WO2022209769A1 - 包装体及びその製造方法 - Google Patents
包装体及びその製造方法 Download PDFInfo
- Publication number
- WO2022209769A1 WO2022209769A1 PCT/JP2022/010970 JP2022010970W WO2022209769A1 WO 2022209769 A1 WO2022209769 A1 WO 2022209769A1 JP 2022010970 W JP2022010970 W JP 2022010970W WO 2022209769 A1 WO2022209769 A1 WO 2022209769A1
- Authority
- WO
- WIPO (PCT)
- Prior art keywords
- metal oxide
- oxide powder
- bag
- powder
- gas
- Prior art date
Links
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 52
- 238000004806 packaging method and process Methods 0.000 title claims abstract description 9
- 239000000843 powder Substances 0.000 claims abstract description 205
- 229910044991 metal oxide Inorganic materials 0.000 claims abstract description 127
- 150000004706 metal oxides Chemical class 0.000 claims abstract description 127
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical group O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 102
- CPLXHLVBOLITMK-UHFFFAOYSA-N Magnesium oxide Chemical compound [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 claims abstract description 73
- 239000007789 gas Substances 0.000 claims abstract description 51
- 239000000377 silicon dioxide Substances 0.000 claims abstract description 50
- 238000007789 sealing Methods 0.000 claims abstract description 40
- 239000000395 magnesium oxide Substances 0.000 claims abstract description 37
- 230000035699 permeability Effects 0.000 claims abstract description 20
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 17
- MYMOFIZGZYHOMD-UHFFFAOYSA-N Dioxygen Chemical compound O=O MYMOFIZGZYHOMD-UHFFFAOYSA-N 0.000 claims abstract description 15
- 229910001873 dinitrogen Inorganic materials 0.000 claims abstract description 15
- 229910001882 dioxygen Inorganic materials 0.000 claims abstract description 15
- 239000002245 particle Substances 0.000 claims description 69
- 238000000034 method Methods 0.000 claims description 32
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 28
- 238000009826 distribution Methods 0.000 claims description 24
- 238000004381 surface treatment Methods 0.000 claims description 23
- 239000006087 Silane Coupling Agent Substances 0.000 claims description 17
- 230000008569 process Effects 0.000 claims description 12
- 238000011282 treatment Methods 0.000 claims description 8
- 238000002203 pretreatment Methods 0.000 claims description 7
- 238000003860 storage Methods 0.000 abstract description 15
- 230000007774 longterm Effects 0.000 abstract description 11
- 229910052756 noble gas Inorganic materials 0.000 abstract 2
- 150000002835 noble gases Chemical class 0.000 abstract 2
- 230000015556 catabolic process Effects 0.000 abstract 1
- 238000006731 degradation reaction Methods 0.000 abstract 1
- 229920005989 resin Polymers 0.000 description 22
- 239000011347 resin Substances 0.000 description 22
- 239000000463 material Substances 0.000 description 10
- 238000010295 mobile communication Methods 0.000 description 10
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 9
- 229910052782 aluminium Inorganic materials 0.000 description 7
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 7
- -1 polybutylene terephthalate Polymers 0.000 description 7
- 230000006866 deterioration Effects 0.000 description 6
- 230000004888 barrier function Effects 0.000 description 5
- 239000007788 liquid Substances 0.000 description 5
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 4
- 238000004220 aggregation Methods 0.000 description 4
- 230000002776 aggregation Effects 0.000 description 4
- XDLMVUHYZWKMMD-UHFFFAOYSA-N 3-trimethoxysilylpropyl 2-methylprop-2-enoate Chemical compound CO[Si](OC)(OC)CCCOC(=O)C(C)=C XDLMVUHYZWKMMD-UHFFFAOYSA-N 0.000 description 3
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 3
- 239000004698 Polyethylene Substances 0.000 description 3
- 239000002131 composite material Substances 0.000 description 3
- 230000001186 cumulative effect Effects 0.000 description 3
- 239000005020 polyethylene terephthalate Substances 0.000 description 3
- 229920000139 polyethylene terephthalate Polymers 0.000 description 3
- 230000008054 signal transmission Effects 0.000 description 3
- 229920000219 Ethylene vinyl alcohol Polymers 0.000 description 2
- 239000004695 Polyether sulfone Substances 0.000 description 2
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 2
- PPBRXRYQALVLMV-UHFFFAOYSA-N Styrene Chemical compound C=CC1=CC=CC=C1 PPBRXRYQALVLMV-UHFFFAOYSA-N 0.000 description 2
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 2
- 229910052786 argon Inorganic materials 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 239000011248 coating agent Substances 0.000 description 2
- 238000000576 coating method Methods 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000005538 encapsulation Methods 0.000 description 2
- 238000010285 flame spraying Methods 0.000 description 2
- 238000004817 gas chromatography Methods 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 239000003973 paint Substances 0.000 description 2
- 239000004417 polycarbonate Substances 0.000 description 2
- 229920000515 polycarbonate Polymers 0.000 description 2
- 229920000728 polyester Polymers 0.000 description 2
- 229920006393 polyether sulfone Polymers 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 229910052710 silicon Inorganic materials 0.000 description 2
- 239000010703 silicon Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- WYTZZXDRDKSJID-UHFFFAOYSA-N (3-aminopropyl)triethoxysilane Chemical compound CCO[Si](OCC)(OCC)CCCN WYTZZXDRDKSJID-UHFFFAOYSA-N 0.000 description 1
- OEPOKWHJYJXUGD-UHFFFAOYSA-N 2-(3-phenylmethoxyphenyl)-1,3-thiazole-4-carbaldehyde Chemical compound O=CC1=CSC(C=2C=C(OCC=3C=CC=CC=3)C=CC=2)=N1 OEPOKWHJYJXUGD-UHFFFAOYSA-N 0.000 description 1
- VXEGSRKPIUDPQT-UHFFFAOYSA-N 4-[4-(4-methoxyphenyl)piperazin-1-yl]aniline Chemical compound C1=CC(OC)=CC=C1N1CCN(C=2C=CC(N)=CC=2)CC1 VXEGSRKPIUDPQT-UHFFFAOYSA-N 0.000 description 1
- NLHHRLWOUZZQLW-UHFFFAOYSA-N Acrylonitrile Chemical compound C=CC#N NLHHRLWOUZZQLW-UHFFFAOYSA-N 0.000 description 1
- 238000004438 BET method Methods 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 229920000106 Liquid crystal polymer Polymers 0.000 description 1
- 239000004977 Liquid-crystal polymers (LCPs) Substances 0.000 description 1
- 239000004677 Nylon Substances 0.000 description 1
- 239000004952 Polyamide Substances 0.000 description 1
- 239000004697 Polyetherimide Substances 0.000 description 1
- 239000004734 Polyphenylene sulfide Substances 0.000 description 1
- 239000004743 Polypropylene Substances 0.000 description 1
- 238000000563 Verneuil process Methods 0.000 description 1
- 239000002250 absorbent Substances 0.000 description 1
- 230000002745 absorbent Effects 0.000 description 1
- 229920000800 acrylic rubber Polymers 0.000 description 1
- 229920000122 acrylonitrile butadiene styrene Polymers 0.000 description 1
- 239000003905 agrochemical Substances 0.000 description 1
- 125000003118 aryl group Chemical group 0.000 description 1
- 239000012298 atmosphere Substances 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 239000002981 blocking agent Substances 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 239000011362 coarse particle Substances 0.000 description 1
- 238000004891 communication Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000005443 coulometric titration Methods 0.000 description 1
- 150000001993 dienes Chemical class 0.000 description 1
- KZHJGOXRZJKJNY-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Si]=O.O=[Al]O[Al]=O.O=[Al]O[Al]=O.O=[Al]O[Al]=O KZHJGOXRZJKJNY-UHFFFAOYSA-N 0.000 description 1
- 239000012776 electronic material Substances 0.000 description 1
- 239000003822 epoxy resin Substances 0.000 description 1
- HQQADJVZYDDRJT-UHFFFAOYSA-N ethene;prop-1-ene Chemical group C=C.CC=C HQQADJVZYDDRJT-UHFFFAOYSA-N 0.000 description 1
- NKSJNEHGWDZZQF-UHFFFAOYSA-N ethenyl(trimethoxy)silane Chemical compound CO[Si](OC)(OC)C=C NKSJNEHGWDZZQF-UHFFFAOYSA-N 0.000 description 1
- 239000004715 ethylene vinyl alcohol Substances 0.000 description 1
- 230000004927 fusion Effects 0.000 description 1
- 230000005484 gravity Effects 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 230000003301 hydrolyzing effect Effects 0.000 description 1
- 238000002347 injection Methods 0.000 description 1
- 239000007924 injection Substances 0.000 description 1
- 239000011810 insulating material Substances 0.000 description 1
- 239000011777 magnesium Substances 0.000 description 1
- 229910052749 magnesium Inorganic materials 0.000 description 1
- ZLNQQNXFFQJAID-UHFFFAOYSA-L magnesium carbonate Chemical compound [Mg+2].[O-]C([O-])=O ZLNQQNXFFQJAID-UHFFFAOYSA-L 0.000 description 1
- 239000001095 magnesium carbonate Substances 0.000 description 1
- 229910000021 magnesium carbonate Inorganic materials 0.000 description 1
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 description 1
- ARYZCSRUUPFYMY-UHFFFAOYSA-N methoxysilane Chemical compound CO[SiH3] ARYZCSRUUPFYMY-UHFFFAOYSA-N 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 229910052863 mullite Inorganic materials 0.000 description 1
- LIBWSLLLJZULCP-UHFFFAOYSA-N n-(3-triethoxysilylpropyl)aniline Chemical compound CCO[Si](OCC)(OCC)CCCNC1=CC=CC=C1 LIBWSLLLJZULCP-UHFFFAOYSA-N 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 229920001778 nylon Polymers 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 239000000049 pigment Substances 0.000 description 1
- 239000002985 plastic film Substances 0.000 description 1
- 229920006255 plastic film Polymers 0.000 description 1
- 229920003207 poly(ethylene-2,6-naphthalate) Polymers 0.000 description 1
- 229920002492 poly(sulfone) Polymers 0.000 description 1
- 229920000058 polyacrylate Polymers 0.000 description 1
- 229920002647 polyamide Polymers 0.000 description 1
- 229920001707 polybutylene terephthalate Polymers 0.000 description 1
- 229920000647 polyepoxide Polymers 0.000 description 1
- 229920001601 polyetherimide Polymers 0.000 description 1
- 229920000573 polyethylene Polymers 0.000 description 1
- 239000011112 polyethylene naphthalate Substances 0.000 description 1
- 229920000069 polyphenylene sulfide Polymers 0.000 description 1
- 229920001155 polypropylene Polymers 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000000790 scattering method Methods 0.000 description 1
- 239000000565 sealant Substances 0.000 description 1
- 238000004062 sedimentation Methods 0.000 description 1
- 238000007873 sieving Methods 0.000 description 1
- FZHAPNGMFPVSLP-UHFFFAOYSA-N silanamine Chemical class [SiH3]N FZHAPNGMFPVSLP-UHFFFAOYSA-N 0.000 description 1
- 239000005049 silicon tetrachloride Substances 0.000 description 1
- 229920002545 silicone oil Polymers 0.000 description 1
- 229920002379 silicone rubber Polymers 0.000 description 1
- 239000004945 silicone rubber Substances 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 235000014347 soups Nutrition 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- JXUKBNICSRJFAP-UHFFFAOYSA-N triethoxy-[3-(oxiran-2-ylmethoxy)propyl]silane Chemical compound CCO[Si](OCC)(OCC)CCCOCC1CO1 JXUKBNICSRJFAP-UHFFFAOYSA-N 0.000 description 1
- ZYMHKOVQDOFPHH-UHFFFAOYSA-N trimethoxy(oct-1-enyl)silane Chemical compound CCCCCCC=C[Si](OC)(OC)OC ZYMHKOVQDOFPHH-UHFFFAOYSA-N 0.000 description 1
- DQZNLOXENNXVAD-UHFFFAOYSA-N trimethoxy-[2-(7-oxabicyclo[4.1.0]heptan-4-yl)ethyl]silane Chemical compound C1C(CC[Si](OC)(OC)OC)CCC2OC21 DQZNLOXENNXVAD-UHFFFAOYSA-N 0.000 description 1
- HBZPRQCNASJKHW-UHFFFAOYSA-N trimethoxysilyl prop-2-enoate Chemical compound CO[Si](OC)(OC)OC(=O)C=C HBZPRQCNASJKHW-UHFFFAOYSA-N 0.000 description 1
- 239000012808 vapor phase Substances 0.000 description 1
- UKRDPEFKFJNXQM-UHFFFAOYSA-N vinylsilane Chemical class [SiH3]C=C UKRDPEFKFJNXQM-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B65—CONVEYING; PACKING; STORING; HANDLING THIN OR FILAMENTARY MATERIAL
- B65D—CONTAINERS FOR STORAGE OR TRANSPORT OF ARTICLES OR MATERIALS, e.g. BAGS, BARRELS, BOTTLES, BOXES, CANS, CARTONS, CRATES, DRUMS, JARS, TANKS, HOPPERS, FORWARDING CONTAINERS; ACCESSORIES, CLOSURES, OR FITTINGS THEREFOR; PACKAGING ELEMENTS; PACKAGES
- B65D81/00—Containers, packaging elements, or packages, for contents presenting particular transport or storage problems, or adapted to be used for non-packaging purposes after removal of contents
- B65D81/24—Adaptations for preventing deterioration or decay of contents; Applications to the container or packaging material of food preservatives, fungicides, pesticides or animal repellants
-
- 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
- C01F5/04—Magnesia by oxidation of metallic magnesium
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B65—CONVEYING; PACKING; STORING; HANDLING THIN OR FILAMENTARY MATERIAL
- B65B—MACHINES, APPARATUS OR DEVICES FOR, OR METHODS OF, PACKAGING ARTICLES OR MATERIALS; UNPACKING
- B65B31/00—Packaging articles or materials under special atmospheric or gaseous conditions; Adding propellants to aerosol containers
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B65—CONVEYING; PACKING; STORING; HANDLING THIN OR FILAMENTARY MATERIAL
- B65D—CONTAINERS FOR STORAGE OR TRANSPORT OF ARTICLES OR MATERIALS, e.g. BAGS, BARRELS, BOTTLES, BOXES, CANS, CARTONS, CRATES, DRUMS, JARS, TANKS, HOPPERS, FORWARDING CONTAINERS; ACCESSORIES, CLOSURES, OR FITTINGS THEREFOR; PACKAGING ELEMENTS; PACKAGES
- B65D81/00—Containers, packaging elements, or packages, for contents presenting particular transport or storage problems, or adapted to be used for non-packaging purposes after removal of contents
- B65D81/18—Containers, packaging elements, or packages, for contents presenting particular transport or storage problems, or adapted to be used for non-packaging purposes after removal of contents providing specific environment for contents, e.g. temperature above or below ambient
- B65D81/20—Containers, packaging elements, or packages, for contents presenting particular transport or storage problems, or adapted to be used for non-packaging purposes after removal of contents providing specific environment for contents, e.g. temperature above or below ambient under vacuum or superatmospheric pressure, or in a special atmosphere, e.g. of inert gas
- B65D81/2069—Containers, packaging elements, or packages, for contents presenting particular transport or storage problems, or adapted to be used for non-packaging purposes after removal of contents providing specific environment for contents, e.g. temperature above or below ambient under vacuum or superatmospheric pressure, or in a special atmosphere, e.g. of inert gas in a special atmosphere
- B65D81/2084—Containers, packaging elements, or packages, for contents presenting particular transport or storage problems, or adapted to be used for non-packaging purposes after removal of contents providing specific environment for contents, e.g. temperature above or below ambient under vacuum or superatmospheric pressure, or in a special atmosphere, e.g. of inert gas in a special atmosphere in a flexible container
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B65—CONVEYING; PACKING; STORING; HANDLING THIN OR FILAMENTARY MATERIAL
- B65D—CONTAINERS FOR STORAGE OR TRANSPORT OF ARTICLES OR MATERIALS, e.g. BAGS, BARRELS, BOTTLES, BOXES, CANS, CARTONS, CRATES, DRUMS, JARS, TANKS, HOPPERS, FORWARDING CONTAINERS; ACCESSORIES, CLOSURES, OR FITTINGS THEREFOR; PACKAGING ELEMENTS; PACKAGES
- B65D85/00—Containers, packaging elements or packages, specially adapted for particular articles or materials
- B65D85/70—Containers, packaging elements or packages, specially adapted for particular articles or materials for materials not otherwise provided for
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- C01B33/113—Silicon oxides; Hydrates thereof
- C01B33/12—Silica; Hydrates thereof, e.g. lepidoic silicic acid
- C01B33/18—Preparation of finely divided silica neither in sol nor in gel form; After-treatment thereof
-
- 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
-
- 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
- C09C1/028—Compounds containing only magnesium as metal
-
- 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
- C09C1/28—Compounds of silicon
- C09C1/30—Silicic acid
- C09C1/3081—Treatment with organo-silicon compounds
-
- 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
- C09C3/12—Treatment with organosilicon compounds
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/12—Surface area
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
- C01P2006/82—Compositional purity water content
Definitions
- the present invention relates to a package for metal oxide powder and a method for manufacturing the package.
- Materials used in mobile communication systems include, for example, metal oxide powders, in particular composites of silica or magnesia powders and resins. Since silica powder and magnesia powder have a low dielectric constant and dielectric loss tangent, a composite material of silica powder or magnesia powder and resin may increase signal propagation speed and reduce signal transmission loss. However, when OH groups are formed on the surface of silica powder and magnesia powder, the dielectric loss tangent of silica powder and magnesia powder increases.
- silica powder and magnesia powder having a low density of OH groups formed on the surface are desired.
- a silica powder having a low OH group density for example, a silica powder described in Patent Document 1 is known as a prior art.
- the density of hydrogen-bonded OH groups in the silica powder described in Patent Document 1 is 0 to 4/nm 2 and the density of isolated OH groups is 3 to 8/nm 2 .
- an object of the present invention is to provide a package of metal oxide powder that can suppress deterioration of the dielectric loss tangent of the metal oxide powder due to long-term storage, and a method of manufacturing the package.
- the present inventors found that the above problems can be solved by storing the metal oxide powder in a bag having a predetermined moisture permeability and filled with a predetermined gas.
- the present invention is based on the above findings, and has the following gist. [1] A metal oxide powder, and a sealed bag containing the metal oxide powder, wherein the bag is selected from the group consisting of rare gas, nitrogen gas, oxygen gas and dry air.
- the bag is filled with at least one kind of gas, the metal oxide powder is silica powder or magnesia powder, and the moisture permeability of the bag measured in accordance with JIS Z 0222-1959 is 0.30 g/(m 2 ⁇ day) a package that is: [2] The package according to [1] above, wherein the water content of at least one gas selected from the group consisting of rare gas, nitrogen gas, oxygen gas and dry air is 3500 mass ppm or less. [3] The package according to the above [1] or [2], wherein the metal oxide powder has a dielectric loss tangent of 0.004 or less.
- the metal oxide powder of [1] to [4] above is a particle size distribution-adjusted product that has undergone a classification process to remove metal oxide particles having a particle size equal to or larger than a predetermined particle size.
- a sealing step of storing and then sealing the bag wherein the metal oxide powder is silica powder or magnesia powder, and the moisture permeability of the bag measured in accordance with JIS Z 0222-1959 is 0.30 g / (m 2 ⁇ day) or less.
- the metal oxide powder is placed in the bag and the bag is sealed [6] or [ 7].
- [11] further comprising a pre-treatment sealing step of placing the metal oxide powder in a bag and sealing the bag within 40 minutes after producing the metal oxide powder in the production step;
- a pre-treatment sealing step of placing the metal oxide powder in a bag and sealing the bag within 40 minutes after producing the metal oxide powder in the production step;
- the present invention it is possible to provide a package of metal oxide powder that can suppress deterioration of the dielectric loss tangent of the metal oxide powder due to long-term storage, and a method of manufacturing the package.
- the package of the present invention includes a metal oxide powder and a sealed bag containing the metal oxide powder, wherein the bag contains a gas selected from the group consisting of rare gas, nitrogen gas, oxygen gas and dry air.
- the metal oxide powder is silica powder or magnesia powder, and the moisture permeability of the bag measured in accordance with JIS Z 0222-1959 is 0.30 g / (m 2 ⁇ day) is as follows. As a result, even if the metal oxide powder is stored for a long time, the dielectric loss tangent of the metal oxide powder does not deteriorate, or if it does deteriorate, the degree of deterioration is small. In addition, aggregation of powder due to long-term storage can be suppressed.
- the metal oxide powder in the package of the present invention is silica powder or magnesia powder.
- Silica powder and magnesia powder have small dielectric constant and dielectric loss tangent. Therefore, by using silica powder or magnesia powder as a material for mobile communication systems, it is possible to increase the speed of signal propagation in mobile communication systems and reduce signal transmission loss.
- silica and magnesia powders are used, for example, in the form of composites with resins. Resins used together with silica powder and magnesia powder are not particularly limited.
- Polyamides such as polyetherimide, polyesters such as polybutylene terephthalate and polyethylene terephthalate, polyphenylene sulfide, wholly aromatic polyester, polysulfone, liquid crystal polymer, polyethersulfone, polycarbonate, maleimide-modified resin, ABS resin, AAS (acrylonitrile-acrylic rubber ⁇ Styrene) resin, AES (acrylonitrile/ethylene/propylene/diene rubber-styrene) resin, and the like.
- the proportions of silica powder and magnesia powder in the resin are appropriately selected according to target physical properties such as dielectric constant and dielectric loss tangent.
- the amount of resin to be used is appropriately selected in the range of 5 to 300 parts by mass with respect to 100 parts by mass of silica powder or magnesia powder.
- the particles are filled in a resin, it is effective to perform surface treatment and particle size distribution adjustment from the viewpoint of compatibility with the resin and viscosity control. Therefore, it is highly necessary to perform a surface treatment step and a particle size distribution adjustment step when manufacturing a package of metal oxide powder to be filled in a resin.
- silica powder is used to increase the viscosity of silicone oil, epoxy resin, etc., to impart thixotropy to liquid paints, to prevent sedimentation of pigments, to reinforce silicone rubber, and to improve fluidity of sealants.
- it can be used to reduce friction resistance or prevent adhesion by coating powder such as powder paint, agricultural chemicals, super absorbent resin, powder soup, and toner. It can also be used as a heat insulating material, a raw material for quartz glass, a catalyst carrier, an anti-blocking agent for films, and the like.
- magnesia powder can also be used as raw materials for high-purity crucibles, substrates for electronic materials, optical materials, sintering aids for ceramics, and the like.
- deterioration of the dielectric loss tangent of the silica powder and the magnesia powder due to long-term storage can be suppressed, as well as aggregation of the powder due to long-term storage can be suppressed. Therefore, even when silica powder and magnesia powder are used for applications other than the materials used in mobile communication systems, the package of the present invention has a remarkable effect.
- the dielectric loss tangent of the metal oxide powder is preferably 0.004 or less.
- the metal oxide powder has a dielectric loss tangent of 0.004 or less, transmission loss can be reduced when a material containing the metal oxide powder is used in a mobile communication system.
- the dielectric loss tangent of the metal oxide powder is more preferably 0.003 or less, and still more preferably 0.001 or less. According to the package of the present invention, even if the metal oxide powder is stored for a long time, the dielectric loss tangent of the metal oxide can be maintained within the above range.
- the dielectric loss tangent of the metal oxide powder can be measured by the method described in Examples below.
- the method for manufacturing the package of the present invention described later further includes a pretreatment sealing step etc., so that the surface treatment and / or Even in the package of the metal oxide powder in which the particle size distribution is adjusted, the dielectric loss tangent of the metal oxide powder in the package can be kept low.
- the dielectric loss tangent of the surface-treated metal oxide powder can be maintained at preferably 0.004 or less, more preferably 0.003 or less.
- the metal oxide powder is preferably surface-treated with a silane coupling agent. This can further suppress aggregation of the metal oxide powder during storage.
- a silane coupling agent can be used for the surface treatment of the metal oxide powder with the silane coupling agent.
- silane coupling agents include epoxysilanes such as ⁇ -glycidoxypropyltriethoxysilane and ⁇ -(3,4-epoxycyclohexyl)ethyltrimethoxysilane, aminopropyltriethoxysilane, N-phenylaminopropyltriethoxysilane, and the like.
- examples include aminosilanes such as methoxysilane, vinylsilanes such as vinyltrimethoxysilane, acrylicsilanes such as acryloxytrimethoxysilane and 3-methacryloxypropyltrimethoxysilane, and octenyltrimethoxysilane.
- the metal oxide powder is preferably a particle size distribution-adjusted product that has undergone a classification process to remove metal oxide particles having a particle size equal to or greater than a predetermined particle size.
- a classification process to remove metal oxide particles having a particle size equal to or greater than a predetermined particle size.
- the classification process includes, for example, classification by a sieve, classification by a gravity classifier, classification by an inertial force classifier, classification by a centrifugal force classifier, and the like.
- sieving is preferred from the viewpoint that coarse particles can be precisely removed.
- the average particle size of the metal oxide powder is preferably 0.7 to 10 ⁇ m, more preferably 0.8 to 6.0 ⁇ m. Moreover, the average particle size of the metal oxide powder is preferably 20 to 150 ⁇ m in the case of magnesia powder.
- the average particle size of the metal oxide powder is the median size of the particle size distribution measured by the laser diffraction scattering method (the particle size when the cumulative frequency of the particle size distribution is 50% by volume (d50)).
- the bag in the package of the present invention contains the metal oxide powder and is sealed.
- the moisture permeability of the bag measured according to JIS Z 0222-1959 is 0.30 g/(m 2 ⁇ day) or less. If the moisture permeability of the bag is higher than 0.30 g/(m 2 ⁇ day), water vapor outside the bag may enter the bag and form OH groups on the surface of the metal oxide powder. As a result, the dielectric loss tangent of the metal oxide powder may deteriorate.
- the moisture permeability of the bag is preferably 0.10 g/(m 2 ⁇ day) or less, more preferably 0.08 g/(m 2 ⁇ day) or less.
- the lower limit of the moisture permeability range of the bag is not particularly limited, but is, for example, 0.04 g/(m 2 ⁇ day). Specifically, the moisture permeability of the bag can be measured by the method described in Examples below.
- Examples of materials for the above-mentioned moisture-permeable bags include films with gas barrier properties such as metal aluminum, alumina, silica, and silicon oxynitride, polyethylene, polypropylene, polycarbonate, polyethylene terephthalate, polyethylene naphthalate, and polyether sulfone. , ethylene-vinyl alcohol copolymer (EVOH), vinylidene chloride, and the like, gas barrier films obtained by coating plastic films, multilayer films of these, and the like. Among these gas barrier films, a multi-layer film is preferable, and a metal aluminum film sandwiched between polyethylene terephthalate films is preferable.
- gas barrier properties such as metal aluminum, alumina, silica, and silicon oxynitride, polyethylene, polypropylene, polycarbonate, polyethylene terephthalate, polyethylene naphthalate, and polyether sulfone.
- EVOH ethylene-vinyl alcohol copolymer
- the thickness of the bag is preferably 0.01 mm or more, more preferably 0.06 mm or more. From the viewpoint of the balance between the effect of suppressing moisture permeation due to the thickness of the bag and the cost, the thickness of the bag is preferably 1.0 mm or less, more preferably 0.7 mm or less.
- the bag in the package of the present invention is filled with at least one gas selected from the group consisting of rare gas, nitrogen gas, oxygen gas and dry air.
- the water content of the gas in the bag is preferably 3500 mass ppm or less, more preferably 1000 mass ppm or less, and still more preferably 500 mass ppm or less.
- the lower limit of the water content range of the gas in the bag is not particularly limited, it is usually 50 mass ppm from the viewpoint of cost.
- the water content in the gas can be measured by the method described in Examples.
- a preferable rare gas is argon gas.
- the method for manufacturing the package of the present invention includes a production step of producing a metal oxide powder, a pretreatment sealing step of storing the metal oxide powder in a bag and temporarily sealing the bag, and a silane coupling agent.
- the pre-treatment sealing step, the surface treatment step, and the particle size distribution adjustment step are optional steps.
- the metal oxide powder is silica powder or magnesia powder, and the moisture permeability of the bag measured according to JIS Z 0222-1959 is 0.30 g/(m 2 ⁇ day) or less.
- silica powder can be produced by a known method.
- silica powder may be produced by hydrolyzing silicon tetrachloride at a high temperature of 1000° C. or higher in an oxygen/hydrogen flame, or silica powder may be produced by flame spraying silica or metallic silicon. good too.
- magnesia powder can be manufactured by a known method.
- magnesia powder may be produced by a basic magnesium carbonate purification method
- magnesia powder may be produced by an underwater spark discharge method
- magnesia powder may be produced by a vapor phase oxidation method
- Magnesium powder may be produced by flame spraying magnesium oxide or magnesium metal.
- the pre-treatment sealing step is a step of placing the metal oxide powder in a bag and then temporarily sealing the bag before performing the surface treatment step and/or the particle size distribution adjustment step.
- the surface treatment step and the particle size distribution adjustment step are optional steps, and the pre-treatment sealing step is also an optional step.
- the bag used in the processing and sealing step is the same as the bag described in the item of the package, so the description is omitted.
- sealing of the bag can be performed, for example, by heat sealing (thermal fusion bonding).
- the metal oxide powder in the manufacturing process it is preferable to put the metal oxide powder in a bag and seal the bag in the pre-treatment sealing step. As a result, it is possible to suppress the formation of OH groups due to moisture in the outside air adhering to the surface of the metal oxide powder. From this point of view, it is preferable to seal within 40 minutes after the metal oxide powder is produced in the production process.
- a surface treatment step is an optional step. As described above, it is preferable to provide a surface treatment step in the production of a package of metal oxide powder to be filled in a resin.
- the method for manufacturing the package of the present invention preferably further includes a surface treatment step of surface-treating the metal oxide powder produced in the production step using a silane coupling agent. This can further suppress aggregation of the metal oxide powder during storage.
- the silane coupling agent used in the surface treatment step is the same as the silane coupling agent explained in the item of the package, so the explanation of the silane coupling agent is omitted.
- the surface treatment of the metal oxide with the silane coupling agent is preferably performed by a dry treatment method.
- the particle size distribution adjustment step is an optional step. As described above, it is preferable to provide a particle size distribution adjustment step in the production of a package of metal oxide powder to be filled in a resin.
- the method for producing the package of the present invention includes a particle size distribution adjusting step of performing a classification treatment for removing metal oxide particles having a particle diameter equal to or larger than a predetermined particle diameter from the metal oxide powder produced in the production process. It is preferable to further include. As a result, when the metal oxide powder is filled in the liquid resin, the viscosity of the liquid resin filled with the metal oxide powder can be kept low, and the metal oxide powder can be highly filled.
- the classification treatment in the particle size distribution adjustment step and the particle size of the particles to be removed in the classification treatment are the same as those explained in the item of the package, so the explanation is omitted.
- the sealing step includes placing the metal oxide powder in a bag filled with at least one gas selected from the group consisting of rare gas, nitrogen gas, oxygen gas and air, and then sealing the bag. is.
- the gas and bag used in the sealing process are the same as the gas and bag explained in the item of the package, so the explanation is omitted. It is preferable that it takes less than 300 hours from the production of the metal oxide powder in the production process to the sealing in the sealing process.
- the metal oxide powder can be stored with a sufficiently low dielectric loss tangent by keeping the time until sealing within 300 hours. If there are optional steps such as the surface treatment step and the particle size distribution adjustment step, the time from the end of the step immediately before the sealing step to the sealing of the bag containing the metal oxide powder should be within 40 minutes. preferable.
- the water content of the gas was measured by gas chromatography.
- the water content in the sealed bag was obtained by piercing the bag with an injection needle and sucking the gas stored in the bag with a syringe. Then, the water content of the sampled gas was measured by gas chromatography.
- the dielectric loss tangent of the metal oxide powder was measured at a frequency of 1.0 GHz using a perturbation-type cavity resonator measurement system (manufactured by KEYENCE CORPORATION).
- the metal oxide powder was placed in a Karl Fischer trace moisture analyzer (trade name “CA-100”, manufactured by Mitsubishi Chemical Corporation), and the moisture generated while heating with an electric heater was measured by the Karl Fischer coulometric titration method. At times, the water generated up to a temperature of 200°C was defined as "physically adsorbed water”. Then, the water content (% by mass) in the metal oxide powder was calculated by dividing the water content of the physically adsorbed water by the mass of the metal oxide powder used for measurement.
- the specific surface area of the metal oxide powder was measured by the BET method using a specific surface area measuring instrument (trade name “Macsorb HM model-1208” manufactured by MACSORB).
- the particle size (d50) at which the cumulative frequency of the particle size distribution of the metal oxide powder becomes 50% is determined as the average particle size. measured as
- silane coupling agent compound name: 3-methacryloxypropyltrimethoxysilane, trade name “KBM-503”, manufactured by Shin-Etsu Chemical Co., Ltd.
- a pot mill (capacity: 10 L) containing 5 kg of ⁇ 10 mm alumina balls was filled with 1.5 kg of silica powder, and 0.51 g of a silane coupling agent was added.
- the surface treatment was performed for 15 minutes by rotating the pot mill. Thereafter, silica powder containing aggregated particles of 1000 ⁇ m or more was removed using a sieve with an opening of 1 mm to prepare silica powder A.
- gas A gas type: nitrogen, water content: 53 mass ppm
- the time from the adjustment of the particle size distribution to the completion of sealing of the bag A was 30 minutes.
- the package 1 was stored for up to 60 days under an environment of a temperature of 50° C., a relative humidity of 90%, and atmospheric pressure to produce a package 1 after storage.
- the silica powder A was taken out from the package 1, and the dielectric loss tangent and water content were measured.
- the dielectric loss tangent was 0.0029, and the water content (200° C.) was 262 mass ppm.
- Silica powder B was produced in the same manner as silica powder A, except that the silica powder was not treated with a silane coupling agent. Then, a package 2 was produced in the same manner as the package 1, except that the silica powder B was used instead of the silica powder A. After being stored for 60 days, the silica powder B was taken out from the package 2, and the dielectric loss tangent and water content were measured. The dielectric loss tangent was 0.0010, and the water content (200° C.) was 535 mass ppm.
- the package 3 was stored for a maximum of 2 months (long-term storage) under an environment of 50° C. temperature, 90% relative humidity and atmospheric pressure to produce a package 3 after storage.
- the magnesia powder A was taken out from the package 3, and the dielectric loss tangent and water content were measured.
- the dielectric loss tangent was 0.0009, and the water content (200° C.) was 126 mass ppm.
- Bag 4 (trade name “Nylon Poly Barrier TL Type 28-40”, moisture permeability: 9.8 g/(m 2 ⁇ day)) was used instead of bag A.
- Package 3 was produced in the same manner as package 1 except for the above. After long-term storage, the silica powder A was taken out from the package 4, and the dielectric loss tangent and water content were measured. The dielectric loss tangent was 0.0048, and the water content (200° C.) was 1310 mass ppm.
- At least one gas selected from the group consisting of rare gas, nitrogen gas, oxygen gas and dry air is filled, and the moisture permeability is 0.30 g / (m 2 day) or less. It was found that by enclosing the metal oxide powder in a certain bag, deterioration of the dielectric loss tangent due to long-term storage of the metal oxide powder can be suppressed.
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Abstract
Description
そこで、本発明は、長時間の保管による金属酸化物粉末の誘電正接の悪化を抑制できる金属酸化物粉末の包装体及びその包装体の製造方法を提供することを目的とする。
本発明は、上記の知見に基づくものであり、以下を要旨とする。
[1]金属酸化物粉末と、前記金属酸化物粉末を収納し、密閉された袋とを含み、前記袋の中は、希ガス、窒素ガス、酸素ガス及び乾燥空気からなる群から選択される少なくとも1種のガスで満たされており、前記金属酸化物粉末はシリカ粉末又はマグネシア粉末であり、JIS Z 0222-1959に準拠して測定した前記袋の透湿度が0.30g/(m2・day)以下である包装体。
[2]前記希ガス、窒素ガス、酸素ガス及び乾燥空気からなる群から選択される少なくとも1種のガスの水分量が3500質量ppm以下である上記[1]に記載の包装体。
[3]前記金属酸化物粉末の誘電正接が0.004以下である上記[1]又は[2]に記載の包装体。
[4]前記金属酸化物粉末は、シランカップリング剤により表面処理されている上記[1]~[3]のいずれか1つに記載の包装体。
[5]前記金属酸化物粉末は、所定の粒子径以上の粒子径を有する金属酸化物粒子を除去するための分級処理が実施された粒度分布調整品である上記[1]~[4]のいずれか1つに記載の包装体。
[6]金属酸化物粉末を製造する製造工程、及び希ガス、窒素ガス、酸素ガス及び乾燥空気からなる群から選択される少なくとも1種のガスが満たされている袋に前記金属酸化物粉末を収納し、その後、前記袋を密封する密封工程を含み、前記金属酸化物粉末がシリカ粉末又はマグネシア粉末であり、JIS Z 0222-1959に準拠して測定した前記袋の透湿度が0.30g/(m2・day)以下である包装体の製造方法。
[7]前記希ガス、窒素ガス、酸素ガス及び乾燥空気からなる群から選択される少なくとも1種のガスの水分量が3500質量ppm以下である上記[6]に記載の包装体の製造方法。
[8]前記製造工程で前記金属酸化物粉末を製造してから300時間以内に、前記密閉工程において、前記金属酸化物粉末を前記袋に収納し、前記袋を密封する上記[6]又は[7]に記載の包装体の製造方法。
[9]シランカップリング剤を用いて前記製造工程で製造した前記金属酸化物粉末の表面処理を実施する表面処理工程をさらに含む上記[6]~[8]のいずれか1つに記載の包装体の製造方法。
[10]前記製造工程で製造した前記金属酸化物粉末から、所定の粒子径以上の粒子径を有する金属酸化物粒子を除去するための分級処理を実施する粒度分布調整工程をさらに含む上記[6]~[9]のいずれか1つに記載の包装体の製造方法。
[11]前記製造工程で前記金属酸化物粉末を製造してから40分以内に、前記金属酸化物粉末を袋に収納し、前記袋を密封する処理前密封工程をさらに有し、前記処理前密封工程後に、密封した前記袋を開封し、前記表面処理工程及び/又は粒度分布調整工程を行う上記[9]又は[10]に記載の包装体の製造方法。
以下、本発明の包装体を説明する。本発明の包装体は、金属酸化物粉末と、金属酸化物粉末を収納し、密閉された袋とを含み、袋の中は、希ガス、窒素ガス、酸素ガス及び乾燥空気からなる群から選択される少なくとも1種のガスで満たされており、金属酸化物粉末はシリカ粉末又はマグネシア粉末であり、JIS Z 0222-1959に準拠して測定した上記袋の透湿度が0.30g/(m2・day)以下である。これにより、金属酸化物粉末を長時間保管しても、金属酸化物粉末の誘電正接は悪化しないか、又は悪化したとしても悪化の程度は小さい。また、長時間保管による粉末の凝集も抑制できる。
本発明の包装体における金属酸化物粉末は、シリカ粉末又はマグネシア粉末である。シリカ粉末及びマグネシア粉末は、誘電率及び誘電正接が小さい。このため、移動通信システムに使用する材料にシリカ粉末もしくはマグネシア粉末を使用することにより、移動通信システムにおける信号伝播を高速化できるとともに、信号の伝送損失を低減することができる。移動通信システムでは、シリカ粉末及びマグネシア粉末は、例えば、樹脂との複合材料の形態で使用される。シリカ粉末及びマグネシア粉末と一緒に使用される樹脂は特に限定されないが、例えば、ポリエチレン、ポリプロピレン、エポキシ樹脂、シリコーン樹脂、フェノール樹脂、メラミン樹脂、ユリア樹脂、不飽和ポリエステル、フッ素樹脂、ポリイミド、ポリアミドイミド、ポリエーテルイミド等のポリアミド、ポリブチレンテレフタレート、ポリエチレンテレフタレート等のポリエステル、ポリフェニレンスルフィド、全芳香族ポリエステル、ポリスルホン、液晶ポリマー、ポリエーテルスルホン、ポリカーボネート、マレイミド変性樹脂、ABS樹脂、AAS(アクリロニトリル-アクリルゴム・スチレン)樹脂、AES(アクリロニトリル・エチレン・プロピレン・ジエンゴム-スチレン)樹脂等が挙げられる。樹脂中におけるシリカ粉末及びマグネシア粉末の割合は、目標とする誘電率や誘電正接等の物性に応じて適宜選択される。例えば、樹脂の使用量は、シリカ粉末もしくはマグネシア粉末100質量部に対して、5~300質量部の範囲で適宜選択される。樹脂に充填される用途においては樹脂との相溶性や粘度制御の観点から表面処理や粒度分布調整を行うことが有効である。したがって、樹脂に充填される金属酸化物粉末の包装体の製造の際には表面処理工程や粒度分布調整工程を行う必要性が高い。
本発明の包装体における袋は、金属酸化物粉末を収納するとともに、密閉されている。そして、JIS Z 0222-1959に準拠して測定した袋の透湿度が0.30g/(m2・day)以下である。袋の透湿度が0.30g/(m2・day)よりも大きいと、袋の外部にある水蒸気が袋の中に侵入し、金属酸化物粉末の表面にOH基を形成する場合がある。その結果、金属酸化物粉末の誘電正接が悪化する場合がある。このような観点から、袋の透湿度は、好ましくは0.10g/(m2・day)以下であり、より好ましくは0.08g/(m2・day)以下である。また、袋の透湿度の範囲の下限値は特に限定されないが、例えば、0.04g/(m2・day)である。袋の透湿度は、具体的には、後述の実施例に記載の方法により測定することができる。
本発明の包装体における袋の中は、希ガス、窒素ガス、酸素ガス及び乾燥空気からなる群から選択される少なくとも1種のガスで満たされている。これにより、袋中のガスの水分によって金属酸化物粉末の表面にOH基が形成され、金属酸化物粉末の誘電正接が悪化することをさらに抑制できる。このような観点から、袋中のガスの水分量は、好ましくは水分量3500質量ppm以下であり、より好ましくは1000質量ppm以下であり、さらに好ましくは500質量ppm以下である。袋中のガスの水分量の範囲の下限値は特に限定されないが、通常、コストの観点から、50質量ppmである。ガス中の水分量は実施例の記載の方法により測定することができる。なお、好ましい希ガスはアルゴンガスである。
以下、本発明の包装体の製造方法を説明する。本発明の包装体の製造方法は、金属酸化物粉末を製造する製造工程、金属酸化物粉末を袋に収納し、その袋を仮に密封する処理前密封工程、シランカップリング剤を用いて、製造工程で製造した金属酸化物粉末の表面処理を実施する表面処理工程、製造工程で製造した金属酸化物粉末から、所定の粒子径以上の粒子径を有する金属酸化物粒子を除去するための分級処理を実施する粒度分布調整工程、及び希ガス、窒素ガス、酸素ガス及び空気からなる群から選択される少なくとも1種のガスが満たされている袋に金属酸化物粉末を収納し、その後、その袋を密封する密封工程を含む。なお、後述するように、処理前密封工程、表面処理工程及び粒度分布調整工程は任意工程であるので、本発明の包装体の製造方法は、処理前密封工程、表面処理工程及び粒度分布調整工程を含まなくてもよい。そして、金属酸化物粉末がシリカ粉末又はマグネシア粉末であり、JIS Z 0222-1959に準拠して測定した袋の透湿度が0.30g/(m2・day)以下である。
製造工程において、シリカ粉末は公知の方法により製造することができる。例えば、四塩化ケイ素を酸素/水素火炎中で1000℃以上の高温下で加水分解することによりシリカ粉末を製造してもよいし、シリカ又は金属シリコンを火炎溶射することによりシリカ粉末を製造してもよい。
処理前密封工程は表面処理工程及び/又は粒度分布調整工程を行う前に、金属酸化物粉末を袋に収納し、その後、その袋を仮に密封する工程である。なお、後述する通り表面処理工程及び粒度分布調整工程は任意工程であり、処理前密封工程も任意工程である。
処理密封工程において使用する袋は、包装体の項目で説明した袋と同様であるので、説明は省略する。なお、袋の密封は、例えばヒートシール(熱融着)により実施することができる。また、空気が入らないように空気を抜きながら金属酸化物粉末を袋詰めすることが好ましい。
表面処理工程は任意工程である。上述の通り、樹脂に充填される金属酸化物粉末の包装体の製造においては、表面処理工程を設けることが好ましい。
本発明の包装体の製造方法は、シランカップリング剤を用いて、製造工程で製造した金属酸化物粉末の表面処理を実施する表面処理工程をさらに含むことが好ましい。これにより、金属酸化物粉末が保管中に凝集することをさらに抑制することができる。なお、表面処理工程で使用するシランカップリング剤は、包装体の項目で説明したシランカップリング剤と同様であるので、シランカップリング剤の説明は省略する。シランカップリング剤による金属酸化物の表面処理は、乾式処理法で行うことが好ましい。
粒度分布調整工程は任意工程である。上述の通り、樹脂に充填される金属酸化物粉末の包装体の製造においては、粒度分布調整工程を設けることが好ましい。
本発明の包装体の製造方法は、製造工程で製造した金属酸化物粉末から、所定の粒子径以上の粒子径を有する金属酸化物粒子を除去するための分級処理を実施する粒度分布調整工程をさらに含むことが好ましい。これにより、金属酸化物粉末を液状樹脂に充填したとき、金属酸化物粉末を充填した液状樹脂の粘度を低く抑えることができ、金属酸化物粉末の高充填が可能となる。なお、粒度分布調整工程における分級処理及び分級処理で除去する粒子の粒径は、包装体の項目で説明したものと同様であるので、説明を省略する。
(密封工程)
密封工程は、希ガス、窒素ガス、酸素ガス及び空気からなる群から選択される少なくとも1種のガスが満たされている袋に前記金属酸化物粉末を収納し、その後、前記袋を密封する工程である。
密封工程で使用するガス及び袋については包装体の項目で説明したガス及び袋と同様であるので、説明は省略する。
製造工程で金属酸化物粉末を製造してから密封工程で密封するまでは300時間以内であることが好ましい。上記表面処理工程や粒度分布調整工程を行う場合であっても、密封までを300時間以内に抑えることで、誘電正接を十分低い状態で金属酸化物粉末を保管できる。
上記表面処理工程や粒度分布調整工程等の任意工程がある場合、密封工程の直前の工程が終了してから金属酸化物粉末を収納した袋を密封するまでの時間は40分以内であることが好ましい。
(袋の透湿度)
JIS Z 0222-1959に準拠して袋の透湿度を測定した。
ガスクロマトグラフィーでガスの水分量を測定した。なお、密閉した袋内の水分量は、袋に注射針を突き刺し、袋の中に保存されたガスを注射器で吸引して採取した。そして、ガスクロマトグラフィーで採取したガスの水分量を測定した。
金属酸化物粉末の誘電正接は、摂動方式空洞共振器測定システム(株式会社キーエンス製)を用いて周波数1.0GHzにて測定した。
カールフィッシャー微量水分測定装置(商品名「CA-100」、三菱化学株式会社製)に金属酸化物粉末を入れ、電気ヒーターで加熱昇温しながら発生した水分をカールフィッシャー電量滴定法にて測定したときに、温度200℃までに発生した水分を「物理的吸着水」と定義した。そして、物理的吸着水の水分量を、測定に用いた金属酸化物粉末の質量で割り算することにより、金属酸化物粉末における水分量(質量%)を算出した。
金属酸化物粉末の比表面積は、比表面積測定機(商品名「Macsorb HM model-1208」、MACSORB社製)を使用して、BET法により測定した。
レーザー式粒度分布測定機(商品名「MT-3300EX」、日機装株式会社製)を使用して、金属酸化物粉末の粒度分布の頻度の累積が50%となる粒子径(d50)を平均粒子径として測定した。
(包装体1)
<シリカ粉末Aの作製>
火炎溶融法を用いて平均粒径0.8μm、比表面積6.0m2/g、d100(粒度分布の頻度の累積が100%となる粒子径)=5.1μmのシリカ粒子を合成した。得られたシリカ粉末は内容積8Lのムライト容器に1.6kg充填し、マッフル炉で大気雰囲気のもと970℃で加熱処理を8時間行った。加熱処理で得られたシリカ粉末は30分以内にアルミ袋へ空気を抜きながら移し替えた(処理前密封工程に相当)。この時の試料温度は23℃であった。
そして、開封して、シランカップリング剤(化合物名:3-メタクリロキシプロピルトリメトキシシラン、商品名「KBM-503」、信越化学工業株式会社製)を用いて表面処理した。具体的には、φ10mmのアルミナボールが5kg入っているポットミル(容量:10L)にシリカ粉末1.5kgを充填し、シランカップリング剤を0.51g添加した。そして、ポットミルを回転させて15分間表面処理を行った。
その後目開き1mmのふるいを使用して、1000μm以上の凝集粒子を含むシリカ粉末を除去し、シリカ粉末Aを作製した。
シリカ粉末A1500gを340mm×480mm×60mmの大きさの袋A(商品名「ラミジップ」、株式会社生産日本社製、透湿度:0.1g/(m2・day)、材質:アルミフィルムにPEをコーティングしたガスバリアフィルム)に収納した。そして、袋Aの中の空気を除去した後、ガスA(ガスの種類:窒素、水分量:53質量ppm)5000mlを袋Aの中に充填し、そして、ヒートシーラー(商品名「FV-801-01」、白光株式会社製)を使用して、袋Aを密封して包装体1を作製した。なお、粒度分布を調整してから袋Aの密封が完了するまでの時間は30分であった。その後、包装体1を50℃の温度、90%の相対湿度及び大気圧の環境下で最大60日間保管し、保管後の包装体1を作製した。
長期間保管後に包装体1からシリカ粉末Aを取り出し、誘電正接及び水分量を測定した。誘電正接は0.0029、水分量(200℃)は262質量ppmであった。
シランカップリング剤処理をしない以外はシリカ粉末Aと同様にしてシリカ粉末Bを製造した。そして、シリカ粉末Aの代わりにシリカ粉末Bを使用した以外は、包装体1と同様にして、包装体2を作製した。60日間保管後に包装体2からシリカ粉末Bを取り出し、誘電正接及び水分量を測定した。誘電正接は0.0010、水分量(200℃)は535質量ppmであった。
<マグネシア粉末Aの作製>
球状マグネシウム(DMG-120、タテホ化学工業株式会社製)を300μm以上の粒子径を有する粒子を除去し、マグネシア粉末を作製した。31℃まで冷却し30分以内にアルミ袋へ空気を抜きながら移し替えた。アルミ袋の封を開けて粒度分布を調整して、マグネシア粉末Aとした。
マグネシア粉末A1000gを340mm×480mm×60mmの大きさの袋A(商品名「ラミジップ」、株式会社生産日本社製、透湿度:0.1g/(m2・day)、材質:アルミフィルムにPEをコーティングしたガスバリアフィルム)に収納した。そして、袋Aの中の空気を除去した後、ガスA(ガスの種類:アルゴン、水分量:30質量ppm)を袋Aの中に充填し、そして、ヒートシーラー(商品名「FV-801-01」、白光株式会社製)を使用して、袋Aを密封して包装体3を作製した。なお、マグネシア粉末Aを製造してから袋Aの密封が完了するまでの時間は25分であった。その後、包装体3を50℃の温度、90%の相対湿度及び大気圧の環境下で最大2か月間保管(長期間保管)し、保管後の包装体3を作製した。長期間保管後に包装体3からマグネシア粉末Aを取り出し、誘電正接及び水分量を測定した。誘電正接は0.0009、水分量(200℃)は126質量ppmであった。
袋Aの代わりに袋B(商品名「ナイロンポリ バリアTLタイプ 28-40」、透湿度:9.8g/(m2・day))を使用した。それ以外は、包装体1と同様な方法で包装体3を作製した。長期間保管後に包装体4からシリカ粉末Aを取り出し、誘電正接及び水分量を測定した。誘電正接は0.0048、水分量(200℃)は1310質量ppmであった。
Claims (11)
- 金属酸化物粉末と、前記金属酸化物粉末を収納し、密閉された袋とを含み、
前記袋の中は、希ガス、窒素ガス、酸素ガス及び乾燥空気からなる群から選択される少なくとも1種のガスで満たされており、
前記金属酸化物粉末はシリカ粉末又はマグネシア粉末であり、
JIS Z 0222-1959に準拠して測定した前記袋の透湿度が0.30g/(m2・day)以下である包装体。 - 前記希ガス、窒素ガス、酸素ガス及び乾燥空気からなる群から選択される少なくとも1種のガスの水分量が3500質量ppm以下である請求項1に記載の包装体。
- 前記金属酸化物粉末の誘電正接が0.004以下である請求項1又は2に記載の包装体。
- 前記金属酸化物粉末は、シランカップリング剤により表面処理されている請求項1~3のいずれか1項に記載の包装体。
- 前記金属酸化物粉末は、所定の粒子径以上の粒子径を有する金属酸化物粒子を除去するための分級処理が実施された粒度分布調整品である請求項1~4のいずれか1項に記載の包装体。
- 金属酸化物粉末を製造する製造工程、及び
希ガス、窒素ガス、酸素ガス及び乾燥空気からなる群から選択される少なくとも1種のガスが満たされている袋に前記金属酸化物粉末を収納し、その後、前記袋を密封する密封工程を含み、
前記金属酸化物粉末がシリカ粉末又はマグネシア粉末であり、
JIS Z 0222-1959に準拠して測定した前記袋の透湿度が0.30g/(m2・day)以下である包装体の製造方法。 - 前記希ガス、窒素ガス、酸素ガス及び乾燥空気からなる群から選択される少なくとも1種のガスの水分量が3500質量ppm以下である請求項6に記載の包装体の製造方法。
- 前記製造工程で前記金属酸化物粉末を製造してから300時間以内に、前記密閉工程において、前記金属酸化物粉末を前記袋に収納し、前記袋を密封する請求項6又は7に記載の包装体の製造方法。
- シランカップリング剤を用いて前記製造工程で製造した前記金属酸化物粉末の表面処理を実施する表面処理工程をさらに含む請求項6~8のいずれか1項に記載の包装体の製造方法。
- 前記製造工程で製造した前記金属酸化物粉末から、所定の粒子径以上の粒子径を有する金属酸化物粒子を除去するための分級処理を実施する粒度分布調整工程をさらに含む請求項6~9のいずれか1項に記載の包装体の製造方法。
- 前記製造工程で前記金属酸化物粉末を製造してから40分以内に、前記金属酸化物粉末を袋に収納し、前記袋を密封する処理前密封工程をさらに有し、
前記処理前密封工程後に、密封した前記袋を開封し、前記表面処理工程及び/又は粒度分布調整工程を行う請求項9又は10に記載の包装体の製造方法。
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JPH1045161A (ja) * | 1996-07-30 | 1998-02-17 | Mitsui Petrochem Ind Ltd | 包装体 |
JP2003026251A (ja) * | 2001-07-18 | 2003-01-29 | Ngk Spark Plug Co Ltd | 吸湿性セラミックスの包装方法及び保管方法 |
JP2016204054A (ja) * | 2011-08-12 | 2016-12-08 | 株式会社日本触媒 | フッ素原子を含むイオン性化合物またはフッ素原子を含むイオン性化合物含有組成物を包装してなる包装体 |
WO2020195205A1 (ja) * | 2019-03-26 | 2020-10-01 | デンカ株式会社 | 球状シリカ粉末 |
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JPH04268085A (ja) * | 1991-02-22 | 1992-09-24 | Mitsubishi Gas Chem Co Inc | 被酸化性粉体の保存方法 |
JPH1045161A (ja) * | 1996-07-30 | 1998-02-17 | Mitsui Petrochem Ind Ltd | 包装体 |
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JP7473725B1 (ja) | 2023-08-25 | 2024-04-23 | デンカ株式会社 | シリカ粉末 |
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