WO2000069647A9 - Ink receptor media suitable for inkjet printing - Google Patents
Ink receptor media suitable for inkjet printingInfo
- Publication number
- WO2000069647A9 WO2000069647A9 PCT/US1999/022505 US9922505W WO0069647A9 WO 2000069647 A9 WO2000069647 A9 WO 2000069647A9 US 9922505 W US9922505 W US 9922505W WO 0069647 A9 WO0069647 A9 WO 0069647A9
- Authority
- WO
- WIPO (PCT)
- Prior art keywords
- particles
- ink receptor
- ink
- silica
- ofthe
- Prior art date
Links
- 238000007641 inkjet printing Methods 0.000 title description 4
- 239000002245 particle Substances 0.000 claims abstract description 234
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 202
- 239000011230 binding agent Substances 0.000 claims abstract description 66
- 239000004094 surface-active agent Substances 0.000 claims abstract description 56
- 239000000758 substrate Substances 0.000 claims abstract description 51
- 239000011148 porous material Substances 0.000 claims abstract description 42
- 238000000034 method Methods 0.000 claims abstract description 41
- 238000001246 colloidal dispersion Methods 0.000 claims abstract description 14
- 239000006185 dispersion Substances 0.000 claims abstract description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 130
- 239000000203 mixture Substances 0.000 claims description 93
- 229910001868 water Inorganic materials 0.000 claims description 80
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 45
- 239000000377 silicon dioxide Substances 0.000 claims description 37
- 239000003795 chemical substances by application Substances 0.000 claims description 34
- 239000000178 monomer Substances 0.000 claims description 21
- 239000004816 latex Substances 0.000 claims description 19
- 229920000126 latex Polymers 0.000 claims description 19
- 125000002091 cationic group Chemical group 0.000 claims description 18
- 239000002904 solvent Substances 0.000 claims description 16
- 239000006184 cosolvent Substances 0.000 claims description 9
- 238000004519 manufacturing process Methods 0.000 claims description 9
- 150000001412 amines Chemical class 0.000 claims description 8
- 150000007524 organic acids Chemical class 0.000 claims description 8
- 229910044991 metal oxide Inorganic materials 0.000 claims description 7
- 238000007639 printing Methods 0.000 claims description 6
- 239000003377 acid catalyst Substances 0.000 claims description 5
- 239000006087 Silane Coupling Agent Substances 0.000 claims description 4
- 230000032683 aging Effects 0.000 claims description 4
- 150000004706 metal oxides Chemical class 0.000 claims description 4
- NIXOWILDQLNWCW-UHFFFAOYSA-M Acrylate Chemical compound [O-]C(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-M 0.000 claims 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 claims description 3
- 125000000129 anionic group Chemical group 0.000 claims description 3
- 235000015165 citric acid Nutrition 0.000 claims description 3
- 230000009477 glass transition Effects 0.000 claims description 3
- 235000014655 lactic acid Nutrition 0.000 claims description 3
- 235000006408 oxalic acid Nutrition 0.000 claims description 3
- 235000002906 tartaric acid Nutrition 0.000 claims description 3
- JOYRKODLDBILNP-UHFFFAOYSA-N Ethyl urethane Chemical compound CCOC(N)=O JOYRKODLDBILNP-UHFFFAOYSA-N 0.000 claims description 2
- 150000001450 anions Chemical class 0.000 claims description 2
- 125000001453 quaternary ammonium group Chemical group 0.000 claims description 2
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 claims description 2
- 229920002554 vinyl polymer Polymers 0.000 claims description 2
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 claims 3
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims 3
- OFOBLEOULBTSOW-UHFFFAOYSA-N Malonic acid Chemical compound OC(=O)CC(O)=O OFOBLEOULBTSOW-UHFFFAOYSA-N 0.000 claims 2
- JVTAAEKCZFNVCJ-UHFFFAOYSA-N lactic acid Chemical compound CC(O)C(O)=O JVTAAEKCZFNVCJ-UHFFFAOYSA-N 0.000 claims 2
- FEWJPZIEWOKRBE-JCYAYHJZSA-N Dextrotartaric acid Chemical compound OC(=O)[C@H](O)[C@@H](O)C(O)=O FEWJPZIEWOKRBE-JCYAYHJZSA-N 0.000 claims 1
- 239000004310 lactic acid Substances 0.000 claims 1
- 239000011975 tartaric acid Substances 0.000 claims 1
- 239000000463 material Substances 0.000 abstract description 45
- 238000009826 distribution Methods 0.000 abstract description 9
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 123
- 239000000976 ink Substances 0.000 description 97
- 239000000243 solution Substances 0.000 description 90
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 58
- LFQCEHFDDXELDD-UHFFFAOYSA-N tetramethyl orthosilicate Chemical compound CO[Si](OC)(OC)OC LFQCEHFDDXELDD-UHFFFAOYSA-N 0.000 description 57
- 239000008367 deionised water Substances 0.000 description 49
- 229910021641 deionized water Inorganic materials 0.000 description 49
- -1 for example Chemical compound 0.000 description 37
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 34
- 238000002360 preparation method Methods 0.000 description 27
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical group [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 26
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 24
- 239000000908 ammonium hydroxide Substances 0.000 description 23
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 description 18
- 239000000499 gel Substances 0.000 description 18
- 239000000725 suspension Substances 0.000 description 18
- 239000000843 powder Substances 0.000 description 17
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 16
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 16
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 description 16
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 15
- 238000002441 X-ray diffraction Methods 0.000 description 15
- 229960000583 acetic acid Drugs 0.000 description 15
- 230000015572 biosynthetic process Effects 0.000 description 15
- 238000003786 synthesis reaction Methods 0.000 description 14
- 239000000839 emulsion Substances 0.000 description 13
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- 239000003054 catalyst Substances 0.000 description 12
- 239000003086 colorant Substances 0.000 description 12
- 239000002253 acid Substances 0.000 description 11
- 238000003756 stirring Methods 0.000 description 11
- 238000006243 chemical reaction Methods 0.000 description 10
- 238000000576 coating method Methods 0.000 description 10
- 239000002002 slurry Substances 0.000 description 10
- WGTYBPLFGIVFAS-UHFFFAOYSA-M tetramethylammonium hydroxide Chemical compound [OH-].C[N+](C)(C)C WGTYBPLFGIVFAS-UHFFFAOYSA-M 0.000 description 10
- DIZPMCHEQGEION-UHFFFAOYSA-H aluminium sulfate (anhydrous) Chemical compound [Al+3].[Al+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O DIZPMCHEQGEION-UHFFFAOYSA-H 0.000 description 9
- 238000001035 drying Methods 0.000 description 9
- IJGRMHOSHXDMSA-UHFFFAOYSA-N nitrogen Substances N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 9
- 239000011164 primary particle Substances 0.000 description 9
- 150000003839 salts Chemical class 0.000 description 9
- 229920003171 Poly (ethylene oxide) Polymers 0.000 description 8
- 239000002585 base Substances 0.000 description 8
- 239000003153 chemical reaction reagent Substances 0.000 description 8
- 239000011521 glass Substances 0.000 description 8
- 229920001983 poloxamer Polymers 0.000 description 8
- 229920000139 polyethylene terephthalate Polymers 0.000 description 8
- 239000005020 polyethylene terephthalate Substances 0.000 description 8
- 239000011248 coating agent Substances 0.000 description 7
- 239000012065 filter cake Substances 0.000 description 7
- 229910052751 metal Inorganic materials 0.000 description 7
- 239000002184 metal Substances 0.000 description 7
- 229920000728 polyester Polymers 0.000 description 7
- 229920000642 polymer Polymers 0.000 description 7
- 229920001451 polypropylene glycol Polymers 0.000 description 7
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 6
- LXEKPEMOWBOYRF-UHFFFAOYSA-N [2-[(1-azaniumyl-1-imino-2-methylpropan-2-yl)diazenyl]-2-methylpropanimidoyl]azanium;dichloride Chemical compound Cl.Cl.NC(=N)C(C)(C)N=NC(C)(C)C(N)=N LXEKPEMOWBOYRF-UHFFFAOYSA-N 0.000 description 6
- 150000007513 acids Chemical class 0.000 description 6
- 125000005210 alkyl ammonium group Chemical group 0.000 description 6
- 239000002105 nanoparticle Substances 0.000 description 6
- 229910052757 nitrogen Inorganic materials 0.000 description 6
- 239000000049 pigment Substances 0.000 description 6
- 229920000098 polyolefin Polymers 0.000 description 6
- 239000011347 resin Substances 0.000 description 6
- 229920005989 resin Polymers 0.000 description 6
- 239000010457 zeolite Substances 0.000 description 6
- RVGRUAULSDPKGF-UHFFFAOYSA-N Poloxamer Chemical compound C1CO1.CC1CO1 RVGRUAULSDPKGF-UHFFFAOYSA-N 0.000 description 5
- 239000004698 Polyethylene Substances 0.000 description 5
- 239000004743 Polypropylene Substances 0.000 description 5
- 230000002378 acidificating effect Effects 0.000 description 5
- 238000003384 imaging method Methods 0.000 description 5
- 229920000573 polyethylene Polymers 0.000 description 5
- 229920001155 polypropylene Polymers 0.000 description 5
- 238000001878 scanning electron micrograph Methods 0.000 description 5
- 238000001228 spectrum Methods 0.000 description 5
- 239000000126 substance Substances 0.000 description 5
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 4
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 4
- 239000000853 adhesive Substances 0.000 description 4
- 230000001070 adhesive effect Effects 0.000 description 4
- 238000001354 calcination Methods 0.000 description 4
- 150000001735 carboxylic acids Chemical class 0.000 description 4
- 239000008119 colloidal silica Substances 0.000 description 4
- 239000000975 dye Substances 0.000 description 4
- 239000007788 liquid Substances 0.000 description 4
- 239000002808 molecular sieve Substances 0.000 description 4
- 239000004570 mortar (masonry) Substances 0.000 description 4
- 230000000737 periodic effect Effects 0.000 description 4
- 229920006267 polyester film Polymers 0.000 description 4
- 229920002451 polyvinyl alcohol Polymers 0.000 description 4
- 239000002244 precipitate Substances 0.000 description 4
- 239000000047 product Substances 0.000 description 4
- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 description 4
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 3
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 3
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 description 3
- JIGUQPWFLRLWPJ-UHFFFAOYSA-N Ethyl acrylate Chemical compound CCOC(=O)C=C JIGUQPWFLRLWPJ-UHFFFAOYSA-N 0.000 description 3
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 3
- VVQNEPGJFQJSBK-UHFFFAOYSA-N Methyl methacrylate Chemical compound COC(=O)C(C)=C VVQNEPGJFQJSBK-UHFFFAOYSA-N 0.000 description 3
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 description 3
- 229920002415 Pluronic P-123 Polymers 0.000 description 3
- 229920002021 Pluronic® F 77 Polymers 0.000 description 3
- 125000000217 alkyl group Chemical group 0.000 description 3
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 3
- 239000003945 anionic surfactant Substances 0.000 description 3
- 238000006555 catalytic reaction Methods 0.000 description 3
- UHZZMRAGKVHANO-UHFFFAOYSA-M chlormequat chloride Chemical compound [Cl-].C[N+](C)(C)CCCl UHZZMRAGKVHANO-UHFFFAOYSA-M 0.000 description 3
- 150000001875 compounds Chemical class 0.000 description 3
- 239000010949 copper Substances 0.000 description 3
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 description 3
- 238000001914 filtration Methods 0.000 description 3
- 238000001879 gelation Methods 0.000 description 3
- 239000012362 glacial acetic acid Substances 0.000 description 3
- 239000003999 initiator Substances 0.000 description 3
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- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 description 3
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- 229920005596 polymer binder Polymers 0.000 description 3
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- 238000010008 shearing Methods 0.000 description 3
- 238000003860 storage Methods 0.000 description 3
- 239000003232 water-soluble binding agent Substances 0.000 description 3
- GMLNSZJUADQSRL-UHFFFAOYSA-H 3-[2-[(1,5-dioxo-6-sulfo-2,4,3-benzodioxalumepin-3-yl)oxycarbonyl]-3-sulfobenzoyl]oxy-1,5-dioxo-2,4,3-benzodioxalumepine-6-sulfonic acid Chemical compound [Al+3].[Al+3].OS(=O)(=O)c1cccc(C([O-])=O)c1C([O-])=O.OS(=O)(=O)c1cccc(C([O-])=O)c1C([O-])=O.OS(=O)(=O)c1cccc(C([O-])=O)c1C([O-])=O GMLNSZJUADQSRL-UHFFFAOYSA-H 0.000 description 2
- QZPSOSOOLFHYRR-UHFFFAOYSA-N 3-hydroxypropyl prop-2-enoate Chemical compound OCCCOC(=O)C=C QZPSOSOOLFHYRR-UHFFFAOYSA-N 0.000 description 2
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 2
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- 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
- BAPJBEWLBFYGME-UHFFFAOYSA-N Methyl acrylate Chemical compound COC(=O)C=C BAPJBEWLBFYGME-UHFFFAOYSA-N 0.000 description 2
- 229910019142 PO4 Inorganic materials 0.000 description 2
- 229920000463 Poly(ethylene glycol)-block-poly(propylene glycol)-block-poly(ethylene glycol) Polymers 0.000 description 2
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- 239000004372 Polyvinyl alcohol Substances 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 description 2
- 238000003917 TEM image Methods 0.000 description 2
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 description 2
- 229910021536 Zeolite Inorganic materials 0.000 description 2
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- BCZMKSMVRLGRFS-UHFFFAOYSA-N [amino(3-trimethoxysilylpropylsulfanyl)methylidene]azanium;chloride Chemical compound Cl.CO[Si](OC)(OC)CCCSC(N)=N BCZMKSMVRLGRFS-UHFFFAOYSA-N 0.000 description 2
- 238000005299 abrasion Methods 0.000 description 2
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- 230000002776 aggregation Effects 0.000 description 2
- 150000008051 alkyl sulfates Chemical class 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
- AMVQGJHFDJVOOB-UHFFFAOYSA-H aluminium sulfate octadecahydrate Chemical compound O.O.O.O.O.O.O.O.O.O.O.O.O.O.O.O.O.O.[Al+3].[Al+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O AMVQGJHFDJVOOB-UHFFFAOYSA-H 0.000 description 2
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- CZDYPVPMEAXLPK-UHFFFAOYSA-N tetramethylsilane Chemical compound C[Si](C)(C)C CZDYPVPMEAXLPK-UHFFFAOYSA-N 0.000 description 2
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- DPBJAVGHACCNRL-UHFFFAOYSA-N 2-(dimethylamino)ethyl prop-2-enoate Chemical class CN(C)CCOC(=O)C=C DPBJAVGHACCNRL-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
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- KFUKRKHCFJBODR-UHFFFAOYSA-J 3-sulfophthalate;zirconium(4+) Chemical compound [Zr+4].OS(=O)(=O)C1=CC=CC(C([O-])=O)=C1C([O-])=O.OS(=O)(=O)C1=CC=CC(C([O-])=O)=C1C([O-])=O KFUKRKHCFJBODR-UHFFFAOYSA-J 0.000 description 1
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- QTBSBXVTEAMEQO-UHFFFAOYSA-M Acetate Chemical compound CC([O-])=O QTBSBXVTEAMEQO-UHFFFAOYSA-M 0.000 description 1
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- UXVMQQNJUSDDNG-UHFFFAOYSA-L Calcium chloride Chemical compound [Cl-].[Cl-].[Ca+2] UXVMQQNJUSDDNG-UHFFFAOYSA-L 0.000 description 1
- CXRFDZFCGOPDTD-UHFFFAOYSA-M Cetrimide Chemical compound [Br-].CCCCCCCCCCCCCC[N+](C)(C)C CXRFDZFCGOPDTD-UHFFFAOYSA-M 0.000 description 1
- LZZYPRNAOMGNLH-UHFFFAOYSA-M Cetrimonium bromide Chemical compound [Br-].CCCCCCCCCCCCCCCC[N+](C)(C)C LZZYPRNAOMGNLH-UHFFFAOYSA-M 0.000 description 1
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- 238000005004 MAS NMR spectroscopy Methods 0.000 description 1
- CERQOIWHTDAKMF-UHFFFAOYSA-N Methacrylic acid Chemical compound CC(=C)C(O)=O CERQOIWHTDAKMF-UHFFFAOYSA-N 0.000 description 1
- WRUZLCLJULHLEY-UHFFFAOYSA-N N-(p-hydroxyphenyl)glycine Chemical group OC(=O)CNC1=CC=C(O)C=C1 WRUZLCLJULHLEY-UHFFFAOYSA-N 0.000 description 1
- 238000005481 NMR spectroscopy Methods 0.000 description 1
- 229910002651 NO3 Inorganic materials 0.000 description 1
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 description 1
- REYJJPSVUYRZGE-UHFFFAOYSA-N Octadecylamine Chemical class CCCCCCCCCCCCCCCCCCN REYJJPSVUYRZGE-UHFFFAOYSA-N 0.000 description 1
- 229920002057 Pluronic® P 103 Polymers 0.000 description 1
- 229920002059 Pluronic® P 104 Polymers 0.000 description 1
- 239000004793 Polystyrene Substances 0.000 description 1
- 239000004820 Pressure-sensitive adhesive Substances 0.000 description 1
- DBMJMQXJHONAFJ-UHFFFAOYSA-M Sodium laurylsulphate Chemical compound [Na+].CCCCCCCCCCCCOS([O-])(=O)=O DBMJMQXJHONAFJ-UHFFFAOYSA-M 0.000 description 1
- BZHJMEDXRYGGRV-UHFFFAOYSA-N Vinyl chloride Chemical compound ClC=C BZHJMEDXRYGGRV-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 150000001242 acetic acid derivatives Chemical class 0.000 description 1
- ZOIORXHNWRGPMV-UHFFFAOYSA-N acetic acid;zinc Chemical compound [Zn].CC(O)=O.CC(O)=O ZOIORXHNWRGPMV-UHFFFAOYSA-N 0.000 description 1
- 239000003929 acidic solution Substances 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000004931 aggregating effect Effects 0.000 description 1
- 238000004220 aggregation Methods 0.000 description 1
- 150000001298 alcohols Chemical class 0.000 description 1
- 150000001335 aliphatic alkanes Chemical class 0.000 description 1
- 229910052783 alkali metal Inorganic materials 0.000 description 1
- 150000008044 alkali metal hydroxides Chemical class 0.000 description 1
- 150000001340 alkali metals Chemical class 0.000 description 1
- 150000001336 alkenes Chemical class 0.000 description 1
- 150000003973 alkyl amines Chemical class 0.000 description 1
- 150000004996 alkyl benzenes Chemical class 0.000 description 1
- 125000005599 alkyl carboxylate group Chemical group 0.000 description 1
- 229940045714 alkyl sulfonate alkylating agent Drugs 0.000 description 1
- 150000008052 alkyl sulfonates Chemical class 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- 229910000323 aluminium silicate Inorganic materials 0.000 description 1
- 150000001408 amides Chemical class 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- CQEYYJKEWSMYFG-UHFFFAOYSA-N butyl acrylate Chemical compound CCCCOC(=O)C=C CQEYYJKEWSMYFG-UHFFFAOYSA-N 0.000 description 1
- 229910052791 calcium Inorganic materials 0.000 description 1
- 239000011575 calcium Substances 0.000 description 1
- 229910001622 calcium bromide Inorganic materials 0.000 description 1
- 239000001110 calcium chloride Substances 0.000 description 1
- 229910001628 calcium chloride Inorganic materials 0.000 description 1
- WGEFECGEFUFIQW-UHFFFAOYSA-L calcium dibromide Chemical compound [Ca+2].[Br-].[Br-] WGEFECGEFUFIQW-UHFFFAOYSA-L 0.000 description 1
- WOWHHFRSBJGXCM-UHFFFAOYSA-M cetyltrimethylammonium chloride Chemical compound [Cl-].CCCCCCCCCCCCCCCC[N+](C)(C)C WOWHHFRSBJGXCM-UHFFFAOYSA-M 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- GRWVQDDAKZFPFI-UHFFFAOYSA-H chromium(III) sulfate Chemical compound [Cr+3].[Cr+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O GRWVQDDAKZFPFI-UHFFFAOYSA-H 0.000 description 1
- 230000000536 complexating effect Effects 0.000 description 1
- 229920001577 copolymer Polymers 0.000 description 1
- SWIBIOWHZRXHEJ-UHFFFAOYSA-L copper;3-sulfophthalate Chemical compound [Cu+2].OS(=O)(=O)C1=CC=CC(C([O-])=O)=C1C([O-])=O SWIBIOWHZRXHEJ-UHFFFAOYSA-L 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- JSWZPVLQSMOJEW-UHFFFAOYSA-H dialuminum 2-sulfobenzene-1,3-dicarboxylate Chemical compound [Al+3].[Al+3].OS(=O)(=O)c1c(cccc1C([O-])=O)C([O-])=O.OS(=O)(=O)c1c(cccc1C([O-])=O)C([O-])=O.OS(=O)(=O)c1c(cccc1C([O-])=O)C([O-])=O JSWZPVLQSMOJEW-UHFFFAOYSA-H 0.000 description 1
- 229910001873 dinitrogen Inorganic materials 0.000 description 1
- 150000002009 diols Chemical class 0.000 description 1
- 238000007598 dipping method Methods 0.000 description 1
- 239000002270 dispersing agent Substances 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 239000012153 distilled water Substances 0.000 description 1
- TVACALAUIQMRDF-UHFFFAOYSA-N dodecyl dihydrogen phosphate Chemical class CCCCCCCCCCCCOP(O)(O)=O TVACALAUIQMRDF-UHFFFAOYSA-N 0.000 description 1
- 230000009977 dual effect Effects 0.000 description 1
- 150000002148 esters Chemical class 0.000 description 1
- 238000002481 ethanol extraction Methods 0.000 description 1
- MEGHWIAOTJPCHQ-UHFFFAOYSA-N ethenyl butanoate Chemical compound CCCC(=O)OC=C MEGHWIAOTJPCHQ-UHFFFAOYSA-N 0.000 description 1
- 150000002170 ethers Chemical class 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 239000011790 ferrous sulphate Substances 0.000 description 1
- 235000003891 ferrous sulphate Nutrition 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 238000007647 flexography Methods 0.000 description 1
- 230000009969 flowable effect Effects 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
- 239000006260 foam Substances 0.000 description 1
- 238000009472 formulation Methods 0.000 description 1
- 229910021485 fumed silica Inorganic materials 0.000 description 1
- 229910052733 gallium Inorganic materials 0.000 description 1
- 229940044658 gallium nitrate Drugs 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 239000008240 homogeneous mixture Substances 0.000 description 1
- QAOWNCQODCNURD-UHFFFAOYSA-M hydrogensulfate Chemical compound OS([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-M 0.000 description 1
- 150000004679 hydroxides Chemical class 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 229910010272 inorganic material Inorganic materials 0.000 description 1
- 239000011147 inorganic material Substances 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 238000011835 investigation Methods 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 1
- BAUYGSIQEAFULO-UHFFFAOYSA-L iron(2+) sulfate (anhydrous) Chemical compound [Fe+2].[O-]S([O-])(=O)=O BAUYGSIQEAFULO-UHFFFAOYSA-L 0.000 description 1
- 229910000359 iron(II) sulfate Inorganic materials 0.000 description 1
- 230000001788 irregular Effects 0.000 description 1
- 150000002576 ketones Chemical class 0.000 description 1
- 239000011777 magnesium Substances 0.000 description 1
- 229910052749 magnesium Inorganic materials 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
- ARQYXIKMMOPJRM-UHFFFAOYSA-L magnesium;3-sulfophthalate Chemical compound [Mg+2].OS(=O)(=O)C1=CC=CC(C([O-])=O)=C1C([O-])=O ARQYXIKMMOPJRM-UHFFFAOYSA-L 0.000 description 1
- 238000003760 magnetic stirring Methods 0.000 description 1
- AUHZEENZYGFFBQ-UHFFFAOYSA-N mesitylene Substances CC1=CC(C)=CC(C)=C1 AUHZEENZYGFFBQ-UHFFFAOYSA-N 0.000 description 1
- 125000001827 mesitylenyl group Chemical group [H]C1=C(C(*)=C(C([H])=C1C([H])([H])[H])C([H])([H])[H])C([H])([H])[H] 0.000 description 1
- JZMJDSHXVKJFKW-UHFFFAOYSA-M methyl sulfate(1-) Chemical compound COS([O-])(=O)=O JZMJDSHXVKJFKW-UHFFFAOYSA-M 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 235000010755 mineral Nutrition 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 239000000983 mordant dye Substances 0.000 description 1
- AJDUTMFFZHIJEM-UHFFFAOYSA-N n-(9,10-dioxoanthracen-1-yl)-4-[4-[[4-[4-[(9,10-dioxoanthracen-1-yl)carbamoyl]phenyl]phenyl]diazenyl]phenyl]benzamide Chemical compound O=C1C2=CC=CC=C2C(=O)C2=C1C=CC=C2NC(=O)C(C=C1)=CC=C1C(C=C1)=CC=C1N=NC(C=C1)=CC=C1C(C=C1)=CC=C1C(=O)NC1=CC=CC2=C1C(=O)C1=CC=CC=C1C2=O AJDUTMFFZHIJEM-UHFFFAOYSA-N 0.000 description 1
- 239000012299 nitrogen atmosphere Substances 0.000 description 1
- 125000004433 nitrogen atom Chemical group N* 0.000 description 1
- 239000004745 nonwoven fabric Substances 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 235000011837 pasties Nutrition 0.000 description 1
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 description 1
- SVTPNELSRGTTOX-UHFFFAOYSA-J phthalate;zirconium(4+) Chemical compound [Zr+4].[O-]C(=O)C1=CC=CC=C1C([O-])=O.[O-]C(=O)C1=CC=CC=C1C([O-])=O SVTPNELSRGTTOX-UHFFFAOYSA-J 0.000 description 1
- 229920000233 poly(alkylene oxides) Polymers 0.000 description 1
- 229920000515 polycarbonate Polymers 0.000 description 1
- 239000004417 polycarbonate Substances 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 229920002223 polystyrene Polymers 0.000 description 1
- 229920000915 polyvinyl chloride Polymers 0.000 description 1
- 239000004800 polyvinyl chloride Substances 0.000 description 1
- LQAZPMXASFNKCD-UHFFFAOYSA-M potassium;dodecane-1-sulfonate Chemical compound [K+].CCCCCCCCCCCCS([O-])(=O)=O LQAZPMXASFNKCD-UHFFFAOYSA-M 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 239000011541 reaction mixture Substances 0.000 description 1
- 230000002441 reversible effect Effects 0.000 description 1
- 102220006493 rs80338873 Human genes 0.000 description 1
- 238000007650 screen-printing Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 229910000077 silane Inorganic materials 0.000 description 1
- 150000004819 silanols Chemical class 0.000 description 1
- 229910002027 silica gel Inorganic materials 0.000 description 1
- 239000000741 silica gel Substances 0.000 description 1
- 238000000235 small-angle X-ray scattering Methods 0.000 description 1
- HFQQZARZPUDIFP-UHFFFAOYSA-M sodium;2-dodecylbenzenesulfonate Chemical compound [Na+].CCCCCCCCCCCCC1=CC=CC=C1S([O-])(=O)=O HFQQZARZPUDIFP-UHFFFAOYSA-M 0.000 description 1
- 238000000527 sonication Methods 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 239000012258 stirred mixture Substances 0.000 description 1
- DIORMHZUUKOISG-UHFFFAOYSA-N sulfoformic acid Chemical class OC(=O)S(O)(=O)=O DIORMHZUUKOISG-UHFFFAOYSA-N 0.000 description 1
- 230000008961 swelling Effects 0.000 description 1
- 229910052715 tantalum Inorganic materials 0.000 description 1
- 239000008399 tap water Substances 0.000 description 1
- 235000020679 tap water Nutrition 0.000 description 1
- 238000010345 tape casting Methods 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 description 1
- 238000002411 thermogravimetry Methods 0.000 description 1
- 229910052718 tin Inorganic materials 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- 239000010936 titanium Substances 0.000 description 1
- 238000004627 transmission electron microscopy Methods 0.000 description 1
- SZHOJFHSIKHZHA-UHFFFAOYSA-N tridecanoic acid Chemical class CCCCCCCCCCCCC(O)=O SZHOJFHSIKHZHA-UHFFFAOYSA-N 0.000 description 1
- 150000004072 triols Chemical class 0.000 description 1
- 239000003039 volatile agent Substances 0.000 description 1
- 230000004580 weight loss Effects 0.000 description 1
- 239000002023 wood Substances 0.000 description 1
- 239000002759 woven fabric Substances 0.000 description 1
- 239000001043 yellow dye Substances 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
- 239000011701 zinc Substances 0.000 description 1
- 239000004246 zinc acetate Substances 0.000 description 1
- 239000011592 zinc chloride Substances 0.000 description 1
- 235000005074 zinc chloride Nutrition 0.000 description 1
- NWONKYPBYAMBJT-UHFFFAOYSA-L zinc sulfate Chemical compound [Zn+2].[O-]S([O-])(=O)=O NWONKYPBYAMBJT-UHFFFAOYSA-L 0.000 description 1
- 229960001763 zinc sulfate Drugs 0.000 description 1
- 229910000368 zinc sulfate Inorganic materials 0.000 description 1
- 229910052726 zirconium Inorganic materials 0.000 description 1
- ZXAUZSQITFJWPS-UHFFFAOYSA-J zirconium(4+);disulfate Chemical compound [Zr+4].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O ZXAUZSQITFJWPS-UHFFFAOYSA-J 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B41—PRINTING; LINING MACHINES; TYPEWRITERS; STAMPS
- B41M—PRINTING, DUPLICATING, MARKING, OR COPYING PROCESSES; COLOUR PRINTING
- B41M5/00—Duplicating or marking methods; Sheet materials for use therein
- B41M5/50—Recording sheets characterised by the coating used to improve ink, dye or pigment receptivity, e.g. for ink-jet or thermal dye transfer recording
- B41M5/52—Macromolecular coatings
-
- 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
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B41—PRINTING; LINING MACHINES; TYPEWRITERS; STAMPS
- B41M—PRINTING, DUPLICATING, MARKING, OR COPYING PROCESSES; COLOUR PRINTING
- B41M5/00—Duplicating or marking methods; Sheet materials for use therein
- B41M5/50—Recording sheets characterised by the coating used to improve ink, dye or pigment receptivity, e.g. for ink-jet or thermal dye transfer recording
- B41M5/52—Macromolecular coatings
- B41M5/5218—Macromolecular coatings characterised by inorganic additives, e.g. pigments, clays
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B41—PRINTING; LINING MACHINES; TYPEWRITERS; STAMPS
- B41M—PRINTING, DUPLICATING, MARKING, OR COPYING PROCESSES; COLOUR PRINTING
- B41M5/00—Duplicating or marking methods; Sheet materials for use therein
- B41M5/50—Recording sheets characterised by the coating used to improve ink, dye or pigment receptivity, e.g. for ink-jet or thermal dye transfer recording
- B41M5/52—Macromolecular coatings
- B41M5/5227—Macromolecular coatings characterised by organic non-macromolecular additives, e.g. UV-absorbers, plasticisers, surfactants
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B41—PRINTING; LINING MACHINES; TYPEWRITERS; STAMPS
- B41M—PRINTING, DUPLICATING, MARKING, OR COPYING PROCESSES; COLOUR PRINTING
- B41M5/00—Duplicating or marking methods; Sheet materials for use therein
- B41M5/50—Recording sheets characterised by the coating used to improve ink, dye or pigment receptivity, e.g. for ink-jet or thermal dye transfer recording
- B41M5/52—Macromolecular coatings
- B41M5/5245—Macromolecular coatings characterised by the use of polymers containing cationic or anionic groups, e.g. mordants
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B41—PRINTING; LINING MACHINES; TYPEWRITERS; STAMPS
- B41M—PRINTING, DUPLICATING, MARKING, OR COPYING PROCESSES; COLOUR PRINTING
- B41M5/00—Duplicating or marking methods; Sheet materials for use therein
- B41M5/50—Recording sheets characterised by the coating used to improve ink, dye or pigment receptivity, e.g. for ink-jet or thermal dye transfer recording
- B41M5/52—Macromolecular coatings
- B41M5/5254—Macromolecular coatings characterised by the use of polymers obtained by reactions only involving carbon-to-carbon unsaturated bonds, e.g. vinyl polymers
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B41—PRINTING; LINING MACHINES; TYPEWRITERS; STAMPS
- B41M—PRINTING, DUPLICATING, MARKING, OR COPYING PROCESSES; COLOUR PRINTING
- B41M5/00—Duplicating or marking methods; Sheet materials for use therein
- B41M5/50—Recording sheets characterised by the coating used to improve ink, dye or pigment receptivity, e.g. for ink-jet or thermal dye transfer recording
- B41M5/52—Macromolecular coatings
- B41M5/5263—Macromolecular coatings characterised by the use of polymers obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
- B41M5/5281—Polyurethanes or polyureas
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B41—PRINTING; LINING MACHINES; TYPEWRITERS; STAMPS
- B41M—PRINTING, DUPLICATING, MARKING, OR COPYING PROCESSES; COLOUR PRINTING
- B41M5/00—Duplicating or marking methods; Sheet materials for use therein
- B41M5/50—Recording sheets characterised by the coating used to improve ink, dye or pigment receptivity, e.g. for ink-jet or thermal dye transfer recording
- B41M5/52—Macromolecular coatings
- B41M5/529—Macromolecular coatings characterised by the use of fluorine- or silicon-containing organic compounds
-
- 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
- Y10T428/249921—Web or sheet containing structurally defined element or component
- Y10T428/249953—Composite having voids in a component [e.g., porous, cellular, etc.]
- Y10T428/249987—With nonvoid component of specified composition
Definitions
- This invention relates to ink receptor media and more particularly to ink receptor media comprising a substrate coated thereon with particles in a binder.
- This invention also relates to surfactant templated silica particles.
- inkjet printers are relatively inexpensive as compared with many other hardcopy output devices, such as electrostatic printers.
- inkjet inks are wholly or partially water-borne.
- Inkjet images may be printed on plain paper or on a suitable ink receptor medium that has been treated or coated to improve its ink receptor properties.
- Such known materials are overhead transparencies and glossy papers, but they can have certain disadvantages such as color bleed, low ink capacity (that is, flooding), a slow ink absorption rate (long dry times), and low color density.
- Porous solids created by nature or by synthetic design have found great utility in the areas of catalysis and separation.
- such porous materials are classified by pore size: microporous having pore sizes of ⁇ 2 nm; macroporous having pore sizes exceeding 50 nm; and mesoporous having pore sizes between 2 and 50 nm.
- Such porous materials can be structurally amorphous, paracrystalline, or crystalline.
- Amorphous materials (for example, silica gel) and paracrystalline materials exhibit wide pore size distributions in the mesoporous range.
- Zeolites and molecular sieves have highly crystalline structures and uniform pore size, but have pore sizes in the microporous range.
- the invention provides ink receptor media comprising a substrate, an ink receptor on the substrate comprising surfactant templated mesoporous particles, and an organic binder.
- the ink receptor media ofthe invention may also have an ink fixing agent in contact with at least a portion ofthe ink receptor.
- surfactant templated mesoporous particles means inorganic materials having substantial intraparticle porosity that are formed with an organic templating agent and have pore sizes of about 1.5 to 50 nm.
- examples of such particles include surfactant templated silica particles (STS), surfactant templated silica- metal oxide particles, non-silica surfactant templated metal oxides, and the like.
- an "ink receptor” comprises a combination of STM particles in an organic binder in a substantially solvent free form to immediately accept ink.
- the invention provides an ink receptor composition comprising a mixture of STM particles and an organic binder.
- the invention provides a method of making an ink receptor medium comprising the step of coating an ink receptor composition comprising STM particles and an organic binder onto a substrate. Further steps may include removing solvent from the composition to form an ink receptor and optionally applying an ink fixing agent on the ink receptor.
- the invention provides a method of printing an image on a substrate comprising the steps of providing a substrate coated with an ink receptor, the ink receptor comprising STM particles and an organic binder, and printing an image onto the ink receptor medium.
- ink receptor media ofthe invention Some features of ink receptor media ofthe invention are that they have a large capacity to absorb ink, provide rapid ink drying times, provide sharp delineation of deposited drop edges in inkjet printed colors, provide good color density, provide waterfastness to the applied ink, are UN and chemically stable, are abrasion resistant, are mechanically flexible, and provide excellent adherence to a substrate.
- optically clear ink receptor coatings may be achieved.
- the invention provides a composition of matter comprising STS particles having a mean particle size of from about 0.01 ⁇ m to about 100 ⁇ m, wherein 90 percent of the particles have a particle size of less than 4 ⁇ m, preferably less than 3 ⁇ m, more preferably less than about 2 ⁇ m, and a pore size of from about 1.5 nm to about 30 nm, preferably from about 2 nm to about 10 nm.
- the STS particles ofthe invention are preferably spherical or ellipsoidal in shape.
- the STS particles ofthe invention are formed using an acid catalyst and may also have a high concentration of surface silanols in an uncalcined state. Such a surface is believed to provide further ink fixing properties.
- STS particles means materials comprising silica having substantial intraparticle porosity that are formed with an organic templating agent.
- organic templating agents used herein are surfactants and block copolymers.
- SEM scanning electron microscopy
- TEM transmission electron microscopy
- XRD X-ray diffraction analysis
- particle size means the largest cross-sectional particle dimension.
- pore size is determined experimentally by a combination of XRD and TEM. Using this method, X-ray diffraction measurements are used to determine the maximal d-spacing for the samples. From the d-spacing data and TEM micrographs, pore size is determined by converting the d-spacing to a lattice constant using information about the symmetry ofthe array of pores, and subtracting from this value the dimension of the pore wall thickness measured from the TEM micrographs. The d-spacing ofthe primary Bragg peak (for example, 100 for a hexagonal array) sets a maximum pore size of the periodic array.
- the invention provides STS particles that are transparent.
- the transparent silica particles can be characterized as having a mean particle size of 100 nm (0.1 ⁇ m) or less, preferably about 10 to about 50 nm (about 0.02 to about 0.05 ⁇ m), and pore sizes of about 1.5 to about 5 nm, preferably from 2 to 4 nm.
- the transparent particles ofthe invention are prepared in a solvent, are preferably unagglomerated (not agglomerated), and can be re-suspended in solvent after the solvent has been decanted. These particles may be either acid or base catalyzed.
- the invention provides a colloidal dispersion of STM particles comprising unagglomerated surfactant templated particles in a solvent.
- the particles have a mean particle size of about 500 nm or less, preferably about 150 nm or less, more preferably about 100 nm or less and pore sizes of about 1.5 to about 30 nm, preferably about 2 to about 10 nm.
- STS particles are preferred.
- the colloidal dispersion is transparent, and more preferably, transparent and stable.
- the preferred mixture containing transparent particles can be characterized as having a pH of about 1 to about 2, as stabilized using an organic acid, and as containing up to about 30 weight percent transparent particles, preferably less than 12 weight percent, more preferably less than 6 weight percent.
- the invention provides a method of making STS particles comprising the steps of forming a mixture comprising water, a silica source, an organic templating agent, and a catalyst; and aging the solution for a sufficient time to form said silica particles.
- the invention provides a method of making surfactant templated silica comprising the steps of forming a mixture comprising water, a silica source, an organic templating agent comprising an ethoxylated fatty amine, and an acid catalyst and aging the solution for a sufficient time to form said silica particles.
- Further steps for methods of making STS include filtering ofthe mixture, drying the mixture, grinding the mixture, calcining the mixture at a temperature sufficient to decompose the templating agent or extracting the templating agent from the particles, and milling or shearing the particles in slurry form to reduce particle size.
- STS particles differ from other forms of silica, for example, colloidal silica, precipitated silica, and conventional zeolites.
- STS particles typically have approximately 50 volume percent intraparticle porosity, whereas colloidal silica or precipitated silica does not have appreciable intraparticle porosity.
- STS particles (formed by aggregating approximately 4 - 10 nm colloidal silica), does have interparticle porosity, but the pore size distribution is quite broad compared to that of STS particles.
- precipitated silica generally forms large friable masses that yield micron-size or larger irregular pieces when ground or shear mixed.
- STS particles typically have a more uniform morphology.
- STS particles differ from conventional molecular sieves in that STS particles have pores that are ⁇ 1.5 to ⁇ 30 nm in size, whereas conventional molecular sieves have pores that are -0.3 to -1.2 nm in size.
- Figure 1 is a scanning electron micrograph of STS particles prepared according to Example 1.
- Figure 2 is a scanning electron micrograph of STS nanoparticles prepared according to Example 25a.
- Figure 3 is a scanning electron micrograph of STS nanoparticles prepared according to Example 25b.
- Figure 4 is a scanning electron micrograph of STS particles prepared according to Example 38.
- Figure 5 is a scanning electron micrograph of STS particles prepared according to Example 40a.
- Figure 6 is an X-ray diffraction spectrum of STS particles prepared as in Example 44. The 100, 200, and 300 peaks are evident and the cell hexagonal constant (pore to pore distance) is approximately 11.5 nm.
- Figure 8 is an X-ray diffraction spectrum of STS nanoparticles prepared as in Example 31 using acetic acid. The peaks at 3.57, 3.13, and 1.79 nm indicate a cubic structure (three-dimensional porosity).
- Ink receptor media ofthe invention comprise a substrate, an ink receptor on the substrate comprising surfactant templated mesoporous particles, and an organic binder.
- an ink fixing agent may be further incorporated into and/or applied to the ink receptor.
- STM particles are broadly suitable for use in the invention, in some cases it may be desirable to use mesoporous particles of such small size that they may be used to prepare transparent ink receptor coatings (that is, transparent STM or STS particles). In other cases, it may be desirable or preferable to use surfactant templated silica particles (that is, STS particles). STS particles are a subset ofthe larger group of STM particles that are useful in the invention.
- the ink receptor media ofthe invention are suitable for inkjet printing, they are also suitable for receiving ink by other printing processes, such as by fountain pen, flexography, screen printing, and the like.
- the receptor compositions ofthe invention contain STM particles. Any STM particles (or combination of STM particles) having a primary unaggregated mean particle size of less than about 100 ⁇ m may be used in the receptor media ofthe invention.
- the STM particles impart additional ink capacity, scratch resistance, dimensional stability, and ink fixing properties to an ink receptor medium.
- Preferred STS particles for use in ink receptors are spherical or ellipsoidal in shape and have a mean particle size range of about less than 0.01 ⁇ m to about 100 ⁇ m, wherein 90 percent ofthe particles have a particle size less than 4 ⁇ m, preferably less than 3 ⁇ m, more preferably less than 2 ⁇ m.
- Preferred STS particles can also be characterized as having at least one low angle Bragg peak in its X-ray diffraction pattern.
- the low angle peak generally occurs in the region between 0.5 and 4.5 degrees two-theta with copper K ⁇ radiation. This corresponds to a d-spacing of approximately 2 to 30 nm. In some cases, 3 or more additional diffraction peaks are observed in the X-ray diffraction pattern in addition to the primary peak.
- the surfaces of useful STS particles typically have a Q3/Q4 signal ratio of greater than 0.5 as measured by 29si NMR with magic angle spinning.
- the signal for ⁇ )4 occurs at about -106 to about -108 ppm relative to a tetramethylsilane (TMS) standard.
- TMS tetramethylsilane
- the ⁇ )3 signal occurs at about -98 to -99 ppm relative to TMS.
- Standard peak fitting programs are used to determine the relative intensities ofthe two peaks. Spectra can be recorded using a resonance frequency of 39.7 MHz, with a 7.25 millisecond pulse at 90T and a pulse delay of 120 seconds using ZrO2 rotors.
- preferred STS particles may be synthesized by combining at least: water, a silica source, an organic templating agent, and a catalyst to form a mixture used to make STS particles ofthe invention. The mixture is then aged for a sufficient time to form the particles.
- Useful silica sources include colloidal silica, precipitated silica, fumed silica, and alkoxysilanes.
- the silica source is an alkoxysilane, with tetramethoxysilane or tetraethoxysilane being preferred;
- the organic templating agent is a C ⁇ 4 or C ⁇ g alkylammonium salt surfactant, preferably the chloride or bromide salt (for example, C ⁇ H33N(CH3)3Br),
- the catalyst is ammonium hydroxide or an alkylammonium hydroxide, and the solvent is a 75 : 25 (wt/wt) water : methanol mixture.
- the water to silica molar ratio is greater that about 5.
- the catalyst is an acid, for example HCl
- typical molar ratios are about 0.02 to about 0.2 moles organic templating agent, 30 to 120 moles water, about 0 to 20 moles co-solvent and about 9 to 20 moles of acid per mole of silica source.
- the catalyst is a base, for example ammonium hydroxide or sodium hydroxide
- typical molar ratios are about 0.1 to about 0.2 moles organic templating agent, 30 to 120 moles water, about 0 to 20 moles co-solvent, and about 0.3 to 0.5 moles of base per mole of silica source.
- Useful organic templating agents include cationic, anionic, and nonionic surfactants.
- Useful cationic surfactants include alkylammonium salts having the formula C n H2n+l N(CH3)3X, where X is OH, Cl, Br, HSO4 or a combination of OH and Cl, and where n is an integer from 8 to 22, and the formula C n H2 n + ⁇ N(C2H5)3X, where n is an integer from 12 to 18; gemini surfactants, for example those having the formula:
- Useful anionic surfactants include alkyl sulfates, for example having the formula C n H2 n +iOSO3-, where n is 12 to 18; alkylsulfonates including C16H33SO3H and
- alkyl phosphates for example C12H25OPO3H, and
- C14H29OPO3K alkylcarboxylic acids, for example C17H35COOH and C 1 H 2 5COOH.
- alkyl sulfates and sulfonates such as sodium dodecyl sulfate and potassium dodecanes
- Useful nonionic surfactants include alkylamines including those having the formula C n H2 n + ⁇ NH2, poly(oxyethylene oxides), poly(octaethylene glycol monodecyl ether) (C ⁇ EOg), poly(octaethylene glyconyl nonhexadecyl ether) (C1 gEOg), and poly(alkylene oxide) triblock copolymers such as poly(ethylene oxide)-poly(propylene oxide)-poly(ethylene oxide) (PEO-PPO-PEO) or the reverse (PPO-PEO-PPO).
- Examples of useful commercially available nonionic copolymer surfactants include those having the tradename PLURONIC and product designations P123, F98, 25R4, and 17R4, available from BASF Corporation, Mount Olive, NJ.
- ethoxylated amines also called ethoxylated fatty amines.
- Useful catalysts are those compounds which promote hydrolysis/dissolution ofthe silica source and can promote "inorganic" polymerization.
- the useful catalysts are generally acids and bases.
- the acids may be organic or inorganic.
- Preferred acids include mineral acids such as hydrochloric, sulfuric, hydrobromic, hydrofluoric, and like acids.
- Useful bases include alkali metal hydroxides such as sodium hydroxide, alkylammonium hydroxides, and like bases.
- a preferred base is ammonium hydroxide.
- a co- solvent may be added to the mixtures used to make STS particles ofthe invention to improve solution homogeneity, to modify particle size, and to modify particle morphology.
- co-solvents examples include alcohols, esters (for example, acetates), ketones, diols, triols, ethers, amides, and amines.
- Preferred co-solvents include methanol, ethanol, isopropanol, ethylene glycol, formamide, N,N-dimethylformamide, tetrahydrofuran, and ethyl acetate.
- a low dielectric constant liquid can be optionally added to the mixtures used to make STS particles ofthe invention to increase the pore size ofthe resulting particles.
- useful low dielectric constant liquids include benzene, toluene, mesitylene, toluene, any many other alkanes, alkenes, and aromatics that are described in U.S. Patent No. 5,057,296 (Beck).
- the resulting mixture is allowed to age from 5 minutes to 1 or more days.
- the resulting physical gel/colloid is suction filtered and washed with water and/or a lower alcohol, such as ethanol.
- the washed filtrate typically is dried overnight in a 100 °C drying oven; mechanically ground (on small scale this may be accomplished in a mortar and pestle); the surfactant is removed by either an extraction means such as with water or an acidic alcohol solution, or by calcining the ground filtrate at a temperature sufficient to decompose the surfactant; and milled or shear mixed as an aqueous slurry to break up any particles that have aggregated into a larger agglomerate.
- the material can be left as an aqueous slurry or dried to a water dispersible powder and then sieved. Slurries are typically 10 - 40 weight percent solids.
- Mean particle size ofthe calcined material prior to milling or shearing is generally within the range of 0.01 - 1000 ⁇ m. After milling or shearing, the mean particle size is typically within the range of 0.01 - 100 ⁇ m, with more preferred mean particle sizes falling in the range of 0.01 -10 ⁇ m.
- transparent STM particles are employed. Transparency results from using particles that have both compatibility with the binder resin and a physical mean size of less than about 100 nm.
- Preferred transparent STM particles ofthe invention are STS particles (also called STS nanoparticles).
- Transparent STS particles ofthe invention are characterized as having a mean particle size of 100 nm (0.1 ⁇ m) or less preferably about 10 to about 50 nm (0.01 to 0.05 ⁇ m) and more preferably about 10 to less than 50 nm (0.01 to 0.05 ⁇ m), and pore sizes of from greater than 1.5 nm to about 5 nm, preferably from 2 to 4 nm. As used herein, only particles having a mean particle size of 100 nm or less are considered transparent. These transparent particles can be used to form unagglomerated colloidal dispersions that are preferably transparent and stable.
- transparent STS particles ofthe invention may be synthesized by combining at least water, a silica source, an organic templating agent, an organic acid, and optionally, an appropriate polar solvent.
- Preferred molar ratios are a polar solvent to water ratio of greater than 1 : 4 and an organic acid to silica molar ratio of greater than about 9 : 1.
- the silica sources, organic templating agents, catalysts, and solvents mentioned above are also useful in making transparent STS particles.
- a preferred silica source is an alkoxy silane; a preferred organic templating agent is a C ⁇ or Ci g alkylammonium salt surfactant, preferably the chloride or bromide salt (for example, C ⁇ gH33N(CH3)3Br); a preferred catalyst is ammonium hydroxide or an alkylammonium hydroxide; and a preferred solvent is a 75 : 25 (wt/wt) water : methanol mixture.
- Useful organic acids include, for example, carboxylic or dicarboxylic acids, for example, acetic, malonic, oxalic, lactic, citric, and tartaric acids with acetic acid being preferred.
- STM and preferably STS particles
- the mean size ofthe particles may range from about 500 nm or less, preferably about 150 nm or less, and more preferably about 100 nm or less.
- the particles have pore sizes of from about 1.5 to about 30 nm, preferably from about 2 to about 10 nm.
- the surface ofthe particles can be functionalized with a silane coupling agent to yield a stable dispersion.
- the surface ofthe particles can be functionalized with a silane coupling agent or stabilized with an appropriate anion of an organic acid to yield a stable dispersion.
- the un-functionalized particles can be allowed to grow, aggregate, and precipitate, at which time the particles can be isolated by filtration.
- Useful silane coupling agents include, for example, cationic alkoxysilanes with N- (trimethoxysilylpropyl)isothiouronium chloride being preferred.
- Useful organic acids include for example, carboxylic or dicarboxylic acids for example, acetic, malonic, oxalic, lactic, citric, and tartaric acids with acetic acid being preferred. Carboxylic acids are believed to catalyze the hydrolysis of a alkoxysilanes and stabilize colloidal dispersions by limiting particle growth.
- STM particles also called ultra-large pore zeolites and mesoporous silica
- STM particles include those described in U.S. Patent Nos. 5,102,643 (Kresge et al); 5,198,203 (Kresge et al.); and 5,098,684 (Kresge et al.); and their methods of making are described in U.S. Patent Nos.
- the receptor compositions ofthe invention contain one or more organic binders.
- the function ofthe binder is to adhere the STM particles to each other and/or to the substrate.
- Preferred binders also provide a receptor that is relatively flexible so to resist cracking and flaking off of the substrate.
- Useful binders have glass transition temperatures in the range of about - ⁇ 125 °C to about 125 °C, and preferably from about -30 °C to about 30 °C. The binders should exhibit good adhesion to the substrate and the STM particles.
- Useful binders are also compatible with the particular dispersing medium used to disperse the STM particles, for example, water so as to not cause particle agglomeration before the mixture is coated onto a substrate.
- the binder is water resistant or insoluble when the receptor is required to be waterfast.
- Such binders are preferred because they are less sensitive to atmospheric humidity changes than are water-soluble binders, and the water resistant or insoluble binders provide receptor integrity under wet conditions.
- a useful water resistant binder is a cationic latex polymer formed from at least one cationic latex emulsion having less than 10 mole percent of a copolymerizable monomer having a tertamino or quaternary ammonium functionality.
- the above latex emulsion may also contain greater than 10 mole percent of a monomer having hydroxy functionality.
- “Cationic” means having a net positive charge.
- “Mole percent” means weight percent of the compound divided by molecular weight ofthe component divided by the total number of moles ofthe composition. Synthesis ofthe cationic latex polymer binder is achieved by formulating a premix of monomers intended as the components of he final polymer, together with an initiator.
- this premix is then added to a vessel containing water, a surfactant, and more initiator. This mixture is then vigorously stirred to create droplets of globules of monomer. After mixing, further monomer and initiator may be added.
- the reaction vessel is heated until formation of a polymer emulsion starts, and then the remainder ofthe premix is added over an extended time period. Following the addition of all ofthe premix, the whole mixture may be maintained at a predetermined temperature for a suitable time period to ensure complete reaction of all monomers.
- the contents ofthe reaction vessel are then cooled and the finished latex polymer emulsion decanted for storage.
- all ofthe reagents should be degassed, and the entire reaction carried out in a nitrogen atmosphere.
- a wide variety of monomers may be used as starting materials for latex emulsion manufacture.
- Vinyl monomers such as inyl acetate, vinyl butyrate, vinyl chloride, and the like may be employed as components of latex emulsions, as may urethane monomers, acrylate monomers, and many others.
- the monomers used are alkyl
- (meth)acrylate monomers such as ethyl acrylate, methyl acrylate, butyl acrylate, methyl methacrylate, hydroxypropyl acrylate, hydroxyethyl acrylate, quaternary salts of dimethylaminoethyl acrylate, and acidic monomers such as acrylic acid and methacrylic acid.
- the above latex emulsions and polymers contain quaternary nitrogen entities, that is, a positively charged quadruple bonded nitrogen atom, and associated therewith a negatively-charged counter ion.
- anionic entities for example, chloride and other halide ions, sulfate ions, phosphate ions, organic acid ion, such as acetic and proprionic, ions combining both traditionally organic entities in combination such as methyl sulfate ions and the like.
- anionic entities for example, chloride and other halide ions, sulfate ions, phosphate ions, organic acid ion, such as acetic and proprionic, ions combining both traditionally organic entities in combination such as methyl sulfate ions and the like.
- the most convenient, but not the only, way of incorporating the desired amount of quaternary nitrogen functions into the latex emulsion is by incorporating a monomer suitably substituted with a quaternary nitrogen in the initial and un-polymerized monomer mixture. Alternatively, a suitable monomer that could be further reacted to attach a quaternary function could also be used.
- the polymer particles in the latex emulsion are generally spherical with mean particle sizes below 500 nm. Emulsions containing particle sizes in this range are nearly or completely transparent. Size may be quite variable but typical mean particle sizes are 50 - 400 nm, preferably from 50 to 150 nm, and more preferably from 75 to 125 nm.
- the binders may be water soluble or water swellable.
- Water soluble or water swellable binders have the advantage in that they can also absorb aqueous inks. However, water soluble or water swellable binders are also more sensitive to atmospheric humidity changes.
- organic binders examples include, but are not limited to, CARBOSETTM GA2136 (an acrylic copolymer, available from B.F. Goodrich, Cleveland, OH); RHOPLEXTM 2438, RHOPLEXTM B-60A, MAINCOTETM HG-54D (acrylic copolymers, available from Rohm & Haas, Philadelphia, PA); and AIRVOLTM
- the binder may be a melt-processable resin which may also function as a substrate.
- the STM particles would be included in the extrudate; that is, extruded with the resin binder/substrate as one unit.
- the extrudate may also include an ink fixing agent or the ink fixing agent may be added afterwards. Examples of such binder/substrate resins include polyethylene and polypropylene.
- the extrudate may also be stretched to induce additional porosity in the substrate.
- the STM particle : binder ratios may range from approximately 1 : 40 to 40 : 1 by weight depending upon the composition ofthe specific particles and binder used.
- a preferred STS particle : binder ratio ranges from 1 :9 to 9:1.
- One of ordinary skill in the art can easily choose the appropriate particle : binder ratio so to optimize scratch resistance, print performance, cost, etc., using the ratios above without undue experimentation.
- the flexibility and scratch resistance ofthe receptor system is largely controlled by the glass transition temperature (Tg) ofthe binder.
- Tg glass transition temperature
- the flexibility ofthe receptor system increases with decreasing Tg, whereas scratch resistance generally increases with increasing Tg.
- these two characteristics are balanced when choosing a binder.
- binder materials having a Tg near —15 °C provide a balance of flexibility and scratch or abrasion resistance for receptor compositions having an STM : binder ratio of approximately 3 : 1 by weight.
- a material that provides further water resistance and pigment or dye fixing may be provided in or over part or all ofthe ink receptor. If an ink fixing agent is desired, the ink fixing agent is preferably incorporated into the receptor composition. Otherwise, if the ink fixing agent is not compatible with any other component in the ink receptor mixture, the ink fixing agent may be provided over the ink receptor.
- These materials are primarily cationic polymers and/or inorganic salts having a multivalent cation. The cationic polymers are believed to mordant dyes and pigment particles.
- the multivalent metal salts are believed to serve as reagents to rapidly destabilize dispersants surrounding the pigment particles in the ink, whereby the pigment particles coagulate or flocculate as the remainder ofthe ink fluid continues along the surfaces ofthe receptor medium.
- the metal salts are soluble in water for both preparing coating solutions and during imaging, but not soluble in water after complexing with the dispersing aid that surrounds the pigment particles in the ink.
- Nonlimiting examples of inorganic multivalent metal salts useful in the present invention include the metal cations from Groups 2 through 16 inclusive in the Periodic
- preferred salts include aluminum sulfate, aluminum nitrate, gallium nitrate, ferrous sulfate, chromium sulfate, zirconium sulfate, magnesium sulfophthalate, copper sulfophthalate, zirconium sulfophthalate, zirconium phthalate, zinc sulfate, zinc acetate, zinc chloride, calcium chloride, calcium bromide, magnesium sulfate, magnesium chloride, aluminum sulfophthalate, aluminum sulfoisophthalate, and combinations thereof. These compounds are typically sold and can be used in the hydrated form. Ofthe various possible salts, aluminum sulfate and aluminum sulfophthalate are presently preferred.
- the amount of salts that can be used in the coating solution for coating the receptors ofthe present invention can range from about 0.1 weight percent to about 50.0 weight percent, and preferably from about 0.5 weight percent to about 10.0 weight percent.
- the substrate ofthe receptor media ofthe invention can have a solid or porous surface which may be composed of, for example, glass, wood, metal, a polymeric film, or a porous material such as a membrane and nonwoven material.
- the substrate may be flexible or rigid and is preferably flexible.
- Useful polymeric films include polyester, polyolefin, polyamide, polycarbonate, polyurethane, polystyrene, polyacrylate, poly(meth)acrylate, polyvinyl chloride, and combinations thereof.
- the substrates may be provided in the form of films, sheets, or tapes, any of which may be provided from a continuous roll with or without perforations.
- porous surface means or includes any material that has voids and includes materials that are considered to be microporous and macroporous.
- Other useful materials include woven and non-woven fabrics (for example, polypropylene, polyethylene, polyester, polyamide, polyurethane, polyacrylate, polymethacrylate, or combinations thereof), membranes, virtually any type of melt-blown or spunbonded fibrous substrates and pulp or paper materials having the desirable strength and integrity.
- the receptor media ofthe invention are very easily made.
- STM particles are first dispersed in a solvent, preferably water, and a polymeric binder and (optionally) a surfactant and/or ink fixing agent is added to the dispersion.
- the homogeneous mixture is coated onto a substrate by means such as knife coating, Mayer rod, spraying, dipping, etc., then dried in an oven at a temperature which evaporates the solvent but does not distort or melt the substrate, preferably about 110 °C.
- a solution of an ink fixing agent (optionally, with additional surfactant) in a solvent, preferably distilled water, may be coated on top ofthe dried receptor composition, followed by drying in an oven at a temperature which evaporates the solvent but does not distort or melt the substrate.
- the STM particles and ink fixing agent if desired may be coextruded with a polyolefin binder using known procedures to form a free standing film.
- This film may also function as the substrate or may be attached (for example, by adhesives or coextrusion) to another substrate as desired.
- An ink receiving medium ofthe present invention has two major opposing surfaces and can be employed for printing (for example, by inkjet methods) on both surfaces.
- one ofthe major surfaces can be dedicated for the purpose of adhering the finished image graphic to a supporting surface such as a wall, a floor, or a ceiling of a building, a sidewall of a truck, a billboard, or any other location where an excellent quality image graphic can be displayed for education, entertainment, or information.
- any of these adhesive surfaces should be protected by a release or storage liner such as those commercially available from Rexam Release, Bedford Park, IL.
- mechanical fasteners can be used if laminated in some known manner to that opposing major surface ofthe receptor ofthe present invention.
- mechanical fasteners include hook and loop, VELCROTM, SCOTCHMATETM, and DUAL LOCKTM fastening systems, as disclosed in published PCT Patent Application No. WO 98/39759 (Loncar).
- an optional layer may be applied to that imaged major surface to protect and enhance the image quality ofthe image on the receptor.
- optional layers are overlaminates and protective clear coatings commercially available from Minnesota Mining and Manufacturing Company from its Commercial Graphics Division and those disclosed in U.S. Patent No. 5,681,660 (Bull et al.). Other products known to those skilled in the art can also be used.
- ADVERA 403 and ADVERA 40 IP are trade designations for zeolites, available from The PQ Corp., Valley Forge, PA.
- AirVOL 523 is a trade designation for polyvinyl alcohol, available from Air Products and Chemicals, Allentown, PA.
- RHOPLEX B-60A "RHOPLEX 2438”, “RHOPLEX AC- 1230M”, and “MAINCOTE HG-54D” are trade designations for latex binder emulsions, available from Rohm and Haas Co.
- CARBOSET GA2136 is a trade designation for a latex binder emulsion, available from B.F. Goodrich Co., Cleveland, OH.
- ZONYL FSO is a trade designation for a fluorinated surfactant, available from E I DuPont de Nemours Corp., Wilmington, DE.
- "ELENES T0703WDO” is a trade designation for a polyester core/ polyethylene sheath fiber spunbonded substrate having a basis weight of 70g/ ⁇ _2 and a thickness of 0.25 mm, available from Unitika, Ltd., Osaka, Japan.
- "REEMAY 2033” is a trade designation for a spunbonded polyester, having a basis weight of 100 g/m ⁇ and 0.44 mm thickness, available from Reemay, Inc., Old Hickory, TN.
- PLURONIC is a trade designation for triblock copolymers of polyethylene oxide - polypropylene oxide - polyethylene oxide, available from BASF Corp. "PLURONIC
- PI 23 is a 30 weight percent polyoxyethylene with a 3600 MW polyoxypropylene segment
- PLURONIC F77 is a 70 weight percent polyoxyethylene with a 2100 MW polyoxypropylene segment
- PLURONIC P85 is 50 weight percent polyoxyethylene with a 2400 MW polyoxypropylene segment
- PLURONIC F98 is an 80 weight percent polyoxyethylene with a 2700 MW polyoxypropylene segment
- PLURONIC P 103 is a
- ETHOMEEN is a trade designation forethoxylated amines having the formula (R-NCH CH2 ⁇ ) ⁇ H (CH2CH O) yH, available from Akzo Nobel, Chicago, IL.
- MAGIC DMPB10 INKJET BANNER FILM is a trade designation for an ink receptor substrate, 10 mil polyethylene base, available from Rexam Graphics Inc., South Hadley, MA.
- PET polyethylene terephthalate
- An imaged substrate to be evaluated was tested by rinsing under tap water on the image and/or soaking the image in a beaker of water. An image was determined to be waterfast if the rinsate was colorless, and the image was not degraded in quality.
- Example 1 This example describes a synthesis of STS particles using ammonium hydroxide and an aqueous slurry of STS particles derived therefrom.
- Tetradecyltrimethylammonium bromide 40 g, abbreviated hereinafter as C14TAB
- C14TAB Tetradecyltrimethylammonium bromide
- 490 g methanol, 980 g deionized water, and 490 g concentrated ammonium hydroxide (27.5 - 29 weight percent aqueous) in a 4-L glass jar. The solution was magnetically stirred until the C ⁇ 4TAB completely dissolved.
- TMOS tetramethoxysilane
- the white gel which had a pH of about 11, was allowed to stand overnight, then filtered and washed with water. The filter cake was dried overnight in a vented 100 °C oven. The dried cake was ground in a large alumina mortar. 74.56 g were calcined in flowing nitrogen at 550 °C for 1.5 hours
- SEM indicated 250 - 400 nm spherical and ellipsoidal primary particles with a small fraction of ⁇ 50 nm primary particles.
- This example describes another preparation of an aqueous slurry of STS particles.
- a sample was prepared with reagent ratios identical to Example 1.
- the TMOS was contained in a separatory funnel and added to the other reagents over 2.5 minutes.
- the reaction was agitated with a high shear mixer for 5 minutes with increasing shear rate from 500 to 14000 rpm.
- the filter cake was dried overnight in a vented 100 °C oven.
- the dried cake was ground in a large mortar. 81.14 g were calcined in flowing air at 550 °C for 6 hours (10 °C ramp rate).
- XRD indicated 1 peak at 3.46 nm in the uncalcined sample.
- SEM indicated 250 - 500 nm spherical and ellipsoidal primary particles with a small fraction of ⁇ 50 nm primary particles. Jagged fracture surfaces were evident on some particles.
- This example describes another preparation of STS particles.
- Cetyltrimethylammonium bromide 36 g, abbreviated hereinbelow as C ⁇ gTAB
- FC-754 surfactant 1470 g deionized water
- 480 g concentrated ammonium hydroxide 27.5 - 29 weight percent aqueous
- the resultant molar weight ratio was 1.00 TMOS : 0.12 CjgTAB : 0.0033 FC-754 surfactant : 120 water : 4.6 ammonium hydroxide.
- the capped jar was allowed to stand quiescent overnight.
- the jar was shaken by hand to break up the resultant gel and suction filtered with a B ⁇ chner funnel.
- the filter cake was thoroughly washed with -1 L of deionized water.
- the cake was dried in air for 3 days. A portion of the dried cake (83.87 g) was ground by hand and loaded into a 6 cm wide x 50 cm long x 2 cm deep hemispherical quartz boat.
- the material was calcined in a large tube furnace (-3 ft hot zone) at 550 °C for 1 hour in a tube furnace with flowing nitrogen.
- the initial ramp from room temperature was 1 hour; the cool down was with the power to the furnace off.
- About 44.1 percent ofthe initial weight was lost.
- the brown tan powder was hand ground with a mortar and pestle.
- the powder was calcined again at 550 °C for 6 hours in a tube furnace with flowing argon and then the same profile with flowing air.
- the initial ramp from room temperature was 50 minutes; the cool down was with the power to the furnace off.
- the recovered white powder 46.512 g was added to 450 mL isopropanol and ground in a ball mill for -1 - 2 hours.
- the isopropanol was evaporated and the dried powder was passed through a No. 100 sieve.
- SEM indicated a bimodal distribution of particle sizes: 100 - 1000 nm spherical and ellipsoidal primary particles plus large 10 - 30 ⁇ m faceted platelets (some substructure).
- This example describes another preparation of STS particles using a modified cosolvent : water molar weight ratio.
- the cake was put into a 100 °C vented drying oven overnight.
- the dried cake was ground by hand and 167.64 g ofthe powder was loaded into a 6 cm wide x 50 cm long x 2 cm deep hemispherical quartz boat.
- the material was calcined with the procedure described in Example 3 above.
- Scanning electron microscopy indicated spherical and ellipsoidal particles 0.05 - 1.30 ⁇ m in size, some with facets.
- This example describes another preparation of STS particles with an aluminosilicate framework using sodium hydroxide catalysis.
- CjgTAB (40 g) was combined with 1862 g deionized water and 19.5 g 50 weight percent aqueous sodium hydroxide in a 4-L glass jar and heated to 50 °C to form a transparent solution.
- 20.79 g aluminum sec-butoxide was combined with 98 g isopropanol and 128.8 g TMOS.
- the solution was mixed for ⁇ 5 minutes. This turbid solution was added to the surfactant solution.
- the resulting opaque white gel (which formed in -10 - 15 seconds) was shaken by hand for about 1 - 2 minutes.
- the final molar weight ratio was 1.00 TMOS : 0.13 Cj ⁇ TAB : 122 water : 1.9 isopropanol : 0.29 sodium hydroxide.
- the capped jar was allowed to stand quiescent overnight.
- the gel was shaken by hand to break it up and suction filtered with a B ⁇ chner funnel.
- the filter cake was thoroughly washed with 200 - 300 mL deionized water.
- the cake was put into a vented drying oven at 100 °C vented and allowed to remain overnight.
- the dried cake was ground by hand and 96.18 g ofthe ground cake was loaded into a 6 cm wide x 50 cm long x 2 cm deep hemispherical quartz boat.
- Example 6 This example describes another preparation of STS particles using a swelling agent.
- the final molar weight ratio was 1.00 TMOS : 0.13 C ⁇ ⁇ TAB : 120 water : 4.6 ammonium hydroxide : 1.5 toluene.
- the stoppered jar was allowed to stand overnight.
- the gel was shaken by hand to break it up and suction filtered with a Buchner funnel.
- the filter cake was thoroughly washed with deionized water.
- the material was calcined with the procedure described in Example 3 above. XRD ofthe calcined powder gave a cell constant of -4.5 nm.
- This example describes another preparation of STS particles using ammonia gas catalysis.
- Ci 4TAB (20 g) was combined with 192.3 g methanol, 735 g deionized water, and
- TMOS 64.5 g TMOS in a 10-L metal bucket.
- the solution was allowed to sit for 5 minutes and then gaseous ammonia was diffused over this rapidly stirred mixture.
- the solution gelled in -25 seconds.
- the final molar weight ratio was 1.00 TMOS : 0.13 C14TAB : 97 water : 25 methanol.
- the beaker was allowed to sit overnight. The gel was shaken by hand to break it up and suction filtered with a Buchner funnel; the pH was > 10. The filter cake was thoroughly washed with deionized water.
- SEM indicated primary particles 50 - 200 nm in size.
- This example describes another preparation of STS particles using tetraethoxysilane as the silica source.
- C14TAB (16.75 g) was combined with 463.2 g methanol and 348 mL concentrated ammonium hydroxide (27.5 - 29 weight percent aqueous). The clear solution was stirred at 200 rpm using a magnetically driven stirrer for several minutes. To this solution was added 64.5 g tetraethoxysilane (abbreviated hereinafter as TEOS). Within 2 minutes, the mixture turned completely white and suspended powder was present. The mixture stirred overnight at 200 rpm. The particles were allowed to settle out and were then filtered. The material was calcined with the procedure described in Example 3 above. SEM indicated primary particles 400 - 1400 nm in size. Some particles were aggregated and necked.
- TEOS tetraethoxysilane
- the initial ramp from room temperature was 50 minutes; the cool down was with the power to the furnace off.
- the resulting powder was partitioned into two samples (135 g and 156 g). Each sample was ball milled in a 1-L mill for 2 - 4 hours. The final suspensions were 23 weight percent solids.
- Particle size analyses with a Coulter 4+ instrument indicated mean particle sizes were 664 nm ⁇ 124 nm and 720 ⁇ 178 nm for the two fractions. The fractions were combined for further use.
- Example 10 This example describes a preparation of STS particles using acid catalysts.
- the sample was suction filtered and washed with 3 L of water plus ethanol.
- the dried powder (23.19 g) was added to 1 L of 0.1M HCl in ethanol and allowed to stir at 400 rpm for 67 hours.
- the suspension was filtered and washed with about 100 mL deionized water.
- the material mixed with 53 g deionized water to form an -30 weight percent suspension. This suspension was milled for about 16 hours.
- This example describes the preparation of STS particles using acetone as the cosolvent.
- Ci gTAB 80 g was combined with 57 mL acetone, 69.5 mL deionized water, and 175 mL concentrated hydrochloric acid (38 weight percent aqueous) in a 4-L beaker and agitated with an overhead stirrer. To this was added rapidly 250 mL TMOS. Within 30 seconds, the solution turned opaque and gelled. The final molar weight ratio was 1.00 TMOS : 0.13 C 16 TAB : 6.6 water : 0.46 acetone : 1.3 HCl.
- the sample was washed with 6 L of water plus ethanol.
- the solution was added to 1.5 L of 0.1M HCl in ethanol and allowed to sit overnight.
- the suspension was filtered and washed with about 300 mL deionized water.
- the material was dried at 150 °C and then mixed with 230 g deionized water to form an -30 weight percent suspension. This suspension was milled for about 3 days. The final pH ofthe suspension was about 1.9.
- the mean particle size as measured with light scattering on a Coulter N4+ is 792 ⁇ 75 nm.
- XRD indicated one very weak peak at about 3.5 nm, indicating a mesoporous material.
- This example describes the preparation of STS particles using acetone as the cosolvent.
- the sample was washed with -2 L water.
- the powder was added to 1.00 L of 0.1M HCl in ethanol and stirred with an overhead stirrer for 1.5 hours.
- the material was dried at 150 °C and then mixed with 348 g deionized water to form an -25 weight percent suspension. This suspension was milled for about 10 hours in a ball mill with a 1-L total capacity.
- the particle size range was 1 - 2 ⁇ m.
- X-ray diffraction indicated one very weak peak at about 3.5 nm, indicating a mesoporous material.
- Example 13 This example describes a preparation of STS particles using TEOS.
- the sample was suction filtered, stirred with -1 L deionized water for 45 minutes, and filtered again.
- the powder was added to 1.00 L of 0.1M HCl in ethanol in a 2-L capacity round-bottom flask and magnetically stirred for 6 hours.
- the material was dried at 150 °C and then 23.3 g was mixed with 69.9 g deionized water to form an -25 weight percent suspension. This suspension was milled for about 13 hours in a ball mill with a 1- L total capacity.
- the sample was quite foamy; 3 mL of ethanol was added to defoam the sample.
- the particle size range was 1 - 6 ⁇ m. Particles were spherical and ellipsoidal. XRD indicated one peak at about 3.58 nm, indicative of a mesoporous material.
- compositions A through C Composition A: A mixture of 75 parts STS powder, 25 parts binder (on a solids basis) and 200 parts water (including water from the binder resin).
- Composition B A mixture of 10 parts aluminum sulfate octadecahydrate and 90 parts water.
- Composition C A mixture of 75 parts STS powder, 20 parts RHOPLEX B-60A (on a solids basis), 5 parts RHOPLEX AC-1230M (on a solids basis), and 300 parts water (including water from the binder resin). Examples 14(a) - 14(c)
- Hewlett-Packard Design Jet 2500CP inkjet printer available from Hewlett-Packard Corp., Palo Alto, CA, using cartridge numbers C1892A, C 1893 A, C1894A, and/or C 1895 A.
- the resulting image exhibited high color density, high gloss, and excellent line sharpness with no bleed or feathering between colors.
- there was no mobility of any color Upon subjecting the image to running water, there was no mobility of any color. Soaking the image in water for 24 hours resulted in no color movement nor any appreciable change in color density.
- Example 14(b) The procedure of Example 14(a) was repeated except that RHOPLEX 2438 was substituted for CARBOSET GA2136. Results were similar in image quality and waterfastness to that of Example 14(a).
- Example 14(a) The procedure of Example 14(a) was repeated except that MAINCOTE HG-54D was substituted for CARBOSET GA2136. Results were similar in image quality and waterfastness to that of Example 14(a).
- Example 14(a) An ink receptive article was prepared according to the procedure of Example 14(a), except that the STS used was prepared according to Example 4, and CARBOSET GA2136 was used as the binder. Results were similar in image quality and waterfastness to that of Example 14(a).
- Example 15(a) The procedure of Example 15(a) was repeated, except that RHOPLEX 2438 was substituted for the CARBOSET GA2136. Results were similar in image quality and waterfastness to that of Example 14(a).
- Example 15(a) The procedure of Example 15(a) was repeated, except that MAINCOTE HG-54D was substituted for the CARBOSET GA2136. Results were similar in image quality and waterfastness to that of Example 14(a).
- This example demonstrates an ink receptive article comprising STS and aluminum sulfate coated onto a polyethylene/PET spunbond substrate.
- Example 14(a) An ink receptive article was prepared according to the procedure of Example 14(a) using STS prepared according to the procedure of Example 1, and CARBOSET GA2136 as the binder. The mixture was coated onto ELEVES T0703WDO spunbond substrate. Results were similar in image quality and waterfastness to that of Example 14(a).
- Example 14(a) An ink receptive article was prepared according to the procedure of Example 14(a) using STS prepared according to the procedure of Example 4, and CARBOSET GA2136 as binder. The mixture was coated onto ELEVES T0703WDO spunbond substrate. Results were similar in image quality and waterfastness to that of Example 14(a).
- Example 18 demonstrate ink receptive articles comprising STS and aluminum sulfate coated onto a polyester film substrate.
- An ink receptive article was prepared according to the procedure of Example 14(a) using STS from Example 3, and CARBOSET GA2136 as binder. Results were similar in image quality and waterfastness to that of Example 14(a).
- the procedure of Example 17(a) was repeated with the addition of 1 weight percent ZONYL FSO surfactant to the STS/binder coating solution. Results were similar in image quality and waterfastness to that of Example 14(a).
- Example 18
- Examples 19(a) - 19(d demonstrate ink receptive articles comprising STS and aluminum sulfate coated onto a polyolefin film substrate.
- Example 14(a) An ink receptive article was prepared according to the procedure of Example 14(a) using STS prepared according to Example 9 with RHOPLEX 2438 binder coated onto a polyolefin film as described in Example 5 of U.S. Patent No. 5,721,086 (Emslander et al.). Results were similar in image quality and waterfastness to that of Example 14(a).
- Example 19(b) The procedure of Example 19(a) was repeated except that a 50/50 blend of MAINCOTE HG-54D/ RHOPLEX 2438 was substituted as binder.
- the resultant ink receptive article when imaged had comparable image quality and improved scratch resistance.
- Example 19(a) The procedure of Example 19(a) was repeated except that RHOPLEX AC- 1230M was substituted as binder.
- the resultant ink receptive article when imaged had comparable image quality and improved scratch resistance.
- Example 19(d) The procedure of Example 19(a) was repeated except that an 80/20 blend of RHOPLEX B-60A/RHOPLEX AC-1230M was substituted as binder.
- the resultant ink receptive article when imaged had comparable image quality and improved scratch resistance.
- Examples 20(a) - 20(c) demonstrate ink receptive articles comprising STS coated onto a polyolefin film substrate.
- Example 20(b) The same procedure as in Example 20(a) except using zeolite type Ca-A (ADNERA 403) as the silica was performed. This material was then printed with UV inks as described in Example 14(a). The resulting image exhibited ink flooding, bleed/feathering between colors and lower color density than that of
- Example 20(a) The same procedure as in Example 20(a) except using zeolite type ⁇ a-A (ADNERA 40 IP) as the silica was performed. This material was then printed as described in Example 14(a). The resulting image exhibited ink flooding, bleed/feathering between colors, lower color density than that of Example 20(a).
- Examples 21 - 24 describe various embodiments of acid-catalyzed STS ink receptive articles without aluminum sulfate
- Example 21 These examples demonstrate ink receptive articles comprising STS with a cationic binder coated onto a polyester substrate.
- the synthesis ofthe cationic latex polymer used in this example is as follows.
- a reaction vessel was fitted with a condenser, a thermometer, a dropping funnel, a mechanical stirrer, and a nitrogen purging system.
- To this vessel was added 393 parts of deionized water, 5 parts of cetyl(trimethyl)ammonium chloride (as a 25 percent solution in water), and 0.4 parts of V-50.
- V-50 is the trade designation for 2,2'-azobis(2- amidinopropane) dihydrochloride, (CAS # 2997-92-4) used by Wako Chemicals USA, Inc., Richmond, VA. The solution was left to stir at 300 rpm.
- Example 14(a) This material was then printed as in Example 14(a).
- the resulting image exhibited high color density, excellent line sharpness with no bleed or feathering in the primary colors, and waterfastness.
- Example 22(b) The same materials as in Example 22(a) was printed using ENCAD NOVAJET PRO printer using Encad Graphic Standard inks (part nos. 206832 cyan dye ink,
- Example 24 The same materials as in Example 23(a) was printed as in Example 22(b). The resulting image exhibited high color density, excellent line sharpness with no bleed or feathering between colors, and waterfastness.
- Example 24 The same materials as in Example 23(a) was printed as in Example 22(b). The resulting image exhibited high color density, excellent line sharpness with no bleed or feathering between colors, and waterfastness.
- This example describes the synthesis of aggregated transparent STS particles.
- Example 26 This example describes the synthesis of aggregated transparent STS particles using
- N-(trimethoxysilylpropyl)isothiouronium chloride abbreviated hereinafter as TIP.
- TMOS was added (that is, 20 seconds after gelation), 1.15 g TIP (50 percent in water) was added to the slightly turbid solution.
- the turbidity ofthe solution remained essentially constant for greater than 1 month, and the solution is assumed to be indefinitely stable.
- Particle size analysis performed 1 month after synthesis indicated a bimodal distribution with most of the particles tightly grouped between
- This example demonstrates the effect of catalyst concentration on transparent STS particle pore size.
- Examples 27(a) through 27(d) gelled to form a white opaque material within 3 seconds after the addition of TMOS;
- Example 27(e) formed a milky white solution, and
- Example 27 (f) formed a slightly turbid solution.
- XRD revealed that Examples 27(a) through 27(d) provided at least three well defined Bragg peaks, with the primary peak at 3.1 - 3.3 nm, indicating a hexagonal lattice of 1-d tubes within each particle.
- Example 27(e) gave a less well defined pattern.
- Example 27(f) clearly showed a weak Bragg peak at about 4.7 nm, which indicated the channel sizes were larger in this material than in Examples 27(a) through 27(d).
- This example describes the synthesis of aggregated transparent STS particles using an acidic ethanol extraction.
- 0.8 g C1 gTAB 6.90 g deionized water, 2.90 g methanol, and 0.040 mL concentrated ammonium hydroxide (29 percent aqueous) to form an alkaline micellar solution.
- TMOS Trimethyl methoxysulfoxide
- To this mixture was added 0.625 mL TMOS with vigorous stirring (1000 rpm). About 2.5 minutes after the TMOS was added (that is, 20 seconds after gelation), 1.15 g TIP (50 percent in water) was added to the slightly turbid solution. The solution gelled overnight. About 4 g ofthe gel was suspended in 127 mL absolute ethanol.
- Example 29 This example describes the synthesis of aggregated transparent STS particles using tetramethylammonium hydroxide (hereinafter referred to as TMAOH).
- TMAOH tetramethylammonium hydroxide
- This example describes the synthesis of aggregated transparent STS particles using tetrabutylammonium hydroxide (hereinafter referred to as TBAOH).
- TBAOH tetrabutylammonium hydroxide
- Example 30(a) turned opaque white after 17 seconds;
- Example 30(b) turned opaque white after 8 seconds; samples turned milky white/opalescent after 15 seconds;
- Example 30(c) turned slightly turbid after 35 seconds.
- Final solution pH varied from 10 - 11 for Examples 30(a) and 30(b) to about 6.1, for Example 30(d).
- Example 30(b) 2.45 2.03
- Example 30(c) 2.45 0.41
- Example 30(d) 2.45 0.082
- This example describes the acid-catalyzed synthesis of aggregated transparent STS particles. Examples were prepared with four different acidic catalysts: hydrochloric acid, acetic acid, sulfuric acid, and phosphoric acid. The general synthetic procedure was as follows:
- the final pH was about 1.6.
- the solution containing acetic acid remained highly transmissive, with no signs of precipitates for greater than 1 month.
- XRD revealed a pattern similar to a cubic, bicontinuous liquid crystalline phase with primary peaks at 40, 3.57, 3.12 and 1.79 nm, in addition to 5 more peaks between 3.0 and 5.5° two-theta and an envelope between 7 and 10° two-theta on a diffractometer equipped with a Cu anode.
- Field emission SEM revealed mostly sub-50 nm particles with a few faceted hexagons (-85 nm on a side).
- TEM revealed -20 nm particles containing regular 2 - 3 nm features (pores) within each particle.
- This example describes the effect of acetic acid concentration on solution stability of transparent STS particles.
- Example 32(a) was cloudy prior to the addition of TMOS, but that after the TMOS was added, the solution was stable and very transmissive for greater than 1.5 months.
- Example 32(b) solution was very slightly turbid after addition of TMOS; after 1.5 months a weak gel formed, but the material was still highly transmissive.
- Examples 32(c) and 32(d) were totally transparent solutions for up to 3 hours; over the course of 1.5 months, the solutions gelled and formed translucent, but still transmissive gels.
- a colloidal suspension was prepared as in Example 31 with acetic acid, but with a scale factor of 10 times.
- the final molar weight ratios were 1.00 TMOS : 0.13 C ⁇ gTAB : 60.6 water : 9.07 acetic acid : 18.1 methanol.
- TEOS 8.6 mL
- ethanol 31 mL
- the mixture was shaken by hand for about 1 minute to form a colloidal suspension of STS particles.
- the final molar weight ratios were 1.00 TEOS : 0.141 CjgTAB : 66.2 water : 10.5 acetic acid :
- This example describes a preparation of STS particles.
- This example describes a preparation of STS particles from a more concentrated synthetic mixture.
- Ci gTAB (0.40 g) was combined with 2.80 mL methanol, 3.50 g deionized water, and 3.50 mL concentrated hydrochloric acid in a 20-mL scintillation vial. To this clear solution was added 1.25 mL TMOS. Within 3 minutes, the solution turned from transparent to opaque gray. The sample was allowed to sit quiescent overnight. The following day, the materials was suction filtered and washed with water and ethanol. The final molar weight ratio was 1.00 TMOS : 0.13 CigTAB : 40 water : 8.1 methanol : 5.4 hydrochloric acid. This solution was approximately 7.9 weight percent silica plus surfactant.
- the dried particles were analyzed with SEM, which revealed 2 - 5 ⁇ m spheres and ellipsoids.
- This example describes a preparation of STS particles using glycerol as the cosolvent.
- Ci gTAB (0.20 g) was combined with 3.10 mL glycerol, 3.80 g deionized water, and 3.50 mL concentrated hydrochloric acid in a 20-mL scintillation vial. To this clear solution was added 0.625 mL TMOS. Within a few seconds, the solution turned from transparent to opaque gray. The sample was allowed to sit quiescent overnight. The following day, the materials were suction filtered and washed with water and ethanol. The dried particles were analyzed with SEM, which revealed aggregated 0.5 - 2 ⁇ m particles. The final molar weight ratio was 1.00 TMOS : 0.13 C ⁇ TAB : 85 water : 18 methanol : 10.5 hydrochloric acid.
- the mean particle size was about 1 ⁇ m with a range of sizes from 0.5 to 2 ⁇ m. Particles were strongly aggregated and had ill-defined shapes.
- This example describes the preparation of STS particles using tetraethoxysilane as the silica source.
- the range of particle sizes was about 3 ⁇ m to 5 ⁇ m. Particles were ellipsoidal and many were intergrown to form doublets.
- This example describes the preparation of STS particles using a synthetic mixture highly concentrated in reagents.
- the solution turned opaque in about 15 seconds.
- the final molar weight ratio was 1.00 TMOS : 0.142 CigTAB : 92.6 water : 19.8 methanol : 11.5 hydrochloric acid.
- Particle size ranged from ⁇ 1 ⁇ m to about 2 ⁇ m.
- This example describes the preparation of STS particles using various glycerol/water molar weight ratios.
- Example 41 This example describes the preparation of STS particles using a glycerol/acetone mixture as the cosolvent.
- Example 42 This example describes the synthesis of templated silica particles using a block copolymer.
- Example 43 The process described above in Example 43 was used to prepare a sample 40 times larger than above.
- the sample was treated hydrothermally (with no prior filtration) at 80 °C for 30 hours.
- the sample was suction filtered, dried in air overnight, and then dried at 100 °C for -24 hours.
- the sample was calcined as above.
- Example 42 The procedure described in Example 42 was used to prepare samples with PLURONIC F77, P85, F98, P103, and P104 surfactants. All ofthe calcined samples exhibited one X-ray diffraction peak with a d spacing between 6.5 and 8.5 nm, indicating periodic porous materials.
- the sample made using PLURONIC F77 surfactant had smooth 1 - 5 ⁇ m spheres and ellipsoids that had very little necking.
- the sample made using PLURONIC P85 surfactant provided particles ranging from irregularly shaped aggregated chunks of less than 1 ⁇ m to rough particles of 6 ⁇ m in size. The above particles have surface textures on the scale of about 50-150 nm.
- the sample made using PLURONIC F77, P85, F98, P103, and P104 surfactants All ofthe calcined samples exhibited one X-ray diffraction peak with a d spacing between 6.5 and 8.5 nm, indicating periodic porous materials
- PLURONIC F98 surfactant provided smooth pieces of 100-200 ⁇ m in size. These pieces have a surface texture on a scale of less than 100 nm.
- the samples made using PLURONIC PI 03 surfactant provided smooth, bent, worm-like particles about 1-2 ⁇ m long by about 0.5 ⁇ m wide.
- the sample made using PLURONIC P104 surfactant provided a significant fraction of particles similar to those made using PLURONIC PI 03 surfactant as well as fused and faceted particles.
- the sample made using PLURONIC P123 surfactant provided faceted, unbent tubules or about 1-1.5 ⁇ m long and about 0.2-0.3 ⁇ m wide.
- This example describes the preparation of large pore STS by templating with ethoxylated fatty amines.
- ETHOMEEN 18/25 (lg) was combined with deionized water (26 g), concentrated hydrochloric acid (5.75 g), and tetraethoxysilane (2.1 g). The mixture was allowed to react at about 35 °C for 20 hours after which time it was placed in an 80 °C oven for 4 hours and then removed. The samples were suction filtered, dried at room temperature, and calcined at 550 °C. The same procedure was carried out concurrently but with 1 g ETHOMEEN. X-ray diffraction revealed 1 Bragg peak at -3.5 nm for the ETHOMEEN 18/25 sample and one peak at -4.0 nm for the ETHOMEEN 18/60 sample.
- Example 47 Both preparations in Example 45 were scaled using ten times the reagents. X-ray diffraction indicated one Bragg peak at 3.9 nm for the ETHOMEEN 18/25 sample and one peak at ⁇ 4.1nm for the ETHOMEEN 18/60 sample.
- Example 47
- This example describes the preparation of transparent STS nanoparticles with expanded pore sizes.
- Ci ⁇ TAB (0.20g), deionized water (4.6 g), glacial acetic acid (2.3 mL), toluene (0.68 mL), and TMOS (0.63 mL) were combined in a 20 mL scintillation vial.
- a transparent sol of STS nanoparticle resulted.
- the sol was aged for 4 days.
- X-ray diffraction indicated Bragg peaks at 4.1 and 3.7 nm, which is consistent with a cubic mesophase that has been swollen by toluene.
- a second sample was prepared identically to the first except that 0.25 mL toluene was used. X-ray diffraction results were identical to those with 0.68 mL toluene.
- This example describes the preparation of surfactant-templated alumina.
- the samples were than suction filtered through filter paper, dried at room temperature for about 2 hours and then calcined at 550 °C for 6 hours.
- X-ray diffraction revealed one Bragg peak at 14.0 nm for the sample reacted at room temperature and at 13.5 nm for the sample reacted at 35 °C.
Abstract
Description
Claims
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1999
- 1999-05-18 US US09/314,794 patent/US6096469A/en not_active Expired - Lifetime
- 1999-09-29 WO PCT/US1999/022505 patent/WO2000069647A1/en not_active Application Discontinuation
- 1999-09-29 EP EP99956497A patent/EP1187724A1/en not_active Withdrawn
- 1999-09-29 JP JP2000618087A patent/JP2002544023A/en not_active Withdrawn
- 1999-09-29 AU AU13095/00A patent/AU1309500A/en not_active Abandoned
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EP1187724A1 (en) | 2002-03-20 |
WO2000069647A1 (en) | 2000-11-23 |
JP2002544023A (en) | 2002-12-24 |
AU1309500A (en) | 2000-12-05 |
US6096469A (en) | 2000-08-01 |
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