TWI744263B - 疏水性矽石粉末、製備彼之方法及用於電子照像之包含彼的調色劑組成物 - Google Patents
疏水性矽石粉末、製備彼之方法及用於電子照像之包含彼的調色劑組成物 Download PDFInfo
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- TWI744263B TWI744263B TW105140266A TW105140266A TWI744263B TW I744263 B TWI744263 B TW I744263B TW 105140266 A TW105140266 A TW 105140266A TW 105140266 A TW105140266 A TW 105140266A TW I744263 B TWI744263 B TW I744263B
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- Prior art keywords
- silica powder
- hydrophobic silica
- water
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- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 title claims abstract description 179
- 239000000377 silicon dioxide Substances 0.000 title claims abstract description 81
- 239000000843 powder Substances 0.000 title claims abstract description 66
- 230000002209 hydrophobic effect Effects 0.000 title claims abstract description 44
- 239000000203 mixture Substances 0.000 title claims description 26
- 238000004519 manufacturing process Methods 0.000 title description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 30
- 239000011164 primary particle Substances 0.000 claims abstract description 11
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 7
- -1 polydimethylsiloxane Polymers 0.000 claims description 33
- 238000000034 method Methods 0.000 claims description 26
- 238000001035 drying Methods 0.000 claims description 17
- 239000003795 chemical substances by application Substances 0.000 claims description 15
- 239000006185 dispersion Substances 0.000 claims description 15
- 230000032683 aging Effects 0.000 claims description 9
- 239000010453 quartz Substances 0.000 claims description 6
- 239000002253 acid Substances 0.000 claims description 5
- 239000008119 colloidal silica Substances 0.000 claims description 5
- 239000004205 dimethyl polysiloxane Substances 0.000 claims description 4
- 229920000435 poly(dimethylsiloxane) Polymers 0.000 claims description 4
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 3
- 239000000126 substance Substances 0.000 claims description 3
- 238000002834 transmittance Methods 0.000 claims description 3
- 239000003513 alkali Substances 0.000 claims description 2
- 150000001343 alkyl silanes Chemical group 0.000 claims description 2
- 235000019353 potassium silicate Nutrition 0.000 claims description 2
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 claims description 2
- 238000005507 spraying Methods 0.000 claims description 2
- 230000007613 environmental effect Effects 0.000 abstract description 8
- 230000003068 static effect Effects 0.000 abstract 1
- 239000002245 particle Substances 0.000 description 16
- 229920001296 polysiloxane Polymers 0.000 description 15
- 239000011347 resin Substances 0.000 description 12
- 229920005989 resin Polymers 0.000 description 12
- 238000000227 grinding Methods 0.000 description 7
- 238000006243 chemical reaction Methods 0.000 description 6
- PPBRXRYQALVLMV-UHFFFAOYSA-N Styrene Chemical compound C=CC1=CC=CC=C1 PPBRXRYQALVLMV-UHFFFAOYSA-N 0.000 description 5
- 239000000654 additive Substances 0.000 description 5
- IISBACLAFKSPIT-UHFFFAOYSA-N bisphenol A Chemical compound C=1C=C(O)C=CC=1C(C)(C)C1=CC=C(O)C=C1 IISBACLAFKSPIT-UHFFFAOYSA-N 0.000 description 5
- 238000006116 polymerization reaction Methods 0.000 description 5
- 125000005372 silanol group Chemical group 0.000 description 5
- SJECZPVISLOESU-UHFFFAOYSA-N 3-trimethoxysilylpropan-1-amine Chemical compound CO[Si](OC)(OC)CCCN SJECZPVISLOESU-UHFFFAOYSA-N 0.000 description 4
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 4
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 4
- 238000010521 absorption reaction Methods 0.000 description 4
- 239000011230 binding agent Substances 0.000 description 4
- 239000003086 colorant Substances 0.000 description 4
- 238000010438 heat treatment Methods 0.000 description 4
- 229920001225 polyester resin Polymers 0.000 description 4
- 239000004645 polyester resin Substances 0.000 description 4
- 150000005846 sugar alcohols Polymers 0.000 description 4
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 3
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 3
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 description 3
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- OFOBLEOULBTSOW-UHFFFAOYSA-N Propanedioic acid Natural products OC(=O)CC(O)=O OFOBLEOULBTSOW-UHFFFAOYSA-N 0.000 description 3
- KDYFGRWQOYBRFD-UHFFFAOYSA-N Succinic acid Natural products OC(=O)CCC(O)=O KDYFGRWQOYBRFD-UHFFFAOYSA-N 0.000 description 3
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 3
- 235000013870 dimethyl polysiloxane Nutrition 0.000 description 3
- 125000000524 functional group Chemical group 0.000 description 3
- 239000007789 gas Substances 0.000 description 3
- 239000002609 medium Substances 0.000 description 3
- 238000002156 mixing Methods 0.000 description 3
- 239000000178 monomer Substances 0.000 description 3
- 229920000728 polyester Polymers 0.000 description 3
- 229920001451 polypropylene glycol Polymers 0.000 description 3
- 150000007519 polyprotic acids Polymers 0.000 description 3
- 229920005792 styrene-acrylic resin Polymers 0.000 description 3
- ARCGXLSVLAOJQL-UHFFFAOYSA-N trimellitic acid Chemical compound OC(=O)C1=CC=C(C(O)=O)C(C(O)=O)=C1 ARCGXLSVLAOJQL-UHFFFAOYSA-N 0.000 description 3
- 229910000859 α-Fe Inorganic materials 0.000 description 3
- WYTZZXDRDKSJID-UHFFFAOYSA-N (3-aminopropyl)triethoxysilane Chemical compound CCO[Si](OCC)(OCC)CCCN WYTZZXDRDKSJID-UHFFFAOYSA-N 0.000 description 2
- DTCCVIYSGXONHU-CJHDCQNGSA-N (z)-2-(2-phenylethenyl)but-2-enedioic acid Chemical compound OC(=O)\C=C(C(O)=O)\C=CC1=CC=CC=C1 DTCCVIYSGXONHU-CJHDCQNGSA-N 0.000 description 2
- ARXKVVRQIIOZGF-UHFFFAOYSA-N 1,2,4-butanetriol Chemical compound OCCC(O)CO ARXKVVRQIIOZGF-UHFFFAOYSA-N 0.000 description 2
- NIXOWILDQLNWCW-UHFFFAOYSA-M Acrylate Chemical compound [O-]C(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-M 0.000 description 2
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- VZCYOOQTPOCHFL-OWOJBTEDSA-N Fumaric acid Chemical compound OC(=O)\C=C\C(O)=O VZCYOOQTPOCHFL-OWOJBTEDSA-N 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 2
- 239000004698 Polyethylene Substances 0.000 description 2
- 239000006087 Silane Coupling Agent Substances 0.000 description 2
- 229920007962 Styrene Methyl Methacrylate Polymers 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- KKEYFWRCBNTPAC-UHFFFAOYSA-N Terephthalic acid Chemical compound OC(=O)C1=CC=C(C(O)=O)C=C1 KKEYFWRCBNTPAC-UHFFFAOYSA-N 0.000 description 2
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 2
- WNLRTRBMVRJNCN-UHFFFAOYSA-N adipic acid Chemical compound OC(=O)CCCCC(O)=O WNLRTRBMVRJNCN-UHFFFAOYSA-N 0.000 description 2
- 238000004220 aggregation Methods 0.000 description 2
- 230000002776 aggregation Effects 0.000 description 2
- 239000003570 air Substances 0.000 description 2
- 125000000217 alkyl group Chemical group 0.000 description 2
- 150000008064 anhydrides Chemical class 0.000 description 2
- 239000012298 atmosphere Substances 0.000 description 2
- WERYXYBDKMZEQL-UHFFFAOYSA-N butane-1,4-diol Chemical compound OCCCCO WERYXYBDKMZEQL-UHFFFAOYSA-N 0.000 description 2
- DFYKHEXCUQCPEB-UHFFFAOYSA-N butyl 2-methylprop-2-enoate;styrene Chemical compound C=CC1=CC=CC=C1.CCCCOC(=O)C(C)=C DFYKHEXCUQCPEB-UHFFFAOYSA-N 0.000 description 2
- TUZBYYLVVXPEMA-UHFFFAOYSA-N butyl prop-2-enoate;styrene Chemical compound C=CC1=CC=CC=C1.CCCCOC(=O)C=C TUZBYYLVVXPEMA-UHFFFAOYSA-N 0.000 description 2
- SXPLZNMUBFBFIA-UHFFFAOYSA-N butyl(trimethoxy)silane Chemical compound CCCC[Si](OC)(OC)OC SXPLZNMUBFBFIA-UHFFFAOYSA-N 0.000 description 2
- 150000001768 cations Chemical class 0.000 description 2
- DCFKHNIGBAHNSS-UHFFFAOYSA-N chloro(triethyl)silane Chemical compound CC[Si](Cl)(CC)CC DCFKHNIGBAHNSS-UHFFFAOYSA-N 0.000 description 2
- IJOOHPMOJXWVHK-UHFFFAOYSA-N chlorotrimethylsilane Chemical compound C[Si](C)(C)Cl IJOOHPMOJXWVHK-UHFFFAOYSA-N 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 229920001577 copolymer Polymers 0.000 description 2
- 239000008367 deionised water Substances 0.000 description 2
- 229910021641 deionized water Inorganic materials 0.000 description 2
- 230000006866 deterioration Effects 0.000 description 2
- FWDBOZPQNFPOLF-UHFFFAOYSA-N ethenyl(triethoxy)silane Chemical compound CCO[Si](OCC)(OCC)C=C FWDBOZPQNFPOLF-UHFFFAOYSA-N 0.000 description 2
- QBKVWLAQSQPTNL-UHFFFAOYSA-N ethyl 2-methylprop-2-enoate;styrene Chemical compound CCOC(=O)C(C)=C.C=CC1=CC=CC=C1 QBKVWLAQSQPTNL-UHFFFAOYSA-N 0.000 description 2
- RRUSYLYDWCIAGO-UHFFFAOYSA-N ethyl prop-2-enoate;styrene Chemical compound CCOC(=O)C=C.C=CC1=CC=CC=C1 RRUSYLYDWCIAGO-UHFFFAOYSA-N 0.000 description 2
- 239000012065 filter cake Substances 0.000 description 2
- 238000001914 filtration Methods 0.000 description 2
- FFUAGWLWBBFQJT-UHFFFAOYSA-N hexamethyldisilazane Chemical compound C[Si](C)(C)N[Si](C)(C)C FFUAGWLWBBFQJT-UHFFFAOYSA-N 0.000 description 2
- 239000001257 hydrogen Substances 0.000 description 2
- 229910052739 hydrogen Inorganic materials 0.000 description 2
- 229910052742 iron Inorganic materials 0.000 description 2
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N iron oxide Inorganic materials [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 description 2
- QQVIHTHCMHWDBS-UHFFFAOYSA-N isophthalic acid Chemical compound OC(=O)C1=CC=CC(C(O)=O)=C1 QQVIHTHCMHWDBS-UHFFFAOYSA-N 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 150000002739 metals Chemical class 0.000 description 2
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 2
- ADFPJHOAARPYLP-UHFFFAOYSA-N methyl 2-methylprop-2-enoate;styrene Chemical compound COC(=O)C(C)=C.C=CC1=CC=CC=C1 ADFPJHOAARPYLP-UHFFFAOYSA-N 0.000 description 2
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 2
- QZUJCEPTAIXZFA-UHFFFAOYSA-N methyl prop-2-enoate;styrene Chemical compound COC(=O)C=C.C=CC1=CC=CC=C1 QZUJCEPTAIXZFA-UHFFFAOYSA-N 0.000 description 2
- KBJFYLLAMSZSOG-UHFFFAOYSA-N n-(3-trimethoxysilylpropyl)aniline Chemical compound CO[Si](OC)(OC)CCCNC1=CC=CC=C1 KBJFYLLAMSZSOG-UHFFFAOYSA-N 0.000 description 2
- 229910052757 nitrogen Inorganic materials 0.000 description 2
- 239000012299 nitrogen atmosphere Substances 0.000 description 2
- BDJRBEYXGGNYIS-UHFFFAOYSA-N nonanedioic acid Chemical compound OC(=O)CCCCCCCC(O)=O BDJRBEYXGGNYIS-UHFFFAOYSA-N 0.000 description 2
- SLYCYWCVSGPDFR-UHFFFAOYSA-N octadecyltrimethoxysilane Chemical compound CCCCCCCCCCCCCCCCCC[Si](OC)(OC)OC SLYCYWCVSGPDFR-UHFFFAOYSA-N 0.000 description 2
- XNGIFLGASWRNHJ-UHFFFAOYSA-N phthalic acid Chemical compound OC(=O)C1=CC=CC=C1C(O)=O XNGIFLGASWRNHJ-UHFFFAOYSA-N 0.000 description 2
- 229920000573 polyethylene Polymers 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 238000007639 printing Methods 0.000 description 2
- CXMXRPHRNRROMY-UHFFFAOYSA-N sebacic acid Chemical compound OC(=O)CCCCCCCCC(O)=O CXMXRPHRNRROMY-UHFFFAOYSA-N 0.000 description 2
- 238000003980 solgel method Methods 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- 125000003944 tolyl group Chemical group 0.000 description 2
- VZCYOOQTPOCHFL-UHFFFAOYSA-N trans-butenedioic acid Natural products OC(=O)C=CC(O)=O VZCYOOQTPOCHFL-UHFFFAOYSA-N 0.000 description 2
- NBXZNTLFQLUFES-UHFFFAOYSA-N triethoxy(propyl)silane Chemical compound CCC[Si](OCC)(OCC)OCC NBXZNTLFQLUFES-UHFFFAOYSA-N 0.000 description 2
- HQYALQRYBUJWDH-UHFFFAOYSA-N trimethoxy(propyl)silane Chemical compound CCC[Si](OC)(OC)OC HQYALQRYBUJWDH-UHFFFAOYSA-N 0.000 description 2
- DQZNLOXENNXVAD-UHFFFAOYSA-N trimethoxy-[2-(7-oxabicyclo[4.1.0]heptan-4-yl)ethyl]silane Chemical compound C1C(CC[Si](OC)(OC)OC)CCC2OC21 DQZNLOXENNXVAD-UHFFFAOYSA-N 0.000 description 2
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 description 2
- 229920002554 vinyl polymer Polymers 0.000 description 2
- DNIAPMSPPWPWGF-VKHMYHEASA-N (+)-propylene glycol Chemical compound C[C@H](O)CO DNIAPMSPPWPWGF-VKHMYHEASA-N 0.000 description 1
- XVOUMQNXTGKGMA-OWOJBTEDSA-N (E)-glutaconic acid Chemical compound OC(=O)C\C=C\C(O)=O XVOUMQNXTGKGMA-OWOJBTEDSA-N 0.000 description 1
- DNIAPMSPPWPWGF-GSVOUGTGSA-N (R)-(-)-Propylene glycol Chemical compound C[C@@H](O)CO DNIAPMSPPWPWGF-GSVOUGTGSA-N 0.000 description 1
- YQJPWWLJDNCSCN-UHFFFAOYSA-N 1,3-diphenyltetramethyldisiloxane Chemical compound C=1C=CC=CC=1[Si](C)(C)O[Si](C)(C)C1=CC=CC=C1 YQJPWWLJDNCSCN-UHFFFAOYSA-N 0.000 description 1
- YPFDHNVEDLHUCE-UHFFFAOYSA-N 1,3-propanediol Substances OCCCO YPFDHNVEDLHUCE-UHFFFAOYSA-N 0.000 description 1
- BNIWGIJIGJJEKG-UHFFFAOYSA-N 1-[dibutyl-(tributylsilylamino)silyl]butane Chemical compound CCCC[Si](CCCC)(CCCC)N[Si](CCCC)(CCCC)CCCC BNIWGIJIGJJEKG-UHFFFAOYSA-N 0.000 description 1
- NSSFZNLWTXERTH-UHFFFAOYSA-N 1-[dipropyl-(tripropylsilylamino)silyl]propane Chemical compound CCC[Si](CCC)(CCC)N[Si](CCC)(CCC)CCC NSSFZNLWTXERTH-UHFFFAOYSA-N 0.000 description 1
- KTZVZZJJVJQZHV-UHFFFAOYSA-N 1-chloro-4-ethenylbenzene Chemical compound ClC1=CC=C(C=C)C=C1 KTZVZZJJVJQZHV-UHFFFAOYSA-N 0.000 description 1
- NKELEQZBIMMAPC-UHFFFAOYSA-N 1-chloro-4-ethenylbenzene;styrene Chemical compound C=CC1=CC=CC=C1.ClC1=CC=C(C=C)C=C1 NKELEQZBIMMAPC-UHFFFAOYSA-N 0.000 description 1
- GGFMVTNGEQRGIO-UHFFFAOYSA-N 1-ethenyl-2-methylbenzene;styrene Chemical compound C=CC1=CC=CC=C1.CC1=CC=CC=C1C=C GGFMVTNGEQRGIO-UHFFFAOYSA-N 0.000 description 1
- DPNGUUBTOATYSA-UHFFFAOYSA-N 1-ethenylnaphthalene;styrene Chemical compound C=CC1=CC=CC=C1.C1=CC=C2C(C=C)=CC=CC2=C1 DPNGUUBTOATYSA-UHFFFAOYSA-N 0.000 description 1
- AHEAPQJDMSHYKL-UHFFFAOYSA-N 1H-indene 5-phenylpenta-2,4-dienenitrile Chemical compound C1=CC=C2CC=CC2=C1.N#CC=CC=CC1=CC=CC=C1 AHEAPQJDMSHYKL-UHFFFAOYSA-N 0.000 description 1
- VSIKJPJINIDELZ-UHFFFAOYSA-N 2,2,4,4,6,6,8,8-octakis-phenyl-1,3,5,7,2,4,6,8-tetraoxatetrasilocane Chemical compound O1[Si](C=2C=CC=CC=2)(C=2C=CC=CC=2)O[Si](C=2C=CC=CC=2)(C=2C=CC=CC=2)O[Si](C=2C=CC=CC=2)(C=2C=CC=CC=2)O[Si]1(C=1C=CC=CC=1)C1=CC=CC=C1 VSIKJPJINIDELZ-UHFFFAOYSA-N 0.000 description 1
- FIADVASZMLCQIF-UHFFFAOYSA-N 2,2,4,4,6,6,8,8-octamethyl-1,3,5,7,2,4,6,8-tetrazatetrasilocane Chemical compound C[Si]1(C)N[Si](C)(C)N[Si](C)(C)N[Si](C)(C)N1 FIADVASZMLCQIF-UHFFFAOYSA-N 0.000 description 1
- VCYDUTCMKSROID-UHFFFAOYSA-N 2,2,4,4,6,6-hexakis-phenyl-1,3,5,2,4,6-trioxatrisilinane Chemical compound O1[Si](C=2C=CC=CC=2)(C=2C=CC=CC=2)O[Si](C=2C=CC=CC=2)(C=2C=CC=CC=2)O[Si]1(C=1C=CC=CC=1)C1=CC=CC=C1 VCYDUTCMKSROID-UHFFFAOYSA-N 0.000 description 1
- WGGNJZRNHUJNEM-UHFFFAOYSA-N 2,2,4,4,6,6-hexamethyl-1,3,5,2,4,6-triazatrisilinane Chemical compound C[Si]1(C)N[Si](C)(C)N[Si](C)(C)N1 WGGNJZRNHUJNEM-UHFFFAOYSA-N 0.000 description 1
- ZAKUVHZFBNPFNP-UHFFFAOYSA-N 2,2,4,4,6-pentamethyl-1,3,5,7,2,4,6,8-tetraoxatetrasilocane Chemical compound C[SiH]1O[SiH2]O[Si](C)(C)O[Si](C)(C)O1 ZAKUVHZFBNPFNP-UHFFFAOYSA-N 0.000 description 1
- DCWFTTYGOKYOOE-UHFFFAOYSA-N 2,4,6,8,10-pentamethyl-2,4,6,8,10-pentakis(3,3,3-trifluoropropyl)-1,3,5,7,9,2,4,6,8,10-pentaoxapentasilecane Chemical compound FC(F)(F)CC[Si]1(C)O[Si](C)(CCC(F)(F)F)O[Si](C)(CCC(F)(F)F)O[Si](C)(CCC(F)(F)F)O[Si](C)(CCC(F)(F)F)O1 DCWFTTYGOKYOOE-UHFFFAOYSA-N 0.000 description 1
- VMAWODUEPLAHOE-UHFFFAOYSA-N 2,4,6,8-tetrakis(ethenyl)-2,4,6,8-tetramethyl-1,3,5,7,2,4,6,8-tetraoxatetrasilocane Chemical compound C=C[Si]1(C)O[Si](C)(C=C)O[Si](C)(C=C)O[Si](C)(C=C)O1 VMAWODUEPLAHOE-UHFFFAOYSA-N 0.000 description 1
- WZJUBBHODHNQPW-UHFFFAOYSA-N 2,4,6,8-tetramethyl-1,3,5,7,2$l^{3},4$l^{3},6$l^{3},8$l^{3}-tetraoxatetrasilocane Chemical compound C[Si]1O[Si](C)O[Si](C)O[Si](C)O1 WZJUBBHODHNQPW-UHFFFAOYSA-N 0.000 description 1
- XOVNCWWRDSAYNE-UHFFFAOYSA-N 2,4,6,8-tetramethyl-2,4,6,8-tetrakis(3,3,3-trifluoropropyl)-1,3,5,7,2,4,6,8-tetraoxatetrasilocane Chemical compound FC(F)(F)CC[Si]1(C)O[Si](C)(CCC(F)(F)F)O[Si](C)(CCC(F)(F)F)O[Si](C)(CCC(F)(F)F)O1 XOVNCWWRDSAYNE-UHFFFAOYSA-N 0.000 description 1
- IRVZFACCNZRHSJ-UHFFFAOYSA-N 2,4,6,8-tetramethyl-2,4,6,8-tetraphenyl-1,3,5,7,2,4,6,8-tetraoxatetrasilocane Chemical compound O1[Si](C)(C=2C=CC=CC=2)O[Si](C)(C=2C=CC=CC=2)O[Si](C)(C=2C=CC=CC=2)O[Si]1(C)C1=CC=CC=C1 IRVZFACCNZRHSJ-UHFFFAOYSA-N 0.000 description 1
- JAHNSTQSQJOJLO-UHFFFAOYSA-N 2-(3-fluorophenyl)-1h-imidazole Chemical compound FC1=CC=CC(C=2NC=CN=2)=C1 JAHNSTQSQJOJLO-UHFFFAOYSA-N 0.000 description 1
- WSFYPFLCEFLXOZ-UHFFFAOYSA-N 2-decylbutanedioic acid Chemical compound CCCCCCCCCCC(C(O)=O)CC(O)=O WSFYPFLCEFLXOZ-UHFFFAOYSA-N 0.000 description 1
- QDCPNGVVOWVKJG-UHFFFAOYSA-N 2-dodec-1-enylbutanedioic acid Chemical compound CCCCCCCCCCC=CC(C(O)=O)CC(O)=O QDCPNGVVOWVKJG-UHFFFAOYSA-N 0.000 description 1
- RKOGJKGQMPZCGG-UHFFFAOYSA-N 2-methoxypropane-1,3-diol Chemical compound COC(CO)CO RKOGJKGQMPZCGG-UHFFFAOYSA-N 0.000 description 1
- ROGIWVXWXZRRMZ-UHFFFAOYSA-N 2-methylbuta-1,3-diene;styrene Chemical compound CC(=C)C=C.C=CC1=CC=CC=C1 ROGIWVXWXZRRMZ-UHFFFAOYSA-N 0.000 description 1
- XYHGSPUTABMVOC-UHFFFAOYSA-N 2-methylbutane-1,2,4-triol Chemical compound OCC(O)(C)CCO XYHGSPUTABMVOC-UHFFFAOYSA-N 0.000 description 1
- HXLAEGYMDGUSBD-UHFFFAOYSA-N 3-[diethoxy(methyl)silyl]propan-1-amine Chemical compound CCO[Si](C)(OCC)CCCN HXLAEGYMDGUSBD-UHFFFAOYSA-N 0.000 description 1
- UNVFWCQQWZUPLB-UHFFFAOYSA-N 3-[dimethoxy(pentan-3-yloxy)silyl]propan-1-amine Chemical compound CCC(CC)O[Si](OC)(OC)CCCN UNVFWCQQWZUPLB-UHFFFAOYSA-N 0.000 description 1
- OFNSCVFOGRGCLA-UHFFFAOYSA-N 3-[heptadecan-9-yloxy(dimethoxy)silyl]propan-1-amine Chemical compound CCCCCCCCC(O[Si](CCCN)(OC)OC)CCCCCCCC OFNSCVFOGRGCLA-UHFFFAOYSA-N 0.000 description 1
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Abstract
本發明關於前所未有之對環境濕度不敏感的疏水性矽石粉末，使用該疏水性矽石粉末之電子照像調色劑可具有導致穩定印刷影像品質之穩定靜電電荷。
該疏水性矽石粉末具有下列物理化學性質：- 平均一次粒徑(D)為30至2000nm，- B*D<430nm，其中B代表當在25℃水分壓比水的平衡蒸氣壓為80%時在矽石(100重量%)上的吸附水蒸氣之重量%，而D代表該矽石粉末之平均一次粒徑(nm)，- B/C<2.7，其中C代表當在25℃水分壓比水的平衡蒸氣壓為20%時在矽石(100重量%)上的吸附水蒸氣之重量%，且- 碳含量>0.30重量%。
Description
本發明關於疏水性矽石、其製備方法，及在調色劑中之用途。
利用電子照像技術之辦公室自動化設備，諸如影印機、雷射印表機等，係藉由電子照像顯影器形成影像。雙組分系統之一般電子照像顯影器使用包含有色細微樹脂粉末及載劑之調色劑。該載劑係由磁性或非磁性粒子製成，用以帶電並攜帶該調色劑。該調色劑及該載劑係在顯影機中攪拌並彼此混合，並因相互摩擦而帶電。已藉由曝光所形成之靜電潛像係利用該帶電來顯影。
因該調色劑呈細微粉末形式，其粉末特性諸如流性及帶電特性亦重要，以使其可在電子照像程序中充分發揮作用。由於慣用類型之調色劑的粒度為10μm或更大，其被當作僅為碎粒來處理。因當前類型之調色劑呈粒度介於5與8μm之更細微粉末形式而達成大幅改善之印刷品質。該調色劑需要各種外部添加劑。
由於調色劑係由摩擦靜電電荷(tribo-electrostatic
charge)控制，該電荷必須在各種不同環境條件下均安定。使用調色劑之環境通常為相對濕度約20%之低濕度環境至相對濕度為80%或更高之高濕度環境。該電荷係藉由該調色劑樹脂及外部添加劑中整合的電荷控制劑來控制。尤其是，外部添加劑扮演關鍵角色。
多年來慣常一般使用之外部添加劑為金屬氧化物粒子，諸如表面改質之矽石及藉由乾燥程序所製造的氧化鈦，原因係彼等顯示低聚集傾向並且容易均勻分散在調色劑表面(JP S58-132757 A、JP S59-034539 A、JP H10-312089 A)。
JP 2002-108001 A提出將藉由所謂溶膠-凝膠法所製造之細微矽石粉末添加至調色劑粒子。雖然該等方法能在適當環境條件下確保提供優異印刷影像，但該細微矽石粉末之表面性質因留在該表面上的矽烷醇基而易於吸濕。該矽烷醇基吸收濕氣，其為調色劑在高濕度環境下靜電荷變差因而使印刷影像變差的原因。
本發明目的係提供前所未有對之對環境濕度不敏感的矽石粉末。其有利於在調色劑中形成極優越外部添加劑。
上述目的係藉由在下述說明、實施例及申請專利範圍中更詳細界定之矽石粉末達成。
因此，本發明關於疏水性矽石粉末，其特徵為下列物理化學性質：
- 以TEM測定之平均一次粒徑(D)為30至2000nm，較佳為40至1000nm，特佳為50至400nm，最佳為50至200nm，- B*D<430nm，較佳為<375nm，特佳係介於65與350nm，其中B代表當在25℃水分壓比水的平衡蒸氣壓為80%時在矽石(100重量%)上的吸附水蒸氣之重量%，而D代表該矽石粉末之平均一次粒徑(以nm計)，- B/C<2.7，較佳為<2.5，特佳係介於1.0與2.4，其中C代表當在25℃水分壓比水的平衡蒸氣壓為20%時在矽石(100重量%)上的吸附水蒸氣之重量%，且- 碳含量>0.30重量%，較佳為>0.40重量%，特佳係介於0.50重量%與5.00重量%。
本發明之疏水性矽石粉末的原粒子之縱橫比可為1.0至1.5，較佳為1.0至1.3，特佳為1.0至1.2。本發明之疏水性矽石的疏水性可高於50%，較佳為高於55%，特佳為高於63%。本發明之疏水性矽石的pH值係介於2.5至9.5，較佳為3.5至8.5，尤佳為4.5至8.0。本發明之疏水性矽石可為粉末。本發明之疏水性矽石可為膠態矽石。
本發明之疏水性矽石粉末前所未有地對環境濕度不敏感，使用該疏水性矽石粉末之調色劑可具有導致穩定印刷影像品質之穩定靜電電荷。
本發明另外關於本發明之疏水性矽石的製備方法a.製備矽石分散液，b.乾燥步驟a之分散液以獲得親水性矽石粉末，
c.在介於100與170℃之溫度，步驟b之親水性矽石粉末的老化處理，且步驟c之溫度高於步驟b之溫度，d.疏水化步驟c之矽石粉末。
步驟a之矽石分散液為單分散膠態矽石分散液。該單分散膠態矽石分散液藉由使用烷氧基矽烷(習知為溶膠-凝膠法或Stöber法(Werner Stöber、Arthur Fink、Ernst Bohn,Controlled growth of monodisperse silica spheres in the micron size range,Journal of Colloid and Interface Science，第26卷，第62至69頁(1968)))，或藉由膠態法使用鹼水玻璃與酸(Ralph K.Iler,The Chemistry of Silica,Wiley,New York，第331至337頁，(1979))獲得。該酸可為例如氫氯酸或硫酸。該等單分散膠態矽石分散液一般已知，且可作為在水及/或有機溶劑中之分散液購得。得自Evonik Industries AG之現有水性分散液為例如IDISILTM EM13530P、EM7530P或EM5530P。
該矽石分散液可藉由一般已知方法在步驟b中，諸如藉由乾燥烘箱、旋轉蒸發器、槳葉式乾燥機、冷凍乾燥機、流體化床乾燥機、及噴霧乾燥機乾燥。該分散液較佳係在步驟b之前藉由陽離子交換劑去離子化，以獲得pH值為2.2至3.8，較佳為2.4至3.5，特佳為2.5至3.2。除了上述直接乾燥法之外，矽石粉末亦可乾燥藉由使用壓濾機之來自分散液的濾餅而獲得。可添加任何已知用劑以加強過濾之前的沉澱、膠凝或聚集。可應用任何已知工具以乾燥該濾餅。應注意的是，乾燥程序b中之環境溫度必須
維持低於在稍後老化步驟c中之溫度。步驟b中之乾燥較佳可在低於150℃之溫度，較佳為低於130℃，特佳為-30℃至100℃進行。步驟b中之乾燥較佳可在冷凍乾燥機、常壓下之乾燥烘箱或減壓下之旋轉蒸發器中進行。步驟b中之矽石可乾燥至該矽石中的濕氣少於5.0重量%，較佳為少於3.0重量%為止。
步驟b之經乾燥矽石在疏水化之前經歷老化程序(步驟c)，且在表面上之矽烷醇基的數目在控制下減少。尤其是，鄰近的矽烷醇基縮合而將此等矽烷醇基留在幾何學上分離之表面上。步驟c可在受控制溫度及濕氣下，在有或無任何觸媒的情況下完成。其係在100℃至170℃之溫度，較佳為110℃至160℃進行。稍後的老化步驟c中之溫度可比乾燥步驟b之溫度高至少10℃，較佳為至少30℃，更佳為至少50℃，特佳為至少70℃。步驟c中之矽石可老化直到矽石中之濕氣為<2.0%，較佳為<1.5%為止。步驟c之老化程序可在周圍空氣或惰性氣體(諸如氮或氬)之下進行。
雖然無特別限制，但用於步驟d以獲得根據本發明之疏水性矽石的疏水劑可為矽氮烷、環狀有機矽氧烷、聚矽氧油及矽烷偶合劑。
矽氮烷包括六甲基二矽氮烷(HMDS)、六乙基二矽氮烷、四甲基二矽氮烷、六丁基二矽氮烷、六丙基二矽氮烷、六戊基二矽氮烷、六甲基環三矽氮烷、1,3-二乙烯基四甲基二矽氮烷、八甲基環四矽氮烷及二乙烯基四甲基二
矽氮烷。
環狀有機矽氧烷包括六苯基環三矽氧烷、八苯基環四矽氧烷、四乙烯基四甲基環四矽氧烷、六甲基環三矽氧烷、八甲基環四矽氧烷、五甲基環四矽氧烷、四甲基環四矽氧烷、八甲基環四矽氧烷、十甲基環五矽氧烷、十二甲基環六矽氧烷、四甲基四氫環四矽氧烷、四甲基四苯基環四矽氧烷、四甲基四(三氟丙基)環四矽氧烷及五甲基五(三氟丙基)環五矽氧烷。
聚矽氧油包括從低黏度至高黏度之有機聚矽氧烷等，諸如二甲基聚矽氧烷、甲苯基聚矽氧烷、甲基氫聚矽氧烷、甲基三甲基氫聚矽氧烷(methyltrimethicone)、甲基矽氧烷/甲苯基矽氧烷之共聚物。此外，亦可使用高聚合度之似橡膠二甲基聚矽氧烷、較高碳烷氧基改質之聚矽氧(諸如硬脂氧基聚矽氧等)、較高碳脂肪酸改質之聚矽氧、烷基改質之聚矽氧、胺基改質之聚矽氧、氟改質之聚矽氧等。亦可能使用在一端或兩端具有反應性官能基之有機聚矽氧烷。以下式(1)表示之有機聚矽氧烷適合使用：Xa-(SiR2O)n-SiR2-Xb (1)該式中之基團R可與由甲基或乙基組成的烷基相同或不同，其一部分由含有包括乙烯基、苯基及胺基之官能基中之一者的烷基取代，基團Xa及Xb可相同或不同且為包括鹵素原子、羥基、烷氧基之反應性官能基。n為顯示矽氧烷鍵聯之聚合度的整數，且係介於1與1000。
矽烷偶合劑包括例如1,3-二乙烯基四甲基二矽氧烷、
1,3-二苯基四甲基二矽氧烷、3-胺丙基三甲氧基矽烷、3-胺丙基甲基二乙氧基矽烷、異丁基三乙氧基矽烷異丁基三甲氧基矽烷、異丙基三乙氧基矽烷、異丙基三甲氧基矽烷、N-β(胺乙基)γ-胺丙基三甲氧基矽烷、N-β(胺乙基)γ-胺丙基甲基二甲氧基矽烷、正十八基三甲氧基矽烷、N-苯基-γ-胺丙基三甲氧基矽烷、正丁基三甲氧基矽烷、正丙基三乙氧基矽烷、正丙基三甲氧基矽烷、正十六基三甲氧基矽烷、鄰甲基苯基三甲氧基矽烷、對甲基苯基三甲氧基矽烷、第三丁基二甲基氯矽烷、a-氯乙基三氯矽烷、β-(3,4-環氧基環己基)乙基三甲氧基矽烷、β-(3,4-環氧基環己基)乙基三甲氧基矽烷、β-氯乙基三氯矽烷、β-(2-胺乙基)胺丙基三甲氧基矽烷、γ-(2-胺乙基)胺丙基甲基二甲氧基矽烷、γ-苯胺基丙基三甲氧基矽烷、γ-胺丙基三乙氧基矽烷、γ-胺丙基三甲氧基矽烷、γ-環氧丙氧基丙基三甲氧基矽烷、γ-環氧丙氧基丙基甲基二乙氧基矽烷、γ-環氧丙氧基丙基甲基二甲氧基矽烷、γ-氯丙基三甲氧基矽烷、γ-氯丙基甲基二甲氧基矽烷、γ-甲基丙烯氧基丙基三甲氧基矽烷、γ-疏基丙基三甲氧基矽烷、胺丙基三乙氧基矽烷、胺丙基三甲氧基矽烷、烯丙基二甲基氯矽烷、烯丙基三乙氧基矽烷、烯丙基苯基二氯矽烷、異丁基三甲氧基矽烷、乙基三乙氧基矽烷、乙基三氯矽烷、乙基三甲氧基矽烷、十八基三乙氧基矽烷、十八基三甲氧基矽烷、辛基三甲氧基矽烷、氯甲基二甲基氯矽烷、二乙基胺丙基三甲氧基矽烷、二乙基二乙氧基矽烷、二乙基二甲氧基矽烷、二辛基
胺丙基三甲氧基矽烷、二苯基二乙氧基矽烷、二苯基二氯矽烷、二苯基二甲氧基矽烷、二丁基胺丙基二甲氧基矽烷、二丁基胺丙基三甲氧基矽烷、二丁基胺丙基二甲氧基矽烷、二丙基胺丙基三甲氧基矽烷、二己基二乙氧基矽烷、二己基二甲氧基矽烷、二甲胺基苯基三乙氧基矽烷、二甲基乙氧基矽烷、二甲基二乙氧基矽烷、二甲基二氯矽烷、二甲基二甲氧基矽烷、癸基三乙氧基矽烷、癸基三甲氧基矽烷、十二基三甲氧基矽烷、三乙基乙氧基矽烷、三乙基氯矽烷、三乙基甲氧基矽烷、三有機矽基丙烯酸酯、三丙基乙氧基矽烷、三丙基氯矽烷、三丙基甲氧基矽烷、三己基乙氧基矽烷、三己基氯矽烷、三甲基乙氧基矽烷、三甲基氯矽烷、三甲基矽烷、三甲基矽基硫醇、三甲基甲氧基矽烷、三甲氧基矽基-γ-丙基苯基胺、三甲氧基矽基-γ-苯基苯甲基胺、萘基三乙氧基矽烷、萘基三甲氧基矽烷、壬基三乙氧基矽烷、羥丙基三甲氧基矽烷、乙烯基二甲基乙醯氧基矽烷、乙烯基三乙醯氧基矽烷、乙烯基三乙氧基矽烷、乙烯基三氯矽烷、乙烯基參(β-甲氧基乙氧基)矽烷、乙烯基三甲氧基矽烷、苯基三乙氧基矽烷、苯基三氯矽烷、苯基三甲氧基矽烷、丁基三乙氧基矽烷、丁基三甲氧基矽烷、丙基三乙氧基矽烷、丙基三甲氧基矽烷、溴甲基二甲基氯矽烷、六甲基二矽氧烷、己基三甲氧基矽烷、苯甲基二甲基氯矽烷、戊基三甲氧基矽烷、氯化甲基丙烯氧基乙基二甲基(3-三甲氧基矽基丙基)銨、甲基三乙氧基矽烷、甲基三氯矽烷、甲基三甲氧基矽烷、甲苯基二
甲氧基矽烷及一丁基胺丙基三甲氧基矽烷。該等疏水劑可獨立使用或與另一或其他的用劑組合使用。
步驟c之親水性矽石粉末的疏水化可以眾所周知的方法進行。當考慮乾式方法時，可將疏水劑噴淋至矽石上或當藉由流動氣體攪拌或流體化時以蒸氣形式引入反應容器。在濕式方法中，步驟c之矽石可分散於溶劑(如甲苯)中，然後在添加疏水劑之後加熱或視需要加熱至回流。或其可在餾除溶劑之後於高溫下進一步加熱。當使用二或多種疏水劑時疏水化方法亦無限制，因此彼等可同時或依序反應。
步驟d之疏水化較佳可藉由將疏水劑噴淋在步驟c之矽石上進行。疏水劑較佳可為烷基矽烷、聚二甲基矽氧烷或矽氮烷，特佳為庚基三甲氧基矽烷或六甲基矽氮烷。
若必要，本發明之矽石可在任何時候，諸如在乾燥(步驟b)、老化處理(步驟c)、或疏水化(步驟d)之後，經歷任何研磨程序。亦可進行超過一次。特佳為包含噴射磨機之研磨系統，其特徵在於該研磨系統中之磨機係在研磨階段中用選自由氣體及/或蒸氣(較佳為蒸汽)及/或包含蒸汽之氣體所組成的群組之操作介質操作；以及研磨室係在加熱階段，即，在用該操作介質實際操作之前加熱，以使該研磨室中及/或在磨機出口之溫度高於蒸汽及/或操作介質的露點。
本發明另外關於包含本發明疏水性矽石粉末之調色劑組成物。根據本發明之調色劑組成物可藉由使用攪拌器，
諸如Henschel混合機，混合有色粒子與本發明疏水性矽石粉末而獲得。
有色粒子可含有黏合劑樹脂及著色劑。其製造方法不受特殊限制，但通常例如以粉碎法(將著色劑熔融至作為黏合劑樹脂組分之熱塑性樹脂中並混合成均勻分散液以形成組成物，然後將該組成物粉碎並分級以獲得有色粒子的方法)，或以聚合法(著色劑係熔融或分散至作為黏合劑樹脂之原材料的可聚合單體中，然後在添加聚合引發劑之後懸浮於含有分散安定劑之水系分散介質中，並將該懸浮液加熱至預定溫度以引發聚合作用，在完成聚合之後藉由過濾、清洗、脫水及乾燥獲得有色粒子的方法)來製造。
黏合劑樹脂包括已廣泛用於調色劑一段時日的樹脂，諸如例如苯乙烯之聚合物及其取代產物，諸如聚苯乙烯、聚對氯苯乙烯及聚乙烯基甲苯；苯乙烯共聚物，諸如苯乙烯-對氯苯乙烯、苯乙烯-丙烯、苯乙烯-乙烯基甲苯、苯乙烯-乙烯基萘、苯乙烯-丙烯酸甲酯、苯乙烯-丙烯酸乙酯、苯乙烯-丙烯酸丁酯、苯乙烯-丙烯酸辛酯、苯乙烯-甲基丙烯酸甲酯、苯乙烯-甲基丙烯酸乙酯、苯乙烯-甲基丙烯酸丁酯、苯乙烯-α-氯甲基丙烯酸甲酯、苯乙烯-丙烯腈、苯乙烯-乙烯基甲醚、苯乙烯-乙烯基乙醚、苯乙烯-乙烯基甲基酮、苯乙烯-丁二烯、苯乙烯-異戊二烯、苯乙烯-丙烯腈-茚、苯乙烯-順丁烯二酸及苯乙烯-順丁烯二酸酯；聚甲基丙烯酸甲酯；聚氯乙烯；聚乙酸乙烯酯；聚乙烯；聚丙烯；聚酯；聚胺甲酸酯；聚醯胺；環氧樹脂；聚乙烯丁
醛；聚丙烯酸系樹脂；松脂；經改質松脂；萜樹脂；酚樹脂；脂族樹脂或脂環烴樹脂；以及芳族石油樹脂。其可獨立或以混合物形式使用。在不違背本發明目的的情況下另外還可將眾所周知的脫模劑、抗靜電劑等添加至所述樹脂。
每一種包括碳黑及鈦白之顏料及/或染料均可用作包含在該有色粒子中的著色劑。該有色粒子可含有任何磁性材料。此處所使用之材料包括鐵氧化物，諸如磁鐵礦、γ-氧化鐵、鐵氧磁體(ferrite)及鐵過量之鐵氧磁體；金屬，諸如鐵、鈷及鎳；或所述金屬與諸如下列金屬之合金及其混合物：鋁、銅、鎂、錫、鋅、鈣、鈦、鎢或釩。根據本發明之每一種調色劑組成物可依原樣，換言之，以單一組分調色劑形式使用。其亦可與載劑混合作為所謂雙組分調色劑。
在電子照像法中，需要調色劑可藉由與帶電物品摩擦而瞬間充電，及調色劑電荷在諸如溫度及濕度之環境條件下長時間安定。一般而言，調色劑材料可含有苯乙烯-丙烯酸系或聚酯樹脂。
苯乙烯-丙烯酸系樹脂為苯乙烯與丙烯酸酯及/或甲基丙烯酸酯之共聚物，且包括例如苯乙烯-丙烯酸甲酯、苯乙烯-丙烯酸乙酯、苯乙烯-丙烯酸丁酯、苯乙烯-丙烯酸辛酯、苯乙烯-甲基丙烯酸甲酯、苯乙烯-甲基丙烯酸乙酯或苯乙烯-甲基丙烯酸丁酯。
聚酯樹脂係由多元醇及多元酸組成，且係藉由聚合視
需要其中至少多元醇或多元酸含有三價或多價組分(交聯組分)的單體組成物而獲得。該等聚酯樹脂可藉由任何普通方法合成。特別是，反應條件可根據所使用之單體的反應選擇，諸如反應溫度(170至250℃)及反應壓力(5mmHg至常壓)，及可於達到指定性質時停止。
用於合成聚酯樹脂之二元醇包括例如乙二醇、三乙二醇、1,2-丙二醇、1,3-丙二醇、1,4-丁二醇、新戊二醇、1,4-丁烯二醇、1,4-雙(羥甲基)環己烷、雙酚A、氫化雙酚A、聚氧乙烯雙酚A、聚氧丙烯(2,2)-2,2’-雙(4-羥苯基)丙烷、聚氧丙烯(3,3)-2,2-雙(4-羥苯基)丙烷、聚氧乙烯(2,2)-2,2-雙(4-羥苯基)丙烷或聚氧丙烯(2,2)-2,2’-雙(4-羥苯基)丙烷。
交聯聚酯中所涉及的三元或多元醇包括例如多元醇、1,2,3,6-己四醇(1,2,3,6-hexanetetrole)、1,4-去水山梨醇、新戊四醇、二新戊四醇、三新戊四醇、蔗糖、1,2,4-丁三醇、1,2,5-戊三醇、甘油、2-甲基丙三醇、2-甲基-1,2,4-丁三醇、三羥甲基乙烷、三羥甲基丙烷或1,3,5-三羥甲基苯。
多元酸包括例如順丁烯二酸、反丁烯二酸、檸康酸、伊康酸、戊烯二酸、酞酸、異酞酸、對酞酸、環己二羧酸、丁二酸、己二酸、癸二酸、壬二酸、丙二酸、烯基丁二酸(諸如正十二烯基丁二酸及正癸基丁二酸)、烷基丁二酸、其他二價有機酸及酐或所述酸之較低碳烷酯。
交聯聚酯所涉及之三價或多價多元酸包括例如1,2,4-
苯三羧酸、1,2,5-苯三羧酸、1,2,4-環己烷三羧酸、2,5,7-萘三羧酸、1,2,4-萘三羧酸、1,2,5-己三羧酸、1,3-二羧基-2-甲基-2-亞甲基羥基丙烷、四(亞甲基羧基)甲烷、1,2,7,8-辛烷四羧酸及前述者之酐。
本發明疏水性矽石之優點係對環境濕度不敏感。
平均一次粒徑係如下計算。藉由分析放大倍率為100,000倍之穿透式電子顯微鏡所獲得的影像，針對超過1,000個隨機選自矽石粉末的粒子測量每一次粒子之長及短軸。長軸及短軸之總粒徑除以(2*粒子數目)以求得平均一次粒徑。縱橫比係由(長軸總和)/(短軸總和)獲得。
表面經改質之疏水性矽石粉末的濕氣吸收量係使用BELSOROP-max於25℃測定。每一樣本係在低於10帕壓力下於150℃加熱3小時以消除所吸收之濕氣作為前置處理。水蒸氣吸收量係在在水蒸氣壓力相對於水平衡蒸氣壓力分別為20%(C)及80%(B)下於25℃測量。
將2g調色劑樣本及48g鐵氧磁體載劑置入玻璃容器(75ml)並且分別在HH環境及在LL環境下靜置24小時。此處之HH環境意指溫度為40℃且相對濕度為85%之氣
氛，而LL環境意指溫度為20℃且相對濕度為20%之氣氛。在所述環境貯存24小時之後，分別藉由TURBULA®搖動機-混合機搖動混合物5分鐘。然後，取0.2g該混合物並使用吹洩電荷測量裝置TB-200(Toshiba Chemical)以空氣吹拂1分鐘來獲得在各HH及LL環境中之調色劑組成物的電荷量。
首先，秤重1g疏水性矽石粉末並置於200ml分液漏斗中，及添加100ml純水。在將蓋放置其上之後，藉由turbular混合機(turbular mixer)搖動該混合物10分鐘。然後該混合物靜置10分鐘。從該漏斗廢棄20至30ml其渾濁下層。將一部分所得之水層分裝至10mm石英槽，然後將該石英槽置入比色計中。疏水性(%)係測量為500nm之波長的透光率(%)。
實施例及對照實例中之經疏水化矽石粉末的碳含量係藉由ISO3262-19測量。
用磁性攪拌器將4g親水性矽石粉末分散於100g去離子水中。以pH計測量該分散液之pH值。
用磁性攪拌器將4g疏水性矽石粉末分散在50g甲醇與50g去離子水之混合物中。以pH計測量該分散液之pH值。
在秤重瓶中秤重1g矽石粉末並在無蓋的乾燥室中105℃加熱兩小時。在加熱之後，用蓋封閉該瓶並貯存於乾燥器中以冷卻至20℃。秤量該矽石粉末之重量。將該粉末之失重除以該樣本的初始重量以測定濕氣含量。
下文，藉由參考實施例及對照實例更明確描述本發明。
市售水性分散液IDISILTM EM13530P、EM7530P或EM5530P(Evonik Industries AG)係藉由陽離子交換器(Lewatit® S 108 H，購自Lanxess AG)去離子，以獲得2.5至3.0之pH值。之後，該分散液係以液態氮冷凍且在第一乾燥步驟中在室溫於0.2mbar之壓力下以Christ Alpha 2-4 LDplus冷凍乾燥機冷凍乾燥超過10小時。就第二乾燥步驟而言，將壓力降至0.05mbar至少2小時以產生親水性矽石粉末。
該粉末於乾燥烘箱中在表1所提之溫度下經歷老化處
理1小時。
在反應容器中，添加100重量份之來自步驟c的老化矽石。該粉末係藉由混合而流體化。如表1所示之氮氣氛下將所述重量份之疏水劑噴淋在該粉末上。該反應混合物係在氮氣氛下於所列溫度及時間流體化。將所得之混合物冷卻以產生疏水性矽石粉末。
使用由藉由研磨方法所製造之平均粒徑為8μm的帶負電苯乙烯-丙烯酸系樹脂所組成的雙組分調色劑粉末。將調色劑粉末及表2之各疏水性矽石粉末混合在一起至具
有以下式所計算的比：矽石(重量份)=矽石粉末之平均一次粒徑(nm)/40
將上述混合物添加至Henschel型混合機(Super Mixer Piccolo SMP-2,Kawata MFG Co.,Ltd.製)，然後在600rpm攪拌1分鐘，然後在3,000rpm攪拌3分鐘，獲得調色劑組成物。
該調色劑組成物之摩擦靜電電荷係在HH及LL條件下測量。結果示於表2。就任何試樣而言，在LL條件下之電荷的絕對值始終較大。其電荷量之比較小意指調色劑組成物在各種不同環境下更為安定。
在表2中，本發明疏水性矽石粉末顯示較低LL/HH比，其造成經改良之對環境濕度的不敏感性。
Claims (12)
- 一種疏水性矽石粉末，其具有下列物理化學性質：- 平均一次粒徑(D)為30至2000nm，- B*D介於65與430，其中B代表當在25℃水分壓比水的平衡蒸氣壓為80%時在矽石(100重量%)上的吸附水蒸氣之重量%，而D代表該矽石粉末之平均一次粒徑(nm)，- B/C介於1.0與2.7，其中C代表當在25℃水分壓比水的平衡蒸氣壓為20%時在矽石(100重量%)上的吸附水蒸氣之重量%，且- 介於0.30與5.00重量%之碳含量。
- 如申請專利範圍第1項之疏水性矽石粉末，其中，如藉由下述方法所測得，其疏水性高於50%：首先，秤重1g疏水性矽石粉末並置於200ml分液漏斗中，及添加100ml純水；在將蓋放置其上之後，藉由turbular混合機(turbular mixer)搖動該混合物10分鐘；然後該混合物靜置10分鐘；從該漏斗廢棄20至30ml之其渾濁下層；將一部分所得之水層分裝至10mm石英槽，然後將該石英槽置入比色計中；以及疏水性(%)係測量為500nm之波長的透光率(%)。
- 如申請專利範圍第1或2項之疏水性矽石粉末，其中，其為膠態矽石粉末。
- 如申請專利範圍第1或2項之疏水性矽石粉末，其中，縱橫比為1.0至1.5。
- 如申請專利範圍第1項之疏水性矽石粉末，其中，如藉由下述方法所測得，疏水性高於55%：首先，秤重1g疏水性矽石粉末並置於200ml分液漏斗中，及添加100ml純水；在將蓋放置其上之後，藉由turbular混合機(turbular mixer)搖動該混合物10分鐘；然後該混合物靜置10分鐘；從該漏斗廢棄20至30ml之其渾濁下層；將一部分所得之水層分裝至10mm石英槽，然後將該石英槽置入比色計中；以及疏水性(%)係測量為500nm之波長的透光率(%)。
- 一種如申請專利範圍第1至5項中任一項之疏水性矽石粉末之製備方法，特徵在於其包含下列步驟：a.製備矽石分散液，b.乾燥步驟a之分散液以獲得親水性矽石粉末，c.在介於100與170℃之溫度，老化處理步驟b之該親水性矽石粉末，且步驟c之溫度高於步驟b之溫度，以及d.疏水化在步驟c中所獲得之該親水性矽石粉末。
- 如申請專利範圍第6項之疏水性矽石粉末之製備方法，其中，步驟a中之該矽石分散液係藉由反應烷氧基矽烷或鹼水玻璃與酸而製備。
- 如申請專利範圍第6或7項之疏水性矽石粉末之製備方法，其中，步驟b之該乾燥係在冷凍乾燥機中進行。
- 如申請專利範圍第6或7項之疏水性矽石粉末之製備方法，其中，步驟c之該老化處理係在乾燥烘箱中進 行。
- 如申請專利範圍第6或7項之疏水性矽石粉末之製備方法，其中，步驟d之該疏水化係藉由將疏水劑噴淋於在步驟c中所獲得之該親水性矽石粉末上來進行。
- 如申請專利範圍第10項之疏水性矽石粉末之製備方法，其中，該疏水劑為烷基矽烷、聚二甲基矽氧烷或矽氮烷。
- 一種用於電子照像之調色劑組成物，其含有至少一種如申請專利範圍第1至5項中任一項之疏水性矽石粉末。
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| JPH04340972A (ja) * | 1991-05-17 | 1992-11-27 | Minolta Camera Co Ltd | 静電荷像現像用トナー |
| US5989768A (en) * | 1997-03-06 | 1999-11-23 | Cabot Corporation | Charge-modified metal oxides with cyclic silazane and electrostatographic systems incorporating same |
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| JP3891265B2 (ja) * | 2001-11-30 | 2007-03-14 | 信越化学工業株式会社 | 疎水性シリカ微粉末及びその製造方法 |
| JP3983234B2 (ja) * | 2004-08-16 | 2007-09-26 | 電気化学工業株式会社 | トナー外添材の製造方法 |
| JP4347201B2 (ja) * | 2004-11-30 | 2009-10-21 | 信越化学工業株式会社 | 静電荷像現像用トナー外添剤およびトナー |
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