CN107188239B - method for extracting iron element from serpentine magnesium extraction residue and preparing ferric oxide - Google Patents

method for extracting iron element from serpentine magnesium extraction residue and preparing ferric oxide Download PDF

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CN107188239B
CN107188239B CN201710592334.6A CN201710592334A CN107188239B CN 107188239 B CN107188239 B CN 107188239B CN 201710592334 A CN201710592334 A CN 201710592334A CN 107188239 B CN107188239 B CN 107188239B
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iron
serpentine
residue
preparing
solution
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CN107188239A (en
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杨祥
薛智勇
乐惠泽
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China University of Geosciences
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China University of Geosciences
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    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01GCOMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G49/00Compounds of iron
    • C01G49/02Oxides; Hydroxides
    • C01G49/06Ferric oxide [Fe2O3]
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2002/00Crystal-structural characteristics
    • C01P2002/70Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
    • C01P2002/72Crystal-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
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2002/00Crystal-structural characteristics
    • C01P2002/80Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70
    • C01P2002/82Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70 by IR- or Raman-data

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

Abstract

The invention discloses a method for extracting iron element from serpentine magnesium extraction residue and preparing ferric oxide, wherein the residue after serpentine magnesium extraction is rich in iron element, and pure iron compound is extracted from the residue by alkali fusion, oxidation, suction filtration and calcination processes; the process flow is simple, and the separation and enrichment of the iron element and other elements in the serpentine iron-rich residue are realized; the experimental cost is low, and pure iron oxide products can be obtained only by using cheap hydrochloric acid, sodium hydroxide and ammonia water, so that the method is favorable for large-scale industrial production; effectively solves the problems of resource waste and environmental pollution caused by stacking of the serpentine magnesium extraction residues.

Description

method for extracting iron element from serpentine magnesium extraction residue and preparing ferric oxide
Technical Field
The invention belongs to the technical fields of development and utilization of nonmetallic ores, treatment of inorganic nonmetallic materials and solid wastes, mineral processing and environmental protection, and particularly relates to a method for extracting iron elements from serpentine magnesium extraction residues and preparing ferric oxide.
Background
the serpentine is a magnesium-rich silicate mineral containing water, has large reserves in China and high economic value, belongs to a 1:1 type layered silicate, consists of silica tetrahedral sheets and magnesia octahedral sheets, and mainly comprises chrysotile, antigorite and lizardite; the main mineral composition of the serpentine, the serpentine tailings and the asbestos tailings is serpentine, the serpentine contains a small amount of magnetite, talc, brucite, dolomite, calcite and the like, and the main chemical composition is SiO2MgO, containing a small amount of Fe2O3、Al2O3、NiO、Cr2O3And the like, wherein the metal oxide is mainly magnesium oxide. People generally concentrate on extracting and preparing magnesium and silicon with high content in serpentine, but the utilization of other valuable elements such as iron element is less, and the valuable elements exist in waste slag in large quantity, so that the resource waste is caused and the environment is polluted.
Disclosure of Invention
In view of the above, embodiments of the present invention provide a method for extracting iron element from serpentine magnesium extraction residue and preparing iron oxide, thereby improving utilization efficiency of serpentine.
In order to solve the above technical problems, an embodiment of the present invention provides a method for extracting iron element from serpentine magnesium extraction residue and preparing iron oxide, comprising the following steps:
(1) Preparing raw materials, namely taking iron-rich residues obtained after conventional serpentine acid leaching for preparing magnesium oxide as raw materials;
(2) adding a sodium hydroxide solution into the raw materials according to the solid-to-liquid ratio of 1:3, and carrying out an alkali-melting reaction under the water-bath heating condition;
(3) Putting the filter residue after the alkali-fusion reaction in a hydrochloric acid solution with the ratio of 1:1, and introducing air under the heating of a water bath to oxidize ferrous ions in the solution;
(4) taking a pH regulating solution prepared from ammonia water and the sodium hydroxide solution, regulating the pH value to 3.0 +/-0.1, and then carrying out suction filtration;
(5) And calcining the filter residue after suction filtration to obtain the ferric oxide.
preferably, in the step (2), the concentration of the sodium hydroxide solution is 2.5mol/L, the heating temperature of the water bath is 55 ℃, and the alkali-melting reaction time is 3 h.
Preferably, in the step (3), the water bath heating temperature is 60 ℃, and the air introducing time is 0.5 h.
preferably, in the step (4), the ammonia water concentration is 30%, and the pH adjusting solution is prepared from 1:5 ammonia water and the sodium hydroxide solution.
preferably, in the step (5), the calcining temperature is 600 ℃ and the time is 2 h.
Compared with the related art, the technical scheme provided by the embodiment of the invention has the following beneficial effects: the method for extracting the iron element from the serpentine magnesium extraction residue and preparing the ferric oxide has simple process flow, and realizes the separation and enrichment of the iron element and other elements in the serpentine iron-rich residue; the experimental cost is low, and pure iron oxide products can be obtained only by using cheap hydrochloric acid, sodium hydroxide and ammonia water, so that the method is favorable for large-scale industrial production; effectively solves the problems of resource waste and environmental pollution caused by stacking of the serpentine magnesium extraction residues.
Drawings
FIG. 1 is a schematic flow chart of a process for producing iron oxide according to an embodiment of the present invention;
FIG. 2 is an XRD spectrum of iron oxide prepared by the preparation method of the embodiment of the invention;
FIG. 3 is an infrared spectrum of iron oxide prepared by the preparation method of the embodiment of the invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, embodiments of the present invention will be further described with reference to the accompanying drawings.
Referring to the attached figure 1, the embodiment of the invention provides a method for extracting iron element from serpentine magnesium extraction residue and preparing ferric oxide, which comprises the following steps:
(1) preparing raw materials, namely taking iron-rich residues obtained after conventional serpentine acid leaching for preparing magnesium oxide as raw materials; diluting hydrochloric acid with water to obtain an acid leaching agent in a ratio of 1:1, adding the acid leaching agent into a three-mouth bottle with a reflux device and an electric stirrer, adding serpentine ore powder clinker (raw ore) into the three-mouth bottle according to a liquid-solid ratio of 5: 1, heating in a water bath, controlling the temperature to be about 90 ℃, stirring for 150min, cooling and filtering, repeatedly washing filter residues with water until the pH value of a washing liquid is 6-7, and washing to obtain an acid-insoluble iron-rich residue raw material;
(2) Adding a sodium hydroxide solution into the raw materials according to the solid-to-liquid ratio of 1:3, and carrying out an alkali-melting reaction under the water-bath heating condition; the concentration of the sodium hydroxide solution is 2.5mol/L, the water bath heating temperature is 55 ℃, and the alkali-fusion reaction time is 3 h; in the alkali melting process, an aluminum-containing compound in the residue reacts with alkali to finally generate aluminum meta-acid, so that aluminum elements in the iron-rich residue are removed;
(3) Putting the filter residue after the alkali-fusion reaction in a hydrochloric acid solution with the ratio of 1:1, and introducing air for 0.5h at the water bath heating temperature of 60 ℃ to oxidize ferrous ions in the solution; dissolving the filter residue after alkali melting in 1:1 hydrochloric acid, and dissolving Fe-containing compounds into Fe under strong acid condition2+、Fe3+,Fe2+Oxidized into Fe in the process of introducing air under acidic condition3+
(4) taking a pH regulating solution prepared from ammonia water and the sodium hydroxide solution, regulating the pH value to 3.0 +/-0.1, and then carrying out suction filtration; the concentration of the ammonia water is 30%, and the pH regulating solution is prepared from 1:5 ammonia water and the sodium hydroxide solution; under strong acid condition, iron exists in ion state, and the pH value of the strong acid solution is adjusted to 3.0 +/-0.1 to generate Fe (OH)3Precipitation of (4);
(5) Taking and filteringAnd calcining the filter residue for 2 hours at the temperature of 600 ℃ to obtain the ferric oxide. The filter residue after suction filtration mainly comprises Fe (OH)3and calcining at high temperature to obtain the iron oxide powder.
The preparation method provided by the embodiment of the invention is simple in process flow, easy to operate and low in cost; effectively solves the problems of resource waste and environmental pollution caused by stacking of the serpentine magnesium-extracted residues.
example two
referring to the attached figure 1, the embodiment of the invention provides a method for extracting iron element from serpentine magnesium extraction residue and preparing ferric oxide, which comprises the following steps:
(1) Preparing raw materials, namely taking iron-rich residues obtained after conventional serpentine acid leaching for preparing magnesium oxide as raw materials;
(2) taking 50g of raw materials, adding 150mL of sodium hydroxide solution, heating in a water bath, and carrying out alkali-melting reaction;
(3) dissolving the filter residue after the alkali-fusion reaction in 300mL of 1:1 hydrochloric acid, and introducing air into a water bath to oxidize ferrous ions;
(4) Adding a pH regulating solution into the solution, and then carrying out suction filtration;
(5) And calcining the filter residue after suction filtration to obtain the ferric oxide. The rest is the same as the first embodiment.
EXAMPLE III
The iron oxide prepared in example one or example two was subjected to X-ray diffraction (XRD) and infrared spectroscopic analysis.
Referring to fig. 2 and 3, it can be seen from XRD spectrum analysis that the iron oxide prepared by the embodiment of the present invention is a mixture of iron sesquioxide and iron oxyhydroxide, wherein the content of iron sesquioxide is 80.26%, the content of iron oxyhydroxide is 19.74%, and the prepared product is a relatively pure iron oxide; the infrared spectrogram analysis shows that the wavelength is 3550cm-1~3149cm-1The absorption peaks are more, which indicates that hydroxyl exists on the surface of the iron oxide in the wavelength range, and the wavelength is 456cm-1And 543cm-1in the presence of Fe2O3The characteristic absorption peak of the present invention shows that the product obtained by the preparation method of the embodiment of the present invention contains ferric oxide. Show the practice of the inventionthe preparation method of the example can prepare pure iron oxide.
In this document, the terms front, back, upper and lower are used to define the components in the drawings and the positions of the components relative to each other, and are used for clarity and convenience of the technical solution. It is to be understood that the use of the directional terms should not be taken to limit the scope of the claims.
The features of the embodiments and embodiments described herein above may be combined with each other without conflict.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents, improvements and the like that fall within the spirit and principle of the present invention are intended to be included therein.

Claims (5)

1. A method for extracting iron element from serpentine magnesium extraction residue and preparing ferric oxide is characterized by comprising the following steps:
(1) Preparing raw materials, namely taking iron-rich residues obtained after conventional serpentine acid leaching for preparing magnesium oxide as raw materials; diluting hydrochloric acid with water to obtain an acid leaching agent in a ratio of 1:1, adding the acid leaching agent into a three-mouth bottle with a reflux device and an electric stirrer, adding serpentine mineral powder clinker into the three-mouth bottle according to a liquid-solid ratio of 5: 1, heating in a water bath, controlling the temperature at 90 ℃, stirring for 150min, cooling and filtering, repeatedly washing filter residues with water until the pH value of a washing solution is 6-7, and washing to obtain a raw material of iron-rich residues;
(2) Adding a sodium hydroxide solution into the raw materials according to the solid-to-liquid ratio of 1:3, and carrying out an alkali-melting reaction under the water-bath heating condition; the concentration of the sodium hydroxide solution is 2.5mol/L, the water bath heating temperature is 55 ℃, and the alkali-fusion reaction time is 3 h; in the alkali melting process, an aluminum-containing compound in the residue reacts with alkali to finally generate aluminum meta-acid, so that aluminum elements in the iron-rich residue are removed;
(3) Putting the filter residue after the alkali-fusion reaction in a hydrochloric acid solution with the ratio of 1:1, and introducing air under the heating of a water bath to oxidize ferrous ions in the solution; the water bath heating temperature is 60 ℃, the air is introduced for 0.5h, and the oxidation is carried outDivalent iron ions in solution; dissolving the filter residue after alkali melting in 1:1 hydrochloric acid, and dissolving Fe-containing compounds into Fe under strong acid condition2+、Fe3+,Fe2+Oxidized into Fe in the process of introducing air under acidic condition3+
(4) Taking a pH regulating solution prepared from ammonia water and the sodium hydroxide solution, regulating the pH value to 3.0 +/-0.1, and then carrying out suction filtration;
(5) And calcining the filter residue after suction filtration to obtain the ferric oxide.
2. The method as claimed in claim 1, wherein the concentration of ammonia water in step (4) is 30%, and the pH adjusting solution is prepared from 1:5 ammonia water and the sodium hydroxide solution.
3. The method for extracting Fe element from the residue of extracting Mg from serpentine and preparing Fe oxide as claimed in claim 1, wherein the calcination temperature in step (5) is 600 ℃ for 2 hours.
4. The method for extracting iron element from the serpentine magnesium extraction residue and preparing iron oxide according to claim 1, wherein in the step (2), the raw material is 50g, and the sodium hydroxide solution is 150 mL.
5. the method for extracting iron element from the serpentine magnesium extraction residue and preparing iron oxide according to claim 1, wherein the 1:1 hydrochloric acid is 300mL in step (3).
CN201710592334.6A 2017-07-19 2017-07-19 method for extracting iron element from serpentine magnesium extraction residue and preparing ferric oxide Expired - Fee Related CN107188239B (en)

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CN100584764C (en) * 2008-04-02 2010-01-27 潘爱芳 Method for reclaiming ferric oxide from coal ash and coal gangue
CN102390869B (en) * 2011-08-08 2014-05-14 山西同华科技有限公司 Method for preparing high-purity ferric oxide by using aluminum oxide red mud
CN103408043B (en) * 2013-08-13 2015-05-13 中国地质大学(武汉) Method for preparing high-purity magnesium oxide with serpentine as raw material
CN103395796B (en) * 2013-08-13 2015-02-25 南阳东方应用化工研究所 Comprehensive utilization method of serpentine and device used by method

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