EP4263432A1 - Procédé de production d'oxyhydroxyde de fer - Google Patents

Procédé de production d'oxyhydroxyde de fer

Info

Publication number
EP4263432A1
EP4263432A1 EP21830664.5A EP21830664A EP4263432A1 EP 4263432 A1 EP4263432 A1 EP 4263432A1 EP 21830664 A EP21830664 A EP 21830664A EP 4263432 A1 EP4263432 A1 EP 4263432A1
Authority
EP
European Patent Office
Prior art keywords
iron
solution
aqueous
iii
solid
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.)
Pending
Application number
EP21830664.5A
Other languages
German (de)
English (en)
Inventor
Andreas Schlegel
Waldemar CZAPLIK
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Lanxess Deutschland GmbH
Original Assignee
Lanxess Deutschland GmbH
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Application filed by Lanxess Deutschland GmbH filed Critical Lanxess Deutschland GmbH
Publication of EP4263432A1 publication Critical patent/EP4263432A1/fr
Pending legal-status Critical Current

Links

Classifications

    • 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
    • C01—INORGANIC CHEMISTRY
    • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G49/00—Compounds of iron
    • C01G49/02—Oxides; Hydroxides
    • 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

Definitions

  • the invention relates to a process for the production of iron oxyhydroxides.
  • Iron oxyhydroxides which are obtained by precipitation of iron(III) salts with an alkaline precipitant or by precipitation of iron(II) salts with an alkaline precipitant and subsequent oxidation, are used as color pigments in numerous ways.
  • other applications for example as adsorbers or catalysts for the production of polymers, are also known areas of use. Particularly when used as catalysts, high demands are placed on the range of by-products.
  • iron oxyhydroxides are described, for example, in EP1582505A1, with either an iron(III) sulfate solution being specified and NaOH being added as a precipitant, or vice versa.
  • An amorphous iron(III) hydroxide, for example, is accessible via the following synthesis route.
  • the product obtained is iron oxyhydroxide with a very high Na content. If the procedure is reversed and the precipitant NaOH is added to the iron salt, the product obtained is iron oxyhydroxide with a very high sulfur content.
  • the iron oxyhydroxides produced according to both variants still have sodium and/or sulfur contents which are too high, particularly for catalyst applications, and which cannot be significantly reduced in each case even by repeated washing.
  • Iron(III) hydroxide Fe(OH) 3 usually precipitates as an aqueous hydrogel of the formula Fe 2 O 3 *n H 2 O (“iron(III) oxy hydrate”).
  • the precipitation is carried out starting from iron(III) chloride
  • the ⁇ -FeOOH (akaganeite) phase is preferably formed, which has high chloride contents due to its special structure.
  • the anions from other iron sources and cations from the precipitants are preferably formed, which has high chloride contents due to its special structure.
  • the object of the present invention was therefore to provide a method with which it is possible to produce iron oxyhydroxides with the lowest possible content of cations originating from the precipitant, in particular alkali metals and/or alkaline earth metals, at the same time
  • SUBSTITUTE SHEET (RULE 26) the lowest possible content of anions originating from the iron salts, in particular sulfur and/or chloride.
  • the invention therefore relates to a process for the production of iron oxyhydroxides, which is characterized in that i) an aqueous iron salt solution (A) and an alkaline, aqueous precipitant solution (B), preferably an alkali hydroxide solution, are mixed with one another, the mixing taking place in such a way that the pH value in the resulting mixture is maintained in the range from 6 to 10 during the addition of (A) and (B) into a receiver, ii) wherein in the case of an aqueous iron salt solution (A) a Fe( ll) salt is introduced during or after the mixing of (A) and (B) oxygen-containing gas to oxidize Fe(II) to Fe(III), iii) the suspension obtained after step i) or ii) is separated from the solid iv) the solid obtained after step iii), in particular the filter cake, is washed with deionized (DI) water, preferably to a filtrate conductivity of less than 2000 pS/
  • the iron oxyhydroxides to be produced by the process according to the invention include the crystalline forms such as FeO, Fe2O3, FesO4 and FeOOH as well as the amorphous forms such as Fe(OH)s and its water-containing hydrogels.
  • Both iron(II) and iron(III) salts can be used as the iron salt of the aqueous iron salt solution (A).
  • ferric salts which are preferred, may preferably be ferric sulphate, ferric nitrate, ferric chloride, ferric phosphate, ferric chloride sulphate or any other Iron (III) salt can be used. Iron(III) sulfate or iron(III) chloride is preferred.
  • ferrous salts ferrous sulfate, ferrous nitrate, ferrous chloride, ferrous phosphate or any other ferrous salt can preferably be used.
  • Iron(II) chloride and iron(II) sulfate are preferred.
  • SUBSTITUTE SHEET (RULE 26)
  • the residual proportion of it in the iron oxyhydroxide obtained can be reduced very greatly using the process according to the invention.
  • This proportion is usually measured, for example, as sulfur content for sulfate, preferably as chloride content for chloride and as nitrate content for nitrate.
  • the aqueous iron salt solution (A) preferably contains from 10 to 1000 g/l, preferably 50 to 800 g/l, of iron salt, based on the aqueous iron salt solution (A).
  • the solution can also contain organic solvents, such as aliphatic alcohols such as methanol, ethanol, propanol such as isopropanol, butanol or others.
  • the proportion of water, based on the total solvent content of the aqueous iron salt solution (A), is preferably from 90 to 100% by weight, preferably from 99 to 100% by weight.
  • Alkaline or alkaline earth metal hydroxides in particular NaOH or KOH or Ca(OH)2, alkali metal or alkaline earth metal carbonates such as Na2COs, K2CO3, CaCOs or MgCOs, alkaline earth metal oxides such as MgO or CaO or NHs or NH4OH are used as the precipitants in the alkaline aqueous precipitant solution (B).
  • An alkali metal hydroxide solution is preferred for component (B).
  • the alkaline, aqueous precipitant solution (B) preferably contains from 10 to 600 g/l, preferably from 50 to 440 g/l, of precipitant, based on the solution.
  • the solution can also contain organic solvents, such as aliphatic alcohols such as methanol, ethanol, propanol such as isopropanol, butanol or others.
  • the proportion of water, based on the total content of solvent in the aqueous precipitant solution (B), is preferably from 90 to 100% by weight, preferably from 99 to 100% by weight.
  • the receiver to which the two solutions (A) and (B) are added is preferably an empty container or a container containing water.
  • the pH can be measured using a pH probe in the reaction mixture, preferably suspension.
  • the mixing can already take place during the addition, for example via a mixing element for the addition streams, or only in the receiver, for example by a mixing element attached there. Stirrers or static mixers are suitable as usual mixing elements.
  • air can be added to the template as a support for good
  • Components (A) and (B) can be added continuously or in portions to the initial charge.
  • Any commercially available pH probe can be used to determine the pH.
  • the two components (A) and (B) are preferably added in such a way that the addition of the two components (A) and (B) results in a pH in the range from 6 to 10, in particular from 6.5 to 9 .5 is maintained during the addition.
  • the addition preferably takes place at a selected pH value with a deviation of +/- 0.5 pH units.
  • the pH generally changes more than the initial pH of the initial charge, so that the pH generally only stabilizes by one value after a short initial time.
  • the pH value in the respective range is therefore preferably adjusted in such a way that it is within this range over 95% of the entire addition period of A) and B) to the receiver; in particular, the desired pH value is preferably with a deviation of + /- 0.5 pH units, in this range.
  • the iron salt solution (A) is preferably added continuously to the initial charge, preferably at a constant addition rate, and the precipitant solution (B) is added in such a way that the desired pH can be maintained in the range mentioned.
  • Mixing preferably takes place with a free temperature profile, particularly preferably at a temperature of from 10 to 100.degree.
  • an aqueous suspension of iron oxyhydroxides is obtained.
  • the solid particles obtained preferably have a BET surface area of from 50 to 400 g/m 2 , preferably from 50 to 300 g/m 2 .
  • oxygen or an oxygen-containing gas, in particular air is preferably added while the two components A) and B) are being mixed. This is preferably done by initiating
  • SUBSTITUTE SHEET (RULE 26) of oxygen or an oxygen-containing gas into the template during the addition of the two components.
  • Oxygen or an oxygen-containing gas can also be introduced into the receiver after the two components A) and B) have been added.
  • the aqueous suspension obtained after step ii) or iii) is separated from the solid, preferably by filtration, for example using a filter press, or by centrifugation.
  • the solid obtained after step iii), in particular the filter cake, is preferably washed with deionized (DI) water, preferably to a filtrate conductivity of ⁇ 1000 pS/cm, in particular ⁇ 300 pS/cm, particularly preferably ⁇ 100 pS/cm.
  • DI deionized
  • the solid obtained after washing in step iv) is usually dried at a temperature of from 60 to 300.degree. C., in particular at from 60 to 100.degree.
  • Usual dryers for pigments are suitable as dryers. Drying is preferably carried out down to a residual moisture content of less than 1% by weight of water, based on the solid.
  • the drying can also be followed by grinding, for example in order to break up the agglomerates and aggregates. This can be advantageous, for example, to enable uniform dispersion in the application medium.
  • Comparative example 1 (similar to example 1 of EP1582505)
  • Comparative example 2 comparison 2 (similar to example 1 of EP1582505)
  • the batch was stirred for a further 15 min.
  • the batch was then washed on a laboratory filter press until the filtrate conductivity was ⁇ 100 pS/cm.
  • the filter cake was dried at 75° C. in a circulating air drying cabinet to constant weight and the solid was lightly ground using a laboratory mill.
  • the suspension obtained was washed on a laboratory filter press until the filtrate conductivity was ⁇ 90 pS/cm.
  • the filter cake was dried at 75° C. in a circulating air drying cabinet and the dried solid was lightly ground using a laboratory mill.
  • the suspension obtained was washed on the laboratory filter press until the filtrate conductivity was ⁇ 90 pS/cm.
  • the filter cake was dried at 75° C. in a circulating air drying cabinet and the dried solid was lightly ground using a laboratory mill.
  • the filter cake was dried at 75° C. in a circulating air drying cabinet and the dried solid was lightly ground using a laboratory mill.
  • the filter cake was dried at 75° C. in a circulating air drying cabinet and the dried solid was lightly ground using a laboratory mill.
  • the suspension was washed on a laboratory filter press until the filtrate conductivity was ⁇ 90 pS/cm.
  • the filter cake was dried at 75° C. in a circulating air drying cabinet and the dried solid was lightly ground using a laboratory mill.
  • the filter cake was dried at 75° C. in a circulating air drying cabinet and the dried solid was lightly ground using a laboratory mill.
  • the filter cake was dried at 75° C. in a circulating air drying cabinet and the dried solid was lightly ground using a laboratory mill.

Landscapes

  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Compounds Of Iron (AREA)

Abstract

L'invention concerne un procédé de production d'oxyhydroxydes de fer par addition d'une solution aqueuse de sel de fer (A) et d'une solution d'agent de précipitation aqueuse alcaline (B) dans un récipient collecteur et maintien du pH dans la plage de 6 à 10.
EP21830664.5A 2020-12-21 2021-12-08 Procédé de production d'oxyhydroxyde de fer Pending EP4263432A1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
EP20216002.4A EP4015459A1 (fr) 2020-12-21 2020-12-21 Procédé de production d'oxyhydroxyde de fer
PCT/EP2021/084720 WO2022135925A1 (fr) 2020-12-21 2021-12-08 Procédé de production d'oxyhydroxyde de fer

Publications (1)

Publication Number Publication Date
EP4263432A1 true EP4263432A1 (fr) 2023-10-25

Family

ID=73856136

Family Applications (2)

Application Number Title Priority Date Filing Date
EP20216002.4A Pending EP4015459A1 (fr) 2020-12-21 2020-12-21 Procédé de production d'oxyhydroxyde de fer
EP21830664.5A Pending EP4263432A1 (fr) 2020-12-21 2021-12-08 Procédé de production d'oxyhydroxyde de fer

Family Applications Before (1)

Application Number Title Priority Date Filing Date
EP20216002.4A Pending EP4015459A1 (fr) 2020-12-21 2020-12-21 Procédé de production d'oxyhydroxyde de fer

Country Status (4)

Country Link
EP (2) EP4015459A1 (fr)
JP (1) JP2024501270A (fr)
CN (1) CN116615392A (fr)
WO (1) WO2022135925A1 (fr)

Family Cites Families (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE4434969A1 (de) * 1994-09-30 1996-04-04 Bayer Ag Hochtransparente, gelbe Eisenoxidpigmente, Verfahren zu ihrer Herstellung sowie deren Verwendung
CN1466548B (zh) 2000-09-26 2013-01-02 朗盛德国有限责任公司 接触剂和吸附剂颗粒
BR0114166B1 (pt) * 2000-09-26 2014-10-14 Lanxess Deutschland Gmbh Unidades susceptíveis ao escoamento de meios e uso das mesmas
DE10115415A1 (de) * 2001-03-29 2002-10-02 Bayer Ag Kontakt- und Adsorber-Granulate
DE102004016601A1 (de) 2004-04-03 2005-10-13 Bayer Chemicals Ag Stabile Adsorber-Granulate
JP2008239399A (ja) * 2007-03-27 2008-10-09 Tdk Corp オキシ水酸化鉄粒子の製造方法
CN101428863A (zh) * 2008-11-27 2009-05-13 天津大学 球形FeOOH纳米粉体的制备方法

Also Published As

Publication number Publication date
CN116615392A (zh) 2023-08-18
JP2024501270A (ja) 2024-01-11
WO2022135925A1 (fr) 2022-06-30
EP4015459A1 (fr) 2022-06-22

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