CN115820945A - Regulating agent for separating and enriching iron in iron and steel dust mud, method and application - Google Patents
Regulating agent for separating and enriching iron in iron and steel dust mud, method and application Download PDFInfo
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- CN115820945A CN115820945A CN202211181690.6A CN202211181690A CN115820945A CN 115820945 A CN115820945 A CN 115820945A CN 202211181690 A CN202211181690 A CN 202211181690A CN 115820945 A CN115820945 A CN 115820945A
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- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 title claims abstract description 300
- 229910052742 iron Inorganic materials 0.000 title claims abstract description 148
- 239000000428 dust Substances 0.000 title claims abstract description 82
- 229910000831 Steel Inorganic materials 0.000 title claims abstract description 56
- 239000010959 steel Substances 0.000 title claims abstract description 56
- 238000000034 method Methods 0.000 title claims abstract description 47
- 239000003795 chemical substances by application Substances 0.000 title claims abstract description 40
- 230000001105 regulatory effect Effects 0.000 title claims abstract description 37
- 239000002244 precipitate Substances 0.000 claims abstract description 57
- 239000011701 zinc Substances 0.000 claims abstract description 46
- 229910052725 zinc Inorganic materials 0.000 claims abstract description 44
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 claims abstract description 43
- 238000000926 separation method Methods 0.000 claims abstract description 38
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 37
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 23
- 229940044631 ferric chloride hexahydrate Drugs 0.000 claims abstract description 17
- NQXWGWZJXJUMQB-UHFFFAOYSA-K iron trichloride hexahydrate Chemical compound O.O.O.O.O.O.[Cl-].Cl[Fe+]Cl NQXWGWZJXJUMQB-UHFFFAOYSA-K 0.000 claims abstract description 17
- ZRTJYPZMXSQDDF-UHFFFAOYSA-K O.O.O.Cl[Fe](Cl)Cl Chemical compound O.O.O.Cl[Fe](Cl)Cl ZRTJYPZMXSQDDF-UHFFFAOYSA-K 0.000 claims abstract description 12
- 239000000376 reactant Substances 0.000 claims abstract description 11
- 238000002156 mixing Methods 0.000 claims abstract description 6
- 238000006243 chemical reaction Methods 0.000 claims description 77
- 239000010802 sludge Substances 0.000 claims description 29
- 238000005406 washing Methods 0.000 claims description 15
- 238000011084 recovery Methods 0.000 claims description 5
- 239000007791 liquid phase Substances 0.000 claims description 4
- 239000007795 chemical reaction product Substances 0.000 claims description 2
- 230000008569 process Effects 0.000 abstract description 20
- 229910021645 metal ion Inorganic materials 0.000 abstract description 14
- 229910052595 hematite Inorganic materials 0.000 abstract description 9
- 239000011019 hematite Substances 0.000 abstract description 9
- LIKBJVNGSGBSGK-UHFFFAOYSA-N iron(3+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Fe+3].[Fe+3] LIKBJVNGSGBSGK-UHFFFAOYSA-N 0.000 abstract description 9
- 229910052500 inorganic mineral Inorganic materials 0.000 abstract description 7
- -1 iron ions Chemical class 0.000 abstract description 7
- 239000011707 mineral Substances 0.000 abstract description 7
- 239000013078 crystal Substances 0.000 abstract description 6
- 239000001257 hydrogen Substances 0.000 abstract description 5
- 229910052739 hydrogen Inorganic materials 0.000 abstract description 5
- 230000007062 hydrolysis Effects 0.000 abstract description 5
- 238000006460 hydrolysis reaction Methods 0.000 abstract description 5
- 229910052751 metal Inorganic materials 0.000 abstract description 5
- 230000006911 nucleation Effects 0.000 abstract description 5
- 238000010899 nucleation Methods 0.000 abstract description 5
- 230000009466 transformation Effects 0.000 abstract description 5
- 238000010306 acid treatment Methods 0.000 abstract description 3
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- 239000000243 solution Substances 0.000 description 19
- 239000012071 phase Substances 0.000 description 12
- 239000002243 precursor Substances 0.000 description 11
- 238000003723 Smelting Methods 0.000 description 6
- 238000002441 X-ray diffraction Methods 0.000 description 6
- 229910001308 Zinc ferrite Inorganic materials 0.000 description 6
- 239000002253 acid Substances 0.000 description 6
- 239000007788 liquid Substances 0.000 description 6
- 235000010755 mineral Nutrition 0.000 description 6
- 239000000047 product Substances 0.000 description 6
- WGEATSXPYVGFCC-UHFFFAOYSA-N zinc ferrite Chemical compound O=[Zn].O=[Fe]O[Fe]=O WGEATSXPYVGFCC-UHFFFAOYSA-N 0.000 description 6
- 238000002386 leaching Methods 0.000 description 5
- 230000000052 comparative effect Effects 0.000 description 4
- 238000004519 manufacturing process Methods 0.000 description 4
- 238000001878 scanning electron micrograph Methods 0.000 description 4
- 229910001341 Crude steel Inorganic materials 0.000 description 3
- 230000008859 change Effects 0.000 description 3
- 238000004663 powder metallurgy Methods 0.000 description 3
- 238000005245 sintering Methods 0.000 description 3
- 239000013543 active substance Substances 0.000 description 2
- 238000004458 analytical method Methods 0.000 description 2
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- 238000005265 energy consumption Methods 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 229910001385 heavy metal Inorganic materials 0.000 description 2
- 238000010335 hydrothermal treatment Methods 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 230000001698 pyrogenic effect Effects 0.000 description 2
- 239000002910 solid waste Substances 0.000 description 2
- 238000001228 spectrum Methods 0.000 description 2
- 229910052596 spinel Inorganic materials 0.000 description 2
- 239000011029 spinel Substances 0.000 description 2
- 238000009865 steel metallurgy Methods 0.000 description 2
- 239000002699 waste material Substances 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 229910021578 Iron(III) chloride Inorganic materials 0.000 description 1
- 239000003082 abrasive agent Substances 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 239000003463 adsorbent Substances 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 229910052783 alkali metal Inorganic materials 0.000 description 1
- 150000001340 alkali metals Chemical class 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 239000012141 concentrate Substances 0.000 description 1
- 230000008094 contradictory effect Effects 0.000 description 1
- 230000001276 controlling effect Effects 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 229940032296 ferric chloride Drugs 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 239000002920 hazardous waste Substances 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 238000002354 inductively-coupled plasma atomic emission spectroscopy Methods 0.000 description 1
- 239000000976 ink Substances 0.000 description 1
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 description 1
- 238000007885 magnetic separation Methods 0.000 description 1
- 238000012423 maintenance Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
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- 238000005096 rolling process Methods 0.000 description 1
- 239000002893 slag Substances 0.000 description 1
- 239000007790 solid phase Substances 0.000 description 1
- 238000009628 steelmaking Methods 0.000 description 1
- 239000011573 trace mineral Substances 0.000 description 1
- 235000013619 trace mineral Nutrition 0.000 description 1
- 239000002912 waste gas Substances 0.000 description 1
- 239000002351 wastewater Substances 0.000 description 1
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
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Abstract
The invention provides a regulating agent for separating and enriching iron in iron and steel dust mud, a method and application thereof. The regulating agent comprises one or more of ferric chloride hexahydrate and ferric chloride trihydrate. The method for separating and enriching iron in the iron and steel dust comprises the following steps: mixing the iron and steel dust mud and a regulating agent to carry out hydrothermal reaction. Adding water into the reactant, centrifugally cleaning and separating to obtain an iron-enriched precipitate and a zinc-containing separation solution. Under the hydrothermal condition, crystal water in the regulating agent is separated and iron ions are hydrolyzed, hydrogen ions generated in the hydrolysis process can enable iron and steel dust mud to generate ore phase transformation to release internal zinc, nucleation and growth of hematite are accelerated by the existence of the regulating agent, iron elements are enriched in precipitates, other metal ions are retained in a solution, and separation and enrichment of the iron elements are realized. The regulating agent can realize effective separation of metal elements by a mineral phase hydrothermal method, thereby avoiding the problem of subsequent acid treatment and reducing pollution; and shortens the process flow.
Description
Technical Field
The invention relates to the technical field of separation and recovery of iron and steel dust and mud, in particular to a regulating agent and a method for separating and enriching iron in iron and steel dust and mud and application thereof.
Background
Iron, which is the second metal in the earth's crust, is currently the most predominant metal material. The iron is widely applied to the fields of pharmacy, pesticides, powder metallurgy, hot hydrogen generators, gel propellants, combustion active agents, catalysts, water cleaning adsorbents, sintering active agents, powder metallurgy products, various mechanical part products, hard alloy material products and the like. Pure iron is used for making the iron cores of generators and motors, reduced iron powder is used for powder metallurgy, and steel is used for making machines and tools. In addition, iron and its compounds are used for preparing magnets, medicines, inks, pigments, abrasives, etc. Iron is also one of the essential trace elements required by the human body, and thus the importance of iron can be seen.
Iron and steel are the basis of industrial products, and the iron and steel smelting industry is an important basic industry of national economy, but the iron and steel smelting industry not only needs to invest a large amount of material resources and energy resources, but also discharges a large amount of waste water, waste gas and solid wastes in the processing and production process. These wastes pose a hazard to the environment and pose a threat to human health. Wherein, the iron and steel smelting can generate a large amount of iron and steel dust mud, which is one of the solid wastes mainly faced by the smelting industry.
The iron and steel dust mud is mainly derived from links of iron making, steel making, sintering, steel rolling and the like in the iron and steel smelting process, contains various alkali metals and heavy metal elements, and is low in recycling rate. The production amount of the dust and mud for iron and steel metallurgy is about 10-12% of the yield of the crude steel, and the produced dust and mud for iron and steel metallurgy reaches 1.065-1.278 hundred million tons calculated by the yield of the crude steel of China being 10.65 hundred million tons in 2020. The zinc-containing dust and mud is typical iron-containing waste slag generated in the steel smelting process. The production amount of the zinc-containing dust and mud is about 10 percent of the yield of crude steel, and the annual yield of the zinc-containing dust and mud in China reaches more than 8000 ten thousand tons.
At present, the method for treating the zinc-containing dust and sludge in the steel plant mainly comprises a fire method, a wet method and a combined method. The method mainly adopts a pyrogenic process for low-zinc dust, wherein the rotary hearth furnace and rotary kiln process are most widely used. Magnetic separation is carried out on the roasted ore obtained by the rotary kiln process to obtain magnetic concentrate with high iron grade and low zinc content; the rotary hearth furnace process can obtain a roasted product with the iron grade of 56.71 percent and the Zn content of 0.07 percent. However, the rotary kiln is easy to form rings, high in operation requirement, low in operation rate, large in equipment investment, high in operation cost and high in energy consumption, and can form nodules after improper operation for 1 month. The elements in the dust produced by the rotary hearth furnace process are complex, and the subsequent treatment and recovery are difficult; and the process has high maintenance cost, high energy consumption and low efficiency. In addition, the pyrogenic process also causes secondary pollution and is poor in environmental protection. In the wet leaching process, the leaching rate of zinc ferrite spinel in the steel dust mud is low, a large amount of acid or alkali is needed for leaching, a large amount of acid mud is generated in the acid leaching process, and the subsequent treatment is difficult.
Disclosure of Invention
The invention mainly aims to provide a regulating agent and a method for separating and enriching iron in iron and steel dust and sludge and application thereof, and aims to solve the technical problems of complex treatment process, low pollution and simple post-treatment of the iron and steel dust and sludge.
In order to achieve the above object, the present invention provides in a first aspect a conditioning agent for iron separation and enrichment in steel dust and sludge, the conditioning agent comprising one or more of ferric chloride hexahydrate and ferric chloride trihydrate.
The second aspect of the invention provides a method for separating and enriching iron in steel dust and sludge, which comprises the following steps:
mixing the iron and steel dust mud with a regulating agent, and carrying out hydrothermal reaction in a closed container, wherein the regulating agent comprises one or more of ferric chloride hexahydrate and ferric chloride trihydrate.
And adding water to the reactant for washing, and separating the precipitate to obtain the iron-enriched precipitate.
According to an embodiment of the present application, the step of washing the reactant with water and separating the precipitate to obtain an iron-enriched precipitate comprises:
and adding water to the reaction product for washing, and centrifugally separating the precipitate to obtain the iron-enriched precipitate.
According to the implementation mode of the application, the reaction temperature of the hydrothermal reaction is 150-200 ℃.
According to an embodiment of the present application, the reaction temperature of the hydrothermal reaction is 180 to 200 ℃.
According to the embodiment of the present application, the hydrothermal reaction time is 2 to 20 hours.
According to the embodiment of the application, the duration of the hydrothermal reaction is 4 to 10 hours.
According to the embodiment of the application, the mass ratio of the regulating agent to the steel dust mud is (1-2): 1.
According to the embodiment of the application, in the step of adding water to wash the reactant and separating the precipitate, the separated liquid phase is collected to obtain the zinc-containing separation liquid.
The third aspect of the invention provides an application of the method for separating and enriching iron from the iron and steel dust mud in the recovery of the iron and steel dust mud.
The regulating agent for separating and enriching iron in the steel dust and sludge comprises one or more of ferric chloride hexahydrate and ferric chloride trihydrate. Under the condition of carrying out hydrothermal reaction, crystal water in the regulating agent is separated and iron ions are hydrolyzed, hydrogen ions generated in the hydrolysis process can enable iron and steel dust mud to generate ore phase transformation to release internal zinc, nucleation and growth of hematite are accelerated by the existence of the regulating agent, iron elements are enriched in precipitates, other metal ions are retained in the solution, and separation and enrichment of the iron elements are realized. The regulating agent can realize effective separation of metal elements by a mineral phase hydrothermal method, thereby avoiding the problem of subsequent acid treatment and reducing pollution; and shortens the process flow.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, it is obvious that the drawings in the following description are only some embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to the structures shown in the drawings without creative efforts.
Fig. 1 is a schematic flow chart of a method for separating and enriching iron from steel dust and sludge by a mineral phase hydrothermal control method according to an embodiment of the present disclosure;
FIG. 2 is an XRD pattern of electric furnace dust and sludge before reaction and iron-enriched precipitate after reaction in example 1, wherein: FIG. 2 (a) is an XRD pattern of electric furnace dust before reaction, and FIG. 2 (b) is an XRD pattern of iron-enriched precipitate after reaction;
FIG. 3 is a scanning electron micrograph of the electric furnace dust and sludge before reaction and the iron-rich precipitate after reaction in example 1, wherein: FIG. 3 (a) is a scanning electron micrograph of electric furnace dust sludge before reaction, and FIG. 3 (b) is a scanning electron micrograph of iron-enriched precipitates after reaction;
FIG. 4 is a graph showing the change of the contents of Fe and Zn in the electric furnace dust and sludge and the Fe-enriched precipitate before and after the reaction in example 1;
FIG. 5 is an XRD pattern of pre-reaction furnace dust and sludge and post-reaction iron-rich precipitate of comparative example 1;
FIG. 6 is an XRD pattern of the pre-reaction furnace dust sludge and the post-reaction iron-enriched precipitate in comparative example 2.
The implementation, functional features and advantages of the present invention will be further explained with reference to the accompanying drawings.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings in the embodiments of the present invention, and it is apparent that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be obtained by a person skilled in the art without any inventive step based on the embodiments of the present invention, are within the scope of the present invention.
It should be noted that all the directional indicators (such as upper and lower 8230; etc.) in the embodiments of the present invention are only used for explaining the relative positional relationship between the components, the motion situation, etc. in a specific posture (as shown in the drawings), and if the specific posture is changed, the directional indicator is changed accordingly.
In addition, the descriptions related to "first", "second", etc. in the present invention are only for descriptive purposes and are not to be construed as indicating or implying relative importance or implicitly indicating the number of technical features indicated. Thus, a feature defined as "first" or "second" may explicitly or implicitly include at least one such feature.
Moreover, the technical solutions in the embodiments of the present invention may be combined with each other, but it is necessary to be able to be realized by a person skilled in the art, and when the technical solutions are contradictory or cannot be realized, the combination of the technical solutions should be considered to be absent, and is not within the protection scope of the present invention.
The invention provides a regulating agent for separating and enriching iron in iron and steel dust mud, which comprises one or more of ferric chloride hexahydrate and ferric chloride trihydrate.
The iron and steel dust mud can be zinc-containing dust mud, and can be one or more of electric furnace dust mud and converter dust mud. The ferric chloride hexahydrate and the ferric chloride trihydrate are both in powder form during use.
The regulating agent for separating and enriching iron in the steel dust and sludge comprises one or more of ferric chloride hexahydrate and ferric chloride trihydrate. Under the hydrothermal condition, crystal water in the regulating agent is separated and iron ions are hydrolyzed, hydrogen ions generated in the hydrolysis process can enable iron and steel dust mud to generate ore phase transformation to release internal zinc, nucleation and growth of hematite are accelerated by the existence of the regulating agent, iron elements are enriched in precipitates, other metal ions are retained in a solution, and separation and enrichment of the iron elements are realized.
In order to complete the separation and enrichment of metal ions in the iron and steel dust and sludge, the invention provides a method for realizing the separation of iron and zinc and the enrichment of iron elements in the iron and steel dust and sludge by mineral phase hydrothermal regulation and control, which comprises the following steps:
s100: mixing the iron and steel dust mud with a regulating agent, and carrying out hydrothermal reaction in a closed container, wherein the regulating agent comprises one or more of ferric chloride hexahydrate and ferric chloride trihydrate.
In the step, the iron and steel dust mud is mixed with a regulating agent to obtain a reaction precursor. The mixing time of the iron and steel dust mud and the regulating agent can be 10-30 min. Thus, the iron and steel dust mud and the regulating agent are uniformly mixed.
The closed container can be opened and closed after the reaction precursor is filled, and can be a hydrothermal reaction kettle, for example. And heating the hydrothermal reaction kettle to perform hydrothermal reaction. In the process, the gas in the closed container expands under heat, and a reaction environment with certain pressure is provided for the reaction precursor.
The hydrothermal reaction is a generic term for chemical reactions that are carried out in a fluid such as water, an aqueous solution, or steam at a certain temperature and pressure.
In one embodiment of the present application, in the heating reaction, a small amount of free water (for convenience, referred to as "water") is formed as crystal water in ferric chloride hexahydrate and ferric chloride trihydrate. The reaction process may also be referred to as a hydrothermal reaction.
Specifically, referring to the above analysis of the controlling agent under hydrothermal conditions, based on the principle of acid production by hydrolysis of metal ions, hydrogen chloride (HCl) generated by hydrolysis of ferric chloride is dissolved in the generated water to form hydrogen ions (H) having a high concentration + ) With ZnFe 2 O 4 Reaction, simultaneously, with formation of Fe 3+ Also hydrolyzes in the seal system as shown in the following equation.
2FeCl 3 + 3H 2 O = Fe 2 O 3 + 6HCl
ZnFe 2 O 4 + 8H + = Zn 2+ + 2Fe 3+ + 4H 2 O
2Fe 3+ + 3H 2 O = Fe 2 O 3 + 6H +
In one embodiment of the present application, a small amount of water may be added to the reaction precursor to perform the hydrothermal reaction.
S200: and adding water to the reactant for washing, and separating the precipitate to obtain the iron-enriched precipitate.
After the iron and steel dust mud and the regulating agent are subjected to hydrothermal reaction, the reactant is in a certain wet state. Under the hydrothermal condition, the regulating agent is hydrolyzed to promote the change of the mineral phase of the iron and steel dust mud, so that the metal ions are effectively removed, and the nucleation growth behavior of the metal ions is regulated by the regulating agent, so that most of iron is converted into Fe 2 O 3 The other metal ions are still in the ionic state. Adding water, fe to the reactants 2 O 3 A precipitate forms and the other metal ions remain in an ionic state and remain in solution.
The precipitate is separated (e.g., centrifuged) to obtain an iron-enriched precipitate. The separated liquid phase may be referred to as a zinc-containing separation liquid. The process can realize the effective separation of iron and zinc elements in the iron and steel dust mud, and solves the technical problems that the iron and steel dust mud is difficult to recycle and the heavy metal is difficult to separate and recycle efficiently. The iron-enriched precipitate can be subjected to several washing and separation processes with water. The metal ions in the reaction solution adsorbed on the surface of the iron-rich precipitate are washed away. Drying treatment can be carried out after cleaning.
Compared with the prior art, the invention has the following advantages:
the invention can realize the effective separation of iron and zinc elements from the iron and steel dust mud, the secondary utilization of hazardous wastes and the improvement of the utilization rate of resources. The invention realizes effective removal of metal ions in the iron and steel dust mud by adopting an ore phase hydrothermal method, and the introduction of the regulating agent successfully realizes effective nucleation and growth of the hematite. Compared with acid leaching treatment, the use of acid is reduced, and the problem of subsequent acid treatment is avoided; the method realizes effective separation of metal elements by a one-step ore-phase hydrothermal method, shortens the process flow, further ensures the separation effectiveness and yield, and enables the iron-containing precipitate to grow in a crystal form under the combined action of hydrothermal conditions and a regulating agent without secondary sintering to obtain the iron-containing precipitate with orderly crystal lattice arrangement, namely the iron-enriched precipitate. The iron-enriched precipitate is a precipitate with high iron content, specifically hematite, and can be reused.
In some embodiments, the reaction temperature of the hydrothermal reaction is from 150 ℃ to 200 ℃. Preferably 180-200 ℃. The zinc ferrite in the steel dust mud is difficult to decompose due to the low temperature.
In some embodiments, the hydrothermal reaction is carried out for a period of 2 to 20 hours. Preferably 4-10h. Too short a period of time can result in incomplete decomposition of the zinc ferrite and incomplete conversion into hematite.
In some embodiments, the mass ratio of the regulating agent to the steel dust mud is (1 to 2): 1. Insufficient use of the regulator can result in incomplete decomposition of the zinc ferrite.
In the foregoing analysis, zinc and other metal ions are mainly in solution, and the metal ions can be reused. Thus, in some embodiments, further comprising: and in the step of adding water to wash the reactant and separating precipitate, collecting the separated liquid phase to obtain the zinc-containing separation liquid.
The zinc-containing separation liquid contains other metal separation liquids, and metal ions are recycled through treatment, so that secondary utilization of resources is realized.
The invention also provides application of the method for separating and enriching iron in the steel dust and sludge in the recovery of the steel dust and sludge.
To facilitate a further understanding of the above embodiments, reference will now be made to the following examples:
example 1
1. And (3) fully mixing electric furnace dust mud (Fe52.4 percent, zn7.96 percent) and ferric chloride hexahydrate for 30 min according to the proportion of 2.
2. And placing the reaction precursor in a reaction kettle for hydrothermal reaction at the reaction temperature of 200 ℃ for 10 hours. And after the reaction is finished, washing for many times to obtain an iron-enriched precipitate and a zinc-containing separation solution. XRD spectrums of the electric furnace dust and mud before reaction and the iron-enriched precipitate after reaction are shown in figure 2, and it can be seen that the electric furnace dust and mud is converted into hematite after hydrothermal reaction, and diffraction peaks of zinc ferrite spinel disappear. Scanning electron micrographs of the electric furnace dust and sludge before the reaction and the iron-enriched precipitate after the reaction are shown in figure 3, and it can be seen that the product after the hydrothermal reaction is spherical hematite and the particles are more uniformly distributed.
3. And (3) digesting the electric furnace dust and mud before reaction and the iron-enriched precipitate after reaction, and quantitatively testing iron and zinc elements in the sample by using ICP-OES. The element content changes are shown in figure 4, and it can be seen that the electric furnace dust mud before reaction contains 52.4% of iron and 7.96% of zinc; the iron-enriched precipitate after the reaction contains 66.63% of iron and 0.11% of zinc. After hydrothermal treatment, the Fe content in the solid phase is close to the theoretical iron content of hematite, and the separation rate of zinc reaches 98%.
Example 2
1. The electric furnace dust sludge of example 1 and ferric chloride hexahydrate were mixed thoroughly for 10 min at a ratio of 1.
2. And placing the reaction precursor in a reaction kettle for hydrothermal reaction at the reaction temperature of 200 ℃ for 8 h. And after the reaction is finished, washing for many times to obtain an iron-enriched precipitate and a zinc-containing separation solution.
3. In the embodiment, the electric furnace dust and sludge before reaction contains 52.4% of iron and 7.96% of zinc; the iron-enriched precipitate after the reaction contains 66.75% of iron and 0.06% of zinc.
Example 3
1. The converter dust sludge (Fe49.7%, zn10.15%) and ferric chloride hexahydrate are fully mixed for 30 min according to the proportion of 2.
2. And placing the reaction precursor in a reaction kettle for hydrothermal reaction at the temperature of 180 ℃ for 10 hours. And after the reaction is finished, washing for many times to obtain an iron-enriched precipitate and a zinc-containing separation solution.
3. In the embodiment, the converter dust before reaction contains 49.7% of iron and 10.15% of zinc; the iron-enriched precipitate after the reaction contains 65.33% of iron and 1.18% of zinc.
Example 4
1. The electric furnace dust sludge of example 1 and ferric chloride trihydrate were mixed thoroughly for 20 min at a ratio of 1.
2. And placing the reaction precursor in a reaction kettle for hydrothermal reaction at the temperature of 180 ℃ for 4 hours. And after the reaction is finished, washing for many times to obtain an iron-enriched precipitate and a zinc-containing separation solution.
3. In the present example, the electric furnace dust before reaction contains 52.4% of iron and 7.96% of zinc; the iron-enriched precipitate after the reaction contains 65.77% of iron and 0.13% of zinc.
Example 5
1. The converter dust sludge of example 3 and ferric chloride hexahydrate were mixed thoroughly for 20 min at a ratio of 2.
2. And placing the reaction precursor in a reaction kettle for hydrothermal reaction at the reaction temperature of 200 ℃ for 2 h. And after the reaction is finished, washing for many times to obtain an iron-enriched precipitate and a zinc-containing separation solution.
3. In the embodiment, the converter dust before reaction contains 49.7% of iron and 10.15% of zinc; the iron-enriched precipitate after the reaction contains 62.43% of iron and 2.01% of zinc.
Example 5
1. The converter dust sludge of example 3 and ferric chloride hexahydrate were mixed thoroughly for 20 min at a ratio of 2.
2. And placing the reaction precursor in a reaction kettle for hydrothermal reaction at the reaction temperature of 150 ℃ for 20 h. And after the reaction is finished, washing for many times to obtain an iron-enriched precipitate and a zinc-containing separation solution.
3. In the embodiment, the converter dust before reaction contains 49.7% of iron and 10.15% of zinc; the iron-enriched precipitate after the reaction contains 64.25% of iron and 1.84% of zinc.
Comparative example 1
1.2 g of the converter dust and sludge (Fe49.7%, zn10.15%) of example 3 was put into a reaction kettle for hydrothermal reaction at 200 ℃ for 10 hours. After the reaction is finished, carrying out solid-liquid separation to obtain an iron-enriched precipitate and a zinc-containing separation solution.
2. XRD spectra of converter dust and sludge before reaction and iron-enriched precipitate after reaction are shown in figure 5, and phases before and after hydrothermal treatment are unchanged.
Compared with example 3, it can be seen that the separation of iron and zinc in mineral phase transformation can not be realized without adding a regulator.
Comparative example 2
1.2 g of the electric furnace dust sludge (Fe52.4%, zn7.96%) of example 1 and ferric chloride hexahydrate were mixed well for 30 min at a ratio of 2.
2. And placing the reaction precursor in a reaction kettle for hydrothermal reaction at 100 ℃ for 10 hours. And after the reaction is finished, washing for many times to obtain an iron-enriched precipitate and a zinc-containing separation solution. The XRD spectrum of the iron-enriched precipitate after the reaction is shown in figure 6, and the phase change is not large after hydrothermal reaction.
Compared with the example 1, the zinc ferrite is not decomposed at the temperature of 100 ℃, and the separation of iron and zinc by mineral phase transformation cannot be realized.
In the above technical solutions of the present invention, the above are only preferred embodiments of the present invention, and the technical scope of the present invention is not limited thereby, and all the technical concepts of the present invention, equivalent structural changes made by using the contents of the description and the drawings of the present invention, or direct/indirect applications in other related technical fields, are included in the scope of the present invention.
Claims (10)
1. A regulating agent for separating and enriching iron in iron and steel dust mud is characterized in that the regulating agent comprises one or more of ferric chloride hexahydrate and ferric chloride trihydrate.
2. A method for separating and enriching iron in iron and steel dust mud is characterized by comprising the following steps:
mixing the iron and steel dust mud with a regulating agent, and carrying out hydrothermal reaction in a closed container, wherein the regulating agent comprises one or more of ferric chloride hexahydrate and ferric chloride trihydrate;
and adding water to the reactant for washing, and separating the precipitate to obtain the iron-enriched precipitate.
3. The method for separating and enriching iron according to claim 2, wherein the step of washing the reactant with water and separating the precipitate to obtain the iron-enriched precipitate comprises:
and adding water to the reaction product for washing, and centrifugally separating the precipitate to obtain the iron-enriched precipitate.
4. The method for separating and enriching iron of claim 2, wherein the reaction temperature of the hydrothermal reaction is 150 ℃ to 200 ℃.
5. The method for iron separation and enrichment according to claim 4, wherein the reaction temperature of the hydrothermal reaction is 180 to 200 ℃.
6. The method for iron separation and enrichment according to claim 4, wherein the hydrothermal reaction is carried out for a period of 2 to 20 hours.
7. The method for iron separation and enrichment according to claim 6, wherein the hydrothermal reaction is carried out for a period of 4 to 10 hours.
8. The method for iron separation and enrichment according to claim 2, wherein the mass ratio of the control agent to the steel dust mud is (1 to 2): 1.
9. The method for separating and enriching iron according to any one of claims 2 to 8, wherein in the step of adding water to wash the reactant and separating the precipitate, the separated liquid phase is collected to obtain a zinc-containing separation solution.
10. Use of the method of any one of claims 2 to 9 for iron separation and enrichment in iron and steel sludge recovery.
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