JP6374601B2 - 赤色酸化鉄顔料の製造 - Google Patents
赤色酸化鉄顔料の製造 Download PDFInfo
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- JP6374601B2 JP6374601B2 JP2017512819A JP2017512819A JP6374601B2 JP 6374601 B2 JP6374601 B2 JP 6374601B2 JP 2017512819 A JP2017512819 A JP 2017512819A JP 2017512819 A JP2017512819 A JP 2017512819A JP 6374601 B2 JP6374601 B2 JP 6374601B2
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- Prior art keywords
- iron
- hematite
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- pigment
- reaction
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- 238000004519 manufacturing process Methods 0.000 title description 11
- 239000001034 iron oxide pigment Substances 0.000 title description 7
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 title description 4
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 250
- LIKBJVNGSGBSGK-UHFFFAOYSA-N iron(3+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Fe+3].[Fe+3] LIKBJVNGSGBSGK-UHFFFAOYSA-N 0.000 claims description 123
- 229910052595 hematite Inorganic materials 0.000 claims description 100
- 239000011019 hematite Substances 0.000 claims description 99
- 229910052742 iron Inorganic materials 0.000 claims description 91
- 238000000034 method Methods 0.000 claims description 86
- 239000007789 gas Substances 0.000 claims description 81
- 230000008569 process Effects 0.000 claims description 77
- 239000000049 pigment Substances 0.000 claims description 73
- 239000000725 suspension Substances 0.000 claims description 68
- MVFCKEFYUDZOCX-UHFFFAOYSA-N iron(2+);dinitrate Chemical compound [Fe+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O MVFCKEFYUDZOCX-UHFFFAOYSA-N 0.000 claims description 58
- 238000006243 chemical reaction Methods 0.000 claims description 47
- 239000007791 liquid phase Substances 0.000 claims description 45
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 27
- 239000001301 oxygen Substances 0.000 claims description 27
- 229910052760 oxygen Inorganic materials 0.000 claims description 27
- 239000011541 reaction mixture Substances 0.000 claims description 23
- 239000000203 mixture Substances 0.000 claims description 15
- 239000002245 particle Substances 0.000 claims description 14
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 12
- 230000035484 reaction time Effects 0.000 claims description 8
- 238000007796 conventional method Methods 0.000 claims description 5
- 229910000859 α-Fe Inorganic materials 0.000 claims description 3
- 230000004048 modification Effects 0.000 claims description 2
- 238000012986 modification Methods 0.000 claims description 2
- 239000007900 aqueous suspension Substances 0.000 claims 4
- MWUXSHHQAYIFBG-UHFFFAOYSA-N nitrogen oxide Inorganic materials O=[N] MWUXSHHQAYIFBG-UHFFFAOYSA-N 0.000 description 48
- 239000000243 solution Substances 0.000 description 34
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 description 33
- GQPLMRYTRLFLPF-UHFFFAOYSA-N Nitrous Oxide Chemical compound [O-][N+]#N GQPLMRYTRLFLPF-UHFFFAOYSA-N 0.000 description 28
- 238000002156 mixing Methods 0.000 description 19
- 235000013980 iron oxide Nutrition 0.000 description 17
- 239000001054 red pigment Substances 0.000 description 14
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 10
- 229910017604 nitric acid Inorganic materials 0.000 description 10
- 230000003647 oxidation Effects 0.000 description 9
- 238000007254 oxidation reaction Methods 0.000 description 9
- 238000012360 testing method Methods 0.000 description 8
- 238000005086 pumping Methods 0.000 description 7
- 238000000576 coating method Methods 0.000 description 6
- 229960001730 nitrous oxide Drugs 0.000 description 6
- 229910000831 Steel Inorganic materials 0.000 description 5
- 239000011248 coating agent Substances 0.000 description 5
- 238000001035 drying Methods 0.000 description 5
- 239000012065 filter cake Substances 0.000 description 5
- 238000005259 measurement Methods 0.000 description 5
- 235000013842 nitrous oxide Nutrition 0.000 description 5
- 238000000926 separation method Methods 0.000 description 5
- 239000007858 starting material Substances 0.000 description 5
- 239000010959 steel Substances 0.000 description 5
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 4
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 4
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 4
- 208000032400 Retinal pigmentation Diseases 0.000 description 4
- 239000007788 liquid Substances 0.000 description 4
- 238000001556 precipitation Methods 0.000 description 4
- 239000007787 solid Substances 0.000 description 4
- 238000003756 stirring Methods 0.000 description 4
- -1 surface coatings Substances 0.000 description 4
- CWYNVVGOOAEACU-UHFFFAOYSA-N Fe2+ Chemical compound [Fe+2] CWYNVVGOOAEACU-UHFFFAOYSA-N 0.000 description 3
- 229910002651 NO3 Inorganic materials 0.000 description 3
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 description 3
- 229920000180 alkyd Polymers 0.000 description 3
- 150000003868 ammonium compounds Chemical class 0.000 description 3
- 239000012298 atmosphere Substances 0.000 description 3
- 150000002505 iron Chemical class 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 229910052751 metal Inorganic materials 0.000 description 3
- 239000002184 metal Substances 0.000 description 3
- 239000001272 nitrous oxide Substances 0.000 description 3
- 230000001590 oxidative effect Effects 0.000 description 3
- 230000002093 peripheral effect Effects 0.000 description 3
- 239000004033 plastic Substances 0.000 description 3
- 229920003023 plastic Polymers 0.000 description 3
- 238000007873 sieving Methods 0.000 description 3
- 239000007921 spray Substances 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 2
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 description 2
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 2
- CBENFWSGALASAD-UHFFFAOYSA-N Ozone Chemical compound [O-][O+]=O CBENFWSGALASAD-UHFFFAOYSA-N 0.000 description 2
- 238000013019 agitation Methods 0.000 description 2
- 239000007864 aqueous solution Substances 0.000 description 2
- 230000008901 benefit Effects 0.000 description 2
- 239000004566 building material Substances 0.000 description 2
- OZECDDHOAMNMQI-UHFFFAOYSA-H cerium(3+);trisulfate Chemical compound [Ce+3].[Ce+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O OZECDDHOAMNMQI-UHFFFAOYSA-H 0.000 description 2
- 229910000333 cerium(III) sulfate Inorganic materials 0.000 description 2
- 229910052804 chromium Inorganic materials 0.000 description 2
- 239000011651 chromium Substances 0.000 description 2
- 229910052802 copper Inorganic materials 0.000 description 2
- 239000010949 copper Substances 0.000 description 2
- 230000001419 dependent effect Effects 0.000 description 2
- 239000000539 dimer Substances 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 238000001914 filtration Methods 0.000 description 2
- 239000005431 greenhouse gas Substances 0.000 description 2
- BAUYGSIQEAFULO-UHFFFAOYSA-L iron(2+) sulfate (anhydrous) Chemical compound [Fe+2].[O-]S([O-])(=O)=O BAUYGSIQEAFULO-UHFFFAOYSA-L 0.000 description 2
- 229910000359 iron(II) sulfate Inorganic materials 0.000 description 2
- 238000004898 kneading Methods 0.000 description 2
- WPBNNNQJVZRUHP-UHFFFAOYSA-L manganese(2+);methyl n-[[2-(methoxycarbonylcarbamothioylamino)phenyl]carbamothioyl]carbamate;n-[2-(sulfidocarbothioylamino)ethyl]carbamodithioate Chemical compound [Mn+2].[S-]C(=S)NCCNC([S-])=S.COC(=O)NC(=S)NC1=CC=CC=C1NC(=S)NC(=O)OC WPBNNNQJVZRUHP-UHFFFAOYSA-L 0.000 description 2
- 150000002739 metals Chemical class 0.000 description 2
- 229910052759 nickel Inorganic materials 0.000 description 2
- 229910052757 nitrogen Inorganic materials 0.000 description 2
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 description 2
- 239000007800 oxidant agent Substances 0.000 description 2
- 239000003973 paint Substances 0.000 description 2
- 239000012071 phase Substances 0.000 description 2
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 2
- 239000004810 polytetrafluoroethylene Substances 0.000 description 2
- 238000003918 potentiometric titration Methods 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 239000000523 sample Substances 0.000 description 2
- 238000004062 sedimentation Methods 0.000 description 2
- 230000009974 thixotropic effect Effects 0.000 description 2
- 239000011800 void material Substances 0.000 description 2
- 238000005406 washing Methods 0.000 description 2
- 239000002351 wastewater Substances 0.000 description 2
- MGWGWNFMUOTEHG-UHFFFAOYSA-N 4-(3,5-dimethylphenyl)-1,3-thiazol-2-amine Chemical compound CC1=CC(C)=CC(C=2N=C(N)SC=2)=C1 MGWGWNFMUOTEHG-UHFFFAOYSA-N 0.000 description 1
- PMVSDNDAUGGCCE-TYYBGVCCSA-L Ferrous fumarate Chemical compound [Fe+2].[O-]C(=O)\C=C\C([O-])=O PMVSDNDAUGGCCE-TYYBGVCCSA-L 0.000 description 1
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 description 1
- IOVCWXUNBOPUCH-UHFFFAOYSA-M Nitrite anion Chemical compound [O-]N=O IOVCWXUNBOPUCH-UHFFFAOYSA-M 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 description 1
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 description 1
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- 230000032683 aging Effects 0.000 description 1
- 229910052783 alkali metal Inorganic materials 0.000 description 1
- 150000001340 alkali metals Chemical class 0.000 description 1
- 229910052784 alkaline earth metal Inorganic materials 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 239000008346 aqueous phase Substances 0.000 description 1
- 229910001566 austenite Inorganic materials 0.000 description 1
- 239000002585 base Substances 0.000 description 1
- 238000005452 bending Methods 0.000 description 1
- 239000011230 binding agent Substances 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 239000011449 brick Substances 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 239000001569 carbon dioxide Substances 0.000 description 1
- 229910002092 carbon dioxide Inorganic materials 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 238000005119 centrifugation Methods 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 239000007795 chemical reaction product Substances 0.000 description 1
- 239000010941 cobalt Substances 0.000 description 1
- 229910017052 cobalt Inorganic materials 0.000 description 1
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 1
- 239000003086 colorant Substances 0.000 description 1
- 238000004737 colorimetric analysis Methods 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 239000000356 contaminant Substances 0.000 description 1
- 239000002872 contrast media Substances 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 230000008878 coupling Effects 0.000 description 1
- 238000010168 coupling process Methods 0.000 description 1
- 238000005859 coupling reaction Methods 0.000 description 1
- 210000003298 dental enamel Anatomy 0.000 description 1
- 230000000779 depleting effect Effects 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 238000005562 fading Methods 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
- 238000004817 gas chromatography Methods 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 229910052598 goethite Inorganic materials 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 230000002706 hydrostatic effect Effects 0.000 description 1
- AEIXRCIKZIZYPM-UHFFFAOYSA-M hydroxy(oxo)iron Chemical compound [O][Fe]O AEIXRCIKZIZYPM-UHFFFAOYSA-M 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 239000003317 industrial substance Substances 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- VBMVTYDPPZVILR-UHFFFAOYSA-N iron(2+);oxygen(2-) Chemical class [O-2].[Fe+2] VBMVTYDPPZVILR-UHFFFAOYSA-N 0.000 description 1
- SZVJSHCCFOBDDC-UHFFFAOYSA-N iron(II,III) oxide Inorganic materials O=[Fe]O[Fe]O[Fe]=O SZVJSHCCFOBDDC-UHFFFAOYSA-N 0.000 description 1
- 239000011553 magnetic fluid Substances 0.000 description 1
- 229910052748 manganese Inorganic materials 0.000 description 1
- 239000011572 manganese Substances 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 238000005555 metalworking Methods 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- DOTMOQHOJINYBL-UHFFFAOYSA-N molecular nitrogen;molecular oxygen Chemical compound N#N.O=O DOTMOQHOJINYBL-UHFFFAOYSA-N 0.000 description 1
- JCXJVPUVTGWSNB-UHFFFAOYSA-N nitrogen dioxide Inorganic materials O=[N]=O JCXJVPUVTGWSNB-UHFFFAOYSA-N 0.000 description 1
- 230000037361 pathway Effects 0.000 description 1
- 239000012256 powdered iron Substances 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 239000012266 salt solution Substances 0.000 description 1
- 239000012488 sample solution Substances 0.000 description 1
- 238000005201 scrubbing Methods 0.000 description 1
- 239000013049 sediment Substances 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 229910052938 sodium sulfate Inorganic materials 0.000 description 1
- 235000011152 sodium sulphate Nutrition 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 229910001220 stainless steel Inorganic materials 0.000 description 1
- 239000010935 stainless steel Substances 0.000 description 1
- 239000010936 titanium Substances 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- 238000004448 titration Methods 0.000 description 1
- 238000003325 tomography Methods 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
- 229910006299 γ-FeOOH Inorganic materials 0.000 description 1
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Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/24—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by centrifugal force
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/26—Drying gases or vapours
- B01D53/266—Drying gases or vapours by filtration
-
- 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
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G49/00—Compounds of iron
- C01G49/02—Oxides; Hydroxides
- C01G49/06—Ferric oxide [Fe2O3]
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
- C09C1/22—Compounds of iron
- C09C1/24—Oxides of iron
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D17/00—Pigment pastes, e.g. for mixing in paints
- C09D17/004—Pigment pastes, e.g. for mixing in paints containing an inorganic pigment
- C09D17/007—Metal oxide
-
- C—CHEMISTRY; METALLURGY
- 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
-
- C—CHEMISTRY; METALLURGY
- 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
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/60—Optical properties, e.g. expressed in CIELAB-values
- C01P2006/63—Optical properties, e.g. expressed in CIELAB-values a* (red-green axis)
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/10—Inorganic compounds
- C02F2101/16—Nitrogen compounds, e.g. ammonia
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Nanotechnology (AREA)
- Inorganic Chemistry (AREA)
- Materials Engineering (AREA)
- Physics & Mathematics (AREA)
- Crystallography & Structural Chemistry (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- General Physics & Mathematics (AREA)
- Analytical Chemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Composite Materials (AREA)
- Life Sciences & Earth Sciences (AREA)
- Wood Science & Technology (AREA)
- Manufacturing & Machinery (AREA)
- Compounds Of Iron (AREA)
- Pigments, Carbon Blacks, Or Wood Stains (AREA)
Description
1.窒素酸化物の放出。窒素酸化物(たとえば、酸化窒素系(nitorous)ガスのNO、NO2、およびN2O4、一般的に「NOx」と呼ばれる)は有毒であり、スモッグの原因となり、UV光の照射により大気中のオゾン層を破壊し、かつ温室効果ガスである。一酸化二窒素は特に、二酸化炭素よりも約300倍も強い温室効果ガスである。それに加えて、一酸化二窒素は、最も強力なオゾン破壊ガスであると今や考えられている。硝酸を使用するPennimanプロセスでは、酸化窒素系ガスのNOおよびNO2、さらには一酸化二窒素もかなりの量で生成する。
2.硝酸を使用するPennimanプロセスは、窒素含有廃水も生成し、それには、顕著な量の硝酸塩、亜硝酸塩、およびアンモニウム化合物が含まれる。
3.硝酸を使用するPennimanプロセスは、エネルギーの消費も極めて高く、なぜなら、外部の熱エネルギーを加えて、大容量の水溶液を60℃〜120℃の温度に上げなければならないからである。それらに加えて、その反応混合物中に酸化剤としての酸素含有ガスを導入することによって(スチームストリッピング)、その反応混合物からエネルギーが除去され、これは、熱として再び導入されなければならない。
・少なくとも鉄を、
・100nm以下の粒径および40m2/g〜150mg2/gのBET比表面積(DIN 66131に従って測定される)を有するヘマタイト核を含むヘマタイト核水性懸濁液、および
・硝酸鉄(II)溶液
と、少なくとも1種の酸素含有ガスの存在下、70〜99℃の温度で反応させて、ヘマタイト顔料の懸濁液を製造することを含む。
・ヘマタイト核懸濁液を少なくとも鉄に添加され、および
・ヘマタイト核懸濁液の添加の前、添加の後、または添加と同時のいずれかで、少なくともヘマタイト核懸濁液および鉄の混合物に対して、硝酸鉄(II)の濃度が無水Fe(NO3)2を基準に計算して0.1〜25g/液相(l)、好ましくは1〜20g/液相(l)であるように、硝酸鉄(II)溶液が添加されて、ヘマタイト顔料の懸濁液を製造することを特徴とする。
A:酸素含有ガス
Fe:鉄
AQ−Fe(NO3)2:硝酸鉄(II)溶液
S−Fe2O3:ヘマタイト核懸濁液
PAQ−Fe2O3:ヘマタイト顔料の懸濁液
H2O:水
NOX:窒素酸化物含有ストリーム(ヘマタイト顔料の懸濁液の製造からのオフガス)
1:ヘマタイト顔料の懸濁液を製造するための反応器
11:反応容器
12:鉄のための支持体(support)
13:ガス導入ユニット
111:硝酸鉄(II)溶液、ヘマタイト核懸濁液の入口
112:NOXの出口
113:ヘマタイト顔料の懸濁液の出口
114:液相の出口
115:液相の入口
2:撹拌装置
21:駆動部
22:駆動部と攪拌機との接続部
23:攪拌機
31:ポンプ
・機械的混合および/または水力学的混合による液相の混合を用いて実施され、および
・少なくとも1種の酸素含有ガスの導入が、6m3以下のガス容積/バッチ容積(m3)/時間、好ましくは0.2〜6m3のガス容積/バッチ容積(m3)/時間、特に好ましくは0.2〜5m3のガス容積/バッチ容積(m3)/時間、極めて特に好ましくは0.2〜3m3のガス容積/バッチ容積(m3)/時間のガス導入容積を用いて実施され、および
・ヘマタイト核懸濁液が少なくとも鉄に添加され、および
・ヘマタイト核懸濁液の添加の前、添加の後、または添加と同時に、少なくともヘマタイト核懸濁液および鉄の混合物に対して、硝酸鉄(II)の濃度が無水Fe(NO3)2を基準に計算して0.1〜25g/液相(l)、好ましくは1〜20g/液相(l)であるように、硝酸鉄(II)溶液が添加されて、ヘマタイト顔料の懸濁液を製造することを特徴とする。
鉄(II)および鉄(III)の定量滴定:
硝酸鉄(II)の含量は、塩酸を用いて酸性化させたサンプル溶液を、硫酸セリウム(III)を用いて電位差滴定することにより、鉄(II)含量を測定することによって間接的に求めることができる。
NOxの測定は、堀場製のガス分析計PG 250(化学ルミネセンス法)を用いて実施した。NOx生成についての情報は、顔料収量に対する比率として報告した(NO2として計算、NO2(g)/顔料(kg))。出発物質のヘマタイト核および硝酸鉄の製造で発生するNOx放出は含まれていない。
笑気ガスの測定は、定量的ガスクロマトグラフィー測定によるか、および/または赤外測定法によって実施した。N2O生成についての情報は、顔料収量に対する比率として報告した(N2O(g)/顔料(kg))。出発物質のヘマタイト核および硝酸鉄の製造で発生するN2O放出は含まれていない。
例1〜8は、同一の反応器において相当のスケール(使用した鉄の量、55〜60kg)で、同一の条件および同一の、出発物質の量対設定溶液の容積の相対比で実施した。使用された鉄は、一般的に過剰に存在する。変化させたパラメーターは次のものであった:単位体積あたりの導入したガスの量;撹拌(あり、なし);攪拌機速度;ポンプ循環(あり、なし);ポンプ輸送による循環量;流速。それぞれの例におけるこれらのパラメーターを表1に示す。
例9〜12は、同一の反応器において相当のスケール(使用した鉄の量、55〜60kg)で、同一の条件および同一の、出発物質の量対設定溶液の容積の相対比で実施した。使用された鉄は、一般的に過剰に存在する。変化させたパラメーターは次のものであった:単位体積あたりの導入ガス量;撹拌(あり、なし);ポンプ循環(あり、なし);硝酸鉄(II)溶液の導入(あり、なし)。それぞれの例におけるこれらのパラメーターを表1に示す。
Claims (7)
- ヘマタイト顔料を製造するためのプロセスであって、少なくとも鉄を、100nm以下の粒径および40m2/g〜150m2/gのBET比表面積(DIN 66131に従って測定される)を有するヘマタイト核を含むヘマタイト核水性懸濁液および硝酸鉄(II)溶液と、少なくとも1種の酸素含有ガスの存在下、70〜99℃の温度で反応させて、ヘマタイト顔料の懸濁液を製造することを含み、
前記ヘマタイト核水性懸濁液が少なくとも鉄に添加され、かつ、前記ヘマタイト核水性懸濁液の添加の前、添加の後、または添加と同時に、前記硝酸鉄(II)溶液が、少なくともヘマタイト核水性懸濁液および鉄の混合物に、無水Fe(NO 3 ) 2 を基準に計算して0.1〜25g/液相(l)の硝酸鉄(II)の濃度が全反応時間の80〜100%であるように添加されることを特徴とする、プロセス。 - 前記ヘマタイト顔料が所望の色合いを有するまで、前記反応が実施されることを特徴とする、請求項1に記載のプロセス。
- 慣用される方法によって、前記反応混合物から前記ヘマタイト顔料を分離することをさらに含む、請求項1または2のいずれか一項に記載のプロセス。
- 前記ヘマタイト顔料の懸濁液中に存在する前記ヘマタイト顔料が、α−Fe2O3変態形を有することを特徴とする、請求項1〜3のいずれか一項に記載のプロセス。
- 最初に少なくとも鉄が仕込まれ、次いで前記ヘマタイト核水性懸濁液が前記鉄に添加されることを特徴とする、請求項1〜4のいずれか一項に記載のプロセス。
- 最初に鉄と水との混合物が仕込まれ、次いで前記ヘマタイト核水性懸濁液が前記鉄と水との混合物に添加されることを特徴とする、請求項1〜5のいずれか一項に記載のプロセス。
- 最初に前記ヘマタイト核水性懸濁液が10〜99℃の温度で少なくとも鉄に添加され、前記添加の完了後、前記硝酸鉄(II)溶液が70〜99℃の前記反応混合物の温度で添加されることを特徴とする、請求項1〜6のいずれか一項に記載のプロセス。
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US10563066B2 (en) * | 2014-09-11 | 2020-02-18 | Lanxess Deutschland Gmbh | Red iron-oxide pigments with improved colour values |
EP3216764A1 (de) | 2016-03-09 | 2017-09-13 | LANXESS Deutschland GmbH | Herstellung von eisenoxid-rot-pigmenten |
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EP3683190B1 (de) * | 2019-01-17 | 2022-03-09 | LANXESS Deutschland GmbH | Verfahren zur herstellung von hämatit pigmenten |
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US5421878A (en) | 1992-10-23 | 1995-06-06 | Bayer Ag | Pure-colored iron oxide direct red pigments, a process for their production and their use |
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JP4182669B2 (ja) | 2001-09-13 | 2008-11-19 | 戸田工業株式会社 | 粒状ヘマタイト粒子粉末の製造法 |
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