EP1277849B1 - Enteisende Fluxsalz-Zusammensetzung für Fluxbäder - Google Patents

Enteisende Fluxsalz-Zusammensetzung für Fluxbäder Download PDF

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Publication number
EP1277849B1
EP1277849B1 EP02008060A EP02008060A EP1277849B1 EP 1277849 B1 EP1277849 B1 EP 1277849B1 EP 02008060 A EP02008060 A EP 02008060A EP 02008060 A EP02008060 A EP 02008060A EP 1277849 B1 EP1277849 B1 EP 1277849B1
Authority
EP
European Patent Office
Prior art keywords
flux
iron
zinc
weight
salt composition
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Expired - Lifetime
Application number
EP02008060A
Other languages
German (de)
English (en)
French (fr)
Other versions
EP1277849A1 (de
Inventor
Georg Bogar
Harald Ernst
Helmut Herwig
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Evonik Operations GmbH
Original Assignee
Goldschmidt GmbH
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Filing date
Publication date
Application filed by Goldschmidt GmbH filed Critical Goldschmidt GmbH
Publication of EP1277849A1 publication Critical patent/EP1277849A1/de
Application granted granted Critical
Publication of EP1277849B1 publication Critical patent/EP1277849B1/de
Anticipated expiration legal-status Critical
Expired - Lifetime legal-status Critical Current

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Classifications

    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C2/00—Hot-dipping or immersion processes for applying the coating material in the molten state without affecting the shape; Apparatus therefor
    • C23C2/30—Fluxes or coverings on molten baths

Definitions

  • the invention relates to a flux salt composition for Flux baths, a particularly simple reprocessing and Fermentation is accessible.
  • Fluxstoff solutions are aqueous salt solutions with a salt content of 300 to 500 g / l.
  • Main components of these flux salts are zinc chloride and ammonium chloride.
  • various alkali and alkaline earth metal chlorides for example KCl, NaCl, MgCl 2 , CaCl 2
  • KCl, NaCl, MgCl 2 , CaCl 2 may be present to a limited extent.
  • the proportion of ammonium chloride is largely replaced by KCl.
  • the flux salt is removed by immersing the Workpiece in the fluxing agent solution applied to the galvanizing. Even when drying occurs through the formation of Hydroxozic acids have a certain pickling effect.
  • the pickling effect is based on the release of hydrochloric acid, which is preferred in the temperature range from 250 to 320 ° C of ammonium chloride. This hydrochloric acid causes the dissolution of oxidic impurities.
  • hydrochloric acid contained in different proportions, whereby iron and alloying elements removed in small quantities from the galvanizing become.
  • Iron which with the flux salt in the galvanizing boiler Hot dip galvanizing is introduced, reacts with the elemental Zinc and forms hard zinc (iron-zinc mixed crystals), which in the Zinc kettle precipitates as a solid. From 1 g of iron arise about 25 g of hard zinc (Böhm, 1974 "Wastewater technology in hot-dip galvanizing plants” 12 (1974) No. 11, 235-239). The zinc losses are so considerably, so that the iron content in the flux bath is not 10 g / l should exceed (Maangled, P formulateker manual "hot-dip galvanizing", 2. Aufl. German publishing house for basic industry, Leipzig 1993, p. 72).
  • the concentration of entrained organic matter Degreasing and pickling in the flux bath is generally low and does not lead to quality degradation in galvanizing.
  • the organic substances are in the zinc kettle with the existing Reactants (for example, zinc, chlorine, ammonium) implemented in an uncontrolled manner so that pollutant-containing reaction products (partly dioxin-containing) may arise in the larger quantities to malfunction in the exhaust air purification lead (blockage of the filter) and recovery of the deposited Make filter dusts difficult or impossible.
  • Contaminated flux baths must therefore be replaced regularly with the iron content leading to replacement in the factories the galvanizing industry in many areas varies (40 to over 80 g / l). Only a small part of the ingredients could in the past in the recovery of such Altfluxe be recovered while the vast majority Share had to be disposed of as hazardous waste.
  • This procedure The prior art is generally based on the fact that in In a multi-step process, first the pH value is set to one value between 3.5 and 4, then by hydrogen peroxide addition, the bivalent iron present in the flux bath Iron (III) hydroxide is precipitated, and then in a due the tricky consistency of these iron hydroxide flakes consuming and lengthy process from the fluxing agent solution Filtration is separated.
  • the object of the present invention is to perform to provide flux salt composition which a simple reprocessing of the fluxing agent solution in one Step and not to external central reprocessing facilities instructed. This allows the flux also in Markets are used for conventional recycling for transport costs are not achievable, for example Overseas countries.
  • a solid deicing flux salt composition for flux baths containing Zinc chloride and alkali metal chloride characterized that they contain at least one or more alkalizing ingredients and one or more in aqueous solution iron (II) to Contains iron (III) oxidizing constituents.
  • Flux salt composition 10 to 80 wt .-% preferably From 25 to 70% by weight, more preferably from 50 to 70% by weight Zinc chloride based on the salt content of the flux salt.
  • the flux salt composition should be 20 to 90% by weight, in particular 30 to 75 wt .-%, more preferably 30 to 50 wt .-% of alkali metal chloride based on the salt content of the fluxing salt.
  • ammonium chloride is particularly preferred here.
  • the alkalizing the flux salt composition of the invention especially zinc oxide, alkali metal hydroxides, especially lithium, sodium and / or potassium hydroxide, Metal carbonates, in particular zinc carbonate or a Combination thereof included, in a preferred embodiment 1 to 20 wt .-%, preferably 2 to 10 wt .-%, particularly preferably 3 to 7 wt .-% zinc oxide based on the flux salt.
  • the oxidizing component is alkali metal permanganate
  • Potassium permanganate is beneficial because it contains both iron and also can oxidize organic contaminants and resulting Manganese (II) as manganese dioxide by methods known per se removable, but it can also metal peroxides and / or metal chlorates such as zinc peroxide or zinc chlorate as oxidizing ingredients are used.
  • the amount of permanganate contained ideally results from the stoichiometric need for oxidation everything contained Iron (II) to iron (III). That is why a salary of 0.1 to 15 wt .-%, preferably 0.5 to 10 wt .-%, particularly preferably From 1 to 5% by weight of alkali metal, in particular potassium permanganate, based on the fluxing salt in the fluxing salt composition of great advantage.
  • reaction temperature exceeds in the reprocessing of the Altfluxes due to the exothermic oxidation of Iron (II) to iron (III) the optimum range when the iron (II) content of the Altfluxes is above 35 to 40 g / l and it must be used coolers.
  • This is the reprocessing sensibly at temperatures below 60 to 70 ° C carried out because above this temperature by evaporation of water Problems in the galvanizing plants occur.
  • a preparation of from the normal operation by Eiseneinschleppung iron-containing Fluxbädern includes, is inventively the Zinc chloride alkali metal chloride ratio and the pH to Iron precipitation and the oxidation of iron (II) to iron (III) by continuous or discontinuous addition of a Flux salt composition as described in one step. This simplifies the procedure compared to the The method described in the prior art considerably and can also decentralized in galvanizing plants also by untrained Staff are made.
  • the flux salt composition can be used to operate the flux bath in solid form and also dissolved in water before being added become.
  • An optimal effect is achieved when going to operation the flux bath with the addition of the flux salt the pH of the flux bath in a range of 3.0 to 4.5 preferably from 3.3 to 4.0, more preferably at 3.8, in the solution galvanized iron (II) to iron (III) oxidized and fails. It is for the reasons described above this is advantageous for an iron content of the Altfluxes of 5 to 40, preferably 10 to 30, particularly preferably 15 to 25 g / l.
  • permanganate can lead to manganese over time in the Altflux accumulate. This manganese should be used from time to time Example by Komproportionierung with potassium permanganate or by oxidation with hydrogen peroxide or otherwise be precipitated and removed.
  • a standard flux was selected, which is sufficient in practice is proven, has good buffering effect and a pH guaranteed from 3 to 3.8. This flux is at the galvanizing plants well introduced and recognized.
  • the flux salt had the following composition (% by weight): 54% Zinc chloride (crystalline) 5% Zinc oxide solid 40% ammonium chloride 2% potassium permanganate
  • This flux bath turned out to be the experimental procedure ideal, because in particular the ratio of zinc chloride to Ammonium chloride deviated strongly from the optimum.
  • the 25 ml removed were again supplemented by 25 ml of a fluxing agent solution according to the invention according to Example 1 with a concentration of 400 g flux / l or 400 kg / m 3 , a usual working concentration in a galvanizing plant, and stirred for about 1 hour.
  • the pH increased from about 3.0 with each addition of flux to about 3.8. This is an optimal value for ferric hydroxide precipitation.
  • the zinc chloride ammonium chloride composition did not changed significantly.
  • the bath would be with consistent application of the de-icing Fluxes iron free in 5 months.
  • the iron and manganese-free bath may then be e.g. with for a year Conventional flux salt operated. From an iron content, preferably 20 g / l, the de-ironing step can be repeated be recorded.
  • Measurement protocol of the flux bath analyzes.

Landscapes

  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Coating With Molten Metal (AREA)
  • Detergent Compositions (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
  • Nonmetallic Welding Materials (AREA)
  • Materials Applied To Surfaces To Minimize Adherence Of Mist Or Water (AREA)
EP02008060A 2001-07-17 2002-04-11 Enteisende Fluxsalz-Zusammensetzung für Fluxbäder Expired - Lifetime EP1277849B1 (de)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE10134812A DE10134812C2 (de) 2001-07-17 2001-07-17 Enteisende Fluxsalz-Zusammensetzung für Fluxbäder
DE10134812 2001-07-17

Publications (2)

Publication Number Publication Date
EP1277849A1 EP1277849A1 (de) 2003-01-22
EP1277849B1 true EP1277849B1 (de) 2005-12-28

Family

ID=7692136

Family Applications (1)

Application Number Title Priority Date Filing Date
EP02008060A Expired - Lifetime EP1277849B1 (de) 2001-07-17 2002-04-11 Enteisende Fluxsalz-Zusammensetzung für Fluxbäder

Country Status (9)

Country Link
US (1) US6802912B2 (da)
EP (1) EP1277849B1 (da)
JP (1) JP2003055752A (da)
AT (1) ATE314502T1 (da)
DE (2) DE10134812C2 (da)
DK (1) DK1277849T3 (da)
ES (1) ES2252346T3 (da)
NO (1) NO20021678L (da)
PL (1) PL200196B1 (da)

Families Citing this family (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE10333165A1 (de) * 2003-07-22 2005-02-24 Daimlerchrysler Ag Pressgehärtetes Bauteil und Verfahren zur Herstellung eines pressgehärteten Bauteils
DE102012100128A1 (de) * 2012-01-10 2013-07-11 Chemische Fabrik Budenheim Kg Kondensierte Eisen(III)phosphate
JP5884200B2 (ja) * 2013-07-31 2016-03-15 Ｊｆｅスチール株式会社 溶融亜鉛めっき用フラックスおよび溶融亜鉛めっき用フラックス浴ならびに溶融亜鉛めっき鋼材の製造方法
JP7252922B2 (ja) * 2019-08-19 2023-04-05 Ｊｆｅスチール株式会社 溶融亜鉛めっき用フラックス液および溶融亜鉛めっき鋼管の製造方法

Family Cites Families (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB543856A (en) * 1939-09-14 1942-03-16 Dewey And Almy Chem Comp Improvements in or relating to soldering, tinning and galvanizing fluxes
DE2852756B2 (de) * 1978-12-06 1980-09-25 Basf Ag, 6700 Ludwigshafen Flußmittel für die Trockenverzinkung
FR2520007B1 (fr) * 1982-01-15 1990-11-02 Asturienne Mines Comp Royale Procede de regeneration en continu de bains de fluxage dans la galvanisation au trempe de pieces en acier
US4496612A (en) * 1982-04-06 1985-01-29 E. I. Du Pont De Nemours And Company Aqueous flux for hot dip metalizing process
DE3630157A1 (de) * 1986-09-04 1988-03-10 Mandl Johannes Verfahren zur reinigung von fluxbaedern, wie sie beim feuerverzinken verwendet werden
JPS63166719A (ja) * 1986-12-27 1988-07-09 Sumitomo Metal Ind Ltd メツキアツシユからの塩化亜鉛製造法
DE3814372A1 (de) * 1988-04-28 1989-11-09 Deca Chemie Gmbh Verfahren zum wirtschaftlichen betreiben einer heissmetallisierungsanlage
US5100486A (en) * 1989-04-14 1992-03-31 The United States Of America As Represented By The United States Department Of Energy Method of coating metal surfaces to form protective metal coating thereon
US5810946A (en) * 1997-02-04 1998-09-22 Metals Recycling Technologies Corp. Method for the production of galvanizing fluxes and flux feedstocks
JP2963091B1 (ja) * 1998-08-20 1999-10-12 東鋼業株式会社 溶融亜鉛−アルミニウム合金めっき方法

Also Published As

Publication number Publication date
EP1277849A1 (de) 2003-01-22
PL200196B1 (pl) 2008-12-31
DE10134812A1 (de) 2003-02-06
DE10134812C2 (de) 2003-06-26
US20030084755A1 (en) 2003-05-08
DK1277849T3 (da) 2006-04-10
US6802912B2 (en) 2004-10-12
PL353298A1 (en) 2003-01-27
DE50205407D1 (de) 2006-02-02
ATE314502T1 (de) 2006-01-15
ES2252346T3 (es) 2006-05-16
NO20021678D0 (no) 2002-04-10
NO20021678L (no) 2003-01-20
JP2003055752A (ja) 2003-02-26

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