JP4550804B2 - 熱分解法二酸化ケイ素粉末およびその分散液 - Google Patents
熱分解法二酸化ケイ素粉末およびその分散液 Download PDFInfo
- Publication number
- JP4550804B2 JP4550804B2 JP2006504689A JP2006504689A JP4550804B2 JP 4550804 B2 JP4550804 B2 JP 4550804B2 JP 2006504689 A JP2006504689 A JP 2006504689A JP 2006504689 A JP2006504689 A JP 2006504689A JP 4550804 B2 JP4550804 B2 JP 4550804B2
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- Prior art keywords
- silicon dioxide
- dioxide powder
- burner
- dispersion
- surface area
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Lifetime
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- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 title claims abstract description 86
- 239000006185 dispersion Substances 0.000 title claims abstract description 58
- DOIRQSBPFJWKBE-UHFFFAOYSA-N dibutyl phthalate Chemical compound CCCCOC(=O)C1=CC=CC=C1C(=O)OCCCC DOIRQSBPFJWKBE-UHFFFAOYSA-N 0.000 claims abstract description 26
- 239000000377 silicon dioxide Substances 0.000 claims abstract description 21
- 235000012239 silicon dioxide Nutrition 0.000 claims abstract description 19
- 238000006243 chemical reaction Methods 0.000 claims abstract description 17
- 239000000203 mixture Substances 0.000 claims abstract description 15
- 239000001257 hydrogen Substances 0.000 claims abstract description 12
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 12
- 239000007789 gas Substances 0.000 claims abstract description 11
- 230000008719 thickening Effects 0.000 claims abstract description 10
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims abstract description 9
- 239000007787 solid Substances 0.000 claims abstract description 9
- 238000010521 absorption reaction Methods 0.000 claims abstract description 7
- LFQCEHFDDXELDD-UHFFFAOYSA-N tetramethyl orthosilicate Chemical compound CO[Si](OC)(OC)OC LFQCEHFDDXELDD-UHFFFAOYSA-N 0.000 claims abstract description 7
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 6
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 6
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 claims abstract description 5
- 239000007795 chemical reaction product Substances 0.000 claims abstract description 3
- 238000000034 method Methods 0.000 claims description 37
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 13
- 239000001301 oxygen Substances 0.000 claims description 13
- 229910052760 oxygen Inorganic materials 0.000 claims description 13
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 13
- 238000004519 manufacturing process Methods 0.000 claims description 11
- 239000002253 acid Substances 0.000 claims description 8
- AZDRQVAHHNSJOQ-UHFFFAOYSA-N alumane Chemical class [AlH3] AZDRQVAHHNSJOQ-UHFFFAOYSA-N 0.000 claims description 8
- 238000000197 pyrolysis Methods 0.000 claims description 8
- 229920006317 cationic polymer Polymers 0.000 claims description 7
- 238000002360 preparation method Methods 0.000 claims description 6
- 239000000047 product Substances 0.000 claims description 6
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 claims description 5
- 238000005498 polishing Methods 0.000 claims description 5
- 239000000126 substance Substances 0.000 claims description 5
- 229910004298 SiO 2 Inorganic materials 0.000 claims description 4
- 230000000694 effects Effects 0.000 claims description 4
- 239000011521 glass Substances 0.000 claims description 4
- 230000006835 compression Effects 0.000 claims description 3
- 238000007906 compression Methods 0.000 claims description 3
- 239000000654 additive Substances 0.000 claims description 2
- 229920001971 elastomer Polymers 0.000 claims description 2
- 239000000945 filler Substances 0.000 claims description 2
- 239000003973 paint Substances 0.000 claims description 2
- 239000004033 plastic Substances 0.000 claims description 2
- 229920003023 plastic Polymers 0.000 claims description 2
- 238000000518 rheometry Methods 0.000 claims description 2
- 239000005060 rubber Substances 0.000 claims description 2
- 229920002379 silicone rubber Polymers 0.000 claims description 2
- 230000000996 additive effect Effects 0.000 claims 1
- 239000012530 fluid Substances 0.000 claims 1
- 239000004945 silicone rubber Substances 0.000 claims 1
- 238000005979 thermal decomposition reaction Methods 0.000 claims 1
- 239000000843 powder Substances 0.000 abstract description 12
- 230000009471 action Effects 0.000 abstract description 6
- 229910052681 coesite Inorganic materials 0.000 abstract 1
- 229910052906 cristobalite Inorganic materials 0.000 abstract 1
- 229910052682 stishovite Inorganic materials 0.000 abstract 1
- 229910052905 tridymite Inorganic materials 0.000 abstract 1
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 description 19
- 239000002245 particle Substances 0.000 description 14
- 230000008569 process Effects 0.000 description 11
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 9
- WGTYBPLFGIVFAS-UHFFFAOYSA-M tetramethylammonium hydroxide Chemical compound [OH-].C[N+](C)(C)C WGTYBPLFGIVFAS-UHFFFAOYSA-M 0.000 description 8
- 238000010008 shearing Methods 0.000 description 7
- 239000008367 deionised water Substances 0.000 description 6
- 229910021641 deionized water Inorganic materials 0.000 description 6
- 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 5
- 150000003377 silicon compounds Chemical class 0.000 description 5
- 239000005049 silicon tetrachloride Substances 0.000 description 5
- 229910001220 stainless steel Inorganic materials 0.000 description 5
- 239000010935 stainless steel Substances 0.000 description 5
- PPBRXRYQALVLMV-UHFFFAOYSA-N Styrene Chemical compound C=CC1=CC=CC=C1 PPBRXRYQALVLMV-UHFFFAOYSA-N 0.000 description 4
- VSCWAEJMTAWNJL-UHFFFAOYSA-K aluminium trichloride Chemical compound Cl[Al](Cl)Cl VSCWAEJMTAWNJL-UHFFFAOYSA-K 0.000 description 4
- 229910000077 silane Inorganic materials 0.000 description 4
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 description 3
- -1 and secondly Chemical compound 0.000 description 3
- 239000002585 base Substances 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 3
- 229910021485 fumed silica Inorganic materials 0.000 description 3
- 230000007062 hydrolysis Effects 0.000 description 3
- 238000006460 hydrolysis reaction Methods 0.000 description 3
- 150000003839 salts Chemical class 0.000 description 3
- 229920006337 unsaturated polyester resin Polymers 0.000 description 3
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 2
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 description 2
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- 230000002378 acidificating effect Effects 0.000 description 2
- NNCOOIBIVIODKO-UHFFFAOYSA-N aluminum;hypochlorous acid Chemical compound [Al].ClO NNCOOIBIVIODKO-UHFFFAOYSA-N 0.000 description 2
- 150000001412 amines Chemical class 0.000 description 2
- 238000004458 analytical method Methods 0.000 description 2
- 150000002431 hydrogen Chemical class 0.000 description 2
- 150000007522 mineralic acids Chemical class 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 150000007524 organic acids Chemical class 0.000 description 2
- 235000005985 organic acids Nutrition 0.000 description 2
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-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
- 230000001698 pyrogenic effect Effects 0.000 description 2
- YGSDEFSMJLZEOE-UHFFFAOYSA-N salicylic acid Chemical compound OC(=O)C1=CC=CC=C1O YGSDEFSMJLZEOE-UHFFFAOYSA-N 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- 239000007858 starting material Substances 0.000 description 2
- 239000002912 waste gas Substances 0.000 description 2
- BNGXYYYYKUGPPF-UHFFFAOYSA-M (3-methylphenyl)methyl-triphenylphosphanium;chloride Chemical compound [Cl-].CC1=CC=CC(C[P+](C=2C=CC=CC=2)(C=2C=CC=CC=2)C=2C=CC=CC=2)=C1 BNGXYYYYKUGPPF-UHFFFAOYSA-M 0.000 description 1
- 229910002012 Aerosil® Inorganic materials 0.000 description 1
- 229910002013 Aerosil® 90 Inorganic materials 0.000 description 1
- 101710134784 Agnoprotein Proteins 0.000 description 1
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 1
- 101100293222 Arabidopsis thaliana XI-K gene Proteins 0.000 description 1
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical group Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 1
- OFOBLEOULBTSOW-UHFFFAOYSA-N Malonic acid Chemical compound OC(=O)CC(O)=O OFOBLEOULBTSOW-UHFFFAOYSA-N 0.000 description 1
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 1
- 229920002873 Polyethylenimine Polymers 0.000 description 1
- ZXRRHFSTAFVGOC-UHFFFAOYSA-N [AlH3].[K] Chemical compound [AlH3].[K] ZXRRHFSTAFVGOC-UHFFFAOYSA-N 0.000 description 1
- HIZLQUSEDILRSC-UHFFFAOYSA-M [N+](=O)([O-])[O-].O[Al+2].[N+](=O)([O-])[O-] Chemical compound [N+](=O)([O-])[O-].O[Al+2].[N+](=O)([O-])[O-] HIZLQUSEDILRSC-UHFFFAOYSA-M 0.000 description 1
- YKTSYUJCYHOUJP-UHFFFAOYSA-N [O--].[Al+3].[Al+3].[O-][Si]([O-])([O-])[O-] Chemical compound [O--].[Al+3].[Al+3].[O-][Si]([O-])([O-])[O-] YKTSYUJCYHOUJP-UHFFFAOYSA-N 0.000 description 1
- HDYRYUINDGQKMC-UHFFFAOYSA-M acetyloxyaluminum;dihydrate Chemical compound O.O.CC(=O)O[Al] HDYRYUINDGQKMC-UHFFFAOYSA-M 0.000 description 1
- 150000007513 acids Chemical class 0.000 description 1
- 239000012190 activator Substances 0.000 description 1
- 239000013543 active substance Substances 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 229940037003 alum Drugs 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- MJWPFSQVORELDX-UHFFFAOYSA-K aluminium formate Chemical compound [Al+3].[O-]C=O.[O-]C=O.[O-]C=O MJWPFSQVORELDX-UHFFFAOYSA-K 0.000 description 1
- WNROFYMDJYEPJX-UHFFFAOYSA-K aluminium hydroxide Chemical compound [OH-].[OH-].[OH-].[Al+3] WNROFYMDJYEPJX-UHFFFAOYSA-K 0.000 description 1
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 1
- DIZPMCHEQGEION-UHFFFAOYSA-H aluminium sulfate (anhydrous) Chemical compound [Al+3].[Al+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O DIZPMCHEQGEION-UHFFFAOYSA-H 0.000 description 1
- 229940009827 aluminum acetate Drugs 0.000 description 1
- QFIGQGUHYKRFAI-UHFFFAOYSA-K aluminum;trichlorate Chemical compound [Al+3].[O-]Cl(=O)=O.[O-]Cl(=O)=O.[O-]Cl(=O)=O QFIGQGUHYKRFAI-UHFFFAOYSA-K 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- LCQXXBOSCBRNNT-UHFFFAOYSA-K ammonium aluminium sulfate Chemical compound [NH4+].[Al+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O LCQXXBOSCBRNNT-UHFFFAOYSA-K 0.000 description 1
- 239000000908 ammonium hydroxide Substances 0.000 description 1
- 125000000129 anionic group Chemical group 0.000 description 1
- 239000012736 aqueous medium Substances 0.000 description 1
- QRUDEWIWKLJBPS-UHFFFAOYSA-N benzotriazole Chemical compound C1=CC=C2N[N][N]C2=C1 QRUDEWIWKLJBPS-UHFFFAOYSA-N 0.000 description 1
- 239000012964 benzotriazole Substances 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- BVKZGUZCCUSVTD-UHFFFAOYSA-N carbonic acid Chemical compound OC(O)=O BVKZGUZCCUSVTD-UHFFFAOYSA-N 0.000 description 1
- 150000001735 carboxylic acids Chemical class 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 125000002091 cationic group Chemical group 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- QGBSISYHAICWAH-UHFFFAOYSA-N dicyandiamide Chemical compound NC(N)=NC#N QGBSISYHAICWAH-UHFFFAOYSA-N 0.000 description 1
- KPUWHANPEXNPJT-UHFFFAOYSA-N disiloxane Chemical class [SiH3]O[SiH3] KPUWHANPEXNPJT-UHFFFAOYSA-N 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 238000002296 dynamic light scattering Methods 0.000 description 1
- 230000001747 exhibiting effect Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- WSFSSNUMVMOOMR-UHFFFAOYSA-N formaldehyde Substances O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 description 1
- 239000008240 homogeneous mixture Substances 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 239000011261 inert gas Substances 0.000 description 1
- 239000003112 inhibitor Substances 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 125000001449 isopropyl group Chemical group [H]C([H])([H])C([H])(*)C([H])([H])[H] 0.000 description 1
- 239000002609 medium Substances 0.000 description 1
- 239000005055 methyl trichlorosilane Substances 0.000 description 1
- JLUFWMXJHAVVNN-UHFFFAOYSA-N methyltrichlorosilane Chemical compound C[Si](Cl)(Cl)Cl JLUFWMXJHAVVNN-UHFFFAOYSA-N 0.000 description 1
- 229910017604 nitric acid Inorganic materials 0.000 description 1
- 239000007800 oxidant agent Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- FJKROLUGYXJWQN-UHFFFAOYSA-N papa-hydroxy-benzoic acid Natural products OC(=O)C1=CC=C(O)C=C1 FJKROLUGYXJWQN-UHFFFAOYSA-N 0.000 description 1
- 150000004965 peroxy acids Chemical class 0.000 description 1
- 125000005496 phosphonium group Chemical class 0.000 description 1
- 229920000083 poly(allylamine) Polymers 0.000 description 1
- 229920000768 polyamine Polymers 0.000 description 1
- 229920000728 polyester Polymers 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 150000003141 primary amines Chemical class 0.000 description 1
- 125000001453 quaternary ammonium group Chemical class 0.000 description 1
- 239000012495 reaction gas Substances 0.000 description 1
- 229960004889 salicylic acid Drugs 0.000 description 1
- 150000003335 secondary amines Chemical class 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- FDNAPBUWERUEDA-UHFFFAOYSA-N silicon tetrachloride Chemical compound Cl[Si](Cl)(Cl)Cl FDNAPBUWERUEDA-UHFFFAOYSA-N 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 230000006641 stabilisation Effects 0.000 description 1
- 238000011105 stabilization Methods 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 230000000153 supplemental effect Effects 0.000 description 1
- 239000000725 suspension Substances 0.000 description 1
- ISIJQEHRDSCQIU-UHFFFAOYSA-N tert-butyl 2,7-diazaspiro[4.5]decane-7-carboxylate Chemical compound C1N(C(=O)OC(C)(C)C)CCCC11CNCC1 ISIJQEHRDSCQIU-UHFFFAOYSA-N 0.000 description 1
- 150000003512 tertiary amines Chemical group 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
- VXYADVIJALMOEQ-UHFFFAOYSA-K tris(lactato)aluminium Chemical compound CC(O)C(=O)O[Al](OC(=O)C(C)O)OC(=O)C(C)O VXYADVIJALMOEQ-UHFFFAOYSA-K 0.000 description 1
- 229920002554 vinyl polymer Polymers 0.000 description 1
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Classifications
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- 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
-
- 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
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J21/00—Catalysts comprising the elements, oxides, or hydroxides of magnesium, boron, aluminium, carbon, silicon, titanium, zirconium, or hafnium
- B01J21/06—Silicon, titanium, zirconium or hafnium; Oxides or hydroxides thereof
- B01J21/08—Silica
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
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- B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
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- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/0072—Preparation of particles, e.g. dispersion of droplets in an oil bath
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- B01J37/08—Heat treatment
- B01J37/082—Decomposition and pyrolysis
- B01J37/086—Decomposition of an organometallic compound, a metal complex or a metal salt of a carboxylic acid
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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
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- C01B33/021—Preparation
- C01B33/023—Preparation by reduction of silica or free silica-containing material
- C01B33/025—Preparation by reduction of silica or free silica-containing material with carbon or a solid carbonaceous material, i.e. carbo-thermal process
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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
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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
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- C01B33/141—Preparation of hydrosols or aqueous dispersions
- C01B33/1415—Preparation of hydrosols or aqueous dispersions by suspending finely divided silica in water
- C01B33/1417—Preparation of hydrosols or aqueous dispersions by suspending finely divided silica in water an aqueous dispersion being obtained
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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
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- C01B33/18—Preparation of finely divided silica neither in sol nor in gel form; After-treatment thereof
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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
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- 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
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Description
− 比表面積1m2あたり、SiO2100gにつきジブチルフタレート1.2g以下の比ジブチルフタレート吸収量および
− 比表面積1m2あたり、15mPas未満の比増粘作用
を示すことを特徴とする、5〜600m2/gの比表面積および500ppm未満の炭素含有率を有する、熱分解法により製造される二酸化ケイ素粉末を提供する。
− 蒸気状のテトラメトキシシラン(TMOS)および/またはテトラエトキシシラン(TEOS)を空気と一緒に、または酸素が富化された空気と一緒に、および別個に
− 水素、
− を、バーナーに供給し、かつ気体の混合物をバーナーに直列に接続された反応室中の火炎中で反応させ、かつ固体の反応生成物を公知の手段により気体流から分離し、
− その際、バーナー中のラムダ値は0.95〜1.5であり、かつ
− その際、反応室中のラムダ値が0.8〜1.6であるために十分な二次空気を反応室へ供給する
ことを特徴とする、本発明による二酸化ケイ素粉末を製造するための方法も提供する。
分析的測定
粉末の比表面積をDIN66131により測定する。
DBP値(g/100g)=(DBP消費量g/粒子の秤量g)×100。
テトラメトキシシラン1.5kg/hを180℃で蒸発させ、かつバーナーの中心管に導入する。さらに空気12m3/hを中心管へ導入する。中心管を取り巻いている管に水素1.8m3/hを供給する。気体混合物は、二次空気17m3/hが付加的に導入される反応室中で燃焼する。
脱イオン水36kgを60lのステンレススチールの回分式容器中に装入する。次いで熱分解法により製造された二酸化ケイ素6.4kgを、Ystral Conti−TDS 3の吸引管を使用して剪断条件下で吸引し、かつ吸引工程の終了時に剪断をさらに3000rpmで15分間継続する。
脱イオン水35.5kgおよび30%のKOH溶液52gを60lのステンレススチールの回分式容器中に装入する。次いで熱分解法により製造された二酸化ケイ素6.4kgを、Ystral Conti−TDS 3の吸引管を使用して剪断条件下で吸引し、かつ吸引工程の終了時に剪断をさらに3000rpmで15分間継続する。この15分間の分散の間にKOH溶液をさらに添加することによりpHを10.4に調節し、かつ維持する。この工程でKOH溶液43gをさらに使用し、かつ水0.4kgの添加により15質量%の固体濃度が確立される。
脱イオン水35kgを60lのステンレススチールの回分式容器中に装入する。次いで熱分解法により製造された二酸化ケイ素6.4kgを、Ystral Conti−TDS 3の吸引管を使用して剪断条件下で吸引する。次いで塩化アルミニウムの1質量%溶液(酸化アルミニウムに対する)640gを分散液と共に添加し、かつ吸引工程の終了時に剪断をさらに3000rpmで15分間継続する。脱イオン水0.1kgおよび1NのNaOH305gを添加してpH3.5を有する15質量%の分散液が得られる。
脱イオン水35.5gおよび30%のKOH溶液52gを60lのステンレススチールの回分式容器中に装入する。次いでAEROSIL (R) 90 5.2kgをYstral Conti−TDS 3の吸引管を使用して剪断条件下で吸引し、かつ吸引工程の終了時に剪断をさらに3000rpmで15分間継続する。この15分間の分散の間に、KOH溶液をさらに添加することによりpHを10.4に調節し、かつ維持する。この工程でさらにKOH溶液を63g使用し、かつ水0.6kgの添加により15質量%の固体濃度が確立される。
60lのステンレススチール回分式容器中の脱イオン水35.5kgを水酸化テトラメチルアンモニウム溶液(25%)によりpH11に調節する。次いで熱分解法により製造された二酸化ケイ素37kgを、Ystral Conti−TDS 3の吸引管を使用して剪断条件下で吸引し、かつ吸引工程の終了時に剪断をさらに3000rpmで15分間継続する。この15分間の分散の間に水酸化テトラメチルアンモニウムをさらに添加することによりpHを10〜11に維持する。必要とされる水の残りの量の添加により50質量%の固体濃度が確立される。
Claims (12)
- 5〜600m2/gの比表面積および500ppm未満の炭素含有量を有する熱分解法により製造された二酸化ケイ素粉末において、
− 比表面積1m2あたり、ジブチルフタレート1.2g/100gSiO2以下の比ジブチルフタレート吸収量、
− 比表面積1m2あたり、15mPas未満の比増粘作用
を有し、かつ塩化物含有量が50ppm未満であることを特徴とする、熱分解法により製造された二酸化ケイ素粉末。 - 比圧縮かさ密度が1000〜10000g/l×m2比表面積である、請求項1記載の二酸化ケイ素粉末。
- 請求項1または2記載の二酸化ケイ素粉末の製造方法において、
− 蒸気状のテトラメトキシシランおよび/またはテトラエトキシシランを空気と一緒に、または酸素が富化された空気と一緒に、および
− 別個に水素、
− を、バーナーに供給し、かつ気体の混合物をバーナーに直列に接続された反応室中の火炎中で反応させ、かつ固体の反応生成物を気体流から分離し、
− その際、バーナー中のラムダ値は0.95〜1.5であり、かつ
− その際、反応室中のラムダ値が0.8〜1.6であるために十分な二次空気を反応室へ供給する
ことを特徴とする、請求項1または2記載の二酸化ケイ素粉末の製造方法。 - バーナー中の酸素/水素の体積比が0.2〜2.8である、請求項3記載の方法。
- バーナーを出る気体の排出速度が少なくとも10ms−1である、請求項3または4記載の方法。
- 請求項1または2記載の二酸化ケイ素粉末を含有する水性分散液。
- 分散液中の二酸化ケイ素の含有率が20〜80質量%である、請求項6記載の水性分散液。
- 分散液中の凝集体の平均直径が200nm未満である、請求項6または7記載の水性分散液。
- 添加剤を含有する、請求項6から8までのいずれか1項記載の水性分散液。
- 請求項6から9までのいずれか1項記載の水性分散液の製造方法において、請求項1または2記載の二酸化ケイ素粉末を分散装置により水中へ混合し、これを塩基またはカチオン性ポリマーまたはアルミニウム塩またはカチオン性ポリマーとアルミニウム塩との混合物または酸の添加により安定化することができ、かつ次いで分散させることを特徴とする、請求項6から9までのいずれか1項記載の水性分散液の製造方法。
- ゴム、シリコーンゴムまたはプラスチック中の充填材として、塗料のレオロジーを調節するため、または、触媒のための担体としての分散液中での請求項1または2記載の二酸化ケイ素粉末の使用。
- ガラス製品を製造するため、化学的機械的研磨のため、または、インクジェット紙を製造するための、請求項6から9までのいずれか1項記載の分散液の使用。
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DE10312970A DE10312970A1 (de) | 2003-03-24 | 2003-03-24 | Pyrogenes Siliciumdioxidpulver und Dispersion hiervon |
PCT/EP2004/002664 WO2004085311A1 (en) | 2003-03-24 | 2004-03-15 | Pyrogenic silicon dioxide powder and dispersion thereof |
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EP (1) | EP1606218B1 (ja) |
JP (1) | JP4550804B2 (ja) |
KR (1) | KR101143130B1 (ja) |
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DE102005027720A1 (de) * | 2005-06-16 | 2006-12-21 | Degussa Ag | Alkalimetalloxid enthaltendes Mischoxidpulver und Siliconkautschuk enthaltend dieses Pulver |
US8087450B2 (en) | 2007-01-29 | 2012-01-03 | Evonik Degussa Corporation | Fumed metal oxides for investment casting |
US7989506B2 (en) | 2007-04-04 | 2011-08-02 | Eastman Kodak Company | Method and apparatus for dispersion of high-surface-area, low-bulk-density fumed silica |
DE502007006418D1 (de) * | 2007-05-21 | 2011-03-17 | Evonik Degussa Gmbh | Pyrogen hergestelltes Siliciumdioxid mit niedriger Verdickungswirkung |
DE102007025685A1 (de) * | 2007-06-01 | 2008-12-04 | Evonik Degussa Gmbh | RTV-Zweikomponenten-Silikonkautschuk |
EP2014622B1 (de) * | 2007-07-06 | 2017-01-18 | Evonik Degussa GmbH | Verfahren zur Herstellung eines Kieselglasgranulats |
CN101185854B (zh) * | 2007-08-29 | 2011-10-05 | 江南大学 | 掺杂二氧化硅的硅橡胶富氧膜及其制备方法 |
DE102007059861A1 (de) * | 2007-12-12 | 2009-06-18 | Evonik Degussa Gmbh | Verfahren zur Herstellung von Siliciumdioxid-Dispersionen |
US8729158B2 (en) | 2008-09-05 | 2014-05-20 | Cabot Corporation | Fumed silica of controlled aggregate size and processes for manufacturing the same |
US8038971B2 (en) | 2008-09-05 | 2011-10-18 | Cabot Corporation | Fumed silica of controlled aggregate size and processes for manufacturing the same |
DE102008064284A1 (de) | 2008-12-20 | 2010-06-24 | Evonik Degussa Gmbh | Niedrigoberflächiges, pyrogen hergestelltes Siliciumdioxidpulver |
JP5774283B2 (ja) * | 2010-04-08 | 2015-09-09 | 株式会社フジミインコーポレーテッド | 研磨用組成物及び研磨方法 |
DE102010031585A1 (de) | 2010-07-21 | 2012-01-26 | Evonik Degussa Gmbh | Siliciumdioxidpulver mit speziellen Oberflächeneigenschaften und dieses Pulver enthaltende Tonerzusammensetzung |
DE102013206266A1 (de) * | 2013-04-10 | 2014-10-16 | Wacker Chemie Ag | Vernetzbare Massen auf der Basis von Organosiliciumverbindungen |
EP3019269B1 (de) * | 2013-07-11 | 2018-08-08 | Evonik Degussa GmbH | Verfahren zur herstellung von kieselsäure mit variabler verdickung |
US10676388B2 (en) | 2015-12-18 | 2020-06-09 | Heraeus Quarzglas Gmbh & Co. Kg | Glass fibers and pre-forms made of homogeneous quartz glass |
JP7044454B2 (ja) | 2015-12-18 | 2022-03-30 | ヘレウス クワルツグラス ゲーエムベーハー ウント コンパニー カーゲー | 石英ガラス調製時の中間体としての炭素ドープ二酸化ケイ素造粒体の調製 |
JP6984897B2 (ja) | 2015-12-18 | 2021-12-22 | ヘレウス クワルツグラス ゲーエムベーハー ウント コンパニー カーゲー | 石英ガラス調製時のケイ素含有量の増大 |
CN109153593A (zh) | 2015-12-18 | 2019-01-04 | 贺利氏石英玻璃有限两合公司 | 合成石英玻璃粉粒的制备 |
WO2017103166A2 (de) | 2015-12-18 | 2017-06-22 | Heraeus Quarzglas Gmbh & Co. Kg | Herstellung eines quarzglaskörpers in einem mehrkammerofen |
US11053152B2 (en) | 2015-12-18 | 2021-07-06 | Heraeus Quarzglas Gmbh & Co. Kg | Spray granulation of silicon dioxide in the preparation of quartz glass |
TWI812586B (zh) | 2015-12-18 | 2023-08-21 | 德商何瑞斯廓格拉斯公司 | 石英玻璃體、其製備方法與應用、及用於控制烘箱出口處之露點 |
KR20180095624A (ko) | 2015-12-18 | 2018-08-27 | 헤래우스 크바르츠글라스 게엠베하 & 컴파니 케이지 | 불투명 실리카 유리 제품의 제조 |
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TWI813534B (zh) | 2015-12-18 | 2023-09-01 | 德商何瑞斯廓格拉斯公司 | 利用露點監測在熔融烘箱中製備石英玻璃體 |
CN109715557A (zh) * | 2017-07-13 | 2019-05-03 | 瓦克化学股份公司 | 用于生产高分散二氧化硅的方法 |
US11499930B2 (en) | 2019-07-25 | 2022-11-15 | Saudi Arabian Oil Company | Measurement of chloride content in catalysts |
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US4292290A (en) * | 1980-04-16 | 1981-09-29 | Cabot Corporation | Process for the production of finely-divided metal and metalloid oxides |
US6193795B1 (en) * | 1993-08-02 | 2001-02-27 | Degussa Corporation | Low structure pyrogenic hydrophilic and hydrophobic metallic oxides, production and use |
DE19530339A1 (de) * | 1995-08-18 | 1997-02-20 | Degussa | Pyrogene Kieselsäure, Verfahren zu ihrer Herstellung und Verwendung |
US6679945B2 (en) * | 2000-08-21 | 2004-01-20 | Degussa Ag | Pyrogenically prepared silicon dioxide |
EP1182168B1 (de) | 2000-08-21 | 2004-05-12 | Degussa AG | Pyrogen hergestelltes Siliciumdioxid |
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US7534409B2 (en) | 2009-05-19 |
US20060201647A1 (en) | 2006-09-14 |
ATE435837T1 (de) | 2009-07-15 |
CN1330571C (zh) | 2007-08-08 |
EP1606218B1 (en) | 2009-07-08 |
KR101143130B1 (ko) | 2012-05-08 |
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