WO2016148446A1 - Procédé de fabrication d'un composé de zinc à partir de poussière de four à arc électrique - Google Patents

Procédé de fabrication d'un composé de zinc à partir de poussière de four à arc électrique Download PDF

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Publication number
WO2016148446A1
WO2016148446A1 PCT/KR2016/002442 KR2016002442W WO2016148446A1 WO 2016148446 A1 WO2016148446 A1 WO 2016148446A1 KR 2016002442 W KR2016002442 W KR 2016002442W WO 2016148446 A1 WO2016148446 A1 WO 2016148446A1
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Prior art keywords
dust
zinc
eafd
filtration
electric
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PCT/KR2016/002442
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English (en)
Korean (ko)
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하종길
신현상
이한샘
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주식회사 정수뉴테크
하종길
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Priority claimed from KR1020150035132A external-priority patent/KR101538746B1/ko
Priority claimed from KR1020150191513A external-priority patent/KR101621967B1/ko
Application filed by 주식회사 정수뉴테크, 하종길 filed Critical 주식회사 정수뉴테크
Publication of WO2016148446A1 publication Critical patent/WO2016148446A1/fr

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    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G9/00—Compounds of zinc
    • C01G9/04—Halides
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B7/00—Working up raw materials other than ores, e.g. scrap, to produce non-ferrous metals and compounds thereof; Methods of a general interest or applied to the winning of more than two metals
    • 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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  • the present invention relates to a method for recovering a zinc (Zn) component containing 15 to 30% as a zinc compound in dust of an electric furnace in the steelmaking industry, and more particularly, hydrochloric acid to dust in an electric furnace of dusty state, which is an industrial waste.
  • a zinc (Zn) component containing 15 to 30% as a zinc compound in dust of an electric furnace in the steelmaking industry, and more particularly, hydrochloric acid to dust in an electric furnace of dusty state, which is an industrial waste.
  • To recover the industrially valuable zinc chloride solution its high-purity powder or zinc sulfate powder and high-purity zinc oxide powder by reacting with a wet process or by reacting dust with sulfuric acid solution.
  • the present invention relates to a method for producing zinc compounds from electric dust that can be utilized as a building material utilizing photocatalytic functions including cement industry by low-chlorination of sludge cakes not dissolved in sulfuric acid.
  • the final product zinc sulfate or zinc chloride is widely used as a trace inorganic nutrient for pigments, fertilizers, feeds, etc.However, when used as a fertilizer, the zinc iron tolerance of zinc sulfate is 0.2% by weight or less, and the zinc iron tolerance of zinc chloride is It is 0.02 weight% or less.
  • zinc sulfate and zinc chloride have been prepared by directly reacting with sulfuric acid or hydrochloric acid using zinc metal.
  • the waste is used to recover the zinc contained in the waste, thereby protecting the environment and economically advantageous.
  • dust or zinc material such as electricity generated in large quantities, but manufacturing using such wastes has various limitations.
  • Furnace dust is generated from scrap metals such as scrap cars due to evaporation of zinc in high temperature furnace at 1800 °C or in scrap cars, and its components may vary depending on the type of scrap metal and the processing company. As shown in Table 1 below, the electric dust (EAFD) composition through X-ray diffraction spectroscopy (XRD) is shown in FIG. 3.
  • EAFD electric dust
  • XRD X-ray diffraction spectroscopy
  • the world steel industry is 1.6 billion tons in 2013, about 45% of which are electric furnaces (Electric World Steel Industry is 1.6 billion tons in 2013, about 45% of which are produced by Electric Arc Furnace. About 11 million tons, or 1.5% of the amount, is generated as dust (EAFD), which contains about 15 to 30% of Zn, which adversely affects the quality of steel making. It is designated as a hazardous waste because it contains harmful heavy metals such as Pb, Cd and Cr. In the past, electric dust cannot be used as it is, so it has been used through special industrial waste companies or mixed with asphalt mortar. Depleting the soil due to various heavy metals generated from the soil and drying the solution containing such leached heavy metals, causing fine powder to scatter and adversely affect the human body. It has emerged as problems.
  • Patent Documents 1 to 5 In order to solve the above problems, many patents have been applied for a method of recovering zinc from dust or zinc material (see Patent Documents 1 to 5).
  • the dust may be treated with electricity to produce an expensive metal zinc or zinc compound.
  • the zinc compound since the iron component is contained in the electric furnace dust in an amount similar to that of zinc,
  • sulfuric acid or hydrochloric acid is used to react with the dust by electricity, not only zinc in the dust but also iron components are reacted together.
  • the dust is analyzed and reacted with sulfuric acid or hydrochloric acid at an equivalent ratio of zinc content in the dust, the zinc component is reacted with acid.
  • Patent Document 1 Patent Application Publication No. 1998-12296
  • Patent Document 2 Patent Document 2: Patent Application Publication No. 1998-15857
  • Patent Document 3 Patent Application No. 1998-39927
  • Patent Document 4 Patent Publication No. 2001-0098080
  • Patent Document 5 Patent Document 5: Patent Publication No. 1538746.
  • the present invention solves various drawbacks and problems caused by zinc oxide (low-purity ZnO) recovery method by dry metallurgy (Pyro metallurgy) from the conventional electric dust in consideration of the above circumstances, and relatively in the wet process (Hydrometallurgy) It improves the difficulty of controlling the co-dissolution of Fe component in economic acid leaching process, and establishes the method to remove trace amount of Fe component by simple method even if trace amount is dissolved and Znferrite component which is impossible to dissolve by SPINEL structure.
  • the problem of recovering more than 90% of Zn contained in electric dust (EAFD) by solving Zn leaching problem of ((ZnFe 3 O 4 ) is completely solved.
  • the method for producing zinc chloride comprises a dust preparation step (S1 step) of preparing dust (EAFD) of the electric furnace; A dust grinding step (S2 step) of grinding the dust (EAFD) with a grinder; A hydrochloric acid reaction step (S3 step) of adding hydrochloric acid to the pulverized dust (EAFD) in a hydrochloric acid reactor; Degassing and neutralization step (S4 step) to remove and neutralize the iron component dissolved in the solution obtained by reacting the dust (EAFD) with hydrochloric acid; A primary filtration step (S5 step) of removing impurities with a filter; A primary drying step (S6 step) of drying the filtrate obtained after the filtration with a hot air spray dryer; A selective dissolution step (S7 step) of adding and dissolving ethyl alcohol (EtOH) to the solid obtained after drying; A secondary filtration step (S8 step) of
  • the present invention is a method for producing a zinc compound from the dust of the electric furnace, the method for producing zinc sulfate and zinc oxide is a pre-treatment step (S21 step) of circulating water in the dust (EAFD) solids of the electric furnace; A primary filtration step (step S22) of filtering the electric dust (EAFD) through the pretreatment step (step S21) with a centrifugal filter; A particle size adjusting step (step S23) of adjusting the particle size of the electric furnace dust (EAFD) by grinding the electric furnace dust (EAFD) with a circular mill; An acid leaching step (S24 step) of reacting dust (EAFD) with a particle size controlled electric furnace in a sulfuric acid solution in a sulfuric acid solution; A de-ironing and neutralization step (S25 step) of removing and neutralizing iron components that may be dissolved in a trace amount in the solution obtained by reacting the electric dust (EAFD) with sulfuric acid solution; A second filtration step (S26) of
  • FIG. 1 is a block conceptual diagram showing a process of a method for producing and recovering zinc chloride from dust of the present invention
  • FIG. 2 is a flowchart illustrating a method for producing and recovering zinc chloride from dust of the present invention.
  • Figure 4 is a flow chart of the execution method of a method for producing zinc sulfate and zinc oxide from dust of the present invention
  • Figure 5 is an X-ray diffraction analysis method (X-ray Diffraction Spectroscopy; XRD) graph showing the electric dust (EAFD) composition
  • Figure 6 is a graph showing the change in pH over the cleaning time of the electric dust (EAFD)
  • Figure 7 is the initial pH conditions of the wash solution the specific alkali metal zinc (Zn) according to the (K, Na, Ca) removal efficiency and the effective metal concentration (M) of (Zn, Fe) graph
  • Figure 8 shows the impact assessment by
  • a vibration ball mill As a mill of the dust crushing step (S2), it is preferable to use a vibration ball mill to completely remove dust particles with electricity of 10 ⁇ m or more, and a ball of a vibration ball mill. It is preferable to use a steel ball having a diameter of 12 mm, and to grind for 100 to 150 minutes so that the average particle diameter is 1 to 2 ⁇ m with a vibration ball mill operated at an amplitude of 5 to 7 mm. .
  • the amount of hydrochloric acid (HCl) added in the hydrochloric acid reaction step (S3 step) is preferably added 500 to 1,000g of 5-12% hydrochloric acid (HCl) per 1,000g of dust (EAFD) in the electric furnace.
  • the iron chloride is oxidized with hydrogen peroxide (H 2 O 2 ) to form Fe 2 O 3 to precipitate and decarburize, and the HCl produced in the oxidation reaction uses potassium hydroxide (KOH). It is preferable to neutralize.
  • the precipitated solid material removed in the first filtration step (S5), cake (Cake) is iron oxide (Fe 2 O 3 ), zinc oxide (ZnO), manganese oxide (MnO), sodium oxide (Na 2 0) and the like,
  • the pH of the filtrate after filtration is preferably about 5.0 to 5.5.
  • the cake (Cake) is preferably to remove the environmental waste of the solid material by recycling as a subsidiary material of building materials manufacturing.
  • the content of chlorine (Cl) is required to be 0.2% by weight or less.
  • the reactivity of the reaction materials was controlled repeatedly to 0.1% by weight or less.
  • the water content of the solid obtained after the first drying step (S6 step) is preferably 0.05 to 0.25%.
  • ethyl alcohol (EtOH) added in the selective dissolution step (S7 step) it is preferable to use more than 99% ethyl alcohol.
  • impurities removed in the secondary filtration step (S8 step) are cake (Cake), potassium chloride (KCl), sodium chloride (NaCl), and the like, and the water content of zinc chloride (ZnCl 2 ) obtained after the second drying step (S11 step).
  • Silver is preferably 0.05 to 0.25%.
  • the zinc (Zn) recovery rate in the high purity powdered zinc chloride (ZnCl 2 ) produced in the second commercialization step (S12 step) is 80% by weight or more.
  • the method for producing zinc sulfate and zinc oxide according to the present invention comprises a pretreatment step (S21 step) of circulating water in the dust (EAFD) solids of the electric furnace; A primary filtration step (step S22) of filtering the electric dust (EAFD) through the pretreatment step (step S21) with a centrifugal filter; A particle size adjusting step (step S23) of adjusting the particle size of the electric furnace dust (EAFD) by grinding the electric furnace dust (EAFD) with a circular mill; An acid leaching step (S24 step) of reacting dust (EAFD) with a particle size controlled electric furnace in a sulfuric acid solution in a sulfuric acid solution; A de-ironing and neutralization step (S25 step) of removing and neutralizing iron components that may be dissolved in a trace amount in the solution obtained by reacting the electric dust (EAFD) with sulfuric acid solution; A second filtration step (S26 step) of separating a liquid phase containing zinc sulfate and zinc
  • the circulating water of the pretreatment step (S21) is added in an in-line mixer or attrition mill (5.0) by adding three to five times the amount of water to the electric dust (EAFD) in an agitation tank. 20 to 30 minutes with a 10 mm ⁇ steel ball) to remove 80 to 90% of the water-soluble impurities.
  • EAFD electric dust
  • the particle size adjusting step (S23 step) is a ratio of the solids and water to the solids obtained by filtration in the first filtration step (S22 step) to 1: 3 to 4 by weight ratio, and then in a stirring tank to an in-line mixer. It is preferable to grind
  • step S24 the sulfuric acid is gradually added to the particle size controlled electric dust (EAFD) to adjust the pH to 2.5 to 3.5, and the reaction is performed for 20 to 60 minutes until the pH becomes 4.0 to 5.0. .
  • EAFD particle size controlled electric dust
  • the cake, the main component of iron oxide removed in the second filtration step (S26), can be recycled as a building material subsidiary material of the photocatalyst function by lowering the residual chlorine flow rate to 1,000 ppm or less, and also 90% of the Zn component.
  • the abnormal recovery allows the Fe in the solid content to be recycled back to the electric furnace.
  • the step of depositing the trace heavy metal (S27 step) to the filtrate obtained after the filtration of the second filtration step (S16 step) to the zinc (Zn) powder at a pH 3 ⁇ 5 of 0.1 ⁇ 0.3% of the electric dust (EAFD) throughput It is preferable to inject
  • the Pb recovered in the third filtration step (S28 step) may be used as a lead acid battery raw material with a purity of about 70%.
  • a high purity zinc sulfate (ZnSO 4 ) solution obtained through the third filtration step (S28 step) is crystallized at 39 ° C. to obtain zinc sulfate 7 hydrochloride (ZnSO 4 7H 2 O). or by drying at 100 ⁇ 120 °C can be commercialized by obtaining a zinc sulfate 1 beard (ZnSO 4 1H 2 O).
  • the zinc sulfate (ZnSO 4 ) may be thermally decomposed at 750 to 800 ° C. to obtain zinc oxide (ZnO) to be commercialized.
  • the present invention economically recovers more than 90% of the Zn component contained in electric dust dust, which is a hazardous waste that is about 11 million tons, which is about 1.5 million tons of low-ferrous materials in electric steel mills in 2013.
  • electric dust dust which is a hazardous waste that is about 11 million tons, which is about 1.5 million tons of low-ferrous materials in electric steel mills in 2013.
  • As a building material that produces zinc compounds with commercial value removes zinc and removes residual dust, the main iron component, in an electric furnace, or utilizes photocatalyst functions such as cement industry by reducing chlorination of sludge cakes not dissolved in sulfuric acid. By making it available, it creates enormous economic added value. Incidentally, it contributes greatly to the improvement of the global environment.
  • FIG. 1 is a block conceptual diagram showing a process of a method for producing and recovering zinc chloride from dust of the present invention
  • FIG. 2 is a flowchart showing a method for producing and recovering zinc chloride from dust of the present invention
  • FIG. 3 is a block conceptual diagram showing a process of a method for producing zinc sulfate and zinc oxide from dust of the present invention
  • FIG. 4 is a flowchart showing a method for producing zinc sulfate and zinc oxide from dust of the present invention
  • EAFD electric dust
  • XRD X-ray diffraction spectroscopy
  • Zinc chloride was produced by the method of producing a zinc compound from the dust of the present invention, and the yield of zinc chloride was investigated.
  • EAFD pulverized dust
  • step S5 filtered through a filter in the first filtration step (step S5), impurities such as cake, iron hydroxide (Fe 2 O 3 ), zinc oxide (ZnO), manganese oxide (MnO), sodium oxide (Na 2 0), and the like.
  • impurities such as cake, iron hydroxide (Fe 2 O 3 ), zinc oxide (ZnO), manganese oxide (MnO), sodium oxide (Na 2 0), and the like.
  • the filtrate was obtained by removing.
  • the filtrate obtained in the first drying step (S6 step) was dried with a hot air spray dryer to obtain a water content of 0.2%, and 99% ethyl alcohol was added to the solid obtained after drying in the selective dissolution step (S7 step).
  • the solid cake (Kake), potassium chloride (KCl), sodium chloride (NaCl), etc. remaining in the filter in the second filtration step (S8 step) were removed to obtain a zinc chloride filtrate dissolved in ethyl alcohol.
  • Zinc sulfate and zinc oxide were produced by the method of producing a zinc compound from the dust of the present invention, and the yields of zinc sulfate and zinc oxide were investigated.
  • a pretreatment step S21
  • 4,000 g of washing water is added to 1,000 g of the electric dust (EAFD) having the composition shown in Table 1 and FIG. 3, and then in-line mixer or attrition mill ( 20 to 30 minutes of washing with an attrition mill; 5.0 to 10 mm ⁇ steel ball) to remove 80 to 90% of the water-soluble impurities, and after confirming that the pH is 8.5 in the first filtration step (S22 step), it was filtered through a centrifugal filter.
  • EAFD electric dust
  • step S23 the electric furnace dust (EAFD) washed in the particle size adjusting step (step S23) was added to 3.0Kg of water in the stirring tank, dispersed, and wet-milled with a bead mill. The grinding was performed so that the thickness was 90% or more.
  • EAFD electric furnace dust
  • the cake, the main component of iron oxide removed in the second filtration step (S26), is washed again by washing with water to recover Zn contained in the liquid phase remaining during filtration, and then the filtrate containing Zn is filtered.
  • Zinc (Zn) powder was added to the filtrate obtained after the filtration in the precipitation step (S27 step) (step S26) at a pH of 4.9, 3 g of 0.3% of the electric dust (EAFD) throughput to obtain Pb and Cd. Heavy metals included were precipitated and precipitated.
  • the Pb recovered as a solid material by executing the third filtration step (S28 step) is used as a lead acid battery raw material, and the high purity obtained through the third filtration step (S28 step) in the screening or drying step (S29 step).
  • the zinc sulfate (ZnSO 4 ) solution was crystallized at 39 ° C. to obtain a powder of zinc sulfate hepatate (ZnSO 4 7H 2 O).
  • the zinc sulfate (ZnSO 4 ) was thermally decomposed at 800 ° C. in a thermal decomposition step (S30) to prepare 311.6 g of high purity zinc oxide (ZnO) of 99% or more. This confirmed a 95.9% recovery of zinc (Zn).
  • the present invention relates to a method for recovering a zinc (Zn) component containing 15 to 30% as a zinc compound in dust of an electric furnace in the steelmaking industry, and more particularly, hydrochloric acid to dust in an electric furnace of dusty state, which is an industrial waste.
  • a zinc (Zn) component containing 15 to 30% as a zinc compound in dust of an electric furnace in the steelmaking industry, and more particularly, hydrochloric acid to dust in an electric furnace of dusty state, which is an industrial waste.
  • To recover the industrially valuable zinc chloride solution its high-purity powder or zinc sulfate powder and high-purity zinc oxide powder by reacting with a wet process or by reacting dust with sulfuric acid solution.
  • the present invention relates to a method for producing zinc compounds from electric dust, which can be utilized as a building material utilizing the photocatalytic function including cement industry by low chlorination of sludge cake not dissolved in sulfuric acid.

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Abstract

La présente invention concerne un procédé de fabrication d'un composé de zinc à partir de poussière de four à arc électrique, constitué par : une étape de prétraitement (étape S21); une étape de filtration primaire (étape S22); une étape de réglage des grosseurs de particule (étape S23); une étape de lixiviation acide (étape S24); une étape de déferrisation/neutralisation (étape S25); une étape de filtration secondaire (étape S26); une étape de précipitation de métaux lourds à l'état de trace (étape S27); une troisième étape de filtration pour éliminer des impuretés résiduelles à l'aide d'un filtre (étape S28); une étape de cristallisation sélective ou de séchage pour cristalliser ou sécher une solution de sulfate de zinc de haute pureté (ZnSO4) obtenue via l'étape de filtration secondaire (étape S29); et une étape de décomposition thermique pour obtenir de l'oxyde de zinc par décomposition thermique du sulfate de zinc (ZnSO4) (étape S30). La présente invention comprend un procédé de déferrisation et de cristallisation de peroxyde d'hydrogène par le fait de permettre la réaction de particules de poussière de four à arc électrique dans une solution d'acide sulfurique d'une concentration de 10-30 %; récupère une poudre de sulfate de zinc monohydraté et de sulfate de zinc heptahydraté et de la poudre d'oxyde de zinc de haute pureté, qui sont hautement utiles d'un point de vue industriel; et réalise l'hypochloration du gâteau de boues non dissous dans l'acide sulfurique et utilise le gâteau de boues en tant que matériau de construction par l'utilisation d'une fonction photocatalytique dans des industries, y compris l'industrie du ciment, ce qui permet d'améliorer les raisons pour lesquelles le gâteau de bouessss ne pouvait pas être commercialisé dans des procédés classiques et de recycler la quantité totale du gâteau de boues. En outre, la présente invention est utile car la présente invention fabrique et récupère du sulfate de zinc et de l'oxyde de zinc, qui sont hautement utiles d'un point de vue industriel et elle permet également d'augmenter le taux de récupération des ingrédients zinciques contenus dans la poussière à raison de 90 % ou plus par la mise en oeuvre d'étapes simples et faciles, ce qui présente un avantage particulier d'excellente faisabilité économique.
PCT/KR2016/002442 2015-03-13 2016-03-11 Procédé de fabrication d'un composé de zinc à partir de poussière de four à arc électrique WO2016148446A1 (fr)

Applications Claiming Priority (4)

Application Number Priority Date Filing Date Title
KR10-2015-0035132 2015-03-13
KR1020150035132A KR101538746B1 (ko) 2015-03-13 2015-03-13 전기로 더스트에 포함되어있는 산화아연으로부터 염화아연을 제조,회수하는 방법
KR1020150191513A KR101621967B1 (ko) 2015-12-31 2015-12-31 전기로 더스트로부터 황산아연 및 산화아연을 제조하는 방법
KR10-2015-0191513 2015-12-31

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
BE1026928B1 (fr) * 2018-12-27 2020-07-28 Hydrometal Procédé hydrométallurgique de traitement de poussières contenant des oxydes métalliques issues de la pyrométallurgie
CN114854989A (zh) * 2022-04-27 2022-08-05 江苏师范大学 一种光催化强化废旧锂离子电池正极活性物质浸出的方法

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
BE1026928B1 (fr) * 2018-12-27 2020-07-28 Hydrometal Procédé hydrométallurgique de traitement de poussières contenant des oxydes métalliques issues de la pyrométallurgie
CN114854989A (zh) * 2022-04-27 2022-08-05 江苏师范大学 一种光催化强化废旧锂离子电池正极活性物质浸出的方法
CN114854989B (zh) * 2022-04-27 2024-05-24 江苏师范大学 一种光催化强化废旧锂离子电池正极活性物质浸出的方法

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