WO2010074516A2 - Procédé de préparation d'oxyde de zinc très pur au moyen de poussière secondaire - Google Patents

Procédé de préparation d'oxyde de zinc très pur au moyen de poussière secondaire Download PDF

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Publication number
WO2010074516A2
WO2010074516A2 PCT/KR2009/007741 KR2009007741W WO2010074516A2 WO 2010074516 A2 WO2010074516 A2 WO 2010074516A2 KR 2009007741 W KR2009007741 W KR 2009007741W WO 2010074516 A2 WO2010074516 A2 WO 2010074516A2
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Prior art keywords
zinc
high purity
zinc oxide
dust
solution
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PCT/KR2009/007741
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English (en)
Korean (ko)
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WO2010074516A3 (fr
Inventor
이재영
변태봉
안중철
박현
박보하
Original Assignee
주식회사 포스코
재단법인 포항산업과학연구원
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Priority to CN200980157304.6A priority Critical patent/CN102325725B/zh
Priority to JP2011543425A priority patent/JP5564514B2/ja
Publication of WO2010074516A2 publication Critical patent/WO2010074516A2/fr
Publication of WO2010074516A3 publication Critical patent/WO2010074516A3/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
    • C01G9/02—Oxides; Hydroxides
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B13/00—Oxygen; Ozone; Oxides or hydroxides in general
    • C01B13/14—Methods for preparing oxides or hydroxides in general
    • C01B13/36—Methods for preparing oxides or hydroxides in general by precipitation reactions in aqueous solutions
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00—Physical properties of inorganic compounds
    • C01P2006/80—Compositional purity

Definitions

  • the present invention relates to a method for producing high purity zinc oxide used in the electronics industry and the rubber industry, and more particularly, by using secondary dust generated in the recycling process of stainless steel by-products. It relates to a method for producing zinc oxide.
  • Dust generated in the steel process usually contains 15-20% of zinc, and the dust is formed together with the reducing material, and then heated and concentrated to recover zinc oxide (Korean Patent 1997-0013538, Japanese Patent Publication 1992). -261590).
  • LD converter steel dust containing zinc and EAF steel dust are used as raw materials, and waste tire dry charcoal, waste activated carbon, or coke is used as a reducing agent, and these components are combined on a stoichiometric basis to prepare ferrets and briquettes. After drying, charged into a liquid fuel heating reduction furnace and smelted at 1000-1500 ° C. for 1-3 hours, and then the evaporated ZnO is recovered in a dust collector.
  • High-purity zinc oxide is usually manufactured by volatilizing high-purity metallic zinc, and wet leaching raw materials such as Zn-containing scraps having high purity, followed by acid extraction, solvent extraction, and then activated carbon treatment to remove impurities.
  • the method of producing a high purity zinc oxide powder characterized in that the solution from which the impurities have been removed is neutralized with an alkali solution to obtain zinc hydroxide, and then the zinc hydroxide is calcined to zinc oxide (Japanese Patent Laid-Open No. 2003-339317). have.
  • the inventors have developed a method for producing high purity zinc oxide from by-products. (Korean Patent Application No. 1998-0056706, Korean Patent Registration No. 409951).
  • the method comprises administering to the Zn plating waste liquid the number of moles of KOH corresponding to 1/200 to 1/50 of the number of moles of Zn in the waste solution, and stirring and aging to allow the impurities to be adsorbed and then filtering them; Filtering and adding the Zn-containing solution from which impurities were removed to the KOH solution to maintain neutralization reaction while maintaining the pH of the solution at 13 or above, followed by stirring for 1 hour to obtain ZnO directly from the aqueous solution; And ZnO manufacturing method comprising the step of drying the obtained oxide after repeated filtration washing.
  • this dust contains high concentrations of Ni, Cr, Mn, Mg, etc. in addition to Fe, and thus it is impossible to produce high purity zinc oxide through a general impurity purification process.
  • An object of the present invention is to provide a method for more economically manufacturing high purity zinc oxide in secondary dust generated in a recycling process of stainless by-products by improving impurity purification techniques.
  • the present invention comprises the steps of leaching secondary dust generated in the process of recycling stainless dust in an acidic aqueous solution to selectively dissolve zinc to make a zinc aqueous solution;
  • Preparing a high purity zinc oxide sludge directly in an aqueous solution by adding a high purity zinc chloride to an aqueous alkaline zinc solution so that the ratio of the number of moles of zinc to the number of moles of zinc is 2.0-3.0;
  • It relates to a method for producing high purity zinc oxide using secondary dust comprising the step of filtering and drying the high purity zinc oxide sludge.
  • Examples of the acidic aqueous solution for leaching the secondary dust include aqueous hydrochloric acid, sulfuric acid and nitric acid, and preferred acidic aqueous solution is hydrochloric acid.
  • Examples of the first group impurities include one or two or more of iron, chromium, nickel, lead, silicon, and fluorine.
  • Examples of the second group impurities include one or two of lead and cadmium.
  • the high-purity zinc chloride is Ni + Cr + Pb + Cd + Mn + Mg + F + Si ⁇ 0.5 wt% by weight of zinc chloride by reacting zinc chloride aqueous solution or zinc by-product obtained by purifying waste zinc plating solution with hydrochloric acid. Purified aqueous zinc chloride solution can be used.
  • the present invention comprises the steps of leaching secondary dust generated in the process of recycling stainless dust in an acidic aqueous solution to selectively dissolve zinc to make a zinc aqueous solution;
  • Preparing a high purity zinc oxide sludge directly in an aqueous solution by adding a high purity zinc chloride to an aqueous alkaline zinc solution so that the ratio of the number of moles of zinc to the number of moles of zinc is 2.0-3.0;
  • It relates to a method for producing high purity zinc oxide using secondary dust comprising the step of filtering and drying the high purity zinc oxide sludge.
  • Examples of the acidic aqueous solution for leaching the secondary dust include aqueous hydrochloric acid, sulfuric acid and nitric acid, and preferred acidic aqueous solution is hydrochloric acid.
  • Examples of the first group impurities include one or two or more of iron, chromium, nickel, lead, silicon, and fluorine.
  • Examples of the second group impurities include one or two of lead and cadmium.
  • Examples of the third group impurity include one or two of manganese and magnesium.
  • the high-purity zinc chloride is Ni + Cr + Pb + Cd + Mn + Mg + F + Si ⁇ 0.5 wt% by weight of zinc chloride by reacting zinc chloride aqueous solution or zinc by-product obtained by purifying waste zinc plating solution with hydrochloric acid. Purified aqueous zinc chloride solution can be used.
  • the present invention is preferably applied to the secondary dust generated in the recycling process of stainless by-products, secondary dust that can be more preferably applied to the present invention
  • T-Fe 1 to 10% by weight, Si: 1 to 6%, Ca: 2 to 8%, Mn: 0.1 to 2.0%, Zn: 20 to 45%, Mg: 1 to 5%, Ni: 0.1 ⁇ 1%, Cr: 0.3-2%, Cd: 0.1-1%, Pb: 1-8%, and K: 3-10%.
  • Table 1 shows the results of analyzing the composition of one example of the secondary dust generated in the recycling process of the stainless by-products applicable to the present invention.
  • the zinc concentration in the secondary dust generated in the recycling process of stainless by-products is very high, about 30%, but Si, Mn, Cr, Ni, Mg, Pb, etc. are very high, and an anion F component ( 5%) and chlorine components (about 10%) are mixed in a large amount.
  • the present invention provides a method for more economically producing high purity zinc oxide in secondary dust generated in the recycling process of stainless by-products by improving impurity purification techniques.
  • hydrochloric acid As the acidic leaching aqueous solution, hydrochloric acid, sulfuric acid, nitric acid aqueous solution and the like can be used, but among these, hydrochloric acid aqueous solution is most preferred.
  • hydrochloric acid as an acidic leaching aqueous solution as above is demonstrated.
  • the secondary dust contains third group impurities such as Mn, so that the neutralizing agent can be used as a neutralizing agent in the neutralization step performed to remove these impurities, and preferably, It can also reduce the environmental load.
  • the leaching reaction and neutralization reaction for each acidic aqueous solution are expressed as follows.
  • ZnNO 3 + Ca (OH) 2 Zn (OH) 2 + Ca (NO 3 ) 2
  • Salts produced by leaching and neutralization by acidic aqueous solution are CaCl 2 , CaSO 4 and Ca (NO 3 ) 2 .
  • aqueous sulfuric acid solution is not preferable because a large amount of solid material CaSO 4 is produced, it is not easy to separate and remove the zinc hydroxide and lower the leaching efficiency and increase the amount of waste sludge during strong alkali leaching.
  • the nitrate produced is soluble in water but is not preferable because biological environment treatment is required.
  • aqueous hydrochloric acid solution which produces a water-soluble salt in the form of calcium chloride, is most effective.
  • the first group impurity is separated and removed by filtering the zinc aqueous solution and the residue obtained by selectively dissolving zinc by leaching the acidic aqueous solution as described above.
  • the residue (sludge) separated from the aqueous zinc solution as described above may be washed with water, filtered, and the filtrate obtained by the filtration may be added to the aqueous zinc solution.
  • the first group impurity is an impurity which is contained in the secondary dust and does not leach into an acidic aqueous solution, and examples thereof include iron, chromium, nickel, lead, silicon and fluorine.
  • the pH at the time of leaching of the secondary dust is preferably 4-6, more preferably
  • Leaching is carried out at a pH of 4-6 with 5-18% weak hydrochloric acid.
  • Leaching with a strongly acidic aqueous solution may cause a sharp drop in pH, which may cause the pH to be 4 or less.
  • the pH of the acidic solution is less than 4 during leaching, a large amount of metallic impurities other than zinc flows into the leaching solution, and especially fluorine is rapidly introduced.
  • the acid dissolution rate is slowed down, which leads to an undesirable result of a slow zinc leaching rate and a low zinc recovery rate.
  • the reason why the leaching rate is good even when leaching with a weakly acidic aqueous solution, for example, a weak hydrochloric acid aqueous solution is as follows.
  • the primary dust generated in the general carbon steel manufacturing process is that zinc is mainly composed of zinc ferrite (ZnOFe 2 O 3 ) spinel phase, so to leach zinc, a strong acidic solution such as strong hydrochloric acid should be used.
  • stainless steel secondary dust is composed of zinc in the ZnO phase and only a part in the ZnOFe 2 O 3 spinel phase.
  • the spinel phase such as (NiPb) O (CrFe) 2 O 3 , has a very high resistance to acids, and therefore, metal ions are dissolved and introduced when leaching with a weak acid at low leaching pH.
  • ZnO has an alkaline property, so even if it is leached at low leaching pH conditions with a weakly acidic aqueous solution such as low concentration hydrochloric acid, there is no problem with zinc leaching.
  • the fluorine component is present in majority in the form of CaF 2, CaF 2 is not a pH of less than 4 because the substantially insoluble nature of leaching when fluoride is dissolved in the ion.
  • Si also exists in the form of SiO 2 and does not dissolve.
  • the dust containing the metal component zinc is thrown into the aqueous zinc solution separated and filtered as described above to remove the second group impurities.
  • the second group impurity is contained in the aqueous zinc solution, and impurities such as Pb, Cd, and the like that can be removed by adding dust containing zinc of a metal component.
  • the dust containing zinc as a metal component to remove lead and cadmium is not particularly limited, but zinc slime generated from dust or electro zinc plating processes having a metal zinc content of 40 to 90% obtained during the smelting of metal zinc ( Zinc ball residues).
  • Dust and sludge (slime) having a metal zinc content of less than 40% are not preferable because the substitution precipitation reaction rate is slow, and dust having a metal zinc content of 90% or more is expensive and thus limited in use.
  • the secondary dust contains a third group impurities such as Mn, Mg, etc. as described above
  • a third group impurities such as Mn, Mg, etc.
  • an alkali agent to the aqueous solution from which the second group impurities have been removed, neutralizing and precipitating zinc and the third group impurities with hydroxides.
  • the step of filtering the aqueous solution to obtain neutral salts and chlorides may optionally be added.
  • the zinc oxide thus produced was very dark in color and was only 95% pure in zinc oxide analysis.
  • the said Mn was a big cause of the whiteness fall, and the said Mg was a big cause of the fall of purity. Therefore, in order to remove said Mn and Mg, a separate purification process is performed.
  • an alkali is added to the aqueous solution from which lead and cadmium are removed as described above to neutralize and precipitate zinc and impurity metal components (Mn, Mg) with hydroxides.
  • the chloride was contained in the dust.
  • Neutralization salts such as calcium chloride are present in the ionic phase and can be removed completely by washing with water.
  • KCl introduced from the dust component in addition to calcium ions is also removed in this washing and filtration process.
  • the alkali agent neutralizing agent
  • slaked lime when used as an alkali agent, slaked lime has an effect of aggregating trace amounts of Si impurities present in addition to Mn and Mg in the solution in the form of CaO ⁇ SiO 2 , thereby achieving a Si removal effect.
  • the third group impurity is contained in the aqueous zinc solution, and, for example, Mn and Mg may be mentioned as impurities which form a hydroxide when an alkali agent is added.
  • NaOH is added to the aqueous solution from which the third group impurities are removed as described above, and the zinc is dissolved in an aqueous alkaline zinc solution at a pH of 14 or more, preferably in a range of 14-15, and filtered.
  • leaching is preferably performed at a high temperature of 30 to 95 ° C, for example.
  • the process of removing the third group impurity as described above is added to the neutralized precipitate (zinc, manganese, magnesium hydroxide) and neutralized salts such as CaCl 2 and the like to remove the pH is 14 or more, preferably The pH is leached in the range of 14-15, dissolving zinc in an aqueous alkaline zinc solution and filtering.
  • Filtration can separate the zinc-containing alkaline solution and impurities such as manganese and magnesium hydroxide sludge.
  • the leaching pH When the leaching pH is less than 14, zinc dissolution is incomplete and the zinc leaching recovery rate is low. Therefore, the leaching should be performed under the condition of strong alkali pH of 14 or more.
  • ZnNa 2 (OH) 4 is an alkali lysate of zinc present in an ionic state.
  • the leaching temperature is less than 30 °C, the leaching rate is bad. If the temperature exceeds 95 °C, it is difficult to select the filtration material because it is strong alkali.
  • zinc oxide ZnCl 2
  • ZnCl 2 zinc oxide
  • zinc chloride Since the purity of zinc chloride is directly related to the purity of zinc oxide, it is preferable to use zinc chloride for industrial high purity (> 99%).
  • the high-purity zinc chloride is Ni + Cr + Pb + Cd + Mn + Mg + F + Si ⁇ 0.5% by weight of zinc chloride by reacting zinc chloride aqueous solution or zinc by-product obtained by purifying waste zinc plating solution with hydrochloric acid Aqueous zinc chloride solution can be used.
  • a secondary dust obtained by secondary evaporation of carbon steel dust as a zinc by-product is used, and the secondary dust is reacted with an acid to form Ni + Cr + Pb + Cd + Mn + relative to the dry weight of zinc chloride.
  • An aqueous zinc chloride solution purified to be Mg + F + Si ⁇ 0.5 wt% may be used.
  • the purified high purity zinc oxide sludge is washed with water to remove NaCl, and the high purity zinc oxide sludge is filtered and dried.
  • the sludge may be prepared in the form of a cake.
  • the sludge is preferably dried after washing with water and filtration once or more.
  • the zinc oxide sludge dried as described above may be pulverized and used in powder form.
  • the hydrochloric acid input rate was adjusted to range the leaching pH to 1.5-6.5.
  • the amount of hydrochloric acid added varies depending on the leaching pH, and the leaching solution is fixed to 1 liter by changing the amount of the final water.
  • the undissolved sludge and the leachate were separated by filtration.
  • Tr. Represents Tr. ≪ 0.01 g / liter.
  • Tr. Represents Tr. ⁇ 0.01 g / liter.
  • the absolute dose of zinc metal should be at least as high as the sum of the moles of Cd and Pb to be removed, as shown in Scheme (4).
  • the zinc oxide is very dark in color and zinc oxide has been found to be less than 95% pure.
  • the purified aqueous zinc solution contained Mn and Mg.
  • Mn was a major cause of whiteness deterioration and Mg was a major cause of purity deterioration.
  • an alkali was added to the purified aqueous solution from which lead and cadmium were separated, and the impurity metal components (Mn, Mg) including zinc were neutralized and precipitated with hydroxides.
  • neutralized salt (CaCl 2 ) and chlorides such as KCl contained in the dust were removed by filtration, and NaOH aqueous solution was added to 100 g (neutral weight: 65 g because of 35% water content) of the neutralized precipitate obtained in the filtration separation step. After leaching at high temperature, the zinc was dissolved in an aqueous alkaline zinc solution.
  • Tr. Represents Tr ⁇ 0.01 g / liter.
  • a lime as a neutralizing agent and NaOH as an alkali leaching agent so that the leaching pH is 14 or more and the leaching temperature is preferably 30 ° C or more.
  • the leaching temperature exceeds 90 o C, problems of the material of the equipment occur, so the leaching temperature is preferably 30 o C-90 o C (inventive material 6,7), and zinc leaching rate by alkali leaching (dissolved zinc Amount / amount of zinc in the hydroxide before the reaction) is almost 100% so that there is almost no zinc in the leach residue.
  • high-purity zinc chloride for the synthesis of zinc oxide is an aqueous zinc chloride solution obtained by purifying the waste zinc plating solution (Korean Patent Application No. 1998-0056706, Korean Patent Registration No. 409951), that is, Zn in waste liquid in an electro zinc plating waste solution. It is also possible to administer moles of KOH corresponding to 1 / 200-1 / 50 of the moles and to prepare a purified high purity zinc chloride aqueous solution. Also known as RHF (Rotary Hearth Furnace), one of zinc by-products, for example, high concentration zinc oxide dust.
  • RHF Rotary Hearth Furnace
  • the secondary dust generated when the carbon steel dust is recycled through RHF has extremely low Mn and Mg content, so that the first group impurities and the second group impurities that are mixed in the recycling process after acid dissolution are dissolved. Even through purification, zinc chloride of good purity can be obtained.

Abstract

La présente invention concerne un procédé de préparation d'oxyde de zinc très pur utilisé dans l'industrie de l'électronique et dans l'industrie du caoutchouc. L'objectif de l'invention est d'utiliser, dans le cadre d'un tel procédé, de la poussière secondaire produite au cours du procédé de recyclage de poussière inoxydable. L'élément clé du procédé de préparation d'oxyde de zinc très pur selon la présente invention est la lixiviation de la poussière secondaire produite au cours du procédé de recyclage de poussière d'acier inoxydable avec une solution aqueuse d'acide chlorhydrique afin de dissoudre de manière sélective le zinc et d'obtenir une solution aqueuse de zinc, les impuretés telles que le fer, le chrome, le fluor, le plomb et le cadmium étant retirées, puis du NaOH est ajouté afin de dissoudre le zinc dans une solution aqueuse de zinc alcaline et une filtration est réalisée dans des conditions de pH de 14-15. Du chlorure de zinc très pur est alors ajouté de manière que le rapport molaire de OH:zinc puisse atteindre 2,0-3,0, afin d'obtenir directement de l'oxyde de zinc très pur, un lavage est effectué afin de retirer NaCl, puis la suspension d'oxyde de zinc très pur est filtrée et séchée afin d'obtenir de l'oxyde de zinc très pur. Selon l'invention, la poussière sous-produit industriel peut être transformée en une ressource permettant d'obtenir de l'oxyde de zinc très pur, ce qui en fait alors un produit à forte valeur ajoutée.
PCT/KR2009/007741 2008-12-23 2009-12-23 Procédé de préparation d'oxyde de zinc très pur au moyen de poussière secondaire WO2010074516A2 (fr)

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Application Number Priority Date Filing Date Title
CN200980157304.6A CN102325725B (zh) 2008-12-23 2009-12-23 用二次粉尘制备高纯度氧化锌的方法
JP2011543425A JP5564514B2 (ja) 2008-12-23 2009-12-23 二次ダストを用いた高純度酸化亜鉛の製造方法

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KR10-2008-0132655 2008-12-23
KR20080132655 2008-12-23

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CN103771489A (zh) * 2013-12-24 2014-05-07 叶礼平 一种由铜烟灰低温制取纳米氧化锌的方法
KR101790697B1 (ko) * 2016-04-05 2017-10-26 (주)덕진 산화아연 입자, 그 제조 방법 및 응용
CN109553124A (zh) * 2019-01-30 2019-04-02 运城学院 一种改性纳米氧化锌的制备方法

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US4992248A (en) * 1988-08-19 1991-02-12 Solex Corporation Of Japan Method for neutralizing sulfuric acid containing zinc ion
US5431713A (en) * 1994-07-19 1995-07-11 Metals Recycling Technologies Crop. Method for the reclamation of metallic compounds from zinc and lead containing dust
US6726889B2 (en) * 2000-07-14 2004-04-27 Noranda, Inc. Production of zinc oxide from acid soluble ore using precipitation method
KR20020020318A (ko) * 2000-09-08 2002-03-15 문상우 제강공장 전기로더스트와 페로망간으로부터 황산아연과황산망간, 황산제1철을 제조하는 방법

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JP5564514B2 (ja) 2014-07-30
WO2010074516A3 (fr) 2010-09-30
CN102325725B (zh) 2016-10-12
JP2012513370A (ja) 2012-06-14
CN102325725A (zh) 2012-01-18
KR20100074071A (ko) 2010-07-01

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