EP0000749A1 - Procédé de préparation d'oxyde ferrique aciculaire ferrimagnétique et son application - Google Patents
Procédé de préparation d'oxyde ferrique aciculaire ferrimagnétique et son application Download PDFInfo
- Publication number
- EP0000749A1 EP0000749A1 EP7878100535A EP78100535A EP0000749A1 EP 0000749 A1 EP0000749 A1 EP 0000749A1 EP 7878100535 A EP7878100535 A EP 7878100535A EP 78100535 A EP78100535 A EP 78100535A EP 0000749 A1 EP0000749 A1 EP 0000749A1
- Authority
- EP
- European Patent Office
- Prior art keywords
- iron
- iii
- acicular
- oxides
- oxide
- 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.)
- Granted
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- UQSXHKLRYXJYBZ-UHFFFAOYSA-N iron oxide Inorganic materials [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 title claims abstract description 24
- 235000013980 iron oxide Nutrition 0.000 title claims abstract description 21
- 238000000034 method Methods 0.000 title claims abstract description 20
- VBMVTYDPPZVILR-UHFFFAOYSA-N iron(2+);oxygen(2-) Chemical class [O-2].[Fe+2] VBMVTYDPPZVILR-UHFFFAOYSA-N 0.000 title claims abstract description 19
- 230000005293 ferrimagnetic effect Effects 0.000 title claims abstract description 11
- 239000000203 mixture Substances 0.000 claims abstract description 28
- 230000005291 magnetic effect Effects 0.000 claims abstract description 26
- AEIXRCIKZIZYPM-UHFFFAOYSA-M hydroxy(oxo)iron Chemical compound [O][Fe]O AEIXRCIKZIZYPM-UHFFFAOYSA-M 0.000 claims abstract description 19
- IEECXTSVVFWGSE-UHFFFAOYSA-M iron(3+);oxygen(2-);hydroxide Chemical class [OH-].[O-2].[Fe+3] IEECXTSVVFWGSE-UHFFFAOYSA-M 0.000 claims abstract description 13
- 230000003647 oxidation Effects 0.000 claims abstract description 11
- 238000007254 oxidation reaction Methods 0.000 claims abstract description 11
- 230000008569 process Effects 0.000 claims abstract description 11
- LIKBJVNGSGBSGK-UHFFFAOYSA-N iron(3+);oxygen(2-) Chemical class [O-2].[O-2].[O-2].[Fe+3].[Fe+3] LIKBJVNGSGBSGK-UHFFFAOYSA-N 0.000 claims abstract description 10
- 238000004519 manufacturing process Methods 0.000 claims abstract description 8
- 229910052598 goethite Inorganic materials 0.000 claims abstract description 7
- 150000002894 organic compounds Chemical class 0.000 claims abstract description 7
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims abstract description 6
- 239000001301 oxygen Substances 0.000 claims abstract description 6
- 229910052760 oxygen Inorganic materials 0.000 claims abstract description 6
- 230000009467 reduction Effects 0.000 claims abstract description 6
- 229910000462 iron(III) oxide hydroxide Inorganic materials 0.000 claims abstract description 5
- 229910021519 iron(III) oxide-hydroxide Inorganic materials 0.000 claims abstract description 5
- 239000007789 gas Substances 0.000 claims abstract description 4
- 239000000696 magnetic material Substances 0.000 claims description 4
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 18
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 15
- 238000006243 chemical reaction Methods 0.000 description 12
- SZVJSHCCFOBDDC-UHFFFAOYSA-N iron(II,III) oxide Inorganic materials O=[Fe]O[Fe]O[Fe]=O SZVJSHCCFOBDDC-UHFFFAOYSA-N 0.000 description 11
- 239000000243 solution Substances 0.000 description 9
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 8
- 239000000126 substance Substances 0.000 description 8
- -1 aliphatic monocarboxylic acids Chemical class 0.000 description 7
- 239000000047 product Substances 0.000 description 7
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 description 6
- 239000011261 inert gas Substances 0.000 description 6
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 6
- 238000003756 stirring Methods 0.000 description 6
- 239000006185 dispersion Substances 0.000 description 5
- 238000006722 reduction reaction Methods 0.000 description 5
- 239000000725 suspension Substances 0.000 description 5
- 238000001035 drying Methods 0.000 description 4
- 229910052757 nitrogen Inorganic materials 0.000 description 4
- 150000003839 salts Chemical class 0.000 description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 4
- RYHBNJHYFVUHQT-UHFFFAOYSA-N 1,4-Dioxane Chemical compound C1COCCO1 RYHBNJHYFVUHQT-UHFFFAOYSA-N 0.000 description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 3
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- 239000011230 binding agent Substances 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 238000005259 measurement Methods 0.000 description 3
- 239000007787 solid Substances 0.000 description 3
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 description 3
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 2
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 description 2
- YNAVUWVOSKDBBP-UHFFFAOYSA-N Morpholine Chemical compound C1COCCN1 YNAVUWVOSKDBBP-UHFFFAOYSA-N 0.000 description 2
- 235000021355 Stearic acid Nutrition 0.000 description 2
- LBPGGVGNNLPHBO-UHFFFAOYSA-N [N].OC Chemical compound [N].OC LBPGGVGNNLPHBO-UHFFFAOYSA-N 0.000 description 2
- WNLRTRBMVRJNCN-UHFFFAOYSA-N adipic acid Chemical compound OC(=O)CCCCC(O)=O WNLRTRBMVRJNCN-UHFFFAOYSA-N 0.000 description 2
- 239000003513 alkali Substances 0.000 description 2
- JZQOJFLIJNRDHK-CMDGGOBGSA-N alpha-irone Chemical compound CC1CC=C(C)C(\C=C\C(C)=O)C1(C)C JZQOJFLIJNRDHK-CMDGGOBGSA-N 0.000 description 2
- 239000012298 atmosphere Substances 0.000 description 2
- 229910001566 austenite Inorganic materials 0.000 description 2
- WERYXYBDKMZEQL-UHFFFAOYSA-N butane-1,4-diol Chemical compound OCCCCO WERYXYBDKMZEQL-UHFFFAOYSA-N 0.000 description 2
- 150000001735 carboxylic acids Chemical class 0.000 description 2
- 239000007795 chemical reaction product Substances 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 229920001577 copolymer Polymers 0.000 description 2
- 235000014113 dietary fatty acids Nutrition 0.000 description 2
- 239000003651 drinking water Substances 0.000 description 2
- 235000020188 drinking water Nutrition 0.000 description 2
- 239000000194 fatty acid Substances 0.000 description 2
- 229930195729 fatty acid Natural products 0.000 description 2
- 150000004665 fatty acids Chemical class 0.000 description 2
- 239000000706 filtrate Substances 0.000 description 2
- 238000001914 filtration Methods 0.000 description 2
- QGPQTSCLUYMZHL-UHFFFAOYSA-N iron(3+);oxygen(2-);hydrate Chemical compound O.[O-2].[O-2].[O-2].[Fe+3].[Fe+3] QGPQTSCLUYMZHL-UHFFFAOYSA-N 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 239000006247 magnetic powder Substances 0.000 description 2
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 2
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 description 2
- OQCDKBAXFALNLD-UHFFFAOYSA-N octadecanoic acid Natural products CCCCCCCC(C)CCCCCCCCC(O)=O OQCDKBAXFALNLD-UHFFFAOYSA-N 0.000 description 2
- 239000003921 oil Substances 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 239000000049 pigment Substances 0.000 description 2
- 229920000728 polyester Polymers 0.000 description 2
- 238000012545 processing Methods 0.000 description 2
- 239000008117 stearic acid Substances 0.000 description 2
- 239000001993 wax Substances 0.000 description 2
- 229910000859 α-Fe Inorganic materials 0.000 description 2
- 229910006540 α-FeOOH Inorganic materials 0.000 description 2
- IIZPXYDJLKNOIY-JXPKJXOSSA-N 1-palmitoyl-2-arachidonoyl-sn-glycero-3-phosphocholine Chemical compound CCCCCCCCCCCCCCCC(=O)OC[C@H](COP([O-])(=O)OCC[N+](C)(C)C)OC(=O)CCC\C=C/C\C=C/C\C=C/C\C=C/CCCCC IIZPXYDJLKNOIY-JXPKJXOSSA-N 0.000 description 1
- IEPRKVQEAMIZSS-UHFFFAOYSA-N Di-Et ester-Fumaric acid Natural products CCOC(=O)C=CC(=O)OCC IEPRKVQEAMIZSS-UHFFFAOYSA-N 0.000 description 1
- IEPRKVQEAMIZSS-WAYWQWQTSA-N Diethyl maleate Chemical compound CCOC(=O)\C=C/C(=O)OCC IEPRKVQEAMIZSS-WAYWQWQTSA-N 0.000 description 1
- VTLYFUHAOXGGBS-UHFFFAOYSA-N Fe3+ Chemical class [Fe+3] VTLYFUHAOXGGBS-UHFFFAOYSA-N 0.000 description 1
- 229910021577 Iron(II) chloride Inorganic materials 0.000 description 1
- 229920002472 Starch Polymers 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- BZHJMEDXRYGGRV-UHFFFAOYSA-N Vinyl chloride Chemical compound ClC=C BZHJMEDXRYGGRV-UHFFFAOYSA-N 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 239000001361 adipic acid Substances 0.000 description 1
- 235000011037 adipic acid Nutrition 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 150000001298 alcohols Chemical class 0.000 description 1
- 229910001854 alkali hydroxide Inorganic materials 0.000 description 1
- 150000008044 alkali metal hydroxides Chemical class 0.000 description 1
- 150000001412 amines Chemical class 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 239000007900 aqueous suspension Substances 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 125000004432 carbon atom Chemical group C* 0.000 description 1
- 239000000969 carrier Substances 0.000 description 1
- 239000003638 chemical reducing agent Substances 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 239000008367 deionised water Substances 0.000 description 1
- 229910021641 deionized water Inorganic materials 0.000 description 1
- LDCRTTXIJACKKU-ARJAWSKDSA-N dimethyl maleate Chemical compound COC(=O)\C=C/C(=O)OC LDCRTTXIJACKKU-ARJAWSKDSA-N 0.000 description 1
- 239000004205 dimethyl polysiloxane Substances 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 239000003925 fat Substances 0.000 description 1
- 230000005294 ferromagnetic effect Effects 0.000 description 1
- 239000011888 foil Substances 0.000 description 1
- 235000011187 glycerol Nutrition 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 229920001519 homopolymer Polymers 0.000 description 1
- 229930195733 hydrocarbon Natural products 0.000 description 1
- 150000002430 hydrocarbons Chemical class 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- NMCUIPGRVMDVDB-UHFFFAOYSA-L iron dichloride Chemical compound Cl[Fe]Cl NMCUIPGRVMDVDB-UHFFFAOYSA-L 0.000 description 1
- 235000010445 lecithin Nutrition 0.000 description 1
- 239000000787 lecithin Substances 0.000 description 1
- 229940067606 lecithin Drugs 0.000 description 1
- 230000005415 magnetization Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000007935 neutral effect Effects 0.000 description 1
- 230000006911 nucleation Effects 0.000 description 1
- 238000010899 nucleation Methods 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- NDLPOXTZKUMGOV-UHFFFAOYSA-N oxo(oxoferriooxy)iron hydrate Chemical compound O.O=[Fe]O[Fe]=O NDLPOXTZKUMGOV-UHFFFAOYSA-N 0.000 description 1
- 229920000435 poly(dimethylsiloxane) Polymers 0.000 description 1
- 229920000139 polyethylene terephthalate Polymers 0.000 description 1
- 239000005020 polyethylene terephthalate Substances 0.000 description 1
- 229920002635 polyurethane Polymers 0.000 description 1
- 239000004814 polyurethane Substances 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 239000012266 salt solution Substances 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 239000000344 soap Substances 0.000 description 1
- 239000008107 starch Substances 0.000 description 1
- 235000019698 starch Nutrition 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 229920001169 thermoplastic Polymers 0.000 description 1
- 239000004416 thermosoftening plastic Substances 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
- 229920002554 vinyl polymer Polymers 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
- 229910006299 γ-FeOOH Inorganic materials 0.000 description 1
Classifications
-
- G—PHYSICS
- G11—INFORMATION STORAGE
- G11B—INFORMATION STORAGE BASED ON RELATIVE MOVEMENT BETWEEN RECORD CARRIER AND TRANSDUCER
- G11B5/00—Recording by magnetisation or demagnetisation of a record carrier; Reproducing by magnetic means; Record carriers therefor
- G11B5/62—Record carriers characterised by the selection of the material
- G11B5/68—Record carriers characterised by the selection of the material comprising one or more layers of magnetisable material homogeneously mixed with a bonding agent
- G11B5/70—Record carriers characterised by the selection of the material comprising one or more layers of magnetisable material homogeneously mixed with a bonding agent on a base layer
- G11B5/706—Record carriers characterised by the selection of the material comprising one or more layers of magnetisable material homogeneously mixed with a bonding agent on a base layer characterised by the composition of the magnetic material
- G11B5/70626—Record carriers characterised by the selection of the material comprising one or more layers of magnetisable material homogeneously mixed with a bonding agent on a base layer characterised by the composition of the magnetic material containing non-metallic substances
- G11B5/70642—Record carriers characterised by the selection of the material comprising one or more layers of magnetisable material homogeneously mixed with a bonding agent on a base layer characterised by the composition of the magnetic material containing non-metallic substances iron oxides
- G11B5/70652—Record carriers characterised by the selection of the material comprising one or more layers of magnetisable material homogeneously mixed with a bonding agent on a base layer characterised by the composition of the magnetic material containing non-metallic substances iron oxides gamma - Fe2 O3
- G11B5/70663—Preparation processes specially adapted therefor, e.g. using stabilising agents
-
- 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]
-
- G—PHYSICS
- G11—INFORMATION STORAGE
- G11B—INFORMATION STORAGE BASED ON RELATIVE MOVEMENT BETWEEN RECORD CARRIER AND TRANSDUCER
- G11B5/00—Recording by magnetisation or demagnetisation of a record carrier; Reproducing by magnetic means; Record carriers therefor
- G11B5/62—Record carriers characterised by the selection of the material
-
- G—PHYSICS
- G11—INFORMATION STORAGE
- G11B—INFORMATION STORAGE BASED ON RELATIVE MOVEMENT BETWEEN RECORD CARRIER AND TRANSDUCER
- G11B5/00—Recording by magnetisation or demagnetisation of a record carrier; Reproducing by magnetic means; Record carriers therefor
- G11B5/62—Record carriers characterised by the selection of the material
- G11B5/68—Record carriers characterised by the selection of the material comprising one or more layers of magnetisable material homogeneously mixed with a bonding agent
- G11B5/70—Record carriers characterised by the selection of the material comprising one or more layers of magnetisable material homogeneously mixed with a bonding agent on a base layer
- G11B5/706—Record carriers characterised by the selection of the material comprising one or more layers of magnetisable material homogeneously mixed with a bonding agent on a base layer characterised by the composition of the magnetic material
- G11B5/70626—Record carriers characterised by the selection of the material comprising one or more layers of magnetisable material homogeneously mixed with a bonding agent on a base layer characterised by the composition of the magnetic material containing non-metallic substances
- G11B5/70642—Record carriers characterised by the selection of the material comprising one or more layers of magnetisable material homogeneously mixed with a bonding agent on a base layer characterised by the composition of the magnetic material containing non-metallic substances iron oxides
- G11B5/70647—Record carriers characterised by the selection of the material comprising one or more layers of magnetisable material homogeneously mixed with a bonding agent on a base layer characterised by the composition of the magnetic material containing non-metallic substances iron oxides with a skin
-
- G—PHYSICS
- G11—INFORMATION STORAGE
- G11B—INFORMATION STORAGE BASED ON RELATIVE MOVEMENT BETWEEN RECORD CARRIER AND TRANSDUCER
- G11B5/00—Recording by magnetisation or demagnetisation of a record carrier; Reproducing by magnetic means; Record carriers therefor
- G11B5/62—Record carriers characterised by the selection of the material
- G11B5/68—Record carriers characterised by the selection of the material comprising one or more layers of magnetisable material homogeneously mixed with a bonding agent
- G11B5/70—Record carriers characterised by the selection of the material comprising one or more layers of magnetisable material homogeneously mixed with a bonding agent on a base layer
- G11B5/706—Record carriers characterised by the selection of the material comprising one or more layers of magnetisable material homogeneously mixed with a bonding agent on a base layer characterised by the composition of the magnetic material
- G11B5/70626—Record carriers characterised by the selection of the material comprising one or more layers of magnetisable material homogeneously mixed with a bonding agent on a base layer characterised by the composition of the magnetic material containing non-metallic substances
- G11B5/70642—Record carriers characterised by the selection of the material comprising one or more layers of magnetisable material homogeneously mixed with a bonding agent on a base layer characterised by the composition of the magnetic material containing non-metallic substances iron oxides
- G11B5/70652—Record carriers characterised by the selection of the material comprising one or more layers of magnetisable material homogeneously mixed with a bonding agent on a base layer characterised by the composition of the magnetic material containing non-metallic substances iron oxides gamma - Fe2 O3
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/10—Particle morphology extending in one dimension, e.g. needle-like
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/54—Particles characterised by their aspect ratio, i.e. the ratio of sizes in the longest to the shortest dimension
-
- 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
- C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
-
- 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
- C01P2004/62—Submicrometer sized, i.e. from 0.1-1 micrometer
-
- 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
- C01P2006/42—Magnetic properties
Definitions
- the invention relates to a process for the production of acicular ferrimagnetic iron oxides by dewatering acicular iron (III) oxide hydroxides.
- acicular iron (III) oxides subsequent reduction of these iron (III) oxides at temperatures between 300 and 650 ° C by means of organic compounds which decompose in this temperature range and oxidation of the resulting products with oxygen-containing gases at 200 to 500 ° C and their use for the production of magnetic recording media.
- Acicular ferrimagnetic iron oxides such as magnetite and gamma-iron (III) oxide
- GB-PS 675 260 already describes a process for the extraction of gamma-iron (III) oxide, in which acicular ⁇ -iron oxide hydroxide (goethite) dehydrates to ⁇ -iron (III) oxide, in a reducing atmosphere "Converted to magnetite at more than 300 ° C and oxidized to acicular gamma-iron (III) oxide in air at temperatures below 4500C.
- this process has been in its individual stages varied several times, and also modified by changing the input materials.
- suitable magnetic iron oxides were obtained in the manner disclosed in DE-PS 801 352, namely by treating non-magnetic iron oxides with the salts of short-chain carboxylic acids and then heating them.
- the magnetite obtained afterwards can also be converted into gamma-iron (III) oxide by oxidation at 200 to 400 ° C.
- 2,900,236 specifies all the corresponding organic substances with particular mention of wax, starch and oil as being useful in DE-AS 12 03 656 salts of soluble soaps precipitated on iron oxide, in DE-OS 20 64 804 Both higher hydrocarbons, higher alcohols and amines, higher fatty acids and their salts, as well as oils, fats and waxes, in DE-PS 91 017 also long-chain carboxylic acids or their salts, in DE-AS 17 71 327 aliphatic monocarboxylic acids with 8 to 24 Carbon- atoms, optionally in a mixture with morpholine and in JP-OS 80 499/1975 organic compounds, such as ethanol, containing inert gases as reducing agents for the production of magnetite from non-magnetic iron oxides.
- the known process mentioned is partly heated in the absence of air, the reaction remaining at the magnetite stage or in the presence of air, as a result of which the magnetite is immediately oxidized to gamma-iron (III) oxide
- the starting materials for the transformation of iron oxides by means of organic substances were predominantly the corresponding ⁇ -modifications, such as ⁇ -FeOOH or a-Fe 2 O 3 , but ⁇ -FeOOH (DE-AS 12 03 656) and ⁇ -FeOOH ( DE-OS 22 12 435) used successfully.
- the invention was therefore based on the object of improving the known acicular ferrimagnetic iron oxides and of eliminating the disadvantages to date.
- the object of the invention was to provide acicular gamma-iron (III) oxide which is distinguished by high values for the coercive field strength and the remanence, by good crystallinity and by mechanical and magnetic stability.
- acicular ferromagnetic iron oxides are formed by dewatering acicular iron (III) oxide hydroxides to acicular iron (III) oxides, then reducing these iron (III) oxides at temperatures between 300 and 650 ° C by means of organic compounds which are decomposable in this temperature range Allow oxidation of the reduction product with oxygen-containing gases at 200 to 500 ° C with the properties required by the task if the needle-shaped iron (III) oxide hydroxide used consists of a mixture of goethite and lepidocrocite with a lepidocrocite content of at least 60% and at temperatures of 200 to 700 ° C is dewatered.
- the acicular iron (III) oxide hydroxides of the mixture have a length to thickness ratio of at least 10 and are dewatered at 300 to 650 ° C.
- the iron (III) oxide hydroxides composed of goethite and lepidocrocite consist of 60 to 98%, preferably 70 to 98%, of lepidocrocite.
- the mixture used for the process according to the invention can be prepared under suitable reaction conditions from iron (III) salt solutions with alkalis with simultaneous oxidation. It has proven particularly expedient to use iron (III) oxide hydrate seeds from an aqueous iron (II) chloride solution using alkalis, such as alkali hydroxide or ammonia, at temperatures between 10 and 32 ° C.
- the solids content of iron (III) oxide hydroxide in the aqueous suspension should be between 10 and 50 g / l, preferably 15 to 45 g / l. After filtering off and washing out the precipitate, the iron (III) oxide hydrate mixture obtained in this way is dried at 60 to 200 ° C.
- Stable crystal needles of the goethite-lepicrocite mixture with at least 60% lepidocrocite, which have almost no dendritic branches, can be obtained by the procedure described by way of example.
- acicular goethite-lepikrokite mixture suitable for use in the method according to the invention are an average particle size of 0.2 to 1.5 and preferably of 0.3 to 1.2 ⁇ m.
- the length-to-thickness ratio is at least 10, with corresponding ratios of 12 to 40 having been found to be expedient.
- the particle surface measured according to BET is between 18 and 70 m2 / g.
- a goethite-lepidocrocite mixture characterized in this way is dewatered according to the invention at temperatures between 200 and 700 ° C., preferably between 300 and 650 ° C. and in particular between 450 and 600 ° C., before further processing into ferrimagnetic iron oxides known per se, surprisingly improve the values for coercive field strength and remanence of the end products obtainable therefrom.
- the dewatering can be carried out both in air and in an inert gas atmosphere.
- the product present after the dewatering step is converted into acicular ferric magnetic at temperatures between 300 and 650 ° C. in a manner known per se with largely ash- and tar-free decomposable organic substances Converted iron oxides.
- the dewatered goethite-lepidocrocite mixture is mechanically mixed with the solid or liquid organic substance or coated in a suitable solution or suspension of the substance and then heated to temperatures of 300 to 650 ° C. under inert gas.
- the method can be carried out by means of gaseous organic substances which are added to the inert gas.
- Organic compounds which can be used in the process according to the invention are all compounds which are stated to be suitable according to the prior art, provided they can be added at temperatures between 300 and 650 ° C. Expediently, higher fatty acids, their derivatives, glycerin, inert gas / alcohol vapor mixtures and also methane are used for this purpose.
- the conversion of the dewatered goethite-lepidocrocite mixture to the acicular magnetite is complete after about 1 to 120 minutes.
- the acicular magnetite obtained after this reduction reaction is usually oxidized to gamma-iron (III) oxide, expediently by passing air over it or adding oxygen at temperatures of 200 to 500 ° C.
- the acicular ferrimagnetic iron oxides produced according to the invention show unexpectedly advantageous properties in the processing Use as magnetic pigments for the production of magnetogram carriers.
- the gamma-iron (III) oxide is dispersed in polymeric binders.
- binders such as homopolymers and copolymers of polyvinyl derivatives, polyurethanes, polyesters and the like.
- the binders are used in solutions in suitable organic solvents, which may optionally contain further additives.
- the magnetic layers are. applied to rigid or flexible supports such as plates, foils and cards.
- the acicular ferrimagnetic iron oxides produced according to the invention differ significantly from the known gamma iron (III) oxides in that they have a more uniform needle shape, since agglomeration is prevented by sintering together. by their improved crystallinity and by the higher coercive field strength and remanence, which can surprisingly be achieved in the process according to the invention. These improvements in the magnetic material are also very noticeable in the magnetic tapes made therefrom.
- the coercive force (H o ) is given in [kA / m]
- the specific remanence (M r / ⁇ ) and the specific magnetization (M m / g) are given in [nT cm 3 / g].
- the suspension is washed on a suction filter with water until the filtrate is chloride-free and then dried at 130 ° C. in a drying cabinet.
- the resulting iron oxide hydroxide is a mixture of 94% lepidocrocite and 6% goethite, has a length-to-thickness ratio of 31 and a BET specific surface area of 34.7 m 2 / g.
- This goethite-lepidocrocite mixture is heated to 490 ° C. for one hour for air dewatering.
- the resulting product is now mixed with 2% by weight of stearic acid, divided into three equal samples 1A, 1B and 1C and converted to magnetite under nitrogen under the conditions specified in Table 1 and to gamma-iron (III) oxide in air oxidized.
- the magnetic properties are also shown in Table 1.
- iron (III) oxide hydroxide mixtures with a lepidocrocite content of 72% with a BET specific surface area of 33.2 m 2 / g are produced. These goethite-lepidocrocite mixtures are dehydrated in air at the temperatures given in Table 2 for one hour each, then at 300 ° C with a nitrogen-methanol vapor mixture reduced to magnetite and then oxidized in air at 400 ° C to gamma-iron (III) oxide.
- the nitrogen-methanol mixture is formed when nitrogen is passed through in an amount of 50 l per hour through a container heated to 105 ° C., to which methanol is added.
- Table 2 The resulting magnetic values of the tests are also shown in Table 2.
- Table 5 shows samples which were dewatered in 30 minutes at the lower dewatering temperature of 400 ° C and then converted to ⁇ -Fe 2 O 3 .
- the germ suspension was heated to 33 ° C. in 20 minutes.
- the amount of air was then increased to 8 m 3 / h and the pH was adjusted to 5.5 by adding aqueous sodium hydroxide solution. and regulated to this value until the end of the reaction.
- the mixture was simultaneously heated to 38 to 39 ° C. in 30 minutes and this temperature was maintained until the end of the growth reaction.
- the oxidation was complete after 1 hour and 40 minutes. After filtration through a filter press, the product is washed with water until the filtrate is chloride-free and then dried at 110 ° C. in a drying cabinet.
- the resulting ferric oxide hydrate sets in.
- Mixture of 92% lepidocrocite and 8% goethite has a length-to-thickness ratio of 16 and a BET specific surface area of 23.3 m 2 / g.
- Magnetic pigment dispersions and then magnetic tapes are produced from the two gamma-iron (III) oxide samples H and J.
- K value 58
- the film After drying, the film carries mecanic'Magnet Mrs of 5 / um thickness. By going The magnetic layer is compacted between heated rollers (80 ° C under a line pressure of approx. 3 kg / cm). The coated film is cut into strips 6.25 mm wide.
- the electroacoustic measurement is carried out in accordance with DIN 45 512, Part II.
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Dermatology (AREA)
- General Health & Medical Sciences (AREA)
- Hard Magnetic Materials (AREA)
- Compounds Of Iron (AREA)
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| DE2735316A DE2735316C3 (de) | 1977-08-05 | 1977-08-05 | Verfahren zur Herstellung von nadeiförmigen, ferrimagnetischen Eisenoxiden |
| DE2735316 | 1977-08-05 |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| EP0000749A1 true EP0000749A1 (fr) | 1979-02-21 |
| EP0000749B1 EP0000749B1 (fr) | 1980-07-23 |
Family
ID=6015703
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| EP78100535A Expired EP0000749B1 (fr) | 1977-08-05 | 1978-07-28 | Procédé de préparation d'oxyde ferrique aciculaire ferrimagnétique et son application |
Country Status (4)
| Country | Link |
|---|---|
| US (1) | US4213959A (fr) |
| EP (1) | EP0000749B1 (fr) |
| JP (1) | JPS5428299A (fr) |
| DE (2) | DE2735316C3 (fr) |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| FR2416868A1 (fr) * | 1978-02-09 | 1979-09-07 | Basf Ag | Procede de preparation d'oxydes de fer ferrimagnetiques aciculaires |
| FR2416869A1 (fr) * | 1978-02-10 | 1979-09-07 | Basf Ag | Procede de preparation d'oxydes de fer ferrimagnetiques aciculaires |
| FR2424910A1 (fr) * | 1978-05-03 | 1979-11-30 | Nippon Shinyaku Co Ltd | Derives de moranoline n-substitues et leur utilisation, notamment pour le traitement de l'hyperglycemie |
| EP0040722A1 (fr) * | 1980-05-23 | 1981-12-02 | BASF Aktiengesellschaft | Procédé pour la production de lépidocrocite synthétique |
Families Citing this family (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE3143870A1 (de) * | 1981-11-05 | 1983-05-11 | Basf Ag, 6700 Ludwigshafen | Verfahren zur herstellung von nadelfoermigen, ferrimagnetischen eisenoxiden |
| JPS58199725A (ja) * | 1982-05-12 | 1983-11-21 | Fuji Photo Film Co Ltd | 強磁性酸化鉄の製造方法 |
| DE3224325A1 (de) * | 1982-06-30 | 1984-01-05 | Basf Ag, 6700 Ludwigshafen | Verfahren zur herstellung von nadelfoermigen, ferrimagnetischen eisenoxiden |
| JPS61106408A (ja) * | 1984-10-25 | 1986-05-24 | Daikin Ind Ltd | 炭化鉄を含有する針状粒子の製造法 |
| US5219554A (en) * | 1986-07-03 | 1993-06-15 | Advanced Magnetics, Inc. | Hydrated biodegradable superparamagnetic metal oxides |
| US5069216A (en) * | 1986-07-03 | 1991-12-03 | Advanced Magnetics Inc. | Silanized biodegradable super paramagnetic metal oxides as contrast agents for imaging the gastrointestinal tract |
| EP0604849B1 (fr) * | 1992-12-29 | 1996-10-16 | Ishihara Sangyo Kaisha, Ltd. | Oxyde de fer magnétique contenant du cobalt et procédé pour sa production |
| US5814164A (en) * | 1994-11-09 | 1998-09-29 | American Scientific Materials Technologies L.P. | Thin-walled, monolithic iron oxide structures made from steels, and methods for manufacturing such structures |
| US6461562B1 (en) | 1999-02-17 | 2002-10-08 | American Scientific Materials Technologies, Lp | Methods of making sintered metal oxide articles |
| JP7132901B2 (ja) | 2019-10-01 | 2022-09-07 | 株式会社Soken | 電力変換装置 |
| CN115676898B (zh) * | 2022-10-31 | 2024-05-07 | 昆明理工大学 | 一种一步碳热还原制备Fe3O4的方法 |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3082067A (en) * | 1959-04-28 | 1963-03-19 | Bayer Ag | Process for the production of isometric ferromagnetic gamma-ferric oxide |
| FR2130407A1 (fr) * | 1971-03-17 | 1972-11-03 | Pfizer |
Family Cites Families (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE1138750B (de) * | 1950-05-26 | 1962-10-31 | Basf Ag | Verfahren zur Herstellung magnetisierbarer Eisenoxyde |
| US2900236A (en) * | 1955-08-03 | 1959-08-18 | Audio Devices Inc | Production of ferromagnetic iron oxide |
| US3117933A (en) * | 1959-06-12 | 1964-01-14 | Bayer Ag | Process for the production of needleshaped, cobalt-containing gamma-ferric oxide crystalline particles |
| JPS5016859B2 (fr) * | 1971-09-30 | 1975-06-17 | ||
| JPS5327719B2 (fr) * | 1972-05-23 | 1978-08-10 | ||
| JPS5241758B2 (fr) * | 1972-09-01 | 1977-10-20 | ||
| JPS5719056B2 (fr) * | 1974-04-08 | 1982-04-20 | ||
| JPS5437680B2 (fr) * | 1975-03-22 | 1979-11-16 |
-
1977
- 1977-08-05 DE DE2735316A patent/DE2735316C3/de not_active Expired
-
1978
- 1978-07-28 DE DE7878100535T patent/DE2860071D1/de not_active Expired
- 1978-07-28 EP EP78100535A patent/EP0000749B1/fr not_active Expired
- 1978-08-03 US US05/930,513 patent/US4213959A/en not_active Expired - Lifetime
- 1978-08-04 JP JP9469578A patent/JPS5428299A/ja active Granted
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3082067A (en) * | 1959-04-28 | 1963-03-19 | Bayer Ag | Process for the production of isometric ferromagnetic gamma-ferric oxide |
| FR2130407A1 (fr) * | 1971-03-17 | 1972-11-03 | Pfizer |
Non-Patent Citations (2)
| Title |
|---|
| ACTA CRYSTALLOGRAPHICA, Teil 13, November 1960, Seiten 932-935, Morphology of synthetic submicroscopic crystals of alpha and gamma FeOOH and of gamma Fe2O3 prepared from FeOOH, G.W. van Oosterhout * |
| JOURNAL OF THE PHYSICAL SOCIETY OF JAPAN, Teil 18, Nr. 1, Januar '63, Seiten 106-116, An electron diffraction study and a theory of the transformation from gamma Fe2O3 to alpha Fe2O3, Sakeji Kachi * |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| FR2416868A1 (fr) * | 1978-02-09 | 1979-09-07 | Basf Ag | Procede de preparation d'oxydes de fer ferrimagnetiques aciculaires |
| FR2416869A1 (fr) * | 1978-02-10 | 1979-09-07 | Basf Ag | Procede de preparation d'oxydes de fer ferrimagnetiques aciculaires |
| FR2424910A1 (fr) * | 1978-05-03 | 1979-11-30 | Nippon Shinyaku Co Ltd | Derives de moranoline n-substitues et leur utilisation, notamment pour le traitement de l'hyperglycemie |
| EP0040722A1 (fr) * | 1980-05-23 | 1981-12-02 | BASF Aktiengesellschaft | Procédé pour la production de lépidocrocite synthétique |
Also Published As
| Publication number | Publication date |
|---|---|
| JPS6140602B2 (fr) | 1986-09-10 |
| EP0000749B1 (fr) | 1980-07-23 |
| DE2735316A1 (de) | 1979-02-08 |
| JPS5428299A (en) | 1979-03-02 |
| DE2735316C3 (de) | 1981-01-29 |
| DE2735316B2 (de) | 1980-04-30 |
| US4213959A (en) | 1980-07-22 |
| DE2860071D1 (en) | 1980-11-13 |
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