CN104114492A - 氢氧化镁微粒 - Google Patents
氢氧化镁微粒 Download PDFInfo
- Publication number
- CN104114492A CN104114492A CN201380006920.8A CN201380006920A CN104114492A CN 104114492 A CN104114492 A CN 104114492A CN 201380006920 A CN201380006920 A CN 201380006920A CN 104114492 A CN104114492 A CN 104114492A
- Authority
- CN
- China
- Prior art keywords
- magnesium hydroxide
- magnesium
- agent
- treated side
- resin
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- VTHJTEIRLNZDEV-UHFFFAOYSA-L magnesium dihydroxide Chemical compound [OH-].[OH-].[Mg+2] VTHJTEIRLNZDEV-UHFFFAOYSA-L 0.000 title claims abstract description 76
- 239000000347 magnesium hydroxide Substances 0.000 title claims abstract description 76
- 229910001862 magnesium hydroxide Inorganic materials 0.000 title claims abstract description 76
- 239000011859 microparticle Substances 0.000 title abstract 3
- 239000002245 particle Substances 0.000 claims abstract description 41
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 21
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 18
- 238000004458 analytical method Methods 0.000 claims abstract description 14
- 238000004519 manufacturing process Methods 0.000 claims abstract description 13
- 229920005989 resin Polymers 0.000 claims description 31
- 239000011347 resin Substances 0.000 claims description 31
- 238000000034 method Methods 0.000 claims description 29
- 238000006243 chemical reaction Methods 0.000 claims description 21
- 239000002994 raw material Substances 0.000 claims description 19
- 159000000003 magnesium salts Chemical class 0.000 claims description 10
- 239000012266 salt solution Substances 0.000 claims description 10
- 229920003002 synthetic resin Polymers 0.000 claims description 10
- 239000000057 synthetic resin Substances 0.000 claims description 10
- 238000000465 moulding Methods 0.000 claims description 9
- 238000012545 processing Methods 0.000 claims description 8
- 239000012756 surface treatment agent Substances 0.000 claims description 7
- 239000007822 coupling agent Substances 0.000 claims description 6
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 5
- 239000002253 acid Substances 0.000 claims description 5
- 150000002632 lipids Chemical class 0.000 claims description 4
- 229920000098 polyolefin Polymers 0.000 claims description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 3
- 239000006087 Silane Coupling Agent Substances 0.000 claims description 3
- 239000013543 active substance Substances 0.000 claims description 3
- 150000004645 aluminates Chemical class 0.000 claims description 3
- 125000000129 anionic group Chemical group 0.000 claims description 3
- 235000014113 dietary fatty acids Nutrition 0.000 claims description 3
- 239000000194 fatty acid Substances 0.000 claims description 3
- 229930195729 fatty acid Natural products 0.000 claims description 3
- 150000004665 fatty acids Chemical class 0.000 claims description 3
- 150000003014 phosphoric acid esters Chemical class 0.000 claims description 3
- 238000004381 surface treatment Methods 0.000 claims description 3
- 238000013459 approach Methods 0.000 claims description 2
- 239000002105 nanoparticle Substances 0.000 abstract description 12
- 239000011163 secondary particle Substances 0.000 abstract 1
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 21
- 239000002002 slurry Substances 0.000 description 20
- -1 (N-aminoethyl-aminoethyl) isopropyl Chemical group 0.000 description 18
- 239000003795 chemical substances by application Substances 0.000 description 17
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 15
- 238000005406 washing Methods 0.000 description 12
- 238000009826 distribution Methods 0.000 description 9
- 238000002156 mixing Methods 0.000 description 9
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 8
- 150000002500 ions Chemical group 0.000 description 7
- 235000011121 sodium hydroxide Nutrition 0.000 description 7
- 238000002296 dynamic light scattering Methods 0.000 description 6
- 238000004945 emulsification Methods 0.000 description 6
- 238000001914 filtration Methods 0.000 description 6
- 238000005342 ion exchange Methods 0.000 description 6
- WALYXZANOBBHCI-UHFFFAOYSA-K magnesium sodium trichloride hydrate Chemical compound O.[Cl-].[Na+].[Mg+2].[Cl-].[Cl-] WALYXZANOBBHCI-UHFFFAOYSA-K 0.000 description 6
- 238000000926 separation method Methods 0.000 description 6
- 239000007787 solid Substances 0.000 description 6
- 239000000654 additive Substances 0.000 description 5
- 150000001408 amides Chemical class 0.000 description 5
- 230000000052 comparative effect Effects 0.000 description 5
- 238000002425 crystallisation Methods 0.000 description 5
- 230000008025 crystallization Effects 0.000 description 5
- 239000000446 fuel Substances 0.000 description 5
- 239000003595 mist Substances 0.000 description 5
- 239000000203 mixture Substances 0.000 description 5
- BDHFUVZGWQCTTF-UHFFFAOYSA-M sulfonate Chemical compound [O-]S(=O)=O BDHFUVZGWQCTTF-UHFFFAOYSA-M 0.000 description 5
- 238000002525 ultrasonication Methods 0.000 description 5
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 4
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 4
- 230000000996 additive effect Effects 0.000 description 4
- 239000012752 auxiliary agent Substances 0.000 description 4
- 238000002485 combustion reaction Methods 0.000 description 4
- 235000013399 edible fruits Nutrition 0.000 description 4
- 150000002148 esters Chemical class 0.000 description 4
- GLDOVTGHNKAZLK-UHFFFAOYSA-N octadecan-1-ol Chemical compound CCCCCCCCCCCCCCCCCCO GLDOVTGHNKAZLK-UHFFFAOYSA-N 0.000 description 4
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 3
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 description 3
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 description 3
- 238000002441 X-ray diffraction Methods 0.000 description 3
- 150000001336 alkenes Chemical class 0.000 description 3
- 239000011248 coating agent Substances 0.000 description 3
- 238000000576 coating method Methods 0.000 description 3
- 239000002131 composite material Substances 0.000 description 3
- 229920001577 copolymer Polymers 0.000 description 3
- 239000011777 magnesium Substances 0.000 description 3
- 229910052749 magnesium Inorganic materials 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 229920005992 thermoplastic resin Polymers 0.000 description 3
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 2
- KAKZBPTYRLMSJV-UHFFFAOYSA-N Butadiene Chemical group C=CC=C KAKZBPTYRLMSJV-UHFFFAOYSA-N 0.000 description 2
- VGGSQFUCUMXWEO-UHFFFAOYSA-N Ethene Chemical compound C=C VGGSQFUCUMXWEO-UHFFFAOYSA-N 0.000 description 2
- TWRXJAOTZQYOKJ-UHFFFAOYSA-L Magnesium chloride Chemical compound [Mg+2].[Cl-].[Cl-] TWRXJAOTZQYOKJ-UHFFFAOYSA-L 0.000 description 2
- CSNNHWWHGAXBCP-UHFFFAOYSA-L Magnesium sulfate Chemical compound [Mg+2].[O-][S+2]([O-])([O-])[O-] CSNNHWWHGAXBCP-UHFFFAOYSA-L 0.000 description 2
- 239000004743 Polypropylene Substances 0.000 description 2
- 239000007864 aqueous solution Substances 0.000 description 2
- 239000006229 carbon black Substances 0.000 description 2
- 238000002050 diffraction method Methods 0.000 description 2
- 239000006185 dispersion Substances 0.000 description 2
- 239000003814 drug Substances 0.000 description 2
- 229940079593 drug Drugs 0.000 description 2
- 239000000428 dust Substances 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 229920001971 elastomer Polymers 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000005038 ethylene vinyl acetate Substances 0.000 description 2
- 229920006225 ethylene-methyl acrylate Polymers 0.000 description 2
- 230000002349 favourable effect Effects 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 229920001903 high density polyethylene Polymers 0.000 description 2
- 239000004700 high-density polyethylene Substances 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 229920001684 low density polyethylene Polymers 0.000 description 2
- 239000004702 low-density polyethylene Substances 0.000 description 2
- YIXJRHPUWRPCBB-UHFFFAOYSA-N magnesium nitrate Chemical compound [Mg+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O YIXJRHPUWRPCBB-UHFFFAOYSA-N 0.000 description 2
- GOQYKNQRPGWPLP-UHFFFAOYSA-N n-heptadecyl alcohol Natural products CCCCCCCCCCCCCCCCCO GOQYKNQRPGWPLP-UHFFFAOYSA-N 0.000 description 2
- 229920001200 poly(ethylene-vinyl acetate) Polymers 0.000 description 2
- 229920001083 polybutene Polymers 0.000 description 2
- 229920000139 polyethylene terephthalate Polymers 0.000 description 2
- 239000005020 polyethylene terephthalate Substances 0.000 description 2
- 229920000306 polymethylpentene Polymers 0.000 description 2
- 239000011116 polymethylpentene Substances 0.000 description 2
- 229920001155 polypropylene Polymers 0.000 description 2
- 239000005060 rubber Substances 0.000 description 2
- 229910000077 silane Inorganic materials 0.000 description 2
- 239000002594 sorbent Substances 0.000 description 2
- 230000003068 static effect Effects 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 230000002194 synthesizing effect Effects 0.000 description 2
- 229920003051 synthetic elastomer Polymers 0.000 description 2
- 229920001187 thermosetting polymer Polymers 0.000 description 2
- 238000002834 transmittance Methods 0.000 description 2
- 238000012982 x-ray structure analysis Methods 0.000 description 2
- WRIDQFICGBMAFQ-UHFFFAOYSA-N (E)-8-Octadecenoic acid Natural products CCCCCCCCCC=CCCCCCCC(O)=O WRIDQFICGBMAFQ-UHFFFAOYSA-N 0.000 description 1
- IEKHISJGRIEHRE-UHFFFAOYSA-N 16-methylheptadecanoic acid;propan-2-ol;titanium Chemical compound [Ti].CC(C)O.CC(C)CCCCCCCCCCCCCCC(O)=O.CC(C)CCCCCCCCCCCCCCC(O)=O.CC(C)CCCCCCCCCCCCCCC(O)=O IEKHISJGRIEHRE-UHFFFAOYSA-N 0.000 description 1
- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-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
- NIXOWILDQLNWCW-UHFFFAOYSA-N 2-Propenoic acid Natural products OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 description 1
- LQJBNNIYVWPHFW-UHFFFAOYSA-N 20:1omega9c fatty acid Natural products CCCCCCCCCCC=CCCCCCCCC(O)=O LQJBNNIYVWPHFW-UHFFFAOYSA-N 0.000 description 1
- SJECZPVISLOESU-UHFFFAOYSA-N 3-trimethoxysilylpropan-1-amine Chemical compound CO[Si](OC)(OC)CCCN SJECZPVISLOESU-UHFFFAOYSA-N 0.000 description 1
- QSBYPNXLFMSGKH-UHFFFAOYSA-N 9-Heptadecensaeure Natural products CCCCCCCC=CCCCCCCCC(O)=O QSBYPNXLFMSGKH-UHFFFAOYSA-N 0.000 description 1
- 239000004925 Acrylic resin Substances 0.000 description 1
- 229920000178 Acrylic resin Polymers 0.000 description 1
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical class [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 description 1
- 239000004709 Chlorinated polyethylene Substances 0.000 description 1
- ZDQWESQEGGJUCH-UHFFFAOYSA-N Diisopropyl adipate Chemical compound CC(C)OC(=O)CCCCC(=O)OC(C)C ZDQWESQEGGJUCH-UHFFFAOYSA-N 0.000 description 1
- 229920002943 EPDM rubber Polymers 0.000 description 1
- 229920002449 FKM Polymers 0.000 description 1
- VHOQXEIFYTTXJU-UHFFFAOYSA-N Isobutylene-isoprene copolymer Chemical group CC(C)=C.CC(=C)C=C VHOQXEIFYTTXJU-UHFFFAOYSA-N 0.000 description 1
- 239000004640 Melamine resin Substances 0.000 description 1
- 229920000877 Melamine resin Polymers 0.000 description 1
- 229920000459 Nitrile rubber Polymers 0.000 description 1
- 239000005642 Oleic acid Substances 0.000 description 1
- ZQPPMHVWECSIRJ-UHFFFAOYSA-N Oleic acid Natural products CCCCCCCCC=CCCCCCCCC(O)=O ZQPPMHVWECSIRJ-UHFFFAOYSA-N 0.000 description 1
- 229930182556 Polyacetal Natural products 0.000 description 1
- 239000004698 Polyethylene Substances 0.000 description 1
- 239000004642 Polyimide Substances 0.000 description 1
- 239000004721 Polyphenylene oxide Substances 0.000 description 1
- 239000004734 Polyphenylene sulfide Substances 0.000 description 1
- 239000004793 Polystyrene Substances 0.000 description 1
- 235000021355 Stearic acid Nutrition 0.000 description 1
- 238000003917 TEM image Methods 0.000 description 1
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 1
- 229920010741 Ultra High Molecular Weight Polyethylene (UHMWPE) Polymers 0.000 description 1
- 229920001807 Urea-formaldehyde Polymers 0.000 description 1
- 229920006311 Urethane elastomer Polymers 0.000 description 1
- XTXRWKRVRITETP-UHFFFAOYSA-N Vinyl acetate Chemical compound CC(=O)OC=C XTXRWKRVRITETP-UHFFFAOYSA-N 0.000 description 1
- BZHJMEDXRYGGRV-UHFFFAOYSA-N Vinyl chloride Chemical group ClC=C BZHJMEDXRYGGRV-UHFFFAOYSA-N 0.000 description 1
- 239000006096 absorbing agent Substances 0.000 description 1
- 125000000218 acetic acid group Chemical group C(C)(=O)* 0.000 description 1
- LCJHLOJKAAQLQW-UHFFFAOYSA-N acetic acid;ethane Chemical compound CC.CC(O)=O LCJHLOJKAAQLQW-UHFFFAOYSA-N 0.000 description 1
- 229920000800 acrylic rubber Polymers 0.000 description 1
- 229920000122 acrylonitrile butadiene styrene Polymers 0.000 description 1
- 229920001895 acrylonitrile-acrylic-styrene Polymers 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 125000003545 alkoxy group Chemical group 0.000 description 1
- HSFWRNGVRCDJHI-UHFFFAOYSA-N alpha-acetylene Natural products C#C HSFWRNGVRCDJHI-UHFFFAOYSA-N 0.000 description 1
- 239000004411 aluminium Substances 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- 229940069428 antacid Drugs 0.000 description 1
- 239000003159 antacid agent Substances 0.000 description 1
- 230000001458 anti-acid effect Effects 0.000 description 1
- 239000003963 antioxidant agent Substances 0.000 description 1
- 230000003078 antioxidant effect Effects 0.000 description 1
- 238000003556 assay Methods 0.000 description 1
- 238000000889 atomisation Methods 0.000 description 1
- 238000012550 audit Methods 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 125000004432 carbon atom Chemical group C* 0.000 description 1
- 150000001732 carboxylic acid derivatives Chemical class 0.000 description 1
- 238000005266 casting Methods 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 229920006026 co-polymeric resin Polymers 0.000 description 1
- 239000003034 coal gas Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000001276 controlling effect Effects 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 238000006477 desulfuration reaction Methods 0.000 description 1
- 230000023556 desulfurization Effects 0.000 description 1
- 150000001993 dienes Chemical class 0.000 description 1
- 150000005690 diesters Chemical class 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 239000000975 dye Substances 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 239000008393 encapsulating agent Substances 0.000 description 1
- 239000003822 epoxy resin Substances 0.000 description 1
- MASNVFNHVJIXLL-UHFFFAOYSA-N ethenyl(ethoxy)silicon Chemical compound CCO[Si]C=C MASNVFNHVJIXLL-UHFFFAOYSA-N 0.000 description 1
- XEKOWRVHYACXOJ-UHFFFAOYSA-N ethyl acetate Substances CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 description 1
- 229920006228 ethylene acrylate copolymer Polymers 0.000 description 1
- 229920006242 ethylene acrylic acid copolymer Polymers 0.000 description 1
- 125000002534 ethynyl group Chemical group [H]C#C* 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
- 235000011194 food seasoning agent Nutrition 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 238000010559 graft polymerization reaction Methods 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 229910052736 halogen Inorganic materials 0.000 description 1
- 150000002367 halogens Chemical class 0.000 description 1
- IPCSVZSSVZVIGE-UHFFFAOYSA-N hexadecanoic acid Chemical compound CCCCCCCCCCCCCCCC(O)=O IPCSVZSSVZVIGE-UHFFFAOYSA-N 0.000 description 1
- 229920001519 homopolymer Polymers 0.000 description 1
- FAHBNUUHRFUEAI-UHFFFAOYSA-M hydroxidooxidoaluminium Chemical compound O[Al]=O FAHBNUUHRFUEAI-UHFFFAOYSA-M 0.000 description 1
- 229920002681 hypalon Polymers 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 239000003112 inhibitor Substances 0.000 description 1
- 150000002484 inorganic compounds Chemical class 0.000 description 1
- 229910010272 inorganic material Inorganic materials 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- QXJSBBXBKPUZAA-UHFFFAOYSA-N isooleic acid Natural products CCCCCCCC=CCCCCCCCCC(O)=O QXJSBBXBKPUZAA-UHFFFAOYSA-N 0.000 description 1
- 125000001449 isopropyl group Chemical group [H]C([H])([H])C([H])(*)C([H])([H])[H] 0.000 description 1
- 239000000314 lubricant Substances 0.000 description 1
- 229910001629 magnesium chloride Inorganic materials 0.000 description 1
- 229910052943 magnesium sulfate Inorganic materials 0.000 description 1
- 235000019341 magnesium sulphate Nutrition 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 239000000113 methacrylic resin Substances 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 235000010755 mineral Nutrition 0.000 description 1
- 230000003472 neutralizing effect Effects 0.000 description 1
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 description 1
- OQCDKBAXFALNLD-UHFFFAOYSA-N octadecanoic acid Natural products CCCCCCCC(C)CCCCCCCCC(O)=O OQCDKBAXFALNLD-UHFFFAOYSA-N 0.000 description 1
- ZQPPMHVWECSIRJ-KTKRTIGZSA-N oleic acid Chemical compound CCCCCCCC\C=C/CCCCCCCC(O)=O ZQPPMHVWECSIRJ-KTKRTIGZSA-N 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 239000005011 phenolic resin Substances 0.000 description 1
- 229920006287 phenoxy resin Polymers 0.000 description 1
- 239000013034 phenoxy resin Substances 0.000 description 1
- 238000005498 polishing Methods 0.000 description 1
- 229920002492 poly(sulfone) Polymers 0.000 description 1
- 229920000058 polyacrylate Polymers 0.000 description 1
- 229920001707 polybutylene terephthalate Polymers 0.000 description 1
- 229920000515 polycarbonate Polymers 0.000 description 1
- 239000004417 polycarbonate Substances 0.000 description 1
- 229920000647 polyepoxide Polymers 0.000 description 1
- 229920000573 polyethylene Polymers 0.000 description 1
- 229920000151 polyglycol Polymers 0.000 description 1
- 239000010695 polyglycol Substances 0.000 description 1
- 229920001721 polyimide Polymers 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 229920006324 polyoxymethylene Polymers 0.000 description 1
- 229920006380 polyphenylene oxide Polymers 0.000 description 1
- 229920000069 polyphenylene sulfide Polymers 0.000 description 1
- 229920005673 polypropylene based resin Polymers 0.000 description 1
- 229920002223 polystyrene Polymers 0.000 description 1
- 239000004800 polyvinyl chloride Substances 0.000 description 1
- 229920000915 polyvinyl chloride Polymers 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- QQONPFPTGQHPMA-UHFFFAOYSA-N propylene Natural products CC=C QQONPFPTGQHPMA-UHFFFAOYSA-N 0.000 description 1
- 238000010298 pulverizing process Methods 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 239000012779 reinforcing material Substances 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 229920002379 silicone rubber Polymers 0.000 description 1
- 239000004945 silicone rubber Substances 0.000 description 1
- PCMORTLOPMLEFB-ONEGZZNKSA-N sinapic acid Chemical compound COC1=CC(\C=C\C(O)=O)=CC(OC)=C1O PCMORTLOPMLEFB-ONEGZZNKSA-N 0.000 description 1
- PCMORTLOPMLEFB-UHFFFAOYSA-N sinapinic acid Natural products COC1=CC(C=CC(O)=O)=CC(OC)=C1O PCMORTLOPMLEFB-UHFFFAOYSA-N 0.000 description 1
- 239000002689 soil Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 229910001220 stainless steel Inorganic materials 0.000 description 1
- 239000010935 stainless steel Substances 0.000 description 1
- 239000008117 stearic acid Substances 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 238000005728 strengthening Methods 0.000 description 1
- 229920003048 styrene butadiene rubber Polymers 0.000 description 1
- 150000005846 sugar alcohols Polymers 0.000 description 1
- 239000005061 synthetic rubber Substances 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 239000010936 titanium Substances 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 1
- 238000012546 transfer Methods 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
- YUYCVXFAYWRXLS-UHFFFAOYSA-N trimethoxysilane Chemical compound CO[SiH](OC)OC YUYCVXFAYWRXLS-UHFFFAOYSA-N 0.000 description 1
- 229920001862 ultra low molecular weight polyethylene Polymers 0.000 description 1
- 229920006337 unsaturated polyester resin Polymers 0.000 description 1
- 239000002966 varnish Substances 0.000 description 1
- 229920002554 vinyl polymer Polymers 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
- 239000004711 α-olefin Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
-
- 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
-
- 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
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K9/00—Use of pretreated ingredients
- C08K9/04—Ingredients treated with organic substances
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B7/00—Insulated conductors or cables characterised by their form
- H01B7/17—Protection against damage caused by external factors, e.g. sheaths or armouring
- H01B7/29—Protection against damage caused by extremes of temperature or by flame
- H01B7/295—Protection against damage caused by extremes of temperature or by flame using material resistant to flame
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/04—Particle morphology depicted by an image obtained by TEM, STEM, STM or AFM
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/51—Particles with a specific particle size distribution
- C01P2004/52—Particles with a specific particle size distribution highly monodisperse size distribution
-
- 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
- C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer
-
- 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
- C01P2006/60—Optical properties, e.g. expressed in CIELAB-values
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2217—Oxides; Hydroxides of metals of magnesium
- C08K2003/2224—Magnesium hydroxide
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/002—Physical properties
- C08K2201/003—Additives being defined by their diameter
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B3/00—Insulators or insulating bodies characterised by the insulating materials; Selection of materials for their insulating or dielectric properties
- H01B3/18—Insulators or insulating bodies characterised by the insulating materials; Selection of materials for their insulating or dielectric properties mainly consisting of organic substances
- H01B3/30—Insulators or insulating bodies characterised by the insulating materials; Selection of materials for their insulating or dielectric properties mainly consisting of organic substances plastics; resins; waxes
- H01B3/44—Insulators or insulating bodies characterised by the insulating materials; Selection of materials for their insulating or dielectric properties mainly consisting of organic substances plastics; resins; waxes vinyl resins; acrylic resins
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
- Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
- Y10T428/00—Stock material or miscellaneous articles
- Y10T428/29—Coated or structually defined flake, particle, cell, strand, strand portion, rod, filament, macroscopic fiber or mass thereof
- Y10T428/2982—Particulate matter [e.g., sphere, flake, etc.]
Abstract
本发明的目的在于提供一种具有纳米粒子级的粒径、碳含量少而白度高、透明性高的氢氧化镁微粒及其制造方法。本发明为一种氢氧化镁微粒,其通过频率分析测定的平均二次粒径为1~100nm,且碳含量不足0.9重量%。
Description
技术领域
本发明涉及一种氢氧化镁微粒及其制造方法。并且涉及一种包含该粒子的树脂组合物及由其形成的成形品。
背景技术
氢氧化镁粒子自古以来便为人所知,其在医药用途、工业用途的广泛领域中被使用。例如,作为医药用途,有抗酸剂、泻药和动物用药剂等,作为工业用途,有混合在热塑性树脂中而赋予该树脂难燃性的难燃剂、含油废水用吸附剂、排烟脱硫剂、排水中和剂和土质改良剂等。
近年来,一直谋求通过作为难燃剂的氢氧化镁的微粒子化和高分散化而提高难燃效果的技术。其原因在于:越为微粒子、分散性越好,难燃效率越上升,可以少的添加量得到高的难燃性。并且,由于电子机器等的应用的小型、薄膜化等也向前发展,因此需要可对应的微粒子难燃剂。作为微粒子难燃剂的微粒子氢氧化镁,提出有平均粒径为10~1000nm的氢氧化镁微粒子(专利文献1)。但是,该氢氧化镁微粒子含有0.9重量%以上的碳量,虽然对于树脂组合物中的混合存在有利的情况,但不适合无需有机处理的混合类或需要氢氧化镁纯度的用途(玻璃等陶瓷中的添加剂、作为镁源的原料等)。
另一方面,已知有利用微反应器制造纳米粒子,微反应器被定义为反应场是边长小于1mm或500μm规模的化学反应装置,并且认为其与以更大规模进行反应的其他装置相比,能量效率、反应速度、产率、安全性、温度控制、高速且均匀地混合、浓度均匀性的提高、规模放大这些部分的细微条件的控制能力优异。细的Y字管的微反应器是有名的,已知可合成纳米粒子,但由于反应场是微小空间,因此产生如氢氧化镁粒子等那样的析晶反应的配管堵塞,存在仅可以非常稀的浓度合成的缺点,而不适合无机化合物的析晶反应。但是,例如专利文献2所示,强制薄膜式微反应器为反应场为1~30μm的非常微小的空间,通过使图3所示的装置图的下方圆盘旋转,利用离心力将所生成的纳米粒子排出至装置外,由此纳米粒子不会堵塞在装置内,而可以容易地以高浓度合成无机化合物纳米粒子。
(专利文献1)日本专利特开2009-62214号
(专利文献2)日本专利特开2009-131831号
发明内容
本发明的目的在于提供一种具有纳米粒子级的粒径、碳含量少而白度高、透明性高的氢氧化镁微粒及其制造方法。
本发明人对得到纳米粒子级的氢氧化镁微粒的方法进行了研究。结果发现:如果在强制薄膜式微反应器中使镁盐水溶液与碱性物质原料反应,则可以得到纳米粒子级的氢氧化镁微粒,并且,所得到的粒子的碳含量极少、纯度优异而白度高,从而完成本发明。
即,本发明为一种氢氧化镁微粒,其通过频率分析测定的平均二次粒径为1~100nm,且碳含量不足0.9重量%。并且,本发明为一种树脂组合物,其含有100重量份的合成树脂和1~95重量份的通过频率分析测定的平均粒径为1~100nm、且碳含量不足0.9重量%的氢氧化镁微粒。并且,本发明为一种由所述树脂组合物形成的成形品。并且,本发明为一种所述氢氧化镁粒子的制造方法,其特征在于:在具有反应场的间隙为1~30μm的强制薄膜式微反应器中,使镁盐水溶液与碱性物质原料反应。
附图说明
图1为实施例2中所得到的氢氧化镁粒子的粒度分布。
图2为实施例2中所得到的氢氧化镁粒子的TEM图像。
图3为强制薄膜式微反应器的一例。
符号说明
1 第1处理面
2 第2处理面
3 排出口
4 旋转圆盘
5 固定圆盘
A 镁盐水溶液
B 碱性物质。
具体实施方式
<氢氧化镁微粒>
本发明的氢氧化镁微粒的平均二次粒径为1~100nm,优选为10~90nm,更优选为15~90nm。粒子的平均二次粒径通过频率分析测定。
本发明的氢氧化镁微粒的碳含量为不足0.9重量%,优选为不足0.8重量%,更优选为不足0.7重量%。
本发明的氢氧化镁微粒可以用表面处理剂进行表面处理。作为表面处理剂,优选为选自由高级脂肪酸类、钛酸酯偶联剂、硅烷偶联剂、铝酸酯偶联剂、多元醇和脂肪酸的磷酸酯类及阴离子类表面活性剂所组成的群中的至少一种。
作为高级脂肪酸类,碳原子数在10以上的脂肪酸,例如,可列举出:硬脂酸、油酸、芥子酸、棕榈酸等及其碱金属盐类。
作为钛酸酯偶联剂,可列举出:三异硬脂酰基钛酸异丙酯、三(二辛基焦磷酰氧基)钛酸异丙酯、三(N-氨乙基-氨乙基)钛酸异丙酯、十三烷基苯磺酰基钛酸异丙酯等。
作为硅烷偶联剂,可列举出:乙烯基乙氧基硅烷、乙烯基-三(2-甲氧基)硅烷、γ-甲基丙烯酰氧丙基三甲氧基硅烷、γ-氨丙基三甲氧基硅烷、β-(3,4-环氧环己基)乙基三甲氧基硅烷、γ-缩水甘油氧基-丙基三甲氧基硅烷、γ-巯基丙基三甲氧基硅烷等。
作为铝酸酯偶联剂,可列举出乙酰烷氧基铝酸二异丙酯等。
作为多元醇的磷酸酯类,可列举出硬脂醇与正磷酸的单酯或二酯或其混合物。
作为阴离子类表面活性剂,可列举出:酰胺键合脂肪族羧酸盐、酰胺键合硫酸酯盐、酰胺键合磺酸盐、酰胺键合烷基烯丙基磺酸盐、硬脂醇等高级醇的硫酸酯盐、聚乙二醇醚的硫酸酯盐、酯键合硫酸酯盐、酯键合磺酸盐、酯键合烷基烯丙基磺酸盐、醚键合烷基烯丙基磺酸盐等。
为了使用表面处理剂进行本发明的氢氧化镁微粒的表面涂布处理,可通过本身公知的湿式法实施。例如作为湿式法,只要是在氢氧化镁微粒的浆料中以液态或乳状添加该表面处理剂,在高达约100℃的温度充分进行机械混合即可。作为干式法,只要是利用韩苏混合机(ヘンシェルミキサー)等混合机,在将氢氧化镁的粉末充分搅拌下以液态、乳状、固态添加表面处理剂,在加热或非加热下充分混合即可。表面处理剂的添加量可适当地选择。
<树脂组合物>
本发明的树脂组合物相对于100重量份的合成树脂,含有1~95重量份的通过频率分析测定的平均粒径为1~100nm且碳含量不足0.9重量%的氢氧化镁微粒。
氢氧化镁微粒的含量相对于100重量份的合成树脂,优选为5~90重量份,更优选为10~85重量份,进一步优选为15~85重量份。
合成树脂只要是通常用作成形品的物质即可,作为其例子,可列举出:聚乙烯、聚丙烯、乙烯/丙烯共聚物、聚丁烯、聚4-甲基-1-戊烯等的C2~C8烯烃(α-烯烃)的聚合物或共聚物、这些烯烃与二烯的共聚物类、乙烯-丙烯酸酯共聚物、聚苯乙烯、ABS树脂、AAS树脂、AS树脂、MBS树脂、乙烯/氯乙烯共聚树脂、乙烯乙酸乙烯酯共聚物树脂、乙烯-氯乙烯-乙酸乙烯酯接枝聚合树脂、偏二氯乙烯、聚氯乙烯、氯化聚乙烯、氯化聚丙烯、氯乙烯-丙烯共聚物、乙酸乙烯酯树脂、苯氧树脂、聚缩醛、聚酰胺、聚酰亚胺、聚碳酸酯、聚砜、聚苯醚、聚苯硫醚、聚对苯二甲酸乙二酯、聚对苯二甲酸丁二酯、甲基丙烯酸类树脂等的热塑性树脂。
作为这些热塑性树脂中优选的例子,有依赖于氢氧化镁粒子的难燃效果、防热劣化效果及保持机械强度特性优异的聚烯烃或其共聚物。具体而言,其为聚丙烯均聚物、乙烯丙烯共聚物之类的聚丙烯类树脂,高密度聚乙烯、低密度聚乙烯、直链低密度聚乙烯、超低密度聚乙烯、EVA(乙烯-乙酸乙烯酯树脂)、EEA(乙烯-丙烯酸乙酯树脂)、EMA(乙烯-丙烯酸甲酯共聚树脂)、EAA(乙烯-丙烯酸共聚树脂)、超高分子量聚乙烯之类的聚乙烯类树脂,以及聚丁烯、聚4-甲基-1-戊烯等的C2~C6的烯烃(α-乙烯)的聚合物或者共聚物。
进一步,可以列举出:环氧树脂、酚树脂、三聚氰胺树脂、不饱和聚酯树脂、醇酸树脂、脲树脂等的热硬化性树脂及EPDM、丁基橡胶、异戊二烯橡胶、SBR、NBR、氯磺化聚乙烯、NIR、氨基甲酸酯橡胶、丁二烯橡胶、丙烯酸类橡胶、硅酮橡胶、氟橡胶等的合成橡胶。合成树脂优选为聚烯烃或其共聚物。
本发明的树脂组合物实质上由所述合成树脂和氢氧化镁微粒形成,但是可以进一步混合难燃助剂。通过混合该难燃助剂,可以降低氢氧化镁微粒的混合比例,并且可以增大难燃效果。
作为难燃助剂,优选为红磷、碳粉末或其混合物。作为红磷,除难燃剂用的通常的红磷以外,例如可使用以热硬化性树脂、聚烯烃、羧酸聚合物、氧化钛或钛铝缩合物表面被覆的红磷。并且,作为碳粉末,可列举碳黑、活性碳或石墨,作为该碳黑,可以为通过油炉法(オイルファーネス法)、煤气炉法(ガスファーネス法)、导槽法(チャンネル法)、热法(サーマル法)或乙炔法中的任一方法制备的物质。
难燃助剂的含量相对于100重量份的合成树脂,优选为0.1~20重量份,更优选为0.5~15重量份。
本发明的树脂组合物也可以混合其他添加剂。例如可列举出:抗氧化剂、抗静电剂、染料、发泡剂、塑化剂、填充剂、补强材、有机卤素难燃剂、交联剂、光稳定剂、紫外线吸收剂、润滑剂等。
<成形品>
本发明包含由所述树脂组合物形成的成形品。作为成形品,可列举出:电线、电缆、散热片材、印刷配线基板、半导体密封剂等电子电气机器用部件、家电部件、车部件、玻璃制品、陶瓷制品等。
<氢氧化镁微粒的制造方法>
本发明的氢氧化镁微粒可在具有反应场的间隙为1~30μm的强制薄膜式微反应器中,使镁盐水溶液与碱性物质原料反应而制造。
本发明的氢氧化镁微粒的制造可使用エム·テクニック株式会社制的微反应器ULREA SS-11。该装置具备在具有反应场的间隙为1~30μm的强制薄膜式微反应器中,通过使圆盘旋转而排出析晶的氢氧化镁浆料的构造。其为在圆盘内进行析晶反应后,立即排出至装置外的连续式的反应装置。因此,即使是细微至1~30μm的反应场间隙,所生成的析晶物也不会堵塞在反应器内,可以高浓度进行反应,而可以得到纳米粒子。
本发明中所使用的强制薄膜式微反应器的一例示于图3。强制薄膜式微反应器如下所述:其具有由相互对向的第1处理面(1)和第2处理面(1)所形成的反应场,可使第1处理面(1)和第2处理面(2)相对地旋转,且相对地接近或背离,通过原料的供给压在使两个处理用面背离的方向上产生力,并且在使两个处理用面接近的方向上另外施加使所述两个处理用面移动的力,而将反应场维持在微小间隔。所谓第1处理面(1)和第2处理面(2),可使一方旋转另一方静止,并且,也可使两者沿反方向旋转。
原料的镁盐水溶液(A)通过既定的压力从反应器的中央部供给至反应场。原料的碱性物质(B)从与镁盐水溶液(A)不同的供给口供给至反应场。含有通过反应生成的微细氢氧化镁的浆料从排出口(3)排出。如果使用强制薄膜式微反应器,则可以薄膜流体的状态进行反应。
图3中,旋转圆盘(4)旋转,固定圆盘(5)不旋转。旋转圆盘(4)固定的转速优选为300~3550rpm,更优选为500~3000rpm。
第1处理面(1)与第2处理面(2)的间隙,即反应场的间隙为1~30μm,优选为3~20μm,更优选为5~15μm。
第1处理面(1)为中空圆板状,固定于圆板状的固定圆盘(4)上。并且,第2处理面(2)为中空圆板状,固定于圆板状的旋转圆盘(4)上。
镁盐水溶液(A)的反应场中的流量优选为10~250ml/秒,更优选为15~200ml/秒。碱性物质(B)的反应场中的流量优选为10~250ml/秒,更优选为15~200ml/秒。
作为原料的镁盐水溶液,使用氯化镁、硝酸镁、硫酸镁等的水溶液。并且,作为碱性物质原料,使用苛性钠、氨、氢氧化钾等的水溶液。
反应的温度优选为5~90℃,更优选为5~60℃,进一步优选为5~50℃。
镁与碱的反应的比例优选为相对于1mol镁,氢氧化物(OH)为0.2~12mol,更优选为0.4~10mol,进一步优选为0.6~8mol。
在本发明的微细氢氧化镁的制造方法中,如上所述,由于使用不含碳的原料,因此作为最终制品的氢氧化镁微粒不含碳。并且,如果需要有机处理,则可以进行用作为现有技术的脂肪酸等的有机表面处理。
实施例
以下,通过实施例和比较例详细说明本发明,但本发明并不仅限定于这些实施例。
另外,实施例中的氢氧化镁粒子的(a)粒度分布和平均二次粒径、(b)TEM观察直径、(c)碳含量、(d)X射线结构分析,和树脂组合物的实施例中的(e)涂膜厚度、(f)雾度测定,显示通过以下所记载的测定法测定的值。
(a)粒度分布和平均二次粒径:
使用日机装的粒度分布装置UPA-UT151(动态光散射法,频率分析)、日机装的Microtrac MT3300EX II(激光衍射法)进行测定。测定时的溶剂用超声波将离子交换水、氢氧化镁浆料处理5分钟后进行测定。合计进行2次测定,将各测定中得到的50%作为样品的平均二次粒径。
(b)TEM观察直径:
使用JEOL公司的JEM-2100。样品为用超声波将氢氧化镁浆料处理5分钟后,滴加至胶棉膜上而制成,并进行观测。
(c)碳含量:
使用岛津制作所的总有机碳计TOC-5000进行测定。
(d)X射线结构分析:
使用リガク社的RINT2200V进行测定。
(e)涂膜厚度
使用高分子计器株式会社的试验片测厚器SDA-25型进行测定。
(f)雾度测定
使用东京电色有限公司的AUTOMATIC HAZEMETER OPTICALUNIT TC-HIIIDP测定全光线透过率、雾度。
实施例1
使用エム·テクニック株式会社制造的强制薄膜式微反应器ULREA SS-11作为反应器。原料为以30ml/分的流量供给1.409mol/L的氯化镁水溶液,以13.3ml/分的流量供给6.045N的苛性钠,并以反应温度35℃、反应场间隙约10μm、旋转圆盘的转速1700rpm进行反应得到氢氧化镁浆料。
用离心分离机将所得到的浆料过滤分离,用离子交换水洗涤。用离子交换水将洗涤后的固体成分乳化,用超声波处理5分钟后,经用日机装的粒度分布装置UPA-UT151(动态光散射法,频率分析)进行测定,得到平均二次粒径为15.8nm的氢氧化镁微粒。经X射线分析,其为氢氧化镁。
实施例2
与实施例1同样地使用ULREA SS-11,原料为以10ml/分的流量供给0.764mol/L的氯化镁水溶液,以250ml/分的流量供给0.264N的苛性钠,以反应温度20℃、反应场间隙约10μm、旋转圆盘的转速1700rpm进行反应得到氢氧化镁浆料。
用离心分离机将所得到的浆料过滤分离,用离子交换水洗涤。用离子交换水将洗涤后的固体成分乳化,用超声波处理5分钟后,经用日机装的粒度分布装置UPA-UT151(动态光散射法,频率分析)进行测定,得到平均二次粒径为38.1nm的氢氧化镁微粒。经X射线分析,其为氢氧化镁。用透射电子显微镜(TEM)可观察50nm以下的分散粒子。
实施例3
与实施例1同样地使用ULREA SS-11,原料为以10ml/分的流量供给0.764mol/L的氯化镁水溶液,以250ml/分的流量供给0.264N的苛性钠,以反应温度77℃、反应场间隙约10μm、旋转圆盘的转速1700rpm进行反应得到氢氧化镁浆料。
用离心分离机将所得到的浆料过滤分离,用离子交换水洗涤。用离子交换水将洗涤后的固体成分乳化,用超声波处理5分钟后,经用日机装的粒度分布装置UPA-UT151(动态光散射法,频率分析)进行测定,得到平均二次粒径为60.1nm的氢氧化镁微粒。经X射线解析,其为氢氧化镁。
实施例4
与实施例1同样地使用ULREA SS-11,原料为以100ml/分的流量供给0.7045mol/L的氯化镁水溶液,以44.3ml/分的流量供给3.023N的苛性钠,以反应温度35℃、反应场间隙约10μm、旋转圆盘的转速1700rpm进行反应得到氢氧化镁浆料。
用离心分离机将所得到的浆料过滤分离,用离子交换水洗涤。用离子交换水将洗涤后的固体成分乳化,用超声波处理5分钟后,经用日机装的粒度分布装置UPA-UT151(动态光散射法,频率分析)进行测定,得到平均二次粒径为69.4nm的氢氧化镁微粒。
实施例5
使用ULREA SS-11,原料为以100ml/分的流量供给1.409mol/L的氯化镁水溶液,以44.3ml/分的流量供给6.045N的苛性钠,以反应温度35℃、反应场间隙约10μm、旋转圆盘的转速1700rpm进行反应得到氢氧化镁浆料。
用离心分离机将所得到的浆料过滤分离,用离子交换水洗涤。用离子交换水将洗涤后的固体成分乳化,用超声波处理5分钟后,经用日机装的粒度分布装置UPA-UT151(动态光散射法,频率分析)进行测定,得到平均二次粒径为89.4nm的氢氧化镁微粒。经X射线分析,其为氢氧化镁。
比较例1
通过在不锈钢制的反应容器中的批反应,经过5分钟将6.045N的苛性钠44.3ml添加于调控温度35℃搅拌下的1.409mol/L的氯化镁水溶液100ml中,得到氢氧化镁浆料。
用离心分离机进行过滤分离,用离子交换水洗涤。用离子交换水将洗涤后的固体成分乳化,经使用日机装的Microtrac MT3300EX II在激光衍射法中进行粒度测定,其平均二次粒径为1280nm。
表1
实施例6
(树脂的混合例)
树脂成分 100phr
实施例4的纳米氢氧化镁粒子 20phr
(树脂组合物的制成)
向株式会社カンペパピオ的水溶性抛光清漆(成分:合成树脂(丙烯酸类)、有机溶剂、水)5.395g(丙烯酸类树脂含量2.460g)中,混合制备成49.2g/L的实施例4的氢氧化镁粒子浆料10ml,用超声波进行1分钟分散处理得到无机有机复合浆料。在厚度为125um的PET板上浇铸无机有机复合浆料1ml,使其自然干燥一晩,得到无机有机复合涂膜。涂膜的厚度为80~160μm。
比较例2
使用平均二次粒径为0.8μm的氢氧化镁粒子浆料(49.2g/L),以与实施例6相同的条件制成树脂组合物。涂膜厚度为70~130μm。
实施例7
进行实施例6与比较例2的涂膜的雾度测定。
表2
实施例6 | 比较例2 | |
全光线透过率(%) | 84.4 | 81.2 |
雾度(雾化度(ヘーズ))(%) | 15.0 | 59.7 |
发明效果
本发明的氢氧化镁微粒的平均二次粒径(通过频率分析法测定)为1~100nm,优选为10~90nm,且不含碳,纯度高。本发明的氢氧化镁微粒由于平均二次粒径非常小,因此可期待应用于小型电子机器或薄膜等迄今为止亚微米级的粒子无法适用的领域。并且,由于粒子尺寸微细,因此透明性也高,也可考虑用于需要透明性的领域。
并且,本发明的氢氧化镁微粒由于平均二次粒径为非常小的100nm以下,且白度高(透明性高),因此难燃效果高于以往的平均二次粒径超过100nm的氢氧化镁,且可得到透明性优异的成形品。
根据本发明的制造方法,可通过使用镁盐水溶液和碱性物质原料在强制薄膜式微反应器中进行反应来制造氢氧化镁微粒。通过粉碎而得到的氢氧化镁存在因与粉碎介质接触而引起的污染,添加包含有机物等的添加剂而得到的氢氧化镁,其添加剂有可能作为杂质而起作用,但是,由于本发明的氢氧化镁微粒由使用以往的氢氧化镁原料的反应而合成,因此无污染,即使不添加添加剂,也可以得到纳米粒子。并且,在使用以往的反应容器的氢氧化镁粒子的反应中,分散性差而完全成为凝聚粒子,但是在本发明的制造方法中,可以得到为微粒子且分散性良好的氢氧化镁粒子。因此,在混合于树脂中的情形下,也显示高的透明性。
(产业上的可利用性)
本发明的氢氧化镁微粒可用作难燃剂、导热剂、耐酸剂(受酸剤)、吸附剂、增粘剂、补强剂等。
Claims (8)
1.一种氢氧化镁微粒,其通过频率分析测定的平均二次粒径为1~100nm,且碳含量不足0.9重量%。
2.根据权利要求1所述的氢氧化镁粒子,其用选自由高级脂肪酸类、钛酸酯偶联剂、硅烷偶联剂、铝酸酯偶联剂、多元醇和脂肪酸的磷酸酯类及阴离子类表面活性剂所组成的组中的至少一种的表面处理剂进行表面处理。
3.一种树脂组合物,其含有100重量份的合成树脂和1~95重量份的通过频率分析测定的平均粒径为1~100nm且碳含量不足0.9重量%的氢氧化镁微粒。
4.根据权利要求3所述的树脂组合物,其中,合成树脂为聚烯烃或其共聚物。
5.一种由根据权利要求3所述的树脂组合物形成的成形品。
6.根据权利要求5所述的成形品,其为电线或电缆。
7.根据权利要求1所述的氢氧化镁微粒的制造方法,其特征在于:在具有反应场的间隙为1~30μm的强制薄膜式微反应器中,使镁盐水溶液与碱性物质原料反应。
8.根据权利要求7所述的制造方法,其中,强制薄膜式微反应器如下所述:其具有由相互对向的第1处理面(1)和第2处理面(2)形成的反应场,可使第1处理面(1)和第2处理面(2)相对地旋转,且相对地接近或背离,通过原料的供给压在使两个处理用面背离的方向上产生力,并且在使两个处理用面接近的方向上另外施加使所述两个处理用面移动的力,而将反应场维持在微小间隔。
Applications Claiming Priority (5)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
JP2012-028480 | 2012-02-13 | ||
JP2012028480 | 2012-02-13 | ||
JP2012-066828 | 2012-03-23 | ||
JP2012066828 | 2012-03-23 | ||
PCT/JP2013/053776 WO2013122239A1 (ja) | 2012-02-13 | 2013-02-08 | 微細水酸化マグネシウム粒子 |
Publications (1)
Publication Number | Publication Date |
---|---|
CN104114492A true CN104114492A (zh) | 2014-10-22 |
Family
ID=48984347
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
CN201380006920.8A Pending CN104114492A (zh) | 2012-02-13 | 2013-02-08 | 氢氧化镁微粒 |
Country Status (8)
Country | Link |
---|---|
US (1) | US20150005429A1 (zh) |
EP (1) | EP2816011A4 (zh) |
JP (1) | JPWO2013122239A1 (zh) |
KR (1) | KR20140128997A (zh) |
CN (1) | CN104114492A (zh) |
RU (1) | RU2014137149A (zh) |
TW (1) | TW201343555A (zh) |
WO (1) | WO2013122239A1 (zh) |
Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN114573956A (zh) * | 2022-01-25 | 2022-06-03 | 浙江恒逸石化研究院有限公司 | 一种纳米氢氧化镁改性可降解共聚酯的制备方法 |
Families Citing this family (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
EP2535105A1 (en) * | 2011-06-14 | 2012-12-19 | Corning Incorporated | Systems and methods for scale-up of microreactors |
RU2561379C2 (ru) * | 2013-10-29 | 2015-08-27 | Открытое Акционерное Общество "Каустик" | Наночастицы антипирена гидроксида магния и способ их производства |
ES2751278T3 (es) * | 2014-08-26 | 2020-03-31 | Kyowa Chem Ind Co Ltd | Nueva solución sólida a base de hidróxido de magnesio y composición de resina y precursor para óxido de magnesio altamente activo que incluye los mismos |
WO2018047841A1 (ja) | 2016-09-07 | 2018-03-15 | 協和化学工業株式会社 | 微粒子複合金属水酸化物、その焼成物、その製造方法及びその樹脂組成物 |
JP7382643B2 (ja) * | 2019-08-02 | 2023-11-17 | 株式会社宮本製作所 | 水酸化マグネシウム懸濁液、その製造方法、水酸化マグネシウム飽和水溶液の製造方法およびpH上昇剤、ならびに、入浴剤、化粧品、医薬品、医薬部外品、除菌剤、防カビ剤およびそれらの製造方法 |
Citations (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JP2006232982A (ja) * | 2005-02-24 | 2006-09-07 | Fuji Xerox Co Ltd | 表面被覆難燃性粒子及びその製造方法、並びに難燃性樹脂組成物及びその製造方法 |
WO2011111487A1 (ja) * | 2010-03-09 | 2011-09-15 | 協和化学工業株式会社 | 合成樹脂用充填剤、合成樹脂組成物、その製造方法、およびその成形品 |
US20110230673A1 (en) * | 2010-03-19 | 2011-09-22 | Fujifilm Corporation | Method for producing fine metal hydroxide particles |
WO2011148463A1 (ja) * | 2010-05-25 | 2011-12-01 | エム・テクニック株式会社 | ドープ元素量を制御された析出物質の製造方法 |
JP2011245474A (ja) * | 2011-02-07 | 2011-12-08 | M Technique Co Ltd | ドープ元素量を制御された析出物質の製造方法 |
Family Cites Families (7)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JP3299921B2 (ja) * | 1997-10-17 | 2002-07-08 | 協和化学工業株式会社 | 水酸化マグネシウムを含有する耐酸性熱可塑性樹脂組成物 |
US6376077B1 (en) * | 1998-04-10 | 2002-04-23 | Kyowa Chemical Industry Co., Ltd. | Process for the production of coupling agent-treated inorganic particles and use thereof |
WO2005103138A1 (ja) * | 2004-04-20 | 2005-11-03 | Yazaki Corporation | ポリオレフィン樹脂組成物及びそれを用いた電線 |
WO2009020188A1 (ja) * | 2007-08-09 | 2009-02-12 | M.Technique Co., Ltd. | 半導体微粒子の製造方法及びその微粒子 |
JP5128882B2 (ja) * | 2007-09-05 | 2013-01-23 | 関東電化工業株式会社 | 水酸化マグネシウム微粒子及びその製造方法 |
JP4986300B2 (ja) | 2007-11-09 | 2012-07-25 | エム・テクニック株式会社 | 微粒子の製造方法 |
WO2012008596A1 (ja) * | 2010-07-13 | 2012-01-19 | 協和化学工業株式会社 | 難燃剤、それを含む樹脂組成物およびその成形品 |
-
2013
- 2013-02-08 US US14/375,585 patent/US20150005429A1/en not_active Abandoned
- 2013-02-08 CN CN201380006920.8A patent/CN104114492A/zh active Pending
- 2013-02-08 WO PCT/JP2013/053776 patent/WO2013122239A1/ja active Application Filing
- 2013-02-08 JP JP2013558764A patent/JPWO2013122239A1/ja active Pending
- 2013-02-08 KR KR1020147022100A patent/KR20140128997A/ko not_active Application Discontinuation
- 2013-02-08 EP EP13748918.3A patent/EP2816011A4/en not_active Withdrawn
- 2013-02-08 RU RU2014137149A patent/RU2014137149A/ru not_active Application Discontinuation
- 2013-02-08 TW TW102105181A patent/TW201343555A/zh unknown
Patent Citations (6)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JP2006232982A (ja) * | 2005-02-24 | 2006-09-07 | Fuji Xerox Co Ltd | 表面被覆難燃性粒子及びその製造方法、並びに難燃性樹脂組成物及びその製造方法 |
WO2011111487A1 (ja) * | 2010-03-09 | 2011-09-15 | 協和化学工業株式会社 | 合成樹脂用充填剤、合成樹脂組成物、その製造方法、およびその成形品 |
US20110230673A1 (en) * | 2010-03-19 | 2011-09-22 | Fujifilm Corporation | Method for producing fine metal hydroxide particles |
JP2011195384A (ja) * | 2010-03-19 | 2011-10-06 | Fujifilm Corp | 金属水酸化物微粒子の製造方法 |
WO2011148463A1 (ja) * | 2010-05-25 | 2011-12-01 | エム・テクニック株式会社 | ドープ元素量を制御された析出物質の製造方法 |
JP2011245474A (ja) * | 2011-02-07 | 2011-12-08 | M Technique Co Ltd | ドープ元素量を制御された析出物質の製造方法 |
Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN114573956A (zh) * | 2022-01-25 | 2022-06-03 | 浙江恒逸石化研究院有限公司 | 一种纳米氢氧化镁改性可降解共聚酯的制备方法 |
CN114573956B (zh) * | 2022-01-25 | 2023-11-24 | 浙江恒逸石化研究院有限公司 | 一种纳米氢氧化镁改性可降解共聚酯的制备方法 |
Also Published As
Publication number | Publication date |
---|---|
EP2816011A1 (en) | 2014-12-24 |
EP2816011A4 (en) | 2015-11-04 |
TW201343555A (zh) | 2013-11-01 |
US20150005429A1 (en) | 2015-01-01 |
WO2013122239A1 (ja) | 2013-08-22 |
KR20140128997A (ko) | 2014-11-06 |
RU2014137149A (ru) | 2016-04-10 |
JPWO2013122239A1 (ja) | 2015-05-18 |
Similar Documents
Publication | Publication Date | Title |
---|---|---|
CN104114492A (zh) | 氢氧化镁微粒 | |
CN104136373A (zh) | 水滑石粒子的制造方法 | |
CN100475893C (zh) | 经表面涂布的阻燃性颗粒及其生产方法以及阻燃性树脂组合物及其生产方法 | |
US20080317794A1 (en) | Agglomerate Particles, Method for Producing Nanocomposites, and the Use Thereof | |
CN108841043B (zh) | 聚氯乙烯材料用纳米化包覆改性复合阻燃剂及其制备方法 | |
JP5911153B2 (ja) | 微細ハイドロタルサイト粒子の製造方法 | |
JP5128882B2 (ja) | 水酸化マグネシウム微粒子及びその製造方法 | |
EP1414914A1 (en) | Inorganic particles and methods of making | |
CN102015534A (zh) | 用于生产可纳米分散的勃姆石的工艺及其在阻燃合成树脂中的用途 | |
ES2751278T3 (es) | Nueva solución sólida a base de hidróxido de magnesio y composición de resina y precursor para óxido de magnesio altamente activo que incluye los mismos | |
CA2873736C (en) | Method for improving the effectiveness of titanium dioxide-containing coatings | |
CN114402043A (zh) | 包含无机氧化物粒子和氰尿酸锌粒子的分散液和涂料组合物 | |
TW201010945A (en) | Process for the production of a storage-stable barium sulphate having good dispersibility | |
JP2005305367A (ja) | 粒子分散体およびその用途 | |
Gong et al. | Synthesis and applications of MANs/poly (MMA-co-BA) nanocomposite latex by miniemulsion polymerization | |
US20140329935A1 (en) | Method for improving the effectiveness of titanium dioxide-containing coatings | |
TWI617627B (zh) | 用於塑膠應用的非微米化顏料 | |
TW202239879A (zh) | 經被覆之板狀鈦酸粒子及其製造方法以及其用途 | |
CN105419399A (zh) | 一种机械力球磨法表面修饰氧化锌的处理方法 | |
EP2204350A1 (en) | Process for production of surface-coated hexaboride particle precursor, surface-coated hexaboride particle precursor, surface-coated hexaboride particles, dispersion of the particles, and structures and articles made by using the particles | |
EP2847284B1 (en) | Method for improving the effectiveness of titanium dioxide containing coatings | |
TW200806758A (en) | Coated magnesium hydroxide produced by mill-drying | |
TW200817282A (en) | Coated aluminum hydroxide particles produced by mill-drying | |
Tunusoğlu | Preparation of nanosized CeO2 particles and their incorporation into transparent acrylate polymers | |
TW200806581A (en) | Coated aluminum hydroxide particles produced by mill drying |
Legal Events
Date | Code | Title | Description |
---|---|---|---|
C06 | Publication | ||
PB01 | Publication | ||
C10 | Entry into substantive examination | ||
SE01 | Entry into force of request for substantive examination | ||
C02 | Deemed withdrawal of patent application after publication (patent law 2001) | ||
WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20141022 |