CN100513303C - dispersoid and antihunt means thereof method, silicon dioxide and modification method, recording medium and surface coat - Google Patents
dispersoid and antihunt means thereof method, silicon dioxide and modification method, recording medium and surface coat Download PDFInfo
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- CN100513303C CN100513303C CNB2004800048471A CN200480004847A CN100513303C CN 100513303 C CN100513303 C CN 100513303C CN B2004800048471 A CNB2004800048471 A CN B2004800048471A CN 200480004847 A CN200480004847 A CN 200480004847A CN 100513303 C CN100513303 C CN 100513303C
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- Prior art keywords
- dioxide
- silicon
- boron
- weight
- dispersion
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- 238000000034 method Methods 0.000 title claims abstract description 42
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 title claims description 299
- 239000000377 silicon dioxide Substances 0.000 title claims description 148
- 235000012239 silicon dioxide Nutrition 0.000 title claims description 134
- 238000002715 modification method Methods 0.000 title 1
- 239000006185 dispersion Substances 0.000 claims abstract description 69
- 229960001866 silicon dioxide Drugs 0.000 claims description 134
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 claims description 82
- 229910052796 boron Inorganic materials 0.000 claims description 82
- 150000001639 boron compounds Chemical class 0.000 claims description 35
- 239000007788 liquid Substances 0.000 claims description 26
- 239000000203 mixture Substances 0.000 claims description 13
- 239000008187 granular material Substances 0.000 claims description 9
- 238000004438 BET method Methods 0.000 claims description 7
- 239000002904 solvent Substances 0.000 claims description 5
- 238000007639 printing Methods 0.000 claims description 4
- 239000007921 spray Substances 0.000 claims description 4
- 238000011068 loading method Methods 0.000 claims description 3
- 238000004381 surface treatment Methods 0.000 claims description 2
- 229910044991 metal oxide Inorganic materials 0.000 abstract description 5
- 150000004706 metal oxides Chemical class 0.000 abstract description 5
- 230000000087 stabilizing effect Effects 0.000 abstract 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 30
- -1 polyoxyethylene Polymers 0.000 description 16
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 description 15
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 15
- 238000006243 chemical reaction Methods 0.000 description 15
- 239000007789 gas Substances 0.000 description 15
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 14
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- 238000002156 mixing Methods 0.000 description 11
- 238000009736 wetting Methods 0.000 description 11
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 10
- IAZDPXIOMUYVGZ-UHFFFAOYSA-N dimethyl sulfoxide Natural products CS(C)=O IAZDPXIOMUYVGZ-UHFFFAOYSA-N 0.000 description 10
- 239000007787 solid Substances 0.000 description 10
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 9
- 239000002253 acid Substances 0.000 description 9
- 229910052500 inorganic mineral Inorganic materials 0.000 description 9
- 239000011707 mineral Substances 0.000 description 9
- 238000000746 purification Methods 0.000 description 9
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 8
- 238000002485 combustion reaction Methods 0.000 description 8
- XBDQKXXYIPTUBI-UHFFFAOYSA-N dimethylselenoniopropionate Natural products CCC(O)=O XBDQKXXYIPTUBI-UHFFFAOYSA-N 0.000 description 8
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 8
- 239000004094 surface-active agent Substances 0.000 description 8
- 239000003513 alkali Substances 0.000 description 7
- 239000001301 oxygen Substances 0.000 description 7
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- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 description 6
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- DNIAPMSPPWPWGF-UHFFFAOYSA-N Propylene glycol Chemical compound CC(O)CO DNIAPMSPPWPWGF-UHFFFAOYSA-N 0.000 description 6
- 229910020175 SiOH Inorganic materials 0.000 description 6
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- 230000000694 effects Effects 0.000 description 6
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 5
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- 125000000217 alkyl group Chemical group 0.000 description 5
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- 125000001495 ethyl group Chemical group [H]C([H])([H])C([H])([H])* 0.000 description 5
- 238000007710 freezing Methods 0.000 description 5
- IXCSERBJSXMMFS-UHFFFAOYSA-N hydrogen chloride Substances Cl.Cl IXCSERBJSXMMFS-UHFFFAOYSA-N 0.000 description 5
- 229910000041 hydrogen chloride Inorganic materials 0.000 description 5
- 238000004519 manufacturing process Methods 0.000 description 5
- VIKNJXKGJWUCNN-XGXHKTLJSA-N norethisterone Chemical compound O=C1CC[C@@H]2[C@H]3CC[C@](C)([C@](CC4)(O)C#C)[C@@H]4[C@@H]3CCC2=C1 VIKNJXKGJWUCNN-XGXHKTLJSA-N 0.000 description 5
- 238000007789 sealing Methods 0.000 description 5
- 238000004062 sedimentation Methods 0.000 description 5
- 230000003019 stabilising effect Effects 0.000 description 5
- WRECIMRULFAWHA-UHFFFAOYSA-N trimethyl borate Chemical compound COB(OC)OC WRECIMRULFAWHA-UHFFFAOYSA-N 0.000 description 5
- LDMOEFOXLIZJOW-UHFFFAOYSA-N 1-dodecanesulfonic acid Chemical compound CCCCCCCCCCCCS(O)(=O)=O LDMOEFOXLIZJOW-UHFFFAOYSA-N 0.000 description 4
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 4
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 4
- SNRUBQQJIBEYMU-UHFFFAOYSA-N Dodecane Natural products CCCCCCCCCCCC SNRUBQQJIBEYMU-UHFFFAOYSA-N 0.000 description 4
- 229920003171 Poly (ethylene oxide) Polymers 0.000 description 4
- 239000004372 Polyvinyl alcohol Substances 0.000 description 4
- GSEJCLTVZPLZKY-UHFFFAOYSA-N Triethanolamine Chemical compound OCCN(CCO)CCO GSEJCLTVZPLZKY-UHFFFAOYSA-N 0.000 description 4
- 229920004890 Triton X-100 Polymers 0.000 description 4
- 239000013543 active substance Substances 0.000 description 4
- 239000000654 additive Substances 0.000 description 4
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 4
- 239000012298 atmosphere Substances 0.000 description 4
- 229910021538 borax Inorganic materials 0.000 description 4
- 125000000484 butyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 4
- 229910052799 carbon Inorganic materials 0.000 description 4
- 239000003093 cationic surfactant Substances 0.000 description 4
- 229960001927 cetylpyridinium chloride Drugs 0.000 description 4
- YMKDRGPMQRFJGP-UHFFFAOYSA-M cetylpyridinium chloride Chemical compound [Cl-].CCCCCCCCCCCCCCCC[N+]1=CC=CC=C1 YMKDRGPMQRFJGP-UHFFFAOYSA-M 0.000 description 4
- 239000003795 chemical substances by application Substances 0.000 description 4
- 125000002704 decyl group Chemical group [H]C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])* 0.000 description 4
- 125000003438 dodecyl group Chemical group [H]C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])* 0.000 description 4
- 239000001257 hydrogen Substances 0.000 description 4
- 229910052739 hydrogen Inorganic materials 0.000 description 4
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 description 4
- 125000000740 n-pentyl group Chemical group [H]C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])* 0.000 description 4
- 230000007935 neutral effect Effects 0.000 description 4
- 150000007524 organic acids Chemical class 0.000 description 4
- 150000007530 organic bases Chemical class 0.000 description 4
- 238000012856 packing Methods 0.000 description 4
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- 239000000843 powder Substances 0.000 description 4
- 235000019260 propionic acid Nutrition 0.000 description 4
- IUVKMZGDUIUOCP-BTNSXGMBSA-N quinbolone Chemical compound O([C@H]1CC[C@H]2[C@H]3[C@@H]([C@]4(C=CC(=O)C=C4CC3)C)CC[C@@]21C)C1=CCCC1 IUVKMZGDUIUOCP-BTNSXGMBSA-N 0.000 description 4
- 239000004328 sodium tetraborate Substances 0.000 description 4
- 235000010339 sodium tetraborate Nutrition 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- FAQYAMRNWDIXMY-UHFFFAOYSA-N trichloroborane Chemical compound ClB(Cl)Cl FAQYAMRNWDIXMY-UHFFFAOYSA-N 0.000 description 4
- 229960004418 trolamine Drugs 0.000 description 4
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 3
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 3
- 238000005054 agglomeration Methods 0.000 description 3
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- 239000002585 base Substances 0.000 description 3
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- 239000002245 particle Substances 0.000 description 3
- 239000000047 product Substances 0.000 description 3
- 238000007086 side reaction Methods 0.000 description 3
- 229910000077 silane Inorganic materials 0.000 description 3
- 238000005507 spraying Methods 0.000 description 3
- 238000003860 storage Methods 0.000 description 3
- PTTPXKJBFFKCEK-UHFFFAOYSA-N 2-Methyl-4-heptanone Chemical compound CC(C)CC(=O)CC(C)C PTTPXKJBFFKCEK-UHFFFAOYSA-N 0.000 description 2
- BTBUEUYNUDRHOZ-UHFFFAOYSA-N Borate Chemical compound [O-]B([O-])[O-] BTBUEUYNUDRHOZ-UHFFFAOYSA-N 0.000 description 2
- XDTMQSROBMDMFD-UHFFFAOYSA-N Cyclohexane Chemical compound C1CCCCC1 XDTMQSROBMDMFD-UHFFFAOYSA-N 0.000 description 2
- IMROMDMJAWUWLK-UHFFFAOYSA-N Ethenol Chemical compound OC=C IMROMDMJAWUWLK-UHFFFAOYSA-N 0.000 description 2
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- 229910004298 SiO 2 Inorganic materials 0.000 description 2
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 description 2
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 2
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 description 2
- 238000013019 agitation Methods 0.000 description 2
- 238000007605 air drying Methods 0.000 description 2
- 150000001335 aliphatic alkanes Chemical class 0.000 description 2
- 239000004411 aluminium Substances 0.000 description 2
- 229910052782 aluminium Inorganic materials 0.000 description 2
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 2
- 150000001408 amides Chemical class 0.000 description 2
- 150000004945 aromatic hydrocarbons Chemical class 0.000 description 2
- 230000005540 biological transmission Effects 0.000 description 2
- 238000003490 calendering Methods 0.000 description 2
- 150000001721 carbon Chemical group 0.000 description 2
- 239000007795 chemical reaction product Substances 0.000 description 2
- 239000011248 coating agent Substances 0.000 description 2
- 238000000576 coating method Methods 0.000 description 2
- 230000008021 deposition Effects 0.000 description 2
- UQGFMSUEHSUPRD-UHFFFAOYSA-N disodium;3,7-dioxido-2,4,6,8,9-pentaoxa-1,3,5,7-tetraborabicyclo[3.3.1]nonane Chemical compound [Na+].[Na+].O1B([O-])OB2OB([O-])OB1O2 UQGFMSUEHSUPRD-UHFFFAOYSA-N 0.000 description 2
- 150000002148 esters Chemical class 0.000 description 2
- 238000001914 filtration Methods 0.000 description 2
- 239000008246 gaseous mixture Substances 0.000 description 2
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- 125000003187 heptyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[H] 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
- 125000004051 hexyl group Chemical group [H]C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])* 0.000 description 2
- 125000001183 hydrocarbyl group Chemical group 0.000 description 2
- 239000011261 inert gas Substances 0.000 description 2
- 125000001972 isopentyl group Chemical group [H]C([H])([H])C([H])(C([H])([H])[H])C([H])([H])C([H])([H])* 0.000 description 2
- 150000002576 ketones Chemical class 0.000 description 2
- 238000010907 mechanical stirring Methods 0.000 description 2
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 2
- 125000003136 n-heptyl group Chemical group [H]C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])* 0.000 description 2
- 125000001280 n-hexyl group Chemical group C(CCCCC)* 0.000 description 2
- 125000004123 n-propyl group Chemical group [H]C([H])([H])C([H])([H])C([H])([H])* 0.000 description 2
- 125000001971 neopentyl group Chemical group [H]C([*])([H])C(C([H])([H])[H])(C([H])([H])[H])C([H])([H])[H] 0.000 description 2
- RZJRJXONCZWCBN-UHFFFAOYSA-N octadecane Chemical compound CCCCCCCCCCCCCCCCCC RZJRJXONCZWCBN-UHFFFAOYSA-N 0.000 description 2
- 125000002347 octyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 2
- 230000003287 optical effect Effects 0.000 description 2
- BMMGVYCKOGBVEV-UHFFFAOYSA-N oxo(oxoceriooxy)cerium Chemical compound [Ce]=O.O=[Ce]=O BMMGVYCKOGBVEV-UHFFFAOYSA-N 0.000 description 2
- 239000003973 paint Substances 0.000 description 2
- 229920006267 polyester film Polymers 0.000 description 2
- 238000012545 processing Methods 0.000 description 2
- 125000001436 propyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])[H] 0.000 description 2
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- 238000010008 shearing Methods 0.000 description 2
- FDNAPBUWERUEDA-UHFFFAOYSA-N silicon tetrachloride Chemical class Cl[Si](Cl)(Cl)Cl FDNAPBUWERUEDA-UHFFFAOYSA-N 0.000 description 2
- 239000011734 sodium Substances 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
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- VXEGSRKPIUDPQT-UHFFFAOYSA-N 4-[4-(4-methoxyphenyl)piperazin-1-yl]aniline Chemical compound C1=CC(OC)=CC=C1N1CCN(C=2C=CC(N)=CC=2)CC1 VXEGSRKPIUDPQT-UHFFFAOYSA-N 0.000 description 1
- 125000006043 5-hexenyl group Chemical group 0.000 description 1
- HOPKHJSQWOIIQO-UHFFFAOYSA-N C[SiH2]C.[O] Chemical group C[SiH2]C.[O] HOPKHJSQWOIIQO-UHFFFAOYSA-N 0.000 description 1
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 1
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- 239000002841 Lewis acid Substances 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 1
- POFAUXBEMGMSAV-UHFFFAOYSA-N [Si].[Cl] Chemical compound [Si].[Cl] POFAUXBEMGMSAV-UHFFFAOYSA-N 0.000 description 1
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- 125000002877 alkyl aryl group Chemical group 0.000 description 1
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- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 description 1
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- QABCGOSYZHCPGN-UHFFFAOYSA-N chloro(dimethyl)silicon Chemical compound C[Si](C)Cl QABCGOSYZHCPGN-UHFFFAOYSA-N 0.000 description 1
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- 125000003963 dichloro group Chemical group Cl* 0.000 description 1
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- LIKFHECYJZWXFJ-UHFFFAOYSA-N dimethyldichlorosilane Chemical compound C[Si](C)(Cl)Cl LIKFHECYJZWXFJ-UHFFFAOYSA-N 0.000 description 1
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- NCWQJOGVLLNWEO-UHFFFAOYSA-N methylsilicon Chemical compound [Si]C NCWQJOGVLLNWEO-UHFFFAOYSA-N 0.000 description 1
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- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 1
- 125000000913 palmityl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 description 1
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- NVIFVTYDZMXWGX-UHFFFAOYSA-N sodium metaborate Chemical compound [Na+].[O-]B=O NVIFVTYDZMXWGX-UHFFFAOYSA-N 0.000 description 1
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- 230000006641 stabilisation Effects 0.000 description 1
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- 125000004079 stearyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
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- 125000002769 thiazolinyl group Chemical group 0.000 description 1
- 239000004408 titanium dioxide Substances 0.000 description 1
- 125000005425 toluyl group Chemical group 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
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- 238000002834 transmittance Methods 0.000 description 1
- IPBRIJAYQVOWRM-UHFFFAOYSA-N trichloromethylsilicon Chemical compound [Si]C(Cl)(Cl)Cl IPBRIJAYQVOWRM-UHFFFAOYSA-N 0.000 description 1
- ZDHXKXAHOVTTAH-UHFFFAOYSA-N trichlorosilane Chemical compound Cl[SiH](Cl)Cl ZDHXKXAHOVTTAH-UHFFFAOYSA-N 0.000 description 1
- 239000005052 trichlorosilane Substances 0.000 description 1
- AJSTXXYNEIHPMD-UHFFFAOYSA-N triethyl borate Chemical compound CCOB(OCC)OCC AJSTXXYNEIHPMD-UHFFFAOYSA-N 0.000 description 1
- BSVBQGMMJUBVOD-UHFFFAOYSA-N trisodium borate Chemical compound [Na+].[Na+].[Na+].[O-]B([O-])[O-] BSVBQGMMJUBVOD-UHFFFAOYSA-N 0.000 description 1
- 238000011144 upstream manufacturing Methods 0.000 description 1
- 239000006200 vaporizer Substances 0.000 description 1
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 description 1
- 229920002554 vinyl polymer Polymers 0.000 description 1
- 239000002912 waste gas Substances 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
- 238000007704 wet chemistry method Methods 0.000 description 1
- 125000005023 xylyl group Chemical group 0.000 description 1
- 239000011787 zinc oxide Substances 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
- B41M5/5218—Macromolecular coatings characterised by inorganic additives, e.g. pigments, clays
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- C—CHEMISTRY; METALLURGY
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- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B13/00—Oxygen; Ozone; Oxides or hydroxides in general
- C01B13/14—Methods for preparing oxides or hydroxides in general
- C01B13/145—After-treatment of oxides or hydroxides, e.g. pulverising, drying, decreasing the acidity
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- C01B33/113—Silicon oxides; Hydrates thereof
- C01B33/12—Silica; Hydrates thereof, e.g. lepidoic silicic acid
- C01B33/18—Preparation of finely divided silica neither in sol nor in gel form; After-treatment thereof
- C01B33/181—Preparation of finely divided silica neither in sol nor in gel form; After-treatment thereof by a dry process
- C01B33/183—Preparation of finely divided silica neither in sol nor in gel form; After-treatment thereof by a dry process by oxidation or hydrolysis in the vapour phase of silicon compounds such as halides, trichlorosilane, monosilane
-
- 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
- B41M5/502—Recording sheets characterised by the coating used to improve ink, dye or pigment receptivity, e.g. for ink-jet or thermal dye transfer recording characterised by structural details, e.g. multilayer materials
- B41M5/508—Supports
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/50—Agglomerated particles
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- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer
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- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/12—Surface area
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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/19—Oil-absorption capacity, e.g. DBP values
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- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
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- C01P2006/22—Rheological behaviour as dispersion, e.g. viscosity, sedimentation stability
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- C01P2006/80—Compositional purity
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- C01P2006/00—Physical properties of inorganic compounds
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Abstract
The invention relates to a method of stabilizing dispersions comprises metal oxide and boric.
Description
Technical field
The present invention relates to a kind of method of stabilising dispersions, a kind of dispersion and manufacture method thereof, a kind of silicon-dioxide and manufacture method thereof.
Background technology
Cabot discloses the aqueous silicon dioxide dispersions enforcement stabilization that is used for application to printed medium (paper) with the aluminium salt pair in EP 1 124 693 A1.Its shortcoming is: having under aluminium existence and the influence at aluminium, non-desired color can take place and change in printing-ink.
Other known methods in order to stabilized chlorine silicon dispersion are regulated high pH value for interpolation alkali and with KOH or NaOH.Its shortcoming is to cause damage to paper.
Summary of the invention
The objective of the invention is to overcome the shortcoming of prior art.
Be surprised to find, boron compound is used for dispersion, silica dispersion especially, and use a kind of silicon-dioxide of boracic, can make the very high silica dispersion of solids content, even it still has anti-freezing gel and anti-sedimentary stability highlightedly after standing storage.
The present invention relates to a kind of method, it is characterized in that this dispersion contains boron in order to stabilising dispersions.
These dispersions preferably can be the dispersion of silicon-dioxide or the dispersion of metal oxide, as aluminum oxide, titanium dioxide, zirconium white (IV), cerium oxide (IV) and zinc oxide.
In method in order to stabilising dispersions, the usage quantity of boron is preferably the boron of 0.00001 to 8 weight %, the boron of 0.0001 to 8 weight % more preferably, be preferably the boron of 0.001 to 5 weight % especially, most preferably be the boron of 0.1 to 5 weight %, wherein boron all is that the gross weight with the boracic dispersion is a benchmark, disperses intravital pure boron to calculate with boracic.
In method in order to stabilising dispersions, the usage quantity of boron is preferably the boron of 0.0001 to 12 weight %, the boron of 0.001 to 10 weight % more preferably, be preferably the boron of 0.1 to 5 weight % especially, wherein boron all is that the gross weight with boracic silicon-dioxide is a benchmark, calculates with the pure boron in the boracic silicon-dioxide.
The invention still further relates to the dispersion that contains silicon-dioxide or metal oxide and contain boron.
Preferably contain above-mentioned silicon-dioxide or metal oxide according to dispersion of the present invention.
When manufacturing contained the dispersion of the present invention of boron, boron was to sneak in the liquid with the form of boron compound.
When manufacturing contains the dispersion of the present invention of boracic silicon-dioxide, be that this boracic silicon-dioxide is sneaked in the liquid.
Liquid is preferably low viscous, more preferably 25 ℃ of following viscosity less than 100 milli pascal seconds, as be preferably water; And other polar protic type liquid mediums, for example pure, as methyl alcohol, ethanol, Virahol, dibasic alcohol and polyvalent alcohol are as ethylene glycol, propylene glycol or glycerol; Aprotic, polar type liquid medium, ether for example, as tetra oxygen furyl, ketone, as acetone, isobutyl ketone, ester, as ethyl acetate, acid amides, as dimethyl formamide, or sulfoxide, as dimethyl sulfoxide (DMSO); And the non-polar liquid body medium, alkane for example, as hexanaphthene, or aromatic hydrocarbons, as toluene.Be preferably water especially.
For making dispersion of the present invention, boron compound can be made an addition in this liquid, and by wetting or by as with swing mixing tank (Taumelmischer) or super mixer is vibrated or make its dispersion by stirring.Under the low silica concentration situation less than 10 weight %, common simple agitation has been enough to make silicon-dioxide to be sneaked in this liquid.Silicon-dioxide sneaking into and disperse preferably under very high shear gradient, to implement in this liquid.What be applicable to this has: the agitator that runs up, rotating speed for example are that the dissolver that runs up of 1 to 50 meter per second, the rotor-stator system that runs up, sonolator, shearing cut off device (Scherspalte), nozzle and ball mill are applicable to this.
This can implement in the method for batch-type or continous way.
Specially suitable system can realize: at first, for example in the container or utensil of a sealing, with effective whipping appts that silicon-dioxide is wetting in addition and sneak in this liquid; In second step, under very high shear gradient, silicon-dioxide is disperseed.This can pass through the dispersion system in first container, or is achieved by the recycle pump in the external pipe that comprises dispersion system, and is wherein preferred under the Circulation of sealing, and this dispersion is sent back this container by this dispersion system from this container.By part circulation and partly taking-up continuously, this working method preferably can be formulated to continous way.
Utilize 5 hertz to 500 kilo hertzs ultrasonic wave to be particularly suitable for making silicon-dioxide in dispersion of the present invention, to disperse, more preferably 10 to 100 kilo hertzs, especially be preferably 15 to 50 kilo hertzs; This ultrasonic dispersing effect can continous way or batch-type enforcement.This can realize by the single ultrasonic generator such as ultrasonic wave spike (Ultraschallspitzen), or as optional by pipeline or the isolating system of tube wall, can comprise in the system for the distribution of commodities of one or more ultrasonic generator and realizing.
The ultrasonic dispersing effect can continous way or batch-type enforcement.
For making dispersion of the present invention, boracic silicon-dioxide can be made an addition in this liquid, and by wetting or by as with swing mixing tank or super mixer is vibrated or make its dispersion by stirring.Under the low silica concentration situation less than 10 weight %, common simple agitation is enough.Sneaking into and disperse preferably under very high shear gradient, to implement of boracic silicon-dioxide.What be applicable to this has: the agitator that runs up, rotating speed for example are the dissolver that runs up of 1 to 50 meter per second, the rotor-stator system that runs up, sonolator, shearing cut off device, nozzle and ball mill.
This can implement in the method for batch-type or continous way.
Specially suitable system can realize: at first, for example in the container or utensil of a sealing, with effective whipping appts that silicon-dioxide is wetting in addition and sneak in this liquid; In second step, under very high shear gradient, silicon-dioxide is disperseed.This can pass through the dispersion system in first container, or is achieved by the recycle pump in the external pipe that comprises dispersion system, and is wherein preferred under the Circulation of sealing, and this dispersion is sent back this container by this dispersion system from this container.By part circulation and partly taking-up continuously, this working method preferably can be formulated to continous way.
Utilize 5 hertz to 500 kilo hertzs ultrasonic wave to be particularly suitable for making silicon-dioxide in dispersion of the present invention, to disperse, more preferably 10 to 100 kilo hertzs, especially be preferably 15 to 50 kilo hertzs; This ultrasonic dispersing effect can continous way or batch-type enforcement.This can realize by the single ultrasonic generator such as the ultrasonic wave spike, or as optional by pipeline or the isolating system of tube wall, can comprise in the system for the distribution of commodities of one or more ultrasonic generator and realizing.
The ultrasonic dispersing effect can continous way or batch-type enforcement.
If dispersion of the present invention contains silicon-dioxide or metal oxide, then the content of boron is preferably the boron of 0.00001 to 8 weight %, the boron of 0.0001 to 8 weight % more preferably, be preferably 0.001 to 5 weight % especially, especially be preferably 0.1 to 5 weight %, most preferably be the boron of 0.5 to 5 weight %, wherein boron all is that the gross weight with the boracic dispersion is a benchmark, disperses intravital pure boron to calculate with boracic.
In dispersion of the present invention, boron content in the boracic silicon-dioxide is preferably the boron of 0.0001 to 12 weight %, 0.001 to 10 weight % more preferably, be preferably 0.1 to 5 weight % especially, most preferably be the boron of 0.5 to 5 weight %, wherein boron all is that the gross weight with boracic silicon-dioxide is a benchmark, calculates with the pure boron in the boracic silicon-dioxide.
The boron that preferably contains the boride form of 0.01 to 5 weight % according to the example of suitable aqueous dispersion of the present invention, and the BET that contains 70 weight % equals the pyrolytic silicon dioxide of 25 to 100 meters squared per gram, or the BET of 50 weight % equals the pyrolytic silicon dioxide of 100 to 200 meters squared per gram, or the BET of 1 to 40 weight % equals the pyrolytic silicon dioxide of 200 to 450 meters squared per gram, other optional silicon-dioxide and optional other thin with solid colloidal, and other additives that contain water and choose wantonly, mineral acid for example is as phosphoric acid; Or organic acid, as oxysuccinic acid or propionic acid; Or mineral alkali, as potassium hydroxide or sodium hydroxide or ammonia; Or organic bases, as trolamine; Or polymkeric substance, as polyoxyethylene glycol, polypropylene glycol; Or tensio-active agent, aniorfic surfactant for example, as dodecane sulfonic acid, or cationic surfactant, as cetylpyridinium chloride, or the neutral surface active agent, as Triton X100.
Example according to boron compound of the present invention is: all dissolve in solvent according to the present invention, decompose or the form dissolved boron compound to decompose, or dissolving in water, decomposition or the form dissolved boron compound to decompose, as the boron compound of hydrolysis.Can use according to the present invention in order to make boracic silicon-dioxide person.Can use the water-soluble boron compound, as water soluble oxidized boron, as B
2O
3Water soluble borate is as B (OH)
3Or HB (OH)
4, HBO
2The salt of boric acid, sodium salt for example is as sodium metaborate, NaBO
3Or borax Na
2B
4O
710H
2O.
The BET that preferably contains 0.1 to 70 weight % according to other examples of aqueous dispersion of the present invention equals the boracic silicon-dioxide of 25 to 100 meters squared per gram, other optional silicon-dioxide and optional other thin with solid colloidal, and other additives that contain water and choose wantonly, mineral acid for example is as phosphoric acid; Or organic acid, as oxysuccinic acid or propionic acid; Or mineral alkali, as potassium hydroxide or sodium hydroxide or ammonia; Or organic bases, as trolamine; Or polymkeric substance, as polyoxyethylene glycol, polypropylene glycol; Or tensio-active agent, aniorfic surfactant for example, as dodecane sulfonic acid, or cationic surfactant, as cetylpyridinium chloride, or the neutral surface active agent, as Triton X100.
The BET that preferably contains 0.1 to 50 weight % according to other examples of aqueous dispersion of the present invention equals the boracic silicon-dioxide of 100 to 200 meters squared per gram, other optional silicon-dioxide and optional other thin with solid colloidal, and other additives that contain water and choose wantonly, mineral acid for example is as phosphoric acid; Or organic acid, as oxysuccinic acid or propionic acid; Or mineral alkali, as potassium hydroxide or sodium hydroxide or ammonia; Or organic bases, as trolamine; Or polymkeric substance, as polyoxyethylene glycol, polypropylene glycol; Or tensio-active agent, aniorfic surfactant for example, as dodecane sulfonic acid, or cationic surfactant, as cetylpyridinium chloride, or the neutral surface active agent, as Triton X100.
The BET that preferably contains 0.1 to 40 weight % according to other examples of aqueous dispersion of the present invention equals the boracic silicon-dioxide of 200 to 450 meters squared per gram, other optional silicon-dioxide and optional other thin with solid colloidal, and other additives that contain water and choose wantonly, mineral acid for example is as phosphoric acid; Or organic acid, as oxysuccinic acid or propionic acid; Or mineral alkali, as potassium hydroxide or sodium hydroxide or ammonia; Or organic bases, as trolamine; Or polymkeric substance, as polyoxyethylene glycol, polypropylene glycol; Or tensio-active agent, aniorfic surfactant for example, as dodecane sulfonic acid, or cationic surfactant, as cetylpyridinium chloride, or the neutral surface active agent, as Triton X100.
Except that aqueous dispersion, also can be preferred dispersion in following medium: other polar protic type liquid mediums, for example pure, as methyl alcohol, ethanol, Virahol, dibasic alcohol and polyvalent alcohol are as ethylene glycol, propylene glycol or glycerol; Aprotic, polar type liquid medium, ether for example, as tetra oxygen furyl, ketone, as acetone, isobutyl ketone, ester, as ethyl acetate, acid amides, as dimethyl formamide, or sulfoxide, as dimethyl sulfoxide (DMSO); And the non-polar liquid body medium, alkane for example, as hexanaphthene, or aromatic hydrocarbons, as toluene.
For being easy to processing and toxic reason, water is specially suitable as liquid medium.
The available in principle diverse ways of boracic silicon-dioxide makes.
Method 1
In the currently known methods of making pyrolytic silicon dioxide, according to temperature is for example to be higher than 1000 ℃ flame method, it comprises the reaction of volatility silane in the flame of for example hydrogen and oxygen combustion such as silicon tetrachloride, trichlorosilane, trichloromethyl silicon or dichloro hydrogen methyl silicon, wherein also can sneak into lower alkyl such as methane less than stoichiometry, and add one or more and plant the vapo(u)rability boron compound, as boron trichloride or trimethyl borate.
The boron in the volatile boron compounds and the ratio of the silicon in the volatility silane are preferably the boron of 0.0001 to 50 weight % corresponding to the amount in the mixture, the boron of 0.1 to 50 weight % more preferably, be preferably the boron of 0.5 to 25 weight % especially, most preferably be the boron of 0.5 to 5 weight %.
The amount of the ratio correspondence of boron is preferably the boron of 0.0001 to 12 weight % in the boracic silicon-dioxide, 0.001 to 10 weight % more preferably, be preferably 0.1 to 5 weight % especially, most preferably be the boron of 0.5 to 2.5 weight %, wherein boron all is that the gross weight with boracic silicon-dioxide is a benchmark, calculates with the pure boron in the boracic silicon-dioxide.
Preferably in the vaporizer that is connected in the burner upstream, add boron compound; Preferably will send into the steam-like composition of burner and gas uniform mixing in addition.
Method 2
In another specific embodiments according to the present invention, with volatility or liquid boron compound or be dissolved in liquid, preferred water-soluble boron compound sprays into, atomizes or sends in order in the flame of making pyrolytic silicon dioxide with the aerocolloidal form that is preferably produced by spraying gun.
The amount of the ratio correspondence of boron is preferably the boron of 0.0001 to 12 weight % in the boracic silicon-dioxide, 0.001 to 10 weight % more preferably, be preferably 0.1 to 5 weight % especially, most preferably be the boron of 0.5 to 2.5 weight %, wherein boron all is that the gross weight with boracic silicon-dioxide is a benchmark, calculates with the pure boron in the boracic silicon-dioxide.
Method 3
In another specific embodiments according to the present invention, plant boron compounds with one or more following silicon-dioxide is implemented post-processed: the silicon-dioxide that makes according to known method, as silicon dioxide gel, silica dioxide gel, without calcining or on incinerating diatomite, wet chemistry made silicon-dioxide, it is so-called deposition of silica, or with the made silicon-dioxide of flame method, promptly so-called pyrolytic silicon dioxide.Optional also can additionally add other and be used for surface-treated reagent, as water-resisting agent, silylating agent, as alkyl chlorosilane, as dimethyldichlorosilane(DMCS), or alkylalkoxy silane, as dimethyldimethoxysil,ne, as the alkyl silazane, as hexamethyldisilazane, or alkyl polysiloxane, as polydimethylsiloxane, its mean chain length degree is less than 100 chain links, it is dimethylsilane oxygen base monomeric unit, and have reactive terminal group, and as the SiOH base, i.e. dimethylsilane alcohol end group for example, or non-reactive end groups, as trimethylsiloxy.
The example of boron compound is the covalency boron compound, as halogenation boron, and as boron trichloride, or the alcoholate of boron, as trimethyl borate or triethyl borate, or the water-soluble salt of boron, as Sodium Tetraborate, as Na
3BO
3Or NaBO
2Or borax.In addition, the boron compound that dissolves in organic solvent also is suitable.
In a special specific embodiments, use wetting ability pyrolytic silicon dioxide made under anhydrous condition as implement basic (initial) product of surface-treated with boron compound.Anhydrous being meant here, in other steps of hydro-thermal manufacture method or this method, as cooling, purify and until finally through purifying, packing and prepare to transport in the storage process of product, the water with extra liquid state or steam-like is not added in this complete processing.In all cases, be benchmark with the gross weight of silicon-dioxide, the addition of water is no more than 5 weight %, preferably adds the least possible water, does not especially preferably add water fully.
The invention still further relates to and a kind ofly apply wetting ability or hydrophobicity or, it is characterized in that, plant volatility, liquid state or soluble boron compounds with one or more described silicon-dioxide is implemented surface treatment through the method for silica silylate.
For example, this boron compound has following general formula
R
1 aBX
b (I)
Or
R
1 cB(OR
2)
d (II)
Wherein a+b=3 or c+d=3,
B is preferably 3,
D is preferably 3,
And
X is a halogen, is preferably chlorine,
R
1Can be identical or different, and optional for single unsaturated or how unsaturated, have 1 to 18 carbon atom, optional through halogenated univalence hydrocarbyl,
R
1Be preferably methyl or ethyl, for be easy to obtain former thereby be preferably methyl especially,
R
2Can be identical or different, and optional for single unsaturated or how unsaturated, have 1 to 12 carbon atom, optional through halogenated univalence hydrocarbyl.
R
1Example be alkyl, as methyl, ethyl; Propyl group is as sec.-propyl or n-propyl; Butyl is as the tertiary butyl or normal-butyl; Amyl group is as neo-pentyl, isopentyl or n-pentyl; Hexyl is as n-hexyl; Heptyl is as n-heptyl; Octyl group is as 2-ethylhexyl or n-octyl; Decyl is as positive decyl; Dodecyl is as dodecyl; Hexadecyl is as n-hexadecyl; Octadecyl is as the Octadecane base; Thiazolinyl is as vinyl, 2-allyl group or 5-hexenyl; Aryl is as phenyl, xenyl or naphthylmethylidyne; Alkylaryl is as phenmethyl, ethylphenyl, toluyl or xylyl; Haloalkyl is as the 3-chloropropyl.
R
1Example be preferably methyl and ethyl, be preferably methyl especially.
R
2Example be alkyl, as methyl, ethyl; Propyl group is as sec.-propyl or n-propyl; Butyl is as the tertiary butyl or normal-butyl; Amyl group is as neo-pentyl, isopentyl or n-pentyl; Hexyl is as n-hexyl; Heptyl is as n-heptyl; Octyl group is as 2-ethylhexyl or n-octyl; Decyl is as positive decyl; And dodecyl, as dodecyl.
R
2Example be preferably methyl and ethyl, be preferably methyl especially.
Particularly preferred boron compound example is boron trichloride and trialkyl borate, wherein most preferably is trimethyl borate.
The amount of the ratio correspondence of boron is preferably the boron of 0.0001 to 12 weight % in the boracic silicon-dioxide, 0.001 to 10 weight % more preferably, be preferably 0.1 to 5 weight % especially, most preferably be the boron of 0.5 to 5 weight %, wherein boron all is that the gross weight with boracic silicon-dioxide is a benchmark, calculates with the pure boron in the boracic silicon-dioxide.
The initial silicon-dioxide of method 3
The primary granule mean sizes of initial silicon-dioxide is preferably less than 100 nanometers, and the primary granule mean sizes is 5 to 50 nanometers more preferably.These primary granules are not to be present in the silicon-dioxide with isolating form, but the composition of bigger aggregate and agglomerate.
The specific surface area of this silicon-dioxide is preferably 25 to 500 meters squared per gram (the BET method according to DIN 66131 and 66132 records).
This silicon-dioxide comprises the aggregate (definition according to DIN 53206) of diameter in 100 to 1000 nanometer range, wherein this silicon-dioxide comprises the agglomerate (definition is according to DIN53206) that contains aggregate, and the agglomerate size that depends on outside shear loading (as measuring condition) is 1 to 500 micron.
The surperficial fractal dimension of this silicon-dioxide is preferably and is less than or equal to 2.3, more preferably is less than or equal to 2.1, is preferably 1.95 to 2.05 especially, wherein should surface fractal dimension D
sBe defined as: the D of granule surface area A and particle radius R
sPower is directly proportional.
The mass-fractal dimension D of this silicon-dioxide
mBe preferably and be less than or equal to 2.8, more preferably be equal to or less than 2.7, be preferably 2.4 to 2.6 especially.This mass-fractal dimension D
mBe defined as: the D of granular mass M and particle radius R
mPower is directly proportional.
The surface density of the silanol group SiOH of this silicon-dioxide is preferably less than 2.5 SiOH/ square nanometers, more preferably less than 2.1 SiOH/ square nanometers, is preferably especially less than 1.9 SiOH/ square nanometers, most preferably is 1.7 to 1.9 SiOH/ square nanometers.
Can use (above 1000 ℃) made silicon-dioxide at high temperature.Be preferably the made silicon-dioxide of pyrolysis method especially.Also can use the upright and outspoken wetting ability silicon-dioxide that makes, temporarily stores or carried out commercial general packing by burner that connects.Also can use hydrophobization or silica silylate, for example commercially available silicon-dioxide.
Can use tap density without compacting less than 60 grams per liters, and through the tap density of the compacting silicon-dioxide greater than 60 grams per liters.
Can use the mixture of different silicon-dioxide, for example: have different B ET specific surface area silicon-dioxide mixture or have the mixture of the silicon-dioxide of different hydrophobization degree or silylanizing degree.
-implement surface modification with boron can adopt discontinuous formula reaction, i.e. batch process, or continuous reaction.For technical reason, be preferably continuous reaction.
-this reaction can be implemented in a step, or implements in two or three steps that are connected mutually.In other words, this reaction can be implemented filling (physical adsorption of boron compound) in advance, and this reaction can be implemented purification step subsequently.Being preferably three successive steps: purifies in reaction-(3), (1) filling-(2).
-filling temperature is preferably-30 ℃ to 350 ℃, more preferably 20 ℃ to 150 ℃, is preferably 60 ℃ to 120 ℃ especially.
-temperature of reaction preferably reaches 50 to 400 ℃, more preferably 50 ℃ to 150 ℃.
-the reaction times is preferably 1 minute to 24 hours, more preferably 10 minutes to 8 hours, is preferably 30 minutes to 4 hours especially.
-reaction pressure can be in the scope of barometric point, high pressure to 10 crust, low pressure to 0.2 crust.
-purification temperature preferably reaches 100 to 400 ℃, more preferably 150 ℃ to 300 ℃.
-silicon-dioxide and boron compound are effectively turned round and thoroughly mixing.This is preferably implemented by machinery or airborne rheomorphism.Can utilize all rare gas elementes to implement the airborne rheomorphism, these rare gas elementes do not react with the silicon-dioxide and the side reaction product of boron compound, silicon-dioxide, boracic, promptly can not cause side reaction, DeR, oxygenizement and flame and explosion phenomenon, as N
2, Ar, other rare gas elementes, CO
2Deng.The blank pipe gas flow rate is preferably in the scope of 0.05 to 5 cel, and 0.05 to 1 cel is more preferably sent into and is used for fluidizing gas.Can pass through wing formula agitator, anchor stirrer and other suitable whipping apptss and implement the mechanical fluidisation effect.
-in a particularly preferred specific embodiments, the amount of sending into gas is preferably less than 10 volume % only in order to keep anoxybiotic atmosphere, more preferably less than the oxygen of 2.5 volume %, implements rheomorphism with pure mechanical mode then.
-this reaction is preferably implemented in the atmosphere that does not cause the oxidation of boracic silicon-dioxide, promptly in the oxygen deficient atmospheres, is preferably the oxygen less than 10 volume %, is preferably especially less than 2.5 volume %, and wherein optimum obtains under the situation less than 1 volume % oxygen.
-boron compound is sent in the silicon-dioxide effectively.This can implement by using the boron compound that is steam-like under application temperature or temperature of reaction.If this boron compound at room temperature and/or be fluid cpds under the temperature of reaction, maybe must be dissolved in the solid chemical compound of solvent, the effective spray application of then preferred use is for example being sprayed in pure nozzle under the pressure of 5 to 20 crust, is spraying in double nozzle under 2 to 20 gases that cling to and liquid pressure, is being implemented fine distribution with spraying gun.
-preferably boron compound is added with thin aerocolloidal form, it is characterized in that this aerocolloidal fall off rate is preferably 0.1 to 20 cel.
-optionally, preferably can add protonic solvent, as liquid or volatile alcohol or water; Typical alcohol is Virahol, ethanol and methyl alcohol.Also can add the mixture of above-mentioned protonic solvent.The preferred water that adds.With silicon-dioxide is benchmark, and the addition of water is preferably 0.1 to 50 weight %; Measure at the weight difference before and after the heating under the situation of 105 ℃ temperature and barometric point two hours by weighing, with the BET specific surface area is that the silicon-dioxide of 100 meters squared per gram is benchmark, the total amount of water or moisture is preferably 0.25 to 2.5 weight % especially, be that the silicon-dioxide of 100 meters squared per gram is 0.25 to 2.5 weight % of benchmark promptly with the BET specific surface area, corresponding to the silicon-dioxide that with the BET specific surface area is 50 meters squared per gram is benchmark and still less 0.125 to 1.25 weight %, and is benchmark and more 0.75 to 7.5 weight % corresponding to the silicon-dioxide that is 300 meters squared per gram with the BET specific surface area.
-optionally, preferably can add acidity or basic catalyst.These catalyzer can have Lewis alkali or
Alkaline characteristic on the meaning of alkali, as ammonia, maybe can have Lewis acid or
Acidic nature on the meaning of acid is as hydrogenchloride.Preferred these catalyzer that add trace are promptly less than 1000ppm.Especially preferably do not add catalyzer.
The feature of-this purification step is running, wherein is preferably slow motion and slight the mixing.
Other features of-this purification step are that the gas amount of sending into is big, are 0.001 to 10 cel corresponding to the blank pipe gas flow rate, are preferably 0.01 to 1 cel.
-this purification step can additionally comprise the mixing effect with mechanical stirring device.In this case, whipping appts is set and makes its running, implementing preferred the mixing and rheomorphism, but not exclusively produce eddy current.
-when adding boron compound, can additionally use the mechanical ramming method, as pressure roller (Presswalzen), ball mill, pan mill, spiral compactor (Schraubenverdichter) or cake compressor (Brikettierer).
-when adding boron compound, can additionally use the agglomeration technique that goes of silicon-dioxide, as pin shredder (Stiftm ü hlen) or mill sieve (Mahlsichtung) device.
-and then method of purification can additionally use the mechanical ramming method of silicon-dioxide afterwards, as pressure roller, or by the compacting of suitable vacuum method by extracting air or gas, or other mechanical ramming methods, as pressure roller, ball mill, pan mill, spiral compactor or cake compressor.
-and then method of purification can additionally use the agglomeration technique that goes of silicon-dioxide afterwards, as pin shredder or mill screen device.
-in a preferred specific embodiments, the boron compound that unreacted is intact, side reaction product, without boron compound, the waste product that comes from purification step and the waste gas of chemical modification and optional excessive interpolation through changing, in homothermic device internal recycle suitably to the coating and the filling step of silicon-dioxide; This can partially or even wholly implement, and is preferably by 50 to 90% of the total volumetric flow rate of gas that purification step produces.
The amount of the ratio correspondence of boron is preferably the boron of 0.0001 to 12 weight % in the boracic silicon-dioxide, 0.001 to 10 weight % more preferably, be preferably 0.1 to 5 weight % especially, most preferably be the boron of 0.5 to 2.5 weight %, wherein boron all is that the gross weight with boracic silicon-dioxide is a benchmark, calculates with the pure boron in the boracic silicon-dioxide.
The invention still further relates to a kind of on the surface or contain the silicon-dioxide of boron at the whole volume of silicon-dioxide, its primary granule mean sizes is less than 100 nanometers, the primary granule mean sizes is preferably 5 to 50 nanometers, wherein these primary granules are not to be present in the silicon-dioxide with isolating form, but the composition of bigger aggregate (definition is according to DIN 53206), the diameter of these aggregates is 100 to 1000 nanometers and forms agglomerate (definition is according to DIN 53206), depend on outside shear loading, this agglomerate is of a size of 1 to 500 micron, its specific surface area is 10 to 500 meters squared per gram (the BET method according to DIN 66131 and 66132 records), and mass-fractal dimension D
mBe less than or equal to 2.8, and boron content is preferably the boron of 0.0001 to 12 weight %, 0.001 to 10 weight % more preferably, be preferably 0.1 to 5 weight % especially, most preferably be the boron of 0.5 to 2.5 weight %, wherein boron all is that the gross weight with boracic silicon-dioxide is a benchmark, calculates with the pure boron in the boracic silicon-dioxide.
Be characterised in that according to other of boracic silicon-dioxide of the present invention, its can make solids content height, viscosity the storage stability height, do not deposit and the aqueous dispersion of not gelation.
The present invention relates to boracic silicon-dioxide according to the present invention is used for powdery solid to improve the flowability of dried powder, promptly improve free-flowing property, promptly as flow promotor; In addition in order to suppressing powder agglomeration and caking, and suppress film bonding and caking.
The invention still further relates to a kind of recording medium, for example: paper or film, this medium are suitable for using the printing of ink-jet printer, particularly glossy paper and high glossiness paper, it is characterized in that, it has according to dispersion of the present invention.
The invention still further relates to the top coat that contains with good grounds dispersion of the present invention.
The present invention relates to according to boracic silicon-dioxide of the present invention and the made thus application of the silica containing aqueous dispersion of boracic in implementing surface-coated, for example: the mineral substrate as metal, as steel or iron, for example has anticorrosion purpose person.
The present invention relates to according to boracic silicon-dioxide of the present invention and the made thus silica containing aqueous dispersion of boracic make paints and paint, synthetic resins, tackiness agent and sealing agent in application, especially be the made person of main component with water.
The present invention relates to according to boracic silicon-dioxide of the present invention and the made thus application of the silica containing aqueous dispersion of boracic in the coating of implementing recording medium, in particular for the paper of contactless printing process.The example is the paper that is used for ink-jet printer, particularly has the paper of high glossiness.
Embodiment
Embodiment
Embodiment 1
Boron trichloride and 74.3Nm with 10.0 kilograms/hour silicon tetrachlorides and 0.8 kilogram/hour
3The primary air of/h and 20.7Nm
3The hydrogen of/h uniform mixing in mixing vessel, and in the burner nozzle of the known configuration in flame it is fed in the combustion chamber.Additionally with 12.0Nm
3The secondary air of/h is blown in this combustion chamber.Leave after the combustion chamber, formed silicon-dioxide-gaseous mixture in the heat exchange system is cooled to 120 to 150 ℃, in the filtering system of a heating, solid silica is separated from the gas phase that contains hydrogenchloride subsequently.Subsequently under the temperature that improves, with the removing residues of hydrogenchloride.BET method according to DIN 66131 and 66132 records, and obtaining specific surface area is the boracic pyrolytic silicon dioxide of 180 meters squared per gram, and concentration is that the pH value (DIN/ISO 787/9) of the dispersion of 4% (weight %) is 4.The boron content of this silicon-dioxide is 1.8 weight %.
Embodiment 2
With 5.0 kilograms/hour silicon tetrachlorides and 74.3Nm
3The primary air of/h and 20.7Nm
3The hydrogen of/h uniform mixing in mixing vessel, and in the burner nozzle of the known configuration in flame it is fed in the combustion chamber.Additionally with 12.0Nm
3The secondary air of/h is blown in this combustion chamber.0.2 kilogram of/hour Sodium Tetraborate that additionally will be dissolved in 1 kilogram of/hour water sprays in this combustion chamber with aerocolloidal form.Leave after the combustion chamber, formed silicon-dioxide-gaseous mixture in the heat exchange system is cooled to 120 to 150 ℃, in the filtering system of a heating, solid silica is separated from the gas phase that contains hydrogenchloride subsequently.Subsequently under the temperature that improves, with the removing residues of hydrogenchloride.BET method according to DIN 66131 and 66132 records, and obtaining specific surface area is the boracic pyrolytic silicon dioxide of 110 meters squared per gram, and concentration is that the pH value (DIN/ISO 787/9) of the dispersion of 4% (weight %) is 6.The boron content of this silicon-dioxide is 0.8 weight %.
Embodiment 3
Under 25 ℃ temperature and at N
2In the inert gas atmosphere, with the trimethyl borate of 200 Grams Per Hours with liquid form in small, broken bits atomizing in the continous way device by pure nozzle (pressure is 10 crust), add mass rate and be 1000 Grams Per Hours, specific surface area is that (trade(brand)name is WACKER HDK T30 for the wetting ability silicon-dioxide of 300 meters squared per gram (the BET method according to DIN 66131 and 66132 records), available from Wacker chemistry company limited, Burghausen, Germany) in, with its wetting be the water of 2.5 weight % to water-content.The silicon-dioxide of so packing into 100 ℃ of following constant temperature 1 hour, is kept 2 hours then so that its reaction under 250 ℃ temperature.Under mechanical stirring and under 150 ℃ temperature, feed N subsequently with gas flow rate less than 0.5 cel
2Situation under, purified 30 minutes.Make the white SiO 2 powder that contains 1.8 weight % boron.
Embodiment 4
Under 25 ℃ temperature and at N
2In the inert gas atmosphere, with the trimethyl borates of 50 grams with liquid form in small, broken bits atomizing in the batch-type device by pure nozzle (pressure be 20 cling to), the specific surface areas that add 100 grams are that (trade(brand)name is WACKER HDK D05 for the wetting ability silicon-dioxide of 50 meters squared per gram (the BET method according to DIN 66131 and 66132 records), available from Wacker chemistry company limited, Burghausen, Germany) in, with its wetting be the water of 0.6 weight % to water-content.The silicon-dioxide of so packing into is amounted to 3 hours at 100 ℃ of following constant temperature, in reactor, under 250 ℃ temperature, kept 2 hours subsequently so that its reaction is sent into N in reaction process under 15 times gaseous interchange
2Making boron content is the white SiO 2 powder of 4.1 weight %.
Embodiment 5
Under 25 ℃ temperature, the boracic silicon-dioxide that 300 grams are made by embodiment 3 makes an addition in 700 milliliters the water with little step in the batch-type device, and with the Ultraturax type rotor-stator diverting device of Jahnke and Kunkel company it is disperseed.Forming boron content is the low viscosity pale aq suspension of 0.5 weight %.This suspension is surpassing the stability that still has anti-deposition and anti-freezing gel in the time of half a year.Conical disc-rotational viscosimeter with RheoStress 600 types of Haake company is measured down at 25 ℃, is under the 100l/s at shear gradient, and the viscosity of this suspension is 120 milli pascal seconds.
By what control by transmittance
Anti-sedimentation Stability is write down in the measurement of type whizzer.
Referring to Fig. 1 (non-reference of the present invention):
With
The recording laser transmissivity distributes and (produces sedimentation by the rotation centrifugal force that is equivalent to 3000G here; Utilize the array of 2000 diodes, in centrifugal separation processes, monitor the sedimentation of this silicon-dioxide) by the laser-transmitting rate.
X-coordinate (X-axis): the longitudinal axis of centrifuge tube is a unit (left side: opening, the right side: the bottom) with the millimeter; Ordinate zou (Y-axis): the optical transmission rate, in percentage (%).
The transmissivity of non-dispersion of the present invention distributes, and uses
Record; Monodisperse silica sphere particle 220 nanometers, Measuring Time 120 minutes, gravity field is 3000G: the strong deposition phenomenon of observing unstable dispersion.
And Fig. 2 (according to embodiments of the invention 5):
With
The recording laser transmissivity distributes and (produces sedimentation by the rotation centrifugal force that is equivalent to 3000G here; Utilize the array of 2000 diodes, in centrifugal separation processes, monitor the sedimentation of this silicon-dioxide) by the laser-transmitting rate.
X-coordinate (X-axis): the longitudinal axis of a centrifuge tube (left side: opening, the right side: the bottom);
Ordinate zou (Y-axis): the optical transmission rate, in percentage (%).
Transmissivity according to the dispersion of the present invention of embodiment 5 distributes, and uses
Record; Measuring Time 120 minutes, gravity field is 3000G: do not observe depositional phenomenon.
Embodiment 6
Under 25 ℃ temperature, the boracic silicon-dioxide that 250 grams are made by embodiment 3 makes an addition in 750 milliliters the water with little step in the batch-type device, and with the fluted disc-dissolver of the Ika company rotating speed with 11.6 meter per seconds it is disperseed.Forming boron content is the low viscosity pale aq suspension of 0.5 weight %.This suspension still has the stability of anti-deposition and anti-freezing gel in surpassing year.Conical disc-rotational viscosimeter with RheoStress 600 types of Haake company is measured down at 25 ℃, is under the 100l/s at shear gradient, and the viscosity of this suspension is 130 milli pascal seconds.
Embodiment 7
Under 25 ℃ temperature, the boracic silicon-dioxide that 2000 grams are made by embodiment 4 makes an addition in 2000 milliliters the water with little step in the batch-type device, and with 6 liters of Unimix type rotor-stator diverting devices of Unimix/Ekator company it is disperseed.Forming boron content is the low viscosity pale aq suspension of 2 weight %.This suspension still has the stability of anti-deposition and anti-freezing gel in surpassing year.Conical disc-rotational viscosimeter with RheoStress 600 types of Haake company is measured down at 25 ℃, is under the 100l/s at shear gradient, and the viscosity of this suspension is 190 milli pascal seconds.
Embodiment 8
Mix in the dispersion that 100 grams make by embodiment 5 being dissolved in 50 grams 8 in water gram polyvinyl alcohol, and mixed, this dispersion contains the silicon-dioxide that 30 grams are made by embodiment 3.The ink-jet japanning that will so make with scraper with manual mode with 77.5 grams/square metre the paper recoat overlay on the paper of uncoated, paper that will be through applying at air drying until the exsiccant feel is arranged.With the calendering of exsiccant paper, and use
Stylus pro Photorealistic prints.Graphical quality is splendid.The glossiness that records this printed matter with 60 ° of miniature-glossmeters of Gardener is 47.
Embodiment 9
Mix in the dispersion that 100 grams make by embodiment 5 being dissolved in the 50 gram gram polyvinyl alcohol of 8 in the water (Mowiol 26-88, Clariant company), and mixed, this dispersion contains the silicon-dioxide that 30 grams are made by embodiment 3.The ink-jet that will so make with scraper with manual mode is coated on the polyester film of 0.2 mm thick with 160 microns wet-film thickness, at 105 ℃ down with the oven dry of the film through applying 15 minutes.With
Stylus Colour 800 prints on this film through applying.Graphical quality is splendid.
Embodiment 10
Under 25 ℃ temperature, with 250 gram BET specific surface areas is that (trade(brand)name is Wacker HDK T30 for the silicon-dioxide of 300 meters squared per gram, available from Wacker chemistry company limited) in the batch-type device, make an addition in the boric acid of 750 milliliters water and 25 grams with little step, and with the Ultraturax type rotor-stator diverting device of Jahnke and the Kunkel company rotating speed with 11000 rev/mins it is disperseed.Forming boron content is the low viscosity pale aq suspension of 0.8 weight %.This suspension is surpassing the stability that still has anti-deposition and anti-freezing gel in the time of half a year.Conical disc-rotational viscosimeter with RheoStress 600 types of Haake company is measured down at 25 ℃, is under the 100l/s at shear gradient, and the viscosity of this suspension is 120 milli pascal seconds.
Embodiment 11
Mix in the dispersion that 100 grams make by embodiment 10 being dissolved in 50 grams 8 in water gram polyvinyl alcohol, and mixed.The ink-jet japanning that will so make with scraper with manual mode with 77.5 grams/square metre the paper recoat overlay on the paper of uncoated, paper that will be through applying at air drying until the exsiccant feel is arranged.With the calendering of exsiccant paper, and use
Stylus proPhotorealistic prints.Graphical quality is splendid.The glossiness that records this printed matter with 60 ° of miniature-glossmeters of Gardener is 47.
Embodiment 12
Mix in the dispersion that 100 grams make by embodiment 10 being dissolved in the 50 gram gram polyvinyl alcohol of 8 in the water (Mowiol 26-88, Clariant company), and mixed.The ink-jet that will so make with scraper with manual mode is coated on the polyester film of 0.2 mm thick with 160 microns wet-film thickness, forms the wet film of 160 micron thickness, at 105 ℃ down with the oven dry of the film through applying 15 minutes.With
Stylus Colour 800 prints on this film through applying.Graphical quality is splendid.
Claims (11)
1, a kind of in order to the stable method that contains the dispersion of silicon-dioxide, it is characterized in that based on the weight of described dispersion, described dispersion contains the boron of 0.00001 to 8 weight %.
2, a kind of in order to the stable method that contains the dispersion of silicon-dioxide, it is characterized in that based on the weight of described silicon-dioxide, described silicon-dioxide contains the boron of 0.0001 to 12 weight %.
3, a kind of dispersion is characterized in that containing silicon-dioxide, and based on the weight of described dispersion, described dispersion contains the boron of 0.00001 to 8 weight %.
4, a kind of dispersion is characterized in that containing the silicon-dioxide of boracic, and based on the weight of described silicon-dioxide, described silicon-dioxide contains the boron of 0.0001 to 12 weight %.
5, a kind of silicon-dioxide, it is characterized in that applying with a kind of boron compound at least, the primary granule mean sizes of this boracic silicon-dioxide is less than 100 nanometers, these primary granules are not to be present in the described silicon-dioxide with isolating form, but according to the composition of the bigger aggregate of DIN 53206 definition, the diameter of these aggregates is 100 to 1000 nanometers and forms the agglomerate that defines according to DIN 53206, depend on outside shear loading, this agglomerate is of a size of 1 to 500 micron, its specific surface area that records according to the BET method of DIN 66131 and 66132 is 10 to 500 meters squared per gram, and mass-fractal dimension D
mBe less than or equal to 2.8, and boron content is 0.0001 to 12 weight %.
6, a kind of usefulness is so that silica modified method, it is characterized in that, plant volatility, liquid state or soluble boron compounds with one or more described silicon-dioxide is implemented surface treatment, be benchmark and calculate that with the gross weight of boracic silicon-dioxide the usage quantity of boron is 0.0001 to 12 weight % with the pure boron in the boracic silicon-dioxide.
7, a kind of usefulness is so that silica modified method, it is characterized in that, in flame, make in the process of pyrolytic silicon dioxide, the boron compound of one or more being planted liquid boron compound or being dissolved in solvent sprays in this flame, be benchmark and calculate that with the gross weight of boracic silicon-dioxide the usage quantity of boron is 0.0001 to 12 weight % with the pure boron in the boracic silicon-dioxide.
8, a kind of recording medium is characterized in that having the dispersion as claim 3 or 4.
9, recording medium as claimed in claim 8 is characterized in that, this recording medium is glossy paper or the high glossiness paper that is suitable for the ink-jet printer printing.
10, recording medium as claimed in claim 8 is characterized in that, this recording medium is the film that is suitable for the ink-jet printer printing.
11, a kind of top coat is characterized in that comprising the dispersion as claim 3 or 4.
Applications Claiming Priority (4)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| DE10307249.7 | 2003-02-20 | ||
| DE2003107249 DE10307249A1 (en) | 2003-02-20 | 2003-02-20 | Stabilizing metal oxide dispersions, especially silica dispersions e.g. for coating paper, comprises incorporating boron in the dispersion |
| DE10311722.9 | 2003-03-17 | ||
| DE10325609.1 | 2003-06-05 |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1753834A CN1753834A (en) | 2006-03-29 |
| CN100513303C true CN100513303C (en) | 2009-07-15 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNB2004800048471A Expired - Fee Related CN100513303C (en) | 2003-02-20 | 2004-02-12 | dispersoid and antihunt means thereof method, silicon dioxide and modification method, recording medium and surface coat |
Country Status (2)
| Country | Link |
|---|---|
| CN (1) | CN100513303C (en) |
| DE (1) | DE10307249A1 (en) |
Family Cites Families (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE2829045A1 (en) * | 1978-07-01 | 1980-01-10 | Degussa | PRESERVED FELLING ACID |
| DE10062945A1 (en) * | 2000-12-16 | 2002-06-20 | Continental Ag | Rubber compound and silica for a rubber compound |
-
2003
- 2003-02-20 DE DE2003107249 patent/DE10307249A1/en not_active Withdrawn
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- 2004-02-12 CN CNB2004800048471A patent/CN100513303C/en not_active Expired - Fee Related
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| CN1753834A (en) | 2006-03-29 |
| DE10307249A1 (en) | 2004-09-09 |
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