KR101682254B1 - 가변성의 기공도 및 표면 모폴로지를 갖는 실리카질 물질 및 이의 합성방법 - Google Patents
가변성의 기공도 및 표면 모폴로지를 갖는 실리카질 물질 및 이의 합성방법 Download PDFInfo
- Publication number
- KR101682254B1 KR101682254B1 KR1020117005699A KR20117005699A KR101682254B1 KR 101682254 B1 KR101682254 B1 KR 101682254B1 KR 1020117005699 A KR1020117005699 A KR 1020117005699A KR 20117005699 A KR20117005699 A KR 20117005699A KR 101682254 B1 KR101682254 B1 KR 101682254B1
- Authority
- KR
- South Korea
- Prior art keywords
- particles
- silica
- solution
- pore
- additive
- 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.)
- Active
Links
- 230000002194 synthesizing effect Effects 0.000 title claims abstract description 8
- 238000000034 method Methods 0.000 title claims description 43
- 239000000463 material Substances 0.000 title description 51
- 239000011148 porous material Substances 0.000 claims abstract description 87
- 238000006243 chemical reaction Methods 0.000 claims abstract description 44
- 229910052751 metal Inorganic materials 0.000 claims abstract description 40
- 239000002184 metal Substances 0.000 claims abstract description 40
- 239000002245 particle Substances 0.000 claims abstract description 27
- 230000015572 biosynthetic process Effects 0.000 claims abstract description 22
- 239000000654 additive Substances 0.000 claims abstract description 21
- 238000003786 synthesis reaction Methods 0.000 claims abstract description 19
- 238000003756 stirring Methods 0.000 claims abstract description 16
- 238000001556 precipitation Methods 0.000 claims abstract description 15
- 230000000996 additive effect Effects 0.000 claims abstract description 12
- 239000000203 mixture Substances 0.000 claims abstract description 11
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 claims abstract description 8
- 230000008859 change Effects 0.000 claims abstract description 7
- 238000002156 mixing Methods 0.000 claims abstract description 5
- 238000001354 calcination Methods 0.000 claims description 15
- 238000001179 sorption measurement Methods 0.000 claims description 15
- 230000008569 process Effects 0.000 claims description 14
- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical compound O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 claims description 11
- 235000012239 silicon dioxide Nutrition 0.000 claims description 11
- 239000004115 Sodium Silicate Substances 0.000 claims description 9
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 claims description 9
- 229910052911 sodium silicate Inorganic materials 0.000 claims description 9
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 8
- 150000003839 salts Chemical class 0.000 claims description 7
- 239000004094 surface-active agent Substances 0.000 claims description 7
- 238000001035 drying Methods 0.000 claims description 6
- 229910001385 heavy metal Inorganic materials 0.000 claims description 5
- KRHYYFGTRYWZRS-UHFFFAOYSA-M Fluoride anion Chemical compound [F-] KRHYYFGTRYWZRS-UHFFFAOYSA-M 0.000 claims description 3
- 230000003247 decreasing effect Effects 0.000 claims description 3
- 229910052757 nitrogen Inorganic materials 0.000 claims description 3
- 150000007530 organic bases Chemical class 0.000 claims description 3
- NWUYHJFMYQTDRP-UHFFFAOYSA-N 1,2-bis(ethenyl)benzene;1-ethenyl-2-ethylbenzene;styrene Chemical compound C=CC1=CC=CC=C1.CCC1=CC=CC=C1C=C.C=CC1=CC=CC=C1C=C NWUYHJFMYQTDRP-UHFFFAOYSA-N 0.000 claims description 2
- 238000013019 agitation Methods 0.000 claims description 2
- 150000007529 inorganic bases Chemical class 0.000 claims description 2
- 239000003456 ion exchange resin Substances 0.000 claims description 2
- 229920003303 ion-exchange polymer Polymers 0.000 claims description 2
- 239000010970 precious metal Substances 0.000 claims description 2
- 229910052761 rare earth metal Inorganic materials 0.000 claims description 2
- 150000002910 rare earth metals Chemical class 0.000 claims description 2
- 229910052723 transition metal Inorganic materials 0.000 claims description 2
- 150000003624 transition metals Chemical class 0.000 claims description 2
- 239000000243 solution Substances 0.000 claims 3
- 239000007864 aqueous solution Substances 0.000 claims 2
- 239000003929 acidic solution Substances 0.000 claims 1
- 230000001939 inductive effect Effects 0.000 claims 1
- 230000000630 rising effect Effects 0.000 claims 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 abstract description 133
- 239000000377 silicon dioxide Substances 0.000 abstract description 59
- 230000002378 acidificating effect Effects 0.000 abstract description 21
- 239000002019 doping agent Substances 0.000 abstract description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 28
- 239000008367 deionised water Substances 0.000 description 26
- 229910021641 deionized water Inorganic materials 0.000 description 26
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 25
- 235000011114 ammonium hydroxide Nutrition 0.000 description 25
- 239000000523 sample Substances 0.000 description 25
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonium chloride Substances [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 description 24
- KDLHZDBZIXYQEI-UHFFFAOYSA-N Palladium Chemical class [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 description 23
- 239000003054 catalyst Substances 0.000 description 20
- 230000005484 gravity Effects 0.000 description 14
- 239000011159 matrix material Substances 0.000 description 14
- 230000000749 insecticidal effect Effects 0.000 description 12
- 229910052763 palladium Inorganic materials 0.000 description 11
- 229910052782 aluminium Inorganic materials 0.000 description 8
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 8
- 230000008901 benefit Effects 0.000 description 8
- 230000004048 modification Effects 0.000 description 8
- 238000012986 modification Methods 0.000 description 8
- 239000000843 powder Substances 0.000 description 8
- YWYZEGXAUVWDED-UHFFFAOYSA-N triammonium citrate Chemical compound [NH4+].[NH4+].[NH4+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O YWYZEGXAUVWDED-UHFFFAOYSA-N 0.000 description 8
- YASYEJJMZJALEJ-UHFFFAOYSA-N Citric acid monohydrate Chemical compound O.OC(=O)CC(O)(C(O)=O)CC(O)=O YASYEJJMZJALEJ-UHFFFAOYSA-N 0.000 description 7
- 229960002303 citric acid monohydrate Drugs 0.000 description 7
- 230000000694 effects Effects 0.000 description 7
- 150000002739 metals Chemical class 0.000 description 7
- 238000003801 milling Methods 0.000 description 7
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical class [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 7
- 239000010936 titanium Chemical class 0.000 description 7
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 6
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical class [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 6
- 239000010949 copper Chemical class 0.000 description 6
- 239000011347 resin Substances 0.000 description 6
- 229920005989 resin Polymers 0.000 description 6
- 229910052719 titanium Inorganic materials 0.000 description 6
- 229910052725 zinc Inorganic materials 0.000 description 6
- 239000011701 zinc Chemical class 0.000 description 6
- 239000012467 final product Substances 0.000 description 5
- 239000000047 product Substances 0.000 description 5
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical class [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 4
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 4
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical class [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 4
- 229910052802 copper Inorganic materials 0.000 description 4
- 238000009826 distribution Methods 0.000 description 4
- 150000002500 ions Chemical class 0.000 description 4
- 229910044991 metal oxide Inorganic materials 0.000 description 4
- 150000004706 metal oxides Chemical class 0.000 description 4
- 230000005012 migration Effects 0.000 description 4
- 238000013508 migration Methods 0.000 description 4
- 150000007524 organic acids Chemical class 0.000 description 4
- -1 platinum ions Chemical class 0.000 description 4
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 3
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 description 3
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- FEWJPZIEWOKRBE-UHFFFAOYSA-N Tartaric acid Natural products [H+].[H+].[O-]C(=O)C(O)C(O)C([O-])=O FEWJPZIEWOKRBE-UHFFFAOYSA-N 0.000 description 3
- 238000005341 cation exchange Methods 0.000 description 3
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 description 3
- 238000010586 diagram Methods 0.000 description 3
- 238000001879 gelation Methods 0.000 description 3
- 239000002917 insecticide Substances 0.000 description 3
- 235000005985 organic acids Nutrition 0.000 description 3
- 229910052697 platinum Inorganic materials 0.000 description 3
- 229920000642 polymer Polymers 0.000 description 3
- 230000009467 reduction Effects 0.000 description 3
- 238000000851 scanning transmission electron micrograph Methods 0.000 description 3
- 238000000926 separation method Methods 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 239000002351 wastewater Substances 0.000 description 3
- 229910018072 Al 2 O 3 Inorganic materials 0.000 description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 2
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 2
- FEWJPZIEWOKRBE-XIXRPRMCSA-N Mesotartaric acid Chemical compound OC(=O)[C@@H](O)[C@@H](O)C(O)=O FEWJPZIEWOKRBE-XIXRPRMCSA-N 0.000 description 2
- 101150003085 Pdcl gene Proteins 0.000 description 2
- 229910004298 SiO 2 Inorganic materials 0.000 description 2
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- 230000002776 aggregation Effects 0.000 description 2
- 238000004220 aggregation Methods 0.000 description 2
- 230000000844 anti-bacterial effect Effects 0.000 description 2
- 150000001732 carboxylic acid derivatives Chemical class 0.000 description 2
- 239000003638 chemical reducing agent Substances 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 239000002131 composite material Substances 0.000 description 2
- 230000007423 decrease Effects 0.000 description 2
- 238000007872 degassing Methods 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 229910001873 dinitrogen Inorganic materials 0.000 description 2
- 229940048879 dl tartaric acid Drugs 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 238000003384 imaging method Methods 0.000 description 2
- 229910010272 inorganic material Inorganic materials 0.000 description 2
- 239000011147 inorganic material Substances 0.000 description 2
- 229910052742 iron Inorganic materials 0.000 description 2
- 238000013507 mapping Methods 0.000 description 2
- 230000007246 mechanism Effects 0.000 description 2
- 229920001467 poly(styrenesulfonates) Polymers 0.000 description 2
- 238000006116 polymerization reaction Methods 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 238000012545 processing Methods 0.000 description 2
- 238000010992 reflux Methods 0.000 description 2
- 229910000077 silane Inorganic materials 0.000 description 2
- 238000005245 sintering Methods 0.000 description 2
- 239000011734 sodium Substances 0.000 description 2
- 238000009827 uniform distribution Methods 0.000 description 2
- ONDPHDOFVYQSGI-UHFFFAOYSA-N zinc nitrate Chemical compound [Zn+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O ONDPHDOFVYQSGI-UHFFFAOYSA-N 0.000 description 2
- NPNPZTNLOVBDOC-UHFFFAOYSA-N 1,1-difluoroethane Chemical compound CC(F)F NPNPZTNLOVBDOC-UHFFFAOYSA-N 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical class [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 description 1
- FEWJPZIEWOKRBE-JCYAYHJZSA-N Dextrotartaric acid Chemical compound OC(=O)[C@H](O)[C@@H](O)C(O)=O FEWJPZIEWOKRBE-JCYAYHJZSA-N 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical class [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 description 1
- 239000002202 Polyethylene glycol Substances 0.000 description 1
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 description 1
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical class [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 1
- KDYFGRWQOYBRFD-UHFFFAOYSA-N Succinic acid Natural products OC(=O)CCC(O)=O KDYFGRWQOYBRFD-UHFFFAOYSA-N 0.000 description 1
- 238000003917 TEM image Methods 0.000 description 1
- 229910010413 TiO 2 Inorganic materials 0.000 description 1
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical class [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 1
- YKTSYUJCYHOUJP-UHFFFAOYSA-N [O--].[Al+3].[Al+3].[O-][Si]([O-])([O-])[O-] Chemical compound [O--].[Al+3].[Al+3].[O-][Si]([O-])([O-])[O-] YKTSYUJCYHOUJP-UHFFFAOYSA-N 0.000 description 1
- 229960000583 acetic acid Drugs 0.000 description 1
- 235000011054 acetic acid Nutrition 0.000 description 1
- 239000003377 acid catalyst Substances 0.000 description 1
- 239000003463 adsorbent Substances 0.000 description 1
- 238000003915 air pollution Methods 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- BWKOZPVPARTQIV-UHFFFAOYSA-N azanium;hydron;2-hydroxypropane-1,2,3-tricarboxylate Chemical compound [NH4+].OC(=O)CC(O)(C(O)=O)CC([O-])=O BWKOZPVPARTQIV-UHFFFAOYSA-N 0.000 description 1
- 230000001580 bacterial effect Effects 0.000 description 1
- 230000004888 barrier function Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229920001400 block copolymer Polymers 0.000 description 1
- KDYFGRWQOYBRFD-NUQCWPJISA-N butanedioic acid Chemical compound O[14C](=O)CC[14C](O)=O KDYFGRWQOYBRFD-NUQCWPJISA-N 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- BVKZGUZCCUSVTD-UHFFFAOYSA-N carbonic acid Chemical class OC(O)=O BVKZGUZCCUSVTD-UHFFFAOYSA-N 0.000 description 1
- 150000001735 carboxylic acids Chemical class 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- WITQLILIVJASEQ-UHFFFAOYSA-N cerium nickel Chemical class [Ni].[Ce] WITQLILIVJASEQ-UHFFFAOYSA-N 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- 229910052804 chromium Inorganic materials 0.000 description 1
- 239000011651 chromium Chemical class 0.000 description 1
- 229960004106 citric acid Drugs 0.000 description 1
- 235000015165 citric acid Nutrition 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 229910017052 cobalt Inorganic materials 0.000 description 1
- 239000010941 cobalt Chemical class 0.000 description 1
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical class [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 1
- 239000008119 colloidal silica Substances 0.000 description 1
- 239000000084 colloidal system Substances 0.000 description 1
- 239000000356 contaminant Substances 0.000 description 1
- 239000000498 cooling water Substances 0.000 description 1
- 238000012937 correction Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- LVYZJEPLMYTTGH-UHFFFAOYSA-H dialuminum chloride pentahydroxide dihydrate Chemical compound [Cl-].[Al+3].[OH-].[OH-].[Al+3].[OH-].[OH-].[OH-].O.O LVYZJEPLMYTTGH-UHFFFAOYSA-H 0.000 description 1
- 238000007865 diluting Methods 0.000 description 1
- 230000003467 diminishing effect Effects 0.000 description 1
- 238000010894 electron beam technology Methods 0.000 description 1
- 239000000839 emulsion Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 238000005189 flocculation Methods 0.000 description 1
- 230000016615 flocculation Effects 0.000 description 1
- XUCNUKMRBVNAPB-UHFFFAOYSA-N fluoroethene Chemical compound FC=C XUCNUKMRBVNAPB-UHFFFAOYSA-N 0.000 description 1
- 238000011010 flushing procedure Methods 0.000 description 1
- 239000006260 foam Substances 0.000 description 1
- 229910021485 fumed silica Inorganic materials 0.000 description 1
- 230000006870 function Effects 0.000 description 1
- 230000000855 fungicidal effect Effects 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 238000005470 impregnation Methods 0.000 description 1
- 238000011065 in-situ storage Methods 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000004973 liquid crystal related substance Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000007734 materials engineering Methods 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 229910021645 metal ion Inorganic materials 0.000 description 1
- 229910052914 metal silicate Inorganic materials 0.000 description 1
- 239000000693 micelle Substances 0.000 description 1
- 239000004530 micro-emulsion Substances 0.000 description 1
- 239000003607 modifier Substances 0.000 description 1
- 239000002808 molecular sieve Substances 0.000 description 1
- 229910052750 molybdenum Inorganic materials 0.000 description 1
- 239000011733 molybdenum Chemical class 0.000 description 1
- 230000008450 motivation Effects 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 239000011368 organic material Substances 0.000 description 1
- 150000002902 organometallic compounds Chemical class 0.000 description 1
- 235000006408 oxalic acid Nutrition 0.000 description 1
- 229940116315 oxalic acid Drugs 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- DCKVFVYPWDKYDN-UHFFFAOYSA-L oxygen(2-);titanium(4+);sulfate Chemical compound [O-2].[Ti+4].[O-]S([O-])(=O)=O DCKVFVYPWDKYDN-UHFFFAOYSA-L 0.000 description 1
- 150000002940 palladium Chemical class 0.000 description 1
- 238000000059 patterning Methods 0.000 description 1
- 230000000737 periodic effect Effects 0.000 description 1
- 238000004375 physisorption Methods 0.000 description 1
- 239000000049 pigment Substances 0.000 description 1
- 238000006068 polycondensation reaction Methods 0.000 description 1
- 229920001223 polyethylene glycol Polymers 0.000 description 1
- 238000005036 potential barrier Methods 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 230000010076 replication Effects 0.000 description 1
- 238000005096 rolling process Methods 0.000 description 1
- 150000004756 silanes Chemical class 0.000 description 1
- SCPYDCQAZCOKTP-UHFFFAOYSA-N silanol Chemical compound [SiH3]O SCPYDCQAZCOKTP-UHFFFAOYSA-N 0.000 description 1
- 125000005372 silanol group Chemical group 0.000 description 1
- 150000004819 silanols Chemical class 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 239000004332 silver Chemical class 0.000 description 1
- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 description 1
- 235000011121 sodium hydroxide Nutrition 0.000 description 1
- ABKQFSYGIHQQLS-UHFFFAOYSA-J sodium tetrachloropalladate Chemical compound [Na+].[Na+].Cl[Pd+2](Cl)(Cl)Cl ABKQFSYGIHQQLS-UHFFFAOYSA-J 0.000 description 1
- 239000008399 tap water Substances 0.000 description 1
- 235000020679 tap water Nutrition 0.000 description 1
- 229960001367 tartaric acid Drugs 0.000 description 1
- 235000002906 tartaric acid Nutrition 0.000 description 1
- 239000011975 tartaric acid Substances 0.000 description 1
- 125000003396 thiol group Chemical group [H]S* 0.000 description 1
- 229910052718 tin Inorganic materials 0.000 description 1
- 239000011135 tin Chemical class 0.000 description 1
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 1
- 229910000348 titanium sulfate Inorganic materials 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
- 229920000428 triblock copolymer Polymers 0.000 description 1
- 229910052720 vanadium Inorganic materials 0.000 description 1
- GPPXJZIENCGNKB-UHFFFAOYSA-N vanadium Chemical class [V]#[V] GPPXJZIENCGNKB-UHFFFAOYSA-N 0.000 description 1
- 239000011800 void material Substances 0.000 description 1
Images
Classifications
-
- 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
-
- 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
- C01B33/126—Preparation of silica of undetermined type
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/10—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J21/00—Catalysts comprising the elements, oxides, or hydroxides of magnesium, boron, aluminium, carbon, silicon, titanium, zirconium, or hafnium
- B01J21/06—Silicon, titanium, zirconium or hafnium; Oxides or hydroxides thereof
- B01J21/08—Silica
-
- 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
- C01B33/14—Colloidal silica, e.g. dispersions, gels, sols
- C01B33/141—Preparation of hydrosols or aqueous dispersions
- C01B33/142—Preparation of hydrosols or aqueous dispersions by acidic treatment of silicates
-
- 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
- C01B33/187—Preparation of finely divided silica neither in sol nor in gel form; After-treatment thereof by acidic treatment of silicates
-
- 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
- C01B33/187—Preparation of finely divided silica neither in sol nor in gel form; After-treatment thereof by acidic treatment of silicates
- C01B33/193—Preparation of finely divided silica neither in sol nor in gel form; After-treatment thereof by acidic treatment of silicates of aqueous solutions of silicates
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B37/00—Compounds having molecular sieve properties but not having base-exchange properties
- C01B37/02—Crystalline silica-polymorphs, e.g. silicalites dealuminated aluminosilicate zeolites
-
- 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
- C01P2006/14—Pore volume
-
- 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
- C01P2006/16—Pore diameter
-
- 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.]
-
- 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.]
- Y10T428/2991—Coated
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Materials Engineering (AREA)
- Engineering & Computer Science (AREA)
- Analytical Chemistry (AREA)
- Dispersion Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Geology (AREA)
- Silicon Compounds (AREA)
- Catalysts (AREA)
- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
Applications Claiming Priority (3)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| US12/209,790 | 2008-09-12 | ||
| US12/209,790 US8790608B2 (en) | 2008-09-12 | 2008-09-12 | Siliceous materials having tunable porosity and surface morphology and methods of synthesizing same |
| PCT/US2009/056659 WO2010030878A2 (en) | 2008-09-12 | 2009-09-11 | Siliceous materials having tunable porosity and surface morphology and methods of synthesizing same |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| KR20110073443A KR20110073443A (ko) | 2011-06-29 |
| KR101682254B1 true KR101682254B1 (ko) | 2016-12-02 |
Family
ID=41572620
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| KR1020117005699A Active KR101682254B1 (ko) | 2008-09-12 | 2009-09-11 | 가변성의 기공도 및 표면 모폴로지를 갖는 실리카질 물질 및 이의 합성방법 |
Country Status (8)
| Country | Link |
|---|---|
| US (1) | US8790608B2 (https=) |
| EP (1) | EP2346782A2 (https=) |
| JP (1) | JP5615281B2 (https=) |
| KR (1) | KR101682254B1 (https=) |
| CN (1) | CN102186772B (https=) |
| MY (1) | MY155398A (https=) |
| TW (1) | TWI527758B (https=) |
| WO (1) | WO2010030878A2 (https=) |
Families Citing this family (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US10227238B2 (en) * | 2006-04-04 | 2019-03-12 | Ecolab Usa Inc. | Production and use of polysilicate particulate materials |
| US8764974B2 (en) | 2010-04-16 | 2014-07-01 | Nalco Company | Processing aids to improve the bitumen recovery and froth quality in oil sands extraction processes |
| US10087081B2 (en) | 2013-03-08 | 2018-10-02 | Ecolab Usa Inc. | Process for producing high solids colloidal silica |
| US10926241B2 (en) | 2014-06-12 | 2021-02-23 | Arizona Board Of Regents On Behalf Of Arizona State University | Carbon dioxide adsorbents |
| EP3325590B1 (en) | 2015-07-18 | 2020-09-30 | Ecolab USA Inc. | Chemical additives to improve oil separation in stillage process operations |
| CN105251446B (zh) * | 2015-11-11 | 2018-02-02 | 中国电建集团中南勘测设计研究院有限公司 | 一种地下水复合重金属污染修复材料 |
| CN105329906B (zh) * | 2015-11-30 | 2017-06-23 | 中海油天津化工研究设计院有限公司 | 一种丙烯腈催化剂用硅溶胶的制备方法 |
| WO2018136695A1 (en) | 2017-01-20 | 2018-07-26 | Seo Dong Kyun | Aluminosilicate nanorods |
| CN106823850B (zh) * | 2017-03-08 | 2019-05-24 | 常州大学 | 一种桥架有机硅膜孔径的调控方法 |
| JP7034435B2 (ja) * | 2017-11-29 | 2022-03-14 | 東洋製罐グループホールディングス株式会社 | 複合体及びその製造方法。 |
| KR102252313B1 (ko) * | 2019-01-23 | 2021-05-14 | 청주대학교 산학협력단 | 중공의 다공성 실리카 나노구 및 그 제조방법 |
| US12006439B2 (en) * | 2019-03-27 | 2024-06-11 | Canon Kabushiki Kaisha | Optical member, optical device and coating liquid |
| CN120137436B (zh) * | 2025-04-22 | 2025-11-11 | 中国科学院宁波材料技术与工程研究所 | 一种硅钛复合防雾涂层及其制备方法与应用 |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6680013B1 (en) | 1999-04-15 | 2004-01-20 | Regents Of The University Of Minnesota | Synthesis of macroporous structures |
Family Cites Families (25)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US2892797A (en) * | 1956-02-17 | 1959-06-30 | Du Pont | Process for modifying the properties of a silica sol and product thereof |
| US2913419A (en) * | 1956-04-18 | 1959-11-17 | Du Pont | Chemical process and composition |
| US2974108A (en) * | 1957-01-14 | 1961-03-07 | Du Pont | Aluminosilicate aquasols and their preparation |
| US3442795A (en) * | 1963-02-27 | 1969-05-06 | Mobil Oil Corp | Method for preparing highly siliceous zeolite-type materials and materials resulting therefrom |
| US3745126A (en) * | 1971-04-22 | 1973-07-10 | Du Pont | Stable positively charged alumina coated silica sols |
| US3864142A (en) * | 1971-04-26 | 1975-02-04 | Nalco Chemical Co | Metal oxide sols |
| US4287086A (en) * | 1975-05-02 | 1981-09-01 | Nl Industries, Inc. | Viscous organic systems containing an organophilic clay gellant without an organic dispersant therefor |
| IT1127311B (it) * | 1979-12-21 | 1986-05-21 | Anic Spa | Materiale sintetico,cristallino,poroso costituito da ossidi di silicio e titanio,metodo per la sua preparazione e suoi usi |
| US4451388A (en) * | 1981-11-02 | 1984-05-29 | Nalco Chemical Company | Preparation of aluminum oxide coated silica sols using ultrafiltration |
| FR2567505B1 (fr) * | 1984-07-11 | 1986-11-21 | Rhone Poulenc Chim Base | Silice a prise d'huile elevee et a structure primaire controlee et procede pour son obtention |
| JPS61158810A (ja) * | 1984-12-28 | 1986-07-18 | Shokubai Kasei Kogyo Kk | 高純度シリカゾルの製造法 |
| US5221497A (en) * | 1988-03-16 | 1993-06-22 | Nissan Chemical Industries, Ltd. | Elongated-shaped silica sol and method for preparing the same |
| ATE207036T1 (de) * | 1992-12-16 | 2001-11-15 | Chevron Usa Inc | Herstellung von aluminosilikatzeolithen |
| JP3517913B2 (ja) * | 1993-10-15 | 2004-04-12 | 日産化学工業株式会社 | 細長い形状のシリカゾルの製造法 |
| JP2908253B2 (ja) * | 1994-09-26 | 1999-06-21 | 日本化学工業株式会社 | 水和珪酸とその製造方法 |
| DE19648798C2 (de) * | 1996-11-26 | 1998-11-19 | Hoechst Ag | Verfahren zur Herstellung von organisch modifizierten Aerogelen durch Oberflächenmodifikation des wäßrigen Gels (ohne vorherigen Lösungsmitteltausch) und anschließender Trocknung |
| US6358882B1 (en) * | 1998-12-08 | 2002-03-19 | The Standard Oil Company | Fluid bed vinyl acetate catalyst |
| US5968473A (en) * | 1998-12-18 | 1999-10-19 | Uop Llc | Stannosilicate molecular sieves |
| US6191323B1 (en) * | 2000-04-25 | 2001-02-20 | Uop Llc | Process for the reduction of ketones and aldehydes to alcohols using a tin substituted zeolite beta |
| JP2002173314A (ja) * | 2000-11-30 | 2002-06-21 | Watanabe Shoko:Kk | 高純度コロイダルシリカ及び高純度合成石英粉の製造方法 |
| JP4976613B2 (ja) * | 2000-12-08 | 2012-07-18 | 水澤化学工業株式会社 | シリカゾルの製造方法 |
| JP2003253154A (ja) * | 2001-12-25 | 2003-09-10 | Asahi Kasei Corp | 無機多孔性微粒子 |
| US6916514B2 (en) * | 2003-07-18 | 2005-07-12 | Eastman Kodak Company | Cationic shelled particle |
| JP4041892B2 (ja) * | 2003-10-03 | 2008-02-06 | 独立行政法人物質・材料研究機構 | 多孔質ガラス微小粒子およびその製造方法 |
| US20070034116A1 (en) * | 2005-08-10 | 2007-02-15 | Mac Donald Dennis L | Silica sols with controlled minimum particle size and preparation thereof |
-
2008
- 2008-09-12 US US12/209,790 patent/US8790608B2/en active Active
-
2009
- 2009-07-09 TW TW098123187A patent/TWI527758B/zh active
- 2009-09-11 WO PCT/US2009/056659 patent/WO2010030878A2/en not_active Ceased
- 2009-09-11 EP EP09792465A patent/EP2346782A2/en active Pending
- 2009-09-11 JP JP2011526992A patent/JP5615281B2/ja active Active
- 2009-09-11 MY MYPI2011001091A patent/MY155398A/en unknown
- 2009-09-11 CN CN200980142127.4A patent/CN102186772B/zh active Active
- 2009-09-11 KR KR1020117005699A patent/KR101682254B1/ko active Active
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6680013B1 (en) | 1999-04-15 | 2004-01-20 | Regents Of The University Of Minnesota | Synthesis of macroporous structures |
Also Published As
| Publication number | Publication date |
|---|---|
| US20100068519A1 (en) | 2010-03-18 |
| TWI527758B (zh) | 2016-04-01 |
| WO2010030878A2 (en) | 2010-03-18 |
| US8790608B2 (en) | 2014-07-29 |
| JP2012501958A (ja) | 2012-01-26 |
| EP2346782A2 (en) | 2011-07-27 |
| CN102186772A (zh) | 2011-09-14 |
| JP5615281B2 (ja) | 2014-10-29 |
| CN102186772B (zh) | 2015-07-22 |
| TW201010942A (en) | 2010-03-16 |
| KR20110073443A (ko) | 2011-06-29 |
| MY155398A (en) | 2015-10-15 |
| WO2010030878A3 (en) | 2010-05-06 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| KR101682254B1 (ko) | 가변성의 기공도 및 표면 모폴로지를 갖는 실리카질 물질 및 이의 합성방법 | |
| Sierra et al. | Synthesis of mesoporous silica with tunable pore size from sodium silicate solutions and a polyethylene oxide surfactant | |
| Huang et al. | Lanthanum-doped ordered mesoporous hollow silica spheres as novel adsorbents for efficient phosphate removal | |
| Cui et al. | Nonionic triblock copolymer synthesis of SBA-15 above the isoelectric point of silica (pH= 2–5) | |
| JP5389660B2 (ja) | 高金属性ケイ質組成物及び同一物を生成する方法 | |
| Misran et al. | Nonsurfactant route of fatty alcohols decomposition for templating of mesoporous silica | |
| Meléndez-Ortiz et al. | Synthesis of spherical SBA-15 mesoporous silica. Influence of reaction conditions on the structural order and stability | |
| Qiao et al. | Control of ordered structure and morphology of large-pore periodic mesoporous organosilicas by inorganic salt | |
| US20110257006A1 (en) | Method for preparing a structured porous material comprising nanoparticles of metal 0 imbedded in the walls thereof | |
| WO2012110995A1 (en) | Silica core-shell microparticles | |
| US9764315B2 (en) | Method for preparation of a group 4 metal silicate and use thereof | |
| Mazinani et al. | Synthesis and photocatalytic performance of hollow sphere particles of SiO2-TiO2 composite of mesocellular foam walls | |
| Hanrahan et al. | Synthesis and swelling of large pore diameter mesoporous silica spheres | |
| Lee et al. | Preparation of NaCl-incorporated plugged mesoporous silica using a cost-effective precursor and applications to the hydrodechlorination of chlorinated hydrocarbons | |
| WO2006060623A2 (en) | Mesoporous inorganic oxide spheres and method of making same | |
| Newalkar et al. | Synthesis and characterization of PSU-1, a novel cage-like mesoporous silica | |
| Aranda et al. | Total oxidation of naphthalene using mesoporous CeO2 catalysts synthesized by nanocasting from two dimensional SBA-15 and three dimensional KIT-6 and MCM-48 silica templates | |
| Isobe et al. | Micropore to macropore structure-designed silicas with regulated condensation of silicic acid nanoparticles | |
| Nowak | Textural and structural properties of niobium-containing micro-, meso-and macroporous molecular sieves | |
| Niu et al. | Chelating template-induced encapsulation of NiO cluster in mesoporous silica via anionic surfactant-templated route | |
| JP5167482B2 (ja) | 複合多孔体及びその製造方法 | |
| Lin et al. | New insights into the mesophase transformation of ethane-bridged PMOs by the influence of different counterions under basic conditions | |
| Martynyuk et al. | Nanostructures constituted by unusually small silica nanoparticles modified with metal oxides as support for ultra-small gold nanoparticles | |
| Carta et al. | Iron–cobalt nanocrystalline alloy supported on a cubic mesostructured silica matrix: FeCo/SBA-16 porous nanocomposites | |
| Rose | Photocatalytically Active Aerogels–Development and Characterization of (Semi-) Crystalline Titania |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PA0105 | International application |
Patent event date: 20110311 Patent event code: PA01051R01D Comment text: International Patent Application |
|
| PG1501 | Laying open of application | ||
| A201 | Request for examination | ||
| PA0201 | Request for examination |
Patent event code: PA02012R01D Patent event date: 20140801 Comment text: Request for Examination of Application |
|
| E902 | Notification of reason for refusal | ||
| PE0902 | Notice of grounds for rejection |
Comment text: Notification of reason for refusal Patent event date: 20151012 Patent event code: PE09021S01D |
|
| E90F | Notification of reason for final refusal | ||
| PE0902 | Notice of grounds for rejection |
Comment text: Final Notice of Reason for Refusal Patent event date: 20160414 Patent event code: PE09021S02D |
|
| E701 | Decision to grant or registration of patent right | ||
| PE0701 | Decision of registration |
Patent event code: PE07011S01D Comment text: Decision to Grant Registration Patent event date: 20160901 |
|
| GRNT | Written decision to grant | ||
| PR0701 | Registration of establishment |
Comment text: Registration of Establishment Patent event date: 20161128 Patent event code: PR07011E01D |
|
| PR1002 | Payment of registration fee |
Payment date: 20161128 End annual number: 3 Start annual number: 1 |
|
| PG1601 | Publication of registration | ||
| PR1001 | Payment of annual fee |
Payment date: 20201028 Start annual number: 5 End annual number: 5 |
|
| PR1001 | Payment of annual fee |
Payment date: 20211027 Start annual number: 6 End annual number: 6 |
|
| PR1001 | Payment of annual fee |
Payment date: 20221017 Start annual number: 7 End annual number: 7 |
|
| PR1001 | Payment of annual fee |
Payment date: 20231017 Start annual number: 8 End annual number: 8 |
|
| PR1001 | Payment of annual fee |
Payment date: 20241016 Start annual number: 9 End annual number: 9 |