts by weight with respect to 90 parts by weight, modifier ⁇ -olefin copolymer (Tuffmer MH7020) 10 parts by weight, phenolic antioxidant (IRGANOX 1010) 0.5 parts by weight And 0.5 part by weight of a sulfur-based antioxidant (DLTDP) were melt-mixed at 160 to 200 ° C. with a continuous kneading extruder, the extruded resin composition strand was cut with a pelletizer, and then 60 ° C. with a vacuum dryer. And dried to prepare pellets.
  • the obtained pellets were blended with 1 part by weight of peroxide (DCP) per 100 parts by weight of the resin component (total of 90 parts by weight of EVA and 10 parts by weight of the modifier ⁇ -olefin copolymer).
  • DCP peroxide
  • the mixture was melt-mixed at 115 ° C. for 10 minutes, taken out in an oval shape, formed into a thickness of 2 mm at 120 ° C. by a hot press, and a crosslinked sheet having a thickness of 1 mm at 180 ° C. was obtained.
  • Comparative Example K Resin composition pellets and a crosslinked sheet were obtained in the same manner as in Example 19 except that the magnesium hydroxide particles used were changed to the magnesium hydroxide particles of Comparative Example A.
  • Example L Preparation of magnesium hydroxide particles having an MV of 4.31 ⁇ m, a D 50 / MV of 0.86, and a BET specific surface area of 30 m 2 / g in advance, except that the magnesium hydroxide particles used are changed to the magnesium hydroxide particles described above. Obtained a resin composition pellet and a crosslinked sheet in the same manner as in Example 19. (Silane-crosslinked resin composition)
  • Example 20 The magnesium hydroxide particles of Example 5 were surface-treated with 0.3% by weight of a silane coupling agent, dried at 105 ° C. for 16 hours, and further dried at 120 ° C. for 2 hours to obtain a silane crosslinkable EVA resin (link).
  • Ron XVF600N (Mitsubishi Chemical Corporation) 135 parts by weight of magnesium hydroxide particles subjected to the above treatment with respect to 87 parts by weight, 10 parts by weight of a modifier ⁇ -olefin copolymer (Tuffmer MH7020), phenolic antioxidant (IRGANOX1010) 0.5 parts by weight and 0.5 parts by weight of a sulfur-based antioxidant (DLTDP) were mixed and melted at 160 to 200 ° C. by a small batch kneader to prepare an oval resin composition.
  • a modifier ⁇ -olefin copolymer (Tuffmer MH7020)
  • phenolic antioxidant IRGANOX101010101010101010101010
  • DLTDP sulfur-based antioxidant
  • the obtained oval resin composition had a resin component of 97 parts by weight (a total of 87 parts by weight of a silane crosslinkable EVA resin and 10 parts by weight of a modifier ⁇ -olefin copolymer) and 3 parts by weight of a crosslinking acceleration catalyst masterbatch.
  • the mixture was melted and mixed at 180 ° C. for 10 minutes with a small batch kneader, and again taken out in an oval shape, formed into a thickness of 2 mm at 160 ° C. and further formed into a thickness of 1 mm at 180 ° C.
  • the molded resin composition was immersed in ion exchange water at 80 ° C. for 24 hours to obtain a crosslinked sheet.
  • Example 21 Magnesium hydroxide particles to be used were changed to the magnesium hydroxide particles of Example 4, and a cross-linked sheet was obtained in the same manner as in Example 20 except that the blending amount was changed to 140 parts.
  • Example 22 A crosslinked sheet was obtained in the same manner as in Example 20 except that the magnesium hydroxide particles used were changed to the magnesium hydroxide particles of Example 4.
  • Comparative Example M Prepare magnesium hydroxide particles having an MV of 0.87 ⁇ m, a D50 / MV of 0.83, and a BET specific surface area of 6 m 2 / g in advance. A crosslinked sheet was obtained in the same manner as in Example 20 except that the amount was changed to 140 parts.
  • Comparative Example N A crosslinked sheet was obtained in the same manner as in Comparative Example M, except that the amount of magnesium hydroxide particles used was changed to 150 parts.
  • Table 5 shows the evaluation of fluidity, colorability and tensile properties of the resin compositions for Examples 18 to 19 and Comparative Examples I to L.
  • Table 6 shows the evaluation of the tensile properties and the flammability of the resin compositions for Examples 20 to 22 and Comparative Examples M to N.
  • the obtained magnesium hydroxide particles have a characteristic that the crystal structure is thermodynamically unstable. Therefore, impurities such as metals such as Cl ions, SO 4 ions, nickel, chromium, lead, zinc, and aluminum can be easily removed from the product in the water washing step.
  • the magnesium hydroxide particles of the present invention have a fine and uniform particle diameter, are highly pure, and are excellent in dispersibility. Since the magnesium hydroxide particles of the present invention are manufactured by heat treatment at a low temperature of 0 to 100 ° C., the crystal structure is thermodynamically unstable and OH is released compared with magnesium hydroxide heat-treated at a higher temperature.
  • the temperature is low. Therefore, it is excellent in flame retardancy.
  • the magnesium hydroxide particles of the present invention have a low content of metals such as Cl ions, SO 4 ions, nickel, chromium, lead, zinc, and aluminum. Further, the magnesium hydroxide particles of the present invention can achieve uniform kneading or uniform coating treatment in applications to organic polymer materials and inorganic materials. In addition, the magnesium oxide particles of the present invention have a fine and uniform particle size, high purity, and excellent dispersibility. The magnesium oxide particles of the present invention have a low content of nickel, chromium, lead, zinc, and aluminum. Moreover, the magnesium oxide particle of this invention can implement
  • the magnesium hydroxide particles of the present invention are useful as a flame retardant for polymer materials and an inorganic filler for separators for non-aqueous secondary batteries.
  • the magnesium oxide particles of the present invention are useful as an acid acceptor for organic polymer materials, a deodorant, an electromagnetic steel material, a resin filler, a catalyst, a catalyst carrier, and the like.
  • the magnesium hydroxide and magnesium oxide particles of the present invention have a small amount of nickel, chromium, lead, zinc, and aluminum, they can be used as additives for electronic materials, pharmaceutical raw materials, and food and beverage products. It can also be used as a synthetic raw material for cosmetics, foods, pharmaceutical pH adjusters, polymer stabilizers, fine particle hydrotalcite, and the like.

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Abstract

La présente invention vise à fournir des particules d'hydroxyde de magnésium et des particules d'oxyde de magnésium, qui ont des diamètres de particules fins et uniformes, tout en ayant une pureté élevée et une excellente dispersibilité. La présente invention concerne un procédé de production de particules d'hydroxyde de magnésium, qui comprend : une étape (i) dans laquelle une solution aqueuse d'un sel soluble de magnésium est mis à réagir avec une solution aqueuse alcaline, ce qui permet de produire une suspension épaisse contenant des particules d'hydroxyde de magnésium ; une étape (ii) dans laquelle la suspension épaisse ainsi obtenue est soumise à un traitement thermique à 0 à 100 °C pendant 5 à 500 heures à la pression atmosphérique ; une étape (iii) dans laquelle un gâteau contenant les particules d'hydroxyde de magnésium est séparé de la suspension épaisse traitée par la chaleur et purifié ; et une étape (iv) dans laquelle le gâteau séparé et purifié est séché, ce qui permet d'obtenir des particules d'hydroxyde de magnésium.
PCT/JP2016/061957 2015-04-10 2016-04-07 Particules d'hydroxyde de magnésium et leur procédé de production WO2016163562A1 (fr)

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Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2018158975A (ja) * 2017-03-22 2018-10-11 協和化学工業株式会社 クロロプレンゴム系接着剤組成物
WO2018221709A1 (fr) * 2017-06-02 2018-12-06 協和化学工業株式会社 Hydroxyde de magnésium utilisé pour séparateur de batterie secondaire non aqueuse, séparateur de batterie secondaire non aqueuse et batterie secondaire non aqueuse
JP2020155294A (ja) * 2019-03-20 2020-09-24 株式会社エンビジョンＡｅｓｃエナジーデバイス 電極、電極の製造方法及び電池
CN115627069A (zh) * 2022-10-22 2023-01-20 营口理工学院 一种改性纳米氢氧化镁复合阻燃尼龙66及其制备方法
CN118399020A (zh) * 2024-07-01 2024-07-26 浙江功能膜材料创新中心有限公司 一种电池隔膜及其制备方法、二次电池和用电装置

Families Citing this family (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110002478A (zh) * 2018-01-05 2019-07-12 上海实业振泰化工有限公司 用后氧化镁制备片状氢氧化镁和球状氧化镁的装置及方法
JP7454334B2 (ja) * 2018-03-28 2024-03-22 タテホ化学工業株式会社 焼鈍分離剤用の酸化マグネシウム及び方向性電磁鋼板の製造方法
JP7454335B2 (ja) * 2018-03-28 2024-03-22 タテホ化学工業株式会社 焼鈍分離剤用の酸化マグネシウム及び方向性電磁鋼板の製造方法
CN113388725B (zh) * 2021-06-18 2022-12-02 协和化学工业株式会社 退火隔离剂的制备方法以及退火隔离剂和方向性电磁钢板

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH0797210A (ja) * 1993-09-29 1995-04-11 Sumitomo Chem Co Ltd 水酸化マグネシウムの製造方法
CN1332116A (zh) * 2001-08-20 2002-01-23 杜以波 均质流体法制备纳米氢氧化镁
JP2012072004A (ja) * 2010-09-28 2012-04-12 Tateho Chemical Industries Co Ltd 水酸化マグネシウム微粒子及び酸化マグネシウム微粒子、並びにそれらの製造方法
WO2014155764A1 (fr) * 2013-03-25 2014-10-02 神島化学工業株式会社 Particules d'oxyde de magnésium, composition de résine, composition de caoutchouc et article moulé
JP2016003174A (ja) * 2014-06-18 2016-01-12 神島化学工業株式会社 高活性な酸化マグネシウム系添加剤、及びその用途

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH0797210A (ja) * 1993-09-29 1995-04-11 Sumitomo Chem Co Ltd 水酸化マグネシウムの製造方法
CN1332116A (zh) * 2001-08-20 2002-01-23 杜以波 均质流体法制备纳米氢氧化镁
JP2012072004A (ja) * 2010-09-28 2012-04-12 Tateho Chemical Industries Co Ltd 水酸化マグネシウム微粒子及び酸化マグネシウム微粒子、並びにそれらの製造方法
WO2014155764A1 (fr) * 2013-03-25 2014-10-02 神島化学工業株式会社 Particules d'oxyde de magnésium, composition de résine, composition de caoutchouc et article moulé
JP2016003174A (ja) * 2014-06-18 2016-01-12 神島化学工業株式会社 高活性な酸化マグネシウム系添加剤、及びその用途

Cited By (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2018158975A (ja) * 2017-03-22 2018-10-11 協和化学工業株式会社 クロロプレンゴム系接着剤組成物
WO2018221709A1 (fr) * 2017-06-02 2018-12-06 協和化学工業株式会社 Hydroxyde de magnésium utilisé pour séparateur de batterie secondaire non aqueuse, séparateur de batterie secondaire non aqueuse et batterie secondaire non aqueuse
JPWO2018221709A1 (ja) * 2017-06-02 2020-05-21 協和化学工業株式会社 非水系二次電池用セパレータに供される水酸化マグネシウム、非水系二次電池用セパレータおよび非水系二次電池
JP2020155294A (ja) * 2019-03-20 2020-09-24 株式会社エンビジョンＡｅｓｃエナジーデバイス 電極、電極の製造方法及び電池
WO2020189298A1 (fr) * 2019-03-20 2020-09-24 株式会社エンビジョンＡｅｓｃエナジーデバイス Électrode, procédé de production d'électrode et batterie
JP7320172B2 (ja) 2019-03-20 2023-08-03 株式会社Ａｅｓｃジャパン 電極、電極の製造方法及び電池
CN115627069A (zh) * 2022-10-22 2023-01-20 营口理工学院 一种改性纳米氢氧化镁复合阻燃尼龙66及其制备方法
CN118399020A (zh) * 2024-07-01 2024-07-26 浙江功能膜材料创新中心有限公司 一种电池隔膜及其制备方法、二次电池和用电装置

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