CN111453775A - Preparation method and application of iron oxide red - Google Patents
Preparation method and application of iron oxide red Download PDFInfo
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- CN111453775A CN111453775A CN202010256905.0A CN202010256905A CN111453775A CN 111453775 A CN111453775 A CN 111453775A CN 202010256905 A CN202010256905 A CN 202010256905A CN 111453775 A CN111453775 A CN 111453775A
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- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 title claims abstract description 172
- 238000002360 preparation method Methods 0.000 title claims abstract description 21
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims abstract description 146
- 229910052742 iron Inorganic materials 0.000 claims abstract description 102
- -1 iron ions Chemical class 0.000 claims abstract description 63
- 239000007864 aqueous solution Substances 0.000 claims abstract description 29
- 239000002244 precipitate Substances 0.000 claims abstract description 25
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 15
- 239000012716 precipitator Substances 0.000 claims abstract description 13
- 238000000576 coating method Methods 0.000 claims abstract description 12
- 238000004040 coloring Methods 0.000 claims abstract description 9
- 239000002537 cosmetic Substances 0.000 claims abstract description 8
- 239000003973 paint Substances 0.000 claims abstract description 8
- 239000004033 plastic Substances 0.000 claims abstract description 8
- 229920003023 plastic Polymers 0.000 claims abstract description 8
- 239000000843 powder Substances 0.000 claims abstract description 7
- 239000000976 ink Substances 0.000 claims abstract description 6
- 239000010985 leather Substances 0.000 claims abstract description 6
- 238000007639 printing Methods 0.000 claims abstract description 6
- 238000000034 method Methods 0.000 claims description 41
- 239000003921 oil Substances 0.000 claims description 35
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 24
- STCOOQWBFONSKY-UHFFFAOYSA-N tributyl phosphate Chemical compound CCCCOP(=O)(OCCCC)OCCCC STCOOQWBFONSKY-UHFFFAOYSA-N 0.000 claims description 15
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims description 12
- 238000001354 calcination Methods 0.000 claims description 12
- 239000000243 solution Substances 0.000 claims description 12
- 239000003085 diluting agent Substances 0.000 claims description 11
- 239000003350 kerosene Substances 0.000 claims description 9
- PHTQWCKDNZKARW-UHFFFAOYSA-N isoamylol Chemical compound CC(C)CCO PHTQWCKDNZKARW-UHFFFAOYSA-N 0.000 claims description 8
- NTIZESTWPVYFNL-UHFFFAOYSA-N Methyl isobutyl ketone Chemical compound CC(C)CC(C)=O NTIZESTWPVYFNL-UHFFFAOYSA-N 0.000 claims description 6
- 239000003513 alkali Substances 0.000 claims description 6
- XTAZYLNFDRKIHJ-UHFFFAOYSA-N n,n-dioctyloctan-1-amine Chemical compound CCCCCCCCN(CCCCCCCC)CCCCCCCC XTAZYLNFDRKIHJ-UHFFFAOYSA-N 0.000 claims description 6
- CDBYLPFSWZWCQE-UHFFFAOYSA-L sodium carbonate Substances [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 6
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 5
- 238000005406 washing Methods 0.000 claims description 5
- UIHCLUNTQKBZGK-UHFFFAOYSA-N Methyl isobutyl ketone Natural products CCC(C)C(C)=O UIHCLUNTQKBZGK-UHFFFAOYSA-N 0.000 claims description 4
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 claims description 4
- 239000002585 base Substances 0.000 claims description 4
- 239000008096 xylene Substances 0.000 claims description 4
- ZFCFOTOVMMPHGK-UHFFFAOYSA-N 2-[methyl(octan-2-yloxy)phosphoryl]oxyoctane Chemical compound CCCCCCC(C)OP(C)(=O)OC(C)CCCCCC ZFCFOTOVMMPHGK-UHFFFAOYSA-N 0.000 claims description 3
- 229910000029 sodium carbonate Inorganic materials 0.000 claims description 3
- 239000012670 alkaline solution Substances 0.000 claims description 2
- 229910021529 ammonia Inorganic materials 0.000 claims description 2
- 229910052799 carbon Inorganic materials 0.000 claims description 2
- 239000000295 fuel oil Substances 0.000 claims description 2
- 230000001376 precipitating effect Effects 0.000 claims description 2
- 239000011248 coating agent Substances 0.000 abstract description 7
- 239000012071 phase Substances 0.000 description 31
- 238000000605 extraction Methods 0.000 description 18
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- 239000002994 raw material Substances 0.000 description 8
- 230000000052 comparative effect Effects 0.000 description 7
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- 239000001054 red pigment Substances 0.000 description 7
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- 239000013078 crystal Substances 0.000 description 5
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- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 5
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 4
- 239000004743 Polypropylene Substances 0.000 description 4
- 238000002441 X-ray diffraction Methods 0.000 description 4
- 230000008901 benefit Effects 0.000 description 4
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- 239000000126 substance Substances 0.000 description 4
- 238000001308 synthesis method Methods 0.000 description 4
- 238000003786 synthesis reaction Methods 0.000 description 4
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 3
- 239000011575 calcium Substances 0.000 description 3
- 229910052791 calcium Inorganic materials 0.000 description 3
- 239000011651 chromium Substances 0.000 description 3
- 229910052500 inorganic mineral Inorganic materials 0.000 description 3
- 150000002500 ions Chemical class 0.000 description 3
- 150000002505 iron Chemical class 0.000 description 3
- SURQXAFEQWPFPV-UHFFFAOYSA-L iron(2+) sulfate heptahydrate Chemical compound O.O.O.O.O.O.O.[Fe+2].[O-]S([O-])(=O)=O SURQXAFEQWPFPV-UHFFFAOYSA-L 0.000 description 3
- 229910000359 iron(II) sulfate Inorganic materials 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 239000011707 mineral Substances 0.000 description 3
- 235000010755 mineral Nutrition 0.000 description 3
- 239000000049 pigment Substances 0.000 description 3
- 238000001878 scanning electron micrograph Methods 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- 239000002699 waste material Substances 0.000 description 3
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 2
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 description 2
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 2
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 2
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- 235000011114 ammonium hydroxide Nutrition 0.000 description 2
- 229910052804 chromium Inorganic materials 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 230000006872 improvement Effects 0.000 description 2
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 230000007774 longterm Effects 0.000 description 2
- 239000011777 magnesium Substances 0.000 description 2
- 229910052749 magnesium Inorganic materials 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
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 229910052759 nickel Inorganic materials 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 150000003839 salts Chemical class 0.000 description 2
- 239000010936 titanium Substances 0.000 description 2
- 229910052719 titanium Inorganic materials 0.000 description 2
- 229910052720 vanadium Inorganic materials 0.000 description 2
- GPPXJZIENCGNKB-UHFFFAOYSA-N vanadium Chemical compound [V]#[V] GPPXJZIENCGNKB-UHFFFAOYSA-N 0.000 description 2
- DKPFZGUDAPQIHT-UHFFFAOYSA-N Butyl acetate Natural products CCCCOC(C)=O DKPFZGUDAPQIHT-UHFFFAOYSA-N 0.000 description 1
- WBLGXIFKKXGJGJ-UHFFFAOYSA-N CC(CCCCCC)(C)OP(O)(=O)C Chemical compound CC(CCCCCC)(C)OP(O)(=O)C WBLGXIFKKXGJGJ-UHFFFAOYSA-N 0.000 description 1
- 229910017518 Cu Zn Inorganic materials 0.000 description 1
- VTLYFUHAOXGGBS-UHFFFAOYSA-N Fe3+ Chemical compound [Fe+3] VTLYFUHAOXGGBS-UHFFFAOYSA-N 0.000 description 1
- 229910002651 NO3 Inorganic materials 0.000 description 1
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 description 1
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 150000001450 anions Chemical class 0.000 description 1
- 239000007900 aqueous suspension Substances 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 239000011324 bead Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229940067573 brown iron oxide Drugs 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 230000000536 complexating effect Effects 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000010790 dilution Methods 0.000 description 1
- 239000012895 dilution Substances 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 239000012153 distilled water Substances 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 229910001447 ferric ion Inorganic materials 0.000 description 1
- SZVJSHCCFOBDDC-UHFFFAOYSA-N ferrosoferric oxide Chemical compound O=[Fe]O[Fe]O[Fe]=O SZVJSHCCFOBDDC-UHFFFAOYSA-N 0.000 description 1
- 239000011790 ferrous sulphate Substances 0.000 description 1
- 235000003891 ferrous sulphate Nutrition 0.000 description 1
- 230000009969 flowable effect Effects 0.000 description 1
- FUZZWVXGSFPDMH-UHFFFAOYSA-N hexanoic acid Chemical compound CCCCCC(O)=O FUZZWVXGSFPDMH-UHFFFAOYSA-N 0.000 description 1
- 238000001027 hydrothermal synthesis Methods 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 238000001746 injection moulding Methods 0.000 description 1
- 239000001023 inorganic pigment Substances 0.000 description 1
- 239000001034 iron oxide pigment Substances 0.000 description 1
- 238000004898 kneading Methods 0.000 description 1
- MOUPNEIJQCETIW-UHFFFAOYSA-N lead chromate Chemical compound [Pb+2].[O-][Cr]([O-])(=O)=O MOUPNEIJQCETIW-UHFFFAOYSA-N 0.000 description 1
- 239000002932 luster Substances 0.000 description 1
- 239000011572 manganese Substances 0.000 description 1
- 238000005272 metallurgy Methods 0.000 description 1
- 238000006386 neutralization reaction Methods 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 239000008188 pellet Substances 0.000 description 1
- DPTATFGPDCLUTF-UHFFFAOYSA-N phosphanylidyneiron Chemical compound [Fe]#P DPTATFGPDCLUTF-UHFFFAOYSA-N 0.000 description 1
- 238000005554 pickling Methods 0.000 description 1
- 239000002985 plastic film Substances 0.000 description 1
- 229920000728 polyester Polymers 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- NIFIFKQPDTWWGU-UHFFFAOYSA-N pyrite Chemical compound [Fe+2].[S-][S-] NIFIFKQPDTWWGU-UHFFFAOYSA-N 0.000 description 1
- 229910052683 pyrite Inorganic materials 0.000 description 1
- 239000011028 pyrite Substances 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 238000005096 rolling process Methods 0.000 description 1
- 239000002893 slag Substances 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 238000009628 steelmaking Methods 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- 239000004408 titanium dioxide Substances 0.000 description 1
- 239000002966 varnish Substances 0.000 description 1
- 239000003039 volatile agent Substances 0.000 description 1
- 239000002351 wastewater Substances 0.000 description 1
- 229910052726 zirconium Inorganic materials 0.000 description 1
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- 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
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G49/00—Compounds of iron
- C01G49/0009—Preparation involving a liquid-liquid extraction, an adsorption or an ion-exchange
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
-
- 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
- C09D167/00—Coating compositions based on polyesters obtained by reactions forming a carboxylic ester link in the main chain; Coating compositions based on derivatives of such polymers
-
- 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
- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
- C09D7/40—Additives
- C09D7/60—Additives non-macromolecular
- C09D7/61—Additives non-macromolecular inorganic
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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- 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
- C01P2006/19—Oil-absorption capacity, e.g. DBP values
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- 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
- C01P2006/80—Compositional purity
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2265—Oxides; Hydroxides of metals of iron
- C08K2003/2272—Ferric oxide (Fe2O3)
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- Chemical Kinetics & Catalysis (AREA)
- Life Sciences & Earth Sciences (AREA)
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Abstract
The invention discloses a preparation method and application of iron oxide red. The preparation method of the iron oxide red comprises the following steps: transferring iron ions from an aqueous solution containing the iron ions into an oil phase by adopting an extracting agent, adding a precipitator into the separated oil phase to form iron precipitate, and then treating the iron precipitate to obtain the iron oxide red. The synthesized iron oxide red is used in the fields of paint, printing ink, plastics, leather coloring, wallpaper, powder coating, cosmetics, food and the like.
Description
Technical Field
The invention relates to the technical field of preparation of iron oxide red, and particularly relates to a preparation method and application of iron oxide red.
Background
Iron oxide red (also called as iron oxide red) with chemical composition of α -Fe2O370% of iron and 30% of oxygen. Iron oxide red is an important chemical pigment, and China is the biggest iron oxide pigment producing country in the world. The existing methods for producing the iron oxide red comprise a dry method and a wet method, wherein the dry method comprises a green vitriol calcining method, an iron oxide yellow calcining method, an iron oxide black calcining method and the like, and the wet method comprises a sulfate and nitrate wet method, a mixed acid method, an ammonia method and the like. The raw materials used are iron filings, iron phosphorus, steel rolling pickling waste liquid, ferrous sulfate produced by titanium dioxide, and the like. The method has the advantages of long process and high cost, needs a large amount of acid liquor or alkali liquor to participate in the reaction, and discharges a large amount of salt-containing wastewater, thereby bringing serious burden to enterprises and causing great pressure to the environment.
With the increase of the market demand and the improvement of the use requirements of customers, researchers at home and abroad also carry out certain deep research on the quality and the synthesis method of the iron pigment. However, most researches focus on using the aqueous solution of iron salt as the raw material, and changing the morphology, particle size, and function of the iron oxide red by different synthesis methods, such as a hydrothermal method, a flame calcination method, and the like, or by adding different additives. However, the inorganic pigments obtained by the current preparation methods generally have the problems of agglomeration caused by kneading, long-term caking, difficult dispersion in a base material, uneven coloring and the like.
In view of this, the invention is particularly proposed.
Disclosure of Invention
The invention aims to overcome the defects in the prior art and provide a preparation method and application of iron oxide red.
The invention is realized by the following steps:
in a first aspect, an embodiment of the present invention provides a method for preparing iron oxide red, including: transferring iron ions from an aqueous solution containing the iron ions to an oil phase by adopting an extracting agent, adding a precipitator into the separated oil phase to form iron precipitate, and then treating the iron precipitate to obtain the iron oxide red.
Currently, the industrial production methods of iron oxide red are divided into two types:
(1) the method comprises the following steps of directly calcining pure copperas, iron mud, pyrite slag and the like serving as raw materials at high temperature to obtain iron oxide red, washing the iron oxide red by using distilled water to remove water-soluble salt, and drying and crushing the iron oxide red to obtain a finished product. But more impurities and poor coloring power.
(2) The method is prepared by taking an iron salt aqueous solution as a raw material and performing alkali neutralization, but the method has the disadvantages of high seed crystal preparation cost, long production period and high product purity dependence on the purity of iron salt.
In order to obtain high-quality iron oxide red, the inventor provides a preparation method of the iron oxide red through long-term practice, and the method has the following thought:
transferring iron ions from an aqueous solution containing the iron ions into an oil phase by using an extractant of the iron ions;
transferring the oil phase containing high-purity iron ions into a synthesis kettle of iron oxide red, adding a precipitator into the system to prepare iron precipitate, and finally carrying out post-treatment to obtain the iron oxide red.
The method is completely different from the current industrial synthesis method, for example, specific iron-containing minerals are not needed to be adopted or experimental steps and parameters are not needed to be controlled to control the growth process of crystals, the raw material for preparing the iron oxide red in the embodiment of the invention is the aqueous solution containing iron ions, firstly, the iron ions in the aqueous solution containing the iron ions are extracted into the oil phase by using the extracting agent, because the current process for extracting the iron ions by using the extracting agent is mature, the high-purity oil phase containing the iron ions can be obtained by using the extracting step, the extraction step is not only unnecessary to limit the source of the aqueous solution containing the iron ions and the composition of the aqueous solution, but also the high-purity iron-containing organic phase can be obtained by extracting, therefore, the extraction step is used for extracting the iron ions, on the one hand, the universality of the raw material source can be greatly improved, and the purity and, on the other hand, different from the complex steps of purification and impurity removal required for the calcination of minerals or the growth of crystals, the high-purity iron ion-containing organic phase can be obtained by extraction in the embodiment of the invention, and the purity of the iron oxide red prepared subsequently is ensured by the high-purity iron ion-containing organic phase, so that the prepared product does not need to be subjected to complex extraction and purity operation;
secondly, after the organic phase obtained by extraction is separated, a precipitator is directly added into the organic phase, under the action of an alkaline precipitator, iron ions in the iron ion extract in the organic phase are dissociated and combined with anions in the alkaline precipitator to obtain iron precipitate, and the iron precipitate is subjected to post-treatment to obtain high-quality iron oxide red.
Therefore, the preparation method of the iron oxide red can widely adopt the aqueous solution containing iron ions as a raw material, and the high-quality iron oxide red can be obtained by extraction and precipitation, so that the iron oxide red with simple preparation process, low cost and high quality is provided.
In an alternative embodiment, the mass concentration of iron ions in the aqueous solution containing iron ions is 1-30%; preferably 10-20%.
In the embodiment of the invention, the raw material for preparing the iron oxide red is an aqueous solution containing iron ions, the aqueous solution containing iron ions can be from mineral leachate generated in the industrial processes of metallurgy, steel making and the like, waste liquid generated in post-treatment, byproducts generated in the process of preparing products and the like, so that the effect of recycling wastes is achieved, the environmental problem is solved, economic benefits are brought, meanwhile, the composition of the aqueous solution containing iron ions is not limited, the solution can also contain one or more of other impurity ions such as titanium, manganese, vanadium, chromium, nickel, calcium, magnesium and the like, as long as a certain amount of iron ions are contained, and in order to ensure that the prepared iron oxide red has a certain yield, the preferred mass concentration of the iron ions in the aqueous solution containing iron ions is at least 1-30%; preferably 10-20%.
In an alternative embodiment, the mass ratio of the extractant to the aqueous solution containing iron ions is 1-6:1, preferably 2-2.5: 1.
In an alternative embodiment, the extractant comprises one or more of tributyl phosphate TBP, di (1-methylheptyl) methylphosphonate P350, methyl isobutyl ketone MIBK, trioctylamine TOA, and a secondary primary amine N1923;
preferably, the fuel oil further comprises a diluent, wherein the diluent comprises one or more of toluene, xylene, isoamyl alcohol and sulfonated kerosene;
preferably, the extractant is selected from tributyl phosphate TBP and the diluent is selected from sulfonated kerosene.
The extraction treatment may be performed by one-stage extraction or by multi-stage extraction, and in the embodiment of the present invention, the multi-stage means at least two stages without specific explanation. After extraction, the organic phases are combined to obtain an iron-rich organic phase.
In the embodiment of the present invention, the specific kind of the iron extractant is not limited as long as it is any organic phase substance capable of extracting ferric ions and separating iron from other ions that may be contained in the solution. In some embodiments, the iron extractant consists, for example, of only an extractant having the extraction function described above, for example, at least one selected from the group consisting of tributyl phosphate, dimethylheptyl methylphosphonate, methyl isobutyl ketone, and trioctylamine. In other embodiments, the iron extractant may also be the extractant described above after dilution, i.e. the iron extractant comprises, in addition to the extractant described above, a diluent, for example at least one selected from the group consisting of toluene, xylene, isoamyl alcohol and sulfonated kerosene. Alternatively, when the iron extractant comprises an extractant and a diluent, the mass ratio of the extractant to the diluent is 1-2:1-2, or 1-2:1, or 1:1-2, such as but not limited to 1:1, 1.5:1, 2:1, 1:1.5, 1: 2.
In an alternative embodiment, the precipitating agent is selected from an alkaline solution;
preferably, the base comprises one or more of sodium hydroxide, aqueous ammonia and sodium carbonate, more preferably, the base is sodium hydroxide.
In an alternative embodiment, the method further comprises: separating, washing and calcining the iron precipitate to obtain iron oxide red; preferably, the temperature of calcination is 550-.
In the preparation process of the iron oxide red provided by the embodiment of the invention, after the iron ion extract compound in the organic phase is precipitated, iron precipitate is obtained, and the iron precipitate is separated, washed and calcined to obtain the iron oxide red.
In an alternative embodiment, the specific steps are as follows:
transferring iron ions in an aqueous solution system with the mass concentration of 1-30% containing iron ions into an oil phase by adopting an extracting agent, controlling the mass ratio of the extracting agent to the aqueous solution containing the iron ions to be 1-6:1, adding an alkali solution into the separated oil phase to form iron precipitate, and then separating, washing and calcining the iron precipitate at the temperature of 550-800 ℃ to obtain the iron oxide red.
In a second aspect, the embodiment of the present invention provides a use of the iron oxide red prepared by the above preparation method, which is used in the fields of paint, printing ink, plastics, leather coloring, wallpaper, powder coating, cosmetics, food, etc., and is especially applied in the fields of cosmetics and food.
The invention has the following beneficial effects:
the invention discloses a preparation method and application of iron oxide red. The method comprises the steps of directionally transferring iron ions in an aqueous solution containing the iron ions to an oil phase for enrichment by adopting an iron extraction agent, adding a precipitator into the separated oil phase to form iron precipitates, and treating the iron precipitates to obtain the iron oxide red. According to the method, because the iron ions extracted into the oil phase are high-purity iron-rich oil phase, a precipitator is further added into the oil phase, and then high-quality iron oxide red can be synthesized through post-treatment, and the synthesized high-quality iron oxide red can be applied to the fields of paint, printing ink, plastics, leather coloring, wallpaper, powder coating, cosmetics or food, especially the fields of cosmetics and food.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings needed to be used in the embodiments will be briefly described below, it should be understood that the following drawings only illustrate some embodiments of the present invention and therefore should not be considered as limiting the scope, and for those skilled in the art, other related drawings can be obtained according to the drawings without inventive efforts.
FIG. 1 is an SEM image of iron oxide red;
FIG. 2 is an XRD pattern of iron oxide red;
fig. 3 shows the effect of iron oxide red in resin.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below. The examples, in which specific conditions are not specified, were conducted under conventional conditions or conditions recommended by the manufacturer. The reagents or instruments used are not indicated by the manufacturer, and are all conventional products available commercially.
The embodiment of the invention provides a method for directly synthesizing iron oxide red from an oil phase containing organic complex iron. The method comprises the following steps: transferring iron ions into an oil phase by adopting an effective extractant to obtain a high-purity iron-rich oil phase, adding a precipitator into the oil phase, and treating the formed precipitate to obtain the high-quality iron oxide red. The method comprises the following specific steps:
transferring iron ions from an aqueous solution containing the iron ions into an oil phase by using an extractant of the iron ions; and (3) directly feeding the oil phase containing high-purity iron ions into a synthesis kettle of the iron oxide red, adding a precipitator into the system to prepare iron precipitate, and finally performing post-treatment to obtain the iron oxide red.
The above-mentioned aqueous solution containing iron ions refers to a solution having an iron ion concentration of 1 to 30% by mass, and the source and composition of the aqueous solution containing iron ions are not particularly limited, and the solution may contain one or more of other impurity ions such as titanium, manganese, vanadium, chromium, nickel, calcium, magnesium, and the like.
The extracting agent in the extraction system is common tributyl phosphate TBP, methyl phosphonic acid di (1-methyl heptyl) ester P350, methyl isobutyl ketone MIBK, trioctylamine TOA, secondary carbon primary amine N1923 and the like, and the diluent in the extraction process is common toluene, xylene, isoamyl alcohol, sulfonated kerosene or the like, preferably the extracting agent is selected from tributyl phosphate TBP, and the diluent is selected from sulfonated kerosene. And the iron extractant and complexing process conditions are well known and can be readily achieved according to the process conditions of the present invention.
The precipitant is alkali solution, and the alkali is one or more selected from sodium hydroxide, ammonia water, and sodium carbonate. Sodium hydroxide is preferred for environmental reasons.
The features and properties of the present invention are described in further detail below with reference to examples.
Example 1
Adding 1000ml of aqueous solution containing 5% of iron ions into an iron extractor, taking tributyl phosphate TBP/sulfonated kerosene (wt) ═ 45:55 as an extraction system at 30 ℃, performing 1-stage extraction on oil phase water compared with O/A ═ 1:1 to obtain an oil phase containing high-purity iron ions, then directly entering an iron oxide red synthesis kettle, adding 20% sodium hydroxide solution into the system to prepare iron precipitate, and finally performing post-treatment to obtain the iron oxide red.
Example 2
Adding 1000ml of aqueous solution containing 20% of iron ions into an extractor, taking tributyl phosphate TBP/sulfonated kerosene (wt) ═ 45:55 as an extraction system at 30 ℃, performing 2-stage extraction on the oil phase water phase ratio O/A ═ 1:1 to obtain an oil phase containing high-purity iron ions, then directly entering an iron oxide red synthesis kettle, adding 20% of sodium hydroxide solution into the system to prepare iron precipitate, and finally performing post-treatment to obtain the iron oxide red.
The composition analysis of the iron oxide red prepared in this example is shown in table 1 below:
TABLE 1 iron oxide Red composition (ppm)
| Fe2O3(％) | Ca | Mg | Al | Mn | V | Cr | Ti | Si | Co |
| 99.89 | 1.2 | 1.1 | 1.6 | 0.9 | - | - | - | 0.02 | 0.01 |
| Ni | Cu | Zn | Cd | Hg | Pb | As | Se | Sb | Ba |
| 0.37 | 0.54 | 0.59 | - | - | - | - | - | - | - |
Note: -: not detected out
As can be seen from table 1 above: the prepared iron oxide red has the following properties:
color: a red flowable powder; fe2O3The content is as follows: 99.89%; water soluble substance: 0.02 percent; screen residue (45 μm): less than 0.01 percent; 105 ℃ volatiles: 0.13 percent; total calcium amount: 0.04 percent;
lead chromate test: is absent;
testing of organic coloring matter: is absent;
pH value of the aqueous suspension: 6-8;
oil absorption: 20-25g/100 g.
Comparative example 1
German brown iron oxide red 4110.
And (3) testing results:
morphology and crystal structure of iron oxide red
Referring to fig. 1, the left image in fig. 1 is an SEM image of the iron oxide red prepared in example 1 of the present invention, and the right image is an SEM image of the iron oxide red in comparative example 1, as can be seen from fig. 1: the morphology of the iron oxide red pigment particles prepared by the method provided by the embodiment of the invention is consistent in the comparative example 1, and the iron oxide red prepared by the embodiment 1 of the invention has better dispersibility.
XRD pattern of iron oxide red referring to fig. 2, from top to bottom in fig. 2, the top is the XRD pattern of iron oxide red prepared in example 1 of the present invention, and the bottom is the XRD pattern of iron oxide red in comparative example 1, as can be seen from fig. 2: the crystal structures of the iron oxide red pigment prepared by the method provided by the embodiment of the invention and the pigment in the comparative example 1 are kept consistent.
Application examples
The iron oxide red pigments obtained in examples 1-2 above are used in the fields of application such as paints, coatings, printing inks, plastics, leather coloring, wallpaper, powder coatings, cosmetics, etc. For example, the addition of the iron oxide red pigments according to the invention to paints or coatings enables the production of coatings having very good color and luster.
Application example 1:
paint spray application as an example:
weigh 4.00 grams of iron oxide red pigment, add 4.0 grams of butyl acetate and 8.0 grams of polyester automotive coating resin, disperse in a high speed stirrer with zirconium beads for 30 minutes, continue to add 84.0 grams of the automotive coating resin system and stir for 5 minutes. The viscosity of the coating was adjusted to 14-15 seconds for Ford 4 cup before spraying. And during spraying, the temperature of a spraying room is controlled to be 25 ℃, and the relative humidity is controlled to be 60%. Spraying twice, flashing for 10 minutes, covering with varnish, flashing again, and baking at 140 ℃ for 30 minutes.
Referring to fig. 3 for the effects of the iron oxide red prepared in example 1 of the present invention and the iron oxide red in comparative example 1 in the resin, the left graph in fig. 3 shows the effects of the iron oxide red prepared in example 1 of the present invention in the resin, and the right graph shows the effects of the iron oxide red in comparative example 1 in the resin, as can be seen from fig. 3: compared with Langshan 4110, the iron oxide red pigment prepared in the embodiment 1 of the invention has the advantages of brighter color and better covering power in resin.
Application example 2:
taking injection molding applications as an example:
200 g of dried polypropylene (PP) material was weighed into a plastic sealed bag, and 1 ml of gloss oil was added and mixed well. Then 5.000 grams of iron oxide red pigment was weighed into a plastic sealed bag to allow the iron oxide red to be well dispersed evenly in the PP pellets. After the temperature of the charging barrel reaches a set value (usually 180-200 ℃), the prepared polypropylene material is added into a hopper, and the operation is carried out according to the set normal process parameter conditions, so that the plastic sheet of iron oxide red with bright color can be obtained.
In summary, the embodiment of the invention provides a preparation method and application of iron oxide red. The preparation method of the iron oxide red is different from the current industrial synthesis method, and the iron ions in the water phase are directionally transferred into the oil phase by adopting an extracting agent, a precipitator is directly added into the separated oil phase to form iron precipitate, and then the iron precipitate is treated to obtain the high-quality iron oxide red. Because the iron ions extracted into the oil phase are high-purity iron-rich oil phase, a precipitator is further added into the oil phase, and then the oil phase is subjected to post-treatment, so that high-quality iron oxide red can be directly synthesized, and the synthesized iron oxide red is used in the fields of paint, printing ink, plastics, leather coloring, wallpaper, powder coating, cosmetics, food and the like.
The above is only a preferred embodiment of the present invention, and is not intended to limit the present invention, and various modifications and changes will occur to those skilled in the art. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (10)
1. A preparation method of iron oxide red is characterized by comprising the following steps: transferring iron ions from an aqueous solution containing the iron ions into an oil phase by adopting an extracting agent, adding a precipitator into the separated oil phase to form iron precipitate, and then treating the iron precipitate to obtain the iron oxide red.
2. The preparation method according to claim 1, wherein the mass concentration of the iron ions in the aqueous solution containing the iron ions is 1 to 30%; preferably 10-20%.
3. The method according to claim 1, wherein the mass ratio of the extractant to the aqueous solution containing iron ions is 1-6:1, preferably 2-2.5: 1.
4. The method of claim 1, wherein the extractant comprises one or more of tributyl phosphate, di (1-methylheptyl) methylphosphonate, methyl isobutyl ketone, trioctylamine, and a secondary carbon primary amine;
preferably, the fuel oil further comprises a diluent, wherein the diluent comprises one or more of toluene, xylene, isoamyl alcohol and sulfonated kerosene.
5. The method of claim 4, wherein the extractant is selected from tributyl phosphate and the diluent is selected from sulfonated kerosene.
6. The method of claim 1, wherein the precipitating agent is selected from an alkaline solution.
7. The method of claim 6, wherein the base comprises one or more of sodium hydroxide, ammonia, and sodium carbonate, preferably sodium hydroxide.
8. The method of claim 1, further comprising: separating, washing and calcining the iron precipitate to obtain iron oxide red; preferably, the temperature of calcination is 550-.
9. The preparation method according to any one of claims 1 to 8, characterized by comprising the following specific steps:
transferring iron ions in an aqueous solution system containing 1-30% of iron ions into an oil phase by adopting an extracting agent, controlling the mass ratio of the extracting agent to the aqueous solution containing the iron ions to be 1-6:1, adding an alkali solution into the separated oil phase to form iron precipitate, and then separating and washing the iron precipitate and calcining at the temperature of 550-800 ℃ to obtain the iron oxide red.
10. Use of the iron oxide red prepared by the preparation process according to any one of claims 1 to 9 in paints, printing inks, plastics, leather colourings, wallpaper, powder coatings, cosmetics or foodstuffs.
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