JP4280712B2 - 熱分解法二酸化ケイ素及びその分散液 - Google Patents
熱分解法二酸化ケイ素及びその分散液 Download PDFInfo
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- JP4280712B2 JP4280712B2 JP2004560434A JP2004560434A JP4280712B2 JP 4280712 B2 JP4280712 B2 JP 4280712B2 JP 2004560434 A JP2004560434 A JP 2004560434A JP 2004560434 A JP2004560434 A JP 2004560434A JP 4280712 B2 JP4280712 B2 JP 4280712B2
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- silicon dioxide
- dioxide powder
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- aqueous dispersion
- gas
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- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 title claims abstract description 69
- 239000006185 dispersion Substances 0.000 title claims abstract description 64
- 239000000377 silicon dioxide Substances 0.000 title abstract description 7
- 235000012239 silicon dioxide Nutrition 0.000 title abstract description 5
- 239000007789 gas Substances 0.000 claims abstract description 56
- 239000000843 powder Substances 0.000 claims abstract description 41
- 239000001301 oxygen Substances 0.000 claims abstract description 28
- 229910052760 oxygen Inorganic materials 0.000 claims abstract description 28
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims abstract description 26
- 239000000203 mixture Substances 0.000 claims abstract description 25
- 150000003377 silicon compounds Chemical class 0.000 claims abstract description 9
- 239000011521 glass Substances 0.000 claims abstract description 5
- 239000000945 filler Substances 0.000 claims abstract description 4
- 229920001971 elastomer Polymers 0.000 claims abstract description 3
- 238000002156 mixing Methods 0.000 claims abstract description 3
- 239000004033 plastic Substances 0.000 claims abstract description 3
- 229920003023 plastic Polymers 0.000 claims abstract description 3
- 239000005060 rubber Substances 0.000 claims abstract description 3
- 229920002379 silicone rubber Polymers 0.000 claims abstract description 3
- 239000007787 solid Substances 0.000 claims abstract description 3
- 238000000034 method Methods 0.000 claims description 23
- 238000004519 manufacturing process Methods 0.000 claims description 15
- 239000002245 particle Substances 0.000 claims description 12
- 239000002253 acid Substances 0.000 claims description 11
- 238000011049 filling Methods 0.000 claims description 11
- AZDRQVAHHNSJOQ-UHFFFAOYSA-N alumane Chemical class [AlH3] AZDRQVAHHNSJOQ-UHFFFAOYSA-N 0.000 claims description 9
- 229920006317 cationic polymer Polymers 0.000 claims description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 9
- 229910004298 SiO 2 Inorganic materials 0.000 claims 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 claims description 5
- 239000005049 silicon tetrachloride Substances 0.000 claims description 5
- 239000000654 additive Substances 0.000 claims description 4
- 239000000567 combustion gas Substances 0.000 claims description 3
- 239000003054 catalyst Substances 0.000 claims description 2
- 239000000975 dye Substances 0.000 claims description 2
- 239000003973 paint Substances 0.000 claims description 2
- 238000005498 polishing Methods 0.000 claims description 2
- 238000000518 rheometry Methods 0.000 claims description 2
- 230000000996 additive effect Effects 0.000 claims 1
- 150000003961 organosilicon compounds Chemical class 0.000 claims 1
- 230000001698 pyrogenic effect Effects 0.000 abstract description 8
- 238000010276 construction Methods 0.000 abstract description 3
- 229910052681 coesite Inorganic materials 0.000 abstract 1
- 229910052906 cristobalite Inorganic materials 0.000 abstract 1
- 239000004945 silicone rubber Substances 0.000 abstract 1
- 229910052682 stishovite Inorganic materials 0.000 abstract 1
- 229910052905 tridymite Inorganic materials 0.000 abstract 1
- DOIRQSBPFJWKBE-UHFFFAOYSA-N dibutyl phthalate Chemical compound CCCCOC(=O)C1=CC=CC=C1C(=O)OCCCC DOIRQSBPFJWKBE-UHFFFAOYSA-N 0.000 description 25
- 238000006243 chemical reaction Methods 0.000 description 10
- WGTYBPLFGIVFAS-UHFFFAOYSA-M tetramethylammonium hydroxide Chemical compound [OH-].C[N+](C)(C)C WGTYBPLFGIVFAS-UHFFFAOYSA-M 0.000 description 8
- 238000001816 cooling Methods 0.000 description 7
- 239000001257 hydrogen Substances 0.000 description 7
- 229910052739 hydrogen Inorganic materials 0.000 description 7
- 238000009826 distribution Methods 0.000 description 6
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 5
- 238000003917 TEM image Methods 0.000 description 5
- 238000010521 absorption reaction Methods 0.000 description 5
- 230000000052 comparative effect Effects 0.000 description 5
- 238000005259 measurement Methods 0.000 description 5
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 4
- -1 aluminum hydroxide chloride Chemical compound 0.000 description 4
- 229910021485 fumed silica Inorganic materials 0.000 description 4
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 4
- 229910003902 SiCl 4 Inorganic materials 0.000 description 3
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 239000002585 base Substances 0.000 description 3
- 238000010191 image analysis Methods 0.000 description 3
- 239000011164 primary particle Substances 0.000 description 3
- 239000000047 product Substances 0.000 description 3
- 150000003839 salts Chemical class 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
- 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
- 150000007513 acids Chemical class 0.000 description 2
- VSCWAEJMTAWNJL-UHFFFAOYSA-K aluminium trichloride Chemical compound Cl[Al](Cl)Cl VSCWAEJMTAWNJL-UHFFFAOYSA-K 0.000 description 2
- 239000007795 chemical reaction product Substances 0.000 description 2
- 238000002485 combustion reaction Methods 0.000 description 2
- 150000002431 hydrogen Chemical class 0.000 description 2
- 230000007062 hydrolysis Effects 0.000 description 2
- 238000006460 hydrolysis reaction Methods 0.000 description 2
- 150000007522 mineralic acids Chemical class 0.000 description 2
- 150000007524 organic acids Chemical class 0.000 description 2
- 235000005985 organic acids Nutrition 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- XNGIFLGASWRNHJ-UHFFFAOYSA-N phthalic acid Chemical class OC(=O)C1=CC=CC=C1C(O)=O XNGIFLGASWRNHJ-UHFFFAOYSA-N 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 239000012495 reaction gas Substances 0.000 description 2
- YGSDEFSMJLZEOE-UHFFFAOYSA-N salicylic acid Chemical class OC(=O)C1=CC=CC=C1O YGSDEFSMJLZEOE-UHFFFAOYSA-N 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- 238000005303 weighing Methods 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
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-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
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-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
- 239000012190 activator Substances 0.000 description 1
- 229940037003 alum Drugs 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
- SMZOGRDCAXLAAR-UHFFFAOYSA-N aluminium isopropoxide Chemical compound [Al+3].CC(C)[O-].CC(C)[O-].CC(C)[O-] SMZOGRDCAXLAAR-UHFFFAOYSA-N 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
- 150000001412 amines Chemical class 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- 239000000908 ammonium hydroxide Substances 0.000 description 1
- BFNBIHQBYMNNAN-UHFFFAOYSA-N ammonium sulfate Chemical compound N.N.OS(O)(=O)=O BFNBIHQBYMNNAN-UHFFFAOYSA-N 0.000 description 1
- 229910052921 ammonium sulfate Inorganic materials 0.000 description 1
- 235000011130 ammonium sulphate Nutrition 0.000 description 1
- 239000002280 amphoteric surfactant Substances 0.000 description 1
- 125000000129 anionic group Chemical group 0.000 description 1
- 239000003945 anionic surfactant Substances 0.000 description 1
- 125000004429 atom Chemical group 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
- BVKZGUZCCUSVTD-UHFFFAOYSA-N carbonic acid Chemical class OC(O)=O BVKZGUZCCUSVTD-UHFFFAOYSA-N 0.000 description 1
- 150000001735 carboxylic acids Chemical class 0.000 description 1
- 125000002091 cationic group Chemical group 0.000 description 1
- 239000003093 cationic surfactant Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 239000007859 condensation product Substances 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- QGBSISYHAICWAH-UHFFFAOYSA-N dicyandiamide Chemical compound NC(N)=NC#N QGBSISYHAICWAH-UHFFFAOYSA-N 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 238000011156 evaluation Methods 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
- 239000000463 material Substances 0.000 description 1
- 239000003345 natural gas Substances 0.000 description 1
- 229910017604 nitric acid Inorganic materials 0.000 description 1
- 239000002736 nonionic surfactant Substances 0.000 description 1
- 239000007800 oxidant agent Substances 0.000 description 1
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 1
- 238000001139 pH measurement Methods 0.000 description 1
- FJKROLUGYXJWQN-UHFFFAOYSA-N papa-hydroxy-benzoic acid Chemical class 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 group 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 229920000083 poly(allylamine) Polymers 0.000 description 1
- 229920000768 polyamine Polymers 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- GRLPQNLYRHEGIJ-UHFFFAOYSA-J potassium aluminium sulfate Chemical compound [Al+3].[K+].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O GRLPQNLYRHEGIJ-UHFFFAOYSA-J 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 150000003141 primary amines Chemical class 0.000 description 1
- 238000000197 pyrolysis Methods 0.000 description 1
- 125000001453 quaternary ammonium group Chemical group 0.000 description 1
- 239000011541 reaction mixture Substances 0.000 description 1
- 229960004889 salicylic acid Drugs 0.000 description 1
- 150000003335 secondary amines Chemical class 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 238000003980 solgel method Methods 0.000 description 1
- 238000003860 storage Methods 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
- 230000008719 thickening Effects 0.000 description 1
- 238000004448 titration Methods 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
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-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C3/00—Glass compositions
- C03C3/04—Glass compositions containing silica
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- C01B33/113—Silicon oxides; Hydrates thereof
- C01B33/12—Silica; Hydrates thereof, e.g. lepidoic silicic acid
- C01B33/18—Preparation of finely divided silica neither in sol nor in gel form; After-treatment thereof
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
- B01F23/00—Mixing according to the phases to be mixed, e.g. dispersing or emulsifying
- B01F23/50—Mixing liquids with solids
-
- 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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- 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
-
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- 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
-
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- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- C01B33/113—Silicon oxides; Hydrates thereof
- C01B33/12—Silica; Hydrates thereof, e.g. lepidoic silicic acid
- C01B33/14—Colloidal silica, e.g. dispersions, gels, sols
- C01B33/141—Preparation of hydrosols or aqueous dispersions
- C01B33/1415—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
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- C01B33/113—Silicon oxides; Hydrates thereof
- C01B33/12—Silica; Hydrates thereof, e.g. lepidoic silicic acid
- C01B33/14—Colloidal silica, e.g. dispersions, gels, sols
- C01B33/146—After-treatment of sols
- C01B33/148—Concentration; Drying; Dehydration; Stabilisation; Purification
- C01B33/1485—Stabilisation, e.g. prevention of gelling; Purification
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- 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
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- Engineering & Computer Science (AREA)
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- Chemical Kinetics & Catalysis (AREA)
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- General Physics & Mathematics (AREA)
- Crystallography & Structural Chemistry (AREA)
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- Silicon Compounds (AREA)
- Medicinal Preparation (AREA)
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- Compositions Of Macromolecular Compounds (AREA)
Description
1. 2H2+O2→2H2O 2. SiCl4+2H2O→SiO2+4HCl
そのガス混合物の均一性のゆえに、反応条件、ひいては製造条件及び成長条件は各SiO2粒子について大部分は同じなので、非常に一様なかつ均一な粒子を形成することができる。よく知られた方法では酸素源として空気が使用される。よく知られた方法により製造される熱分解法シリカは、10〜600m2/gの比表面積を有する。
− 30〜90m2/gのBET表面積、
− 80以下のDBP指数
− 25000nm2の平均凝集体面積
− 1000nm未満の平均凝集体周囲長
を有し、その際、その凝集体の少なくとも70%が1300nm未満の周囲長を有する粉末によって解決される。
− 遊離酸素含有ガスの酸素含量を、ラムダ値が1以上であるように調整し、
− ガンマ値が1.2〜1.8であり、
− 処理量が0.1〜0.3kgのSiO2/m3(コアガス混合物)であり、
− 燃焼器口の高さでの火炎管における平均正規化ガス流速が少なくとも5m/秒である
ことを特徴とする方法を提供する。
− 四塩化ケイ素を使用すること、
− ラムダ値が1<ラムダ≦1.2であること、
− ガンマ値が1.6〜1.8であること、
− 処理量が0.1〜0.3kgのSiO2/m3(コアガス混合物)であること、
− 更に、燃焼器に導入される遊離酸素含有ガスの量に対して少なくとも二倍量の空気を火炎管に導入すること、及び
− 燃焼器口での供給原料のガス流速が40〜65m/秒(標準条件に関して)であること、及び
− 燃焼器口の高さでの火炎管における平均正規化ガス流速が8〜12m/秒であること
である。
BET表面積はDIN66131に従って測定される。
DBP指数(g/100g)=(消費されたDBP(g)/粒子の初期質量(g))×100
複雑な流動挙動を試験するためにプログラム可能で、標準的な回転棒を備えたレオメーターを粘度測定のために利用できた。
測定温度:室温(23℃)
分散速濃度:30質量%
手順:500mlの分散液を600mlのガラスビーカー中に入れ、そして室温で(測定センサによる統計的な温度記録)種々の剪断速度において試験する。
最大充填度=添加された粉末量[g]/(添加された粉末量[g]+最初に導入された水の量[g])×100
実施例1(比較例):
500kg/hのSiCl4を約90℃で気化させ、そして公知の構造の燃焼器の内管に輸送する。また145Nm3/hの水素と、35容量%の酸素含量を有する207Nm3/hの空気をこの管中に導入する。このガス混合物を水冷燃焼器の火炎管中で点火させ、燃焼させる。燃焼器口の高さでの火炎管における平均正規化ガス流速は0.7m/秒である。反応ガスの冷却後に、熱分解法二酸化ケイ素粉末をフィルタ及び/又はサイクロンを用いて塩化水素酸含有ガスから分離する。熱分解法二酸化ケイ素粉末を脱酸装置中で水蒸気及び空気で処理する。
実施例5(作業例):
400kg/hのSiCl4を約90℃で気化させ、そして公知の構造の燃焼器の内管に輸送する。また195Nm3/hの水素と、30容量%の酸素含量を有する303Nm3/hの空気をこの管中に導入する。このガス混合物を水冷燃焼器の火炎管中で点火させ、燃焼させる。燃焼器口の高さでの火炎管における平均正規化ガス流速は10m/秒である。反応ガスの冷却後に、熱分解二酸化ケイ素粉末をフィルタ及び/又はサイクロンを用いて塩化水素酸含有ガスから分離する。熱分解法二酸化ケイ素粉末を脱酸装置中で水蒸気及び空気で処理する。
実施例5からの本発明による二酸化ケイ素粉末を、分散条件下で少しずつ246.5kgの完全脱塩水に導入し、水酸化テトラメチルアンモニウムでpH11に調整した。Ystral社製のConti−TDS5型のローター−ステーター装置を用いて分散液にする。pHは水酸化テトラメチルアンモニウムを添加することにより10〜11の値に維持する。粉末の完全な取り込み後に、更に12分間の間、分散を継続する。
Claims (31)
- 熱分解法二酸化ケイ素粉末であって、
− 30〜90m2/gのBET表面積、
− 80以下のDBP指数
− 25000nm2未満の平均凝集体面積
− 1000nm未満の平均凝集体周囲長
を有し、その際、その凝集体の少なくとも70%が1300nm未満の周囲長を有する二酸化ケイ素粉末。 - BET表面積が35〜75m2/gである、請求項1記載の二酸化ケイ素粉末。
- DBP指数が60〜80である、請求項1又は2記載の二酸化ケイ素粉末。
- BET表面積が40〜60m2/gであり、かつDBP指数が60〜80である、請求項1から3までのいずれか1項記載の二酸化ケイ素粉末。
- 本発明による二酸化ケイ素粉末が多くとも20000nm2の平均凝集体面積を有する、請求項1から4までのいずれか1項記載の二酸化ケイ素粉末。
- BET表面積が40〜60m2/gであり、DBP指数が60〜80であり、かつ平均凝集体面積が15000〜20000nm2である、請求項1から5までのいずれか1項記載の二酸化ケイ素粉末。
- 1000nm未満の平均凝集体周囲長を有する、請求項1から6までのいずれか1項記載の二酸化ケイ素粉末。
- BET表面積が40〜60m2/gであり、DBP指数が60〜80であり、平均凝集体面積が1500〜20000nm2であり、かつ平均凝集体周囲長が600〜1000nmである、請求項1から7までのいずれか1項記載の二酸化ケイ素粉末。
- 水性分散液中の粉末の充填度が90質量%までである、請求項1から8までのいずれか1項記載の二酸化ケイ素粉末。
- 30質量%の水性分散液に関して剪断速度5rpmで100mPas未満の粘度を有する、請求項1から9までのいずれか1項記載の二酸化ケイ素粉末。
- 4%濃度の水性分散液中で測定されてpH3.8〜5を有する、請求項1から10までのいずれか1項記載の二酸化ケイ素粉末。
- 請求項1から11までのいずれか1項記載の本発明による二酸化ケイ素粉末の製造方法であって、蒸気状態の少なくとも1種のケイ素化合物、遊離酸素含有ガス及び燃焼ガスを公知の構造の燃焼器中で混合し、このガス混合物を燃焼器口で点火させ、そして燃焼器の火炎管内で燃焼させ、得られた固体をガス混合物から分離し、そして場合により精製することを含み、その際、
− 遊離酸素含有ガスの酸素含量を、ラムダ値が1以上であるように調整し、
− ガンマ値が1.2〜1.8であり、
− 処理量が0.1〜0.3kgのSiO2/m3(コアガス混合物)であり、
− 燃焼器口の高さでの火炎管における平均正規化ガス流速が少なくとも5m/秒である
ことを特徴とする方法。 - 遊離酸素含有ガスの酸素含量が40容量%以下である、請求項12記載の方法。
- 1<ラムダ≦1.2である、請求項12又は13記載の方法。
- 1.6<ガンマ≦1.8である、請求項12から14までのいずれか1項記載の方法。
- 燃焼器口の高さでの火炎管における平均正規化ガス流速が8m/秒より高い、請求項12から15までのいずれか1項記載の方法。
- 燃焼器口でのガス混合物の平均排出速度が少なくとも30m/秒である、請求項12から16までのいずれか1項記載の方法。
- 付加的な空気(二次空気)を火炎管中に導入する、請求項12から17までのいずれか1項記載の方法。
- 四塩化ケイ素及び/又は少なくとも1種の有機ケイ素化合物をケイ素化合物として使用する、請求項12から18までのいずれか1項記載の方法。
- 四塩化ケイ素を使用し、1<ラムダ≦1.2であり、1.6<ガンマ<1.8であり、処理量が0.1〜0.3kgのSiO2/m3(コアガス混合物)であり、更に、燃焼器に導入される遊離酸素含有ガスの量に対して少なくとも二倍量の空気を火炎管に導入し、かつ燃焼器口での供給原料の流速が40〜65m/秒であり、燃焼器口の高さでの火炎管における平均正規化ガス流速が8〜12m/秒である、請求項12から19までのいずれか1項記載の方法。
- 請求項1から11までのいずれか1項記載の二酸化ケイ素粉末を含有する水性分散液。
- 二酸化ケイ素粉末の濃度が20〜80質量%である、請求項21記載の水性分散液。
- 二酸化ケイ素粉末の濃度が40〜60質量%である、請求項21記載の水性分散液。
- 50質量%の分散液の粘度が剪断速度50rpmで2500mPas未満である、請求項21から23までのいずれか1項記載の水性分散液。
- 二酸化ケイ素粉末の平均粒径が200nm未満である、請求項21から24までのいずれか1項記載の水性分散液。
- 塩基の添加か、又はカチオン系ポリマーの添加か、又はアルミニウム塩の添加か、又はカチオン系ポリマーとアルミニウム塩との混合物の添加か、又は酸の添加によって安定化されている、請求項21から25までのいずれか1項記載の水性分散液。
- 添加剤を含有する、請求項21から26までのいずれか1項記載の水性分散液。
- 請求項21から27までのいずれか1項記載の水性分散液の製造方法であって、請求項1から4までのいずれか1項記載の二酸化ケイ素粉末を、分散装置を用いて水中に導入し、これを塩基の添加か、又はカチオン系ポリマーの添加か、又はアルミニウム塩の添加か、又はカチオン系ポリマーとアルミニウム塩との混合物の添加か、又は酸の添加により安定化してよく、かつ次いで更に5〜30分間分散させることを特徴とする方法。
- 分散装置としてローター−ステーター装置を使用する、請求項28記載の方法。
- 請求項1から11までのいずれか1項記載の二酸化ケイ素粉末の使用であって、ゴム、シリコーンゴム及びプラスチックにおける充填剤としての、染料及び塗料のレオロジーを調節するための、及び触媒の担体としての使用。
- 請求項21から27までのいずれか1項記載の分散液の使用であって、ガラス製品の製造のための、化学的−機械的ポリシングのための、及びインクジェット紙の製造のための使用。
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DE102005001410A1 (de) * | 2005-01-12 | 2006-07-20 | Degussa Ag | Pyrogen hergestelltes Siliciumdioxidpulver und Dispersion hiervon |
EP1700824A1 (en) | 2005-03-09 | 2006-09-13 | Degussa AG | Granules based on pyrogenically prepared silicon dioxide, method for their preparation and use thereof |
EP1700832A1 (en) * | 2005-03-09 | 2006-09-13 | Degussa AG | A method of producing glass of optical quality |
PL1700831T3 (pl) | 2005-03-09 | 2008-03-31 | Degussa Novara Tech S P A | Sposób wytwarzania monolitów za pomocą procesu zol-żel |
EP1700830A1 (en) | 2005-03-09 | 2006-09-13 | Novara Technology S.R.L. | Process for the production of monoliths by means of the invert sol-gel process |
EP1700828A1 (en) | 2005-03-09 | 2006-09-13 | Degussa AG | Method for producing ultra-high purity, optical quality, glass articles |
EP1700829A1 (en) * | 2005-03-09 | 2006-09-13 | Degussa AG | Process for the production of glass-monoliths by means of the sol-gel process |
EP1717202A1 (en) * | 2005-04-29 | 2006-11-02 | Degussa AG | Sintered silicon dioxide materials |
DE102006005093A1 (de) * | 2006-02-04 | 2007-08-09 | Degussa Ag | Siliciumdioxid und Polycarboxylatether enthaltende Dispersion |
DE102006030002A1 (de) * | 2006-06-29 | 2008-01-03 | Wacker Chemie Ag | Herstellung pyrogener Metalloxide in temperierten Reaktionskammern |
DE102006054156A1 (de) * | 2006-11-16 | 2008-05-21 | Wacker Chemie Ag | Pyrogene Kieselsäure hergestellt in einer Produktions-Anlage mit großer Kapazität |
ATE497483T1 (de) * | 2007-05-21 | 2011-02-15 | Evonik Degussa Gmbh | Pyrogen hergestelltes siliciumdioxid mit niedriger verdickungswirkung |
EP2088128B1 (en) | 2007-12-10 | 2015-04-08 | Cristal Materials Corporation | Method for the production of glassy monoliths via the sol-gel process |
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CN103712951B (zh) * | 2013-12-31 | 2016-03-09 | 清华大学深圳研究生院 | 一种基于三维结构纳米阵列生物芯片的制备方法及其应用 |
US10730780B2 (en) | 2015-12-18 | 2020-08-04 | Heraeus Quarzglas Gmbh & Co. Kg | Preparation of a quartz glass body in a multi-chamber oven |
WO2017103120A1 (de) | 2015-12-18 | 2017-06-22 | Heraeus Quarzglas Gmbh & Co. Kg | Herstellung einer synthetischen quarzglaskörnung |
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JP6881776B2 (ja) | 2015-12-18 | 2021-06-02 | 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 | 不透明石英ガラス体の調製 |
KR20180095619A (ko) | 2015-12-18 | 2018-08-27 | 헤래우스 크바르츠글라스 게엠베하 & 컴파니 케이지 | 실리카 유리 제조 동안 규소 함량의 증가 |
US11053152B2 (en) | 2015-12-18 | 2021-07-06 | Heraeus Quarzglas Gmbh & Co. Kg | Spray granulation of silicon dioxide in the preparation of quartz glass |
TWI794150B (zh) | 2015-12-18 | 2023-03-01 | 德商何瑞斯廓格拉斯公司 | 自二氧化矽顆粒製備石英玻璃體 |
US11339076B2 (en) | 2015-12-18 | 2022-05-24 | Heraeus Quarzglas Gmbh & Co. Kg | Preparation of carbon-doped silicon dioxide granulate as an intermediate in the preparation of quartz glass |
EP3390308B1 (de) | 2015-12-18 | 2024-08-28 | Heraeus Quarzglas GmbH & Co. KG | Glasfasern aus quarzglas mit geringem oh-, cl- und al-gehalt |
WO2017103115A2 (de) | 2015-12-18 | 2017-06-22 | Heraeus Quarzglas Gmbh & Co. Kg | Herstellung eines quarzglaskörpers in einem schmelztiegel aus refraktärmetall |
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US6679945B2 (en) * | 2000-08-21 | 2004-01-20 | Degussa Ag | Pyrogenically prepared silicon dioxide |
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DE10326049A1 (de) | 2003-06-10 | 2004-12-30 | Degussa Ag | Flammenhydrolytisch hergestelltes Siliciumdioxid, Verfahren zu seiner Herstellung und Verwendung |
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