EP0968322A1 - Procede et dispositif pour l'exploitation de bains de fraisage - Google Patents

Procede et dispositif pour l'exploitation de bains de fraisage

Info

Publication number
EP0968322A1
EP0968322A1 EP98916915A EP98916915A EP0968322A1 EP 0968322 A1 EP0968322 A1 EP 0968322A1 EP 98916915 A EP98916915 A EP 98916915A EP 98916915 A EP98916915 A EP 98916915A EP 0968322 A1 EP0968322 A1 EP 0968322A1
Authority
EP
European Patent Office
Prior art keywords
milling
bath
complex
milling medium
mixture
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.)
Granted
Application number
EP98916915A
Other languages
German (de)
English (en)
Other versions
EP0968322B1 (fr
Inventor
Karsten LÖHR
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.)
Mercedes Benz Group AG
Original Assignee
DaimlerChrysler AG
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Application filed by DaimlerChrysler AG filed Critical DaimlerChrysler AG
Publication of EP0968322A1 publication Critical patent/EP0968322A1/fr
Application granted granted Critical
Publication of EP0968322B1 publication Critical patent/EP0968322B1/fr
Anticipated expiration legal-status Critical
Expired - Lifetime legal-status Critical Current

Links

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
    • C23F—NON-MECHANICAL REMOVAL OF METALLIC MATERIAL FROM SURFACE; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL; MULTI-STEP PROCESSES FOR SURFACE TREATMENT OF METALLIC MATERIAL INVOLVING AT LEAST ONE PROCESS PROVIDED FOR IN CLASS C23 AND AT LEAST ONE PROCESS COVERED BY SUBCLASS C21D OR C22F OR CLASS C25
    • C23F1/00—Etching metallic material by chemical means
    • C23F1/46—Regeneration of etching compositions

Definitions

  • the invention relates to a method for operating milling baths, in which a metal workpiece to be milled is immersed in a milling bath containing a milling medium, the metal is oxidized by a chemical reaction between the metal and the milling medium and converted into a soluble complex, the resulting mixture of a separation is subjected to, by which excess milling medium is separated from the complex, the recovered milling medium is used again to operate milling baths, and the complex is subjected to a preparation process.
  • the milling bath described there is an alkaline milling bath in which aluminum workpieces are dissolved using sodium hydroxide solution according to the following equation:
  • the milling bath mixture which is highly concentrated in the metal ion complex, is treated in such a way that a dialysis step is carried out first.
  • a dialysis step a large part of the sodium hydroxide is separated from the aluminate complex.
  • the sodium hydroxide solution obtained in the dialysis step is still sufficiently concentrated to be able to be returned to a milling bath.
  • the aluminate solution has been considerably diluted by the dialysis step. The concentration was cut in half.
  • the processing process of the complex now consists in splitting the aluminate complex into water-insoluble aluminum hydroxide and sodium hydroxide solution by adding water, which takes place according to the following equilibrium reaction:
  • the precipitated aluminum hydroxide is a valuable substance that is used, for example, in the aluminum industry. It roughly corresponds to the substance that is produced by the usual Bayer process.
  • a disadvantage of the process mentioned at the outset is that large amounts of water are required in the dialysis step, that is to say the so-called diffusion dialytic removal of the sodium hydroxide solution, in order to maintain the concentration gradient for the operation of the dialysis.
  • the dialysis speeds are extremely low and a very large membrane area is required in order to be able to convert corresponding amounts.
  • WO 85/01 670 A1 describes a process for treating aqueous waste solutions containing metal ions.
  • the process products are separated and separated from the solvent water by a combination of reverse osmosis and a “water splitting” process, for example electrodialysis.
  • the process products are separated from one another by means of ion-selective electrodialysis and the water is separated from the process products by means of reverse osmosis, the
  • the various process streams are at least partially recycled.
  • Reverse osmosis is not ion-selective and can therefore only be used in combination with another process such as electrodialysis for the separation of process products.
  • the combination of two processes requires increased process engineering. The problem of electrodialysis has already been pointed out.
  • milling is understood not only as a slight surface etching or pickling of a metal piece, but also as a very defined, substantial amount of material removal, which is otherwise only achieved by machining.
  • the milling baths are very large, contents of 60 m 3 are possible in order to be able to treat such large components. As a result, very high amounts of milling baths are processed.
  • the object is achieved in that a mixture of dissolved complexed metal ion and milling medium is removed from the milling bath at a concentration of dissolved complexed metal ion which is far below its saturation limit that the separation is a nanofiltration, in which the milling medium is separated from the mixture using the principle of reverse osmosis, with concurrent concentration of the residue of complexed metal ion taking place.
  • the mixture of dissolved complexed metal ion and milling medium is thus removed even at a relatively low concentration of complexed metal ion.
  • etching or milling conditions can be achieved with relatively low concentrations of dissolved metal complex, which become increasingly unfavorable with increasing concentration and are difficult to grasp in terms of control technology.
  • the second important aspect of the invention now opens up the possibility of a subsequent economically meaningful preparation because the separation by means of nanofiltration simultaneously results in a concentration of the residue on the complexed metal ion.
  • the medium to be filtered is pressurized and ion-selective membrane separation takes place.
  • hyperfiltration and low-pressure reverse osmosis also exist for the term nanofiltration.
  • Small molecules such as sodium hydroxide or water can easily pass through the membrane, larger molecules such as the metal complex can only pass through the membrane with difficulty.
  • both water and the milling medium for example sodium hydroxide solution, can be separated from the milling bath mixture, which then increases the concentration of metal complex in the remaining solution.
  • sodium hydroxide solution is produced again.
  • the aqueous filtrate contains sodium hydroxide solution and also residual amounts of sodium aluminate complex.
  • the sodium hydroxide which was still bound in the aluminate complex during the previous nanofiltration, can now also be separated off and returned to the milling bath. This makes it possible to circulate the entire necessary sodium hydroxide solution, which means a considerable economic and ecological effect in large-scale plants.
  • the complex is prepared by diluting with water and precipitating and separating the metal as hydroxide
  • the water addition is controlled so that the filtrate resulting from the separation compensates for the evaporation loss of the milling bath.
  • Milling baths are often carried out at high temperatures, for example in the range of 75-80 ° C., so that a considerable amount of the water in the milling bath evaporates gradually.
  • an appropriately diluted filtrate from the preparation process of the complex appropriate amounts of water can be added to the nanofiltration, which together with the sodium hydroxide solution pass through the membrane of the nanofiltration and thus ensure adequate water supply to the milling bath.
  • the mixture of dissolved complexed metal ion and milling medium is removed from the milling bath either continuously or in batches. Depending on the size of the system and the control technology, the mixture can be removed accordingly.
  • the concentration of alkali in the milling bath is in the range from 1 10-150 g / l sodium hydroxide.
  • the sodium hydroxide created during the nanofiltration is continuously recycled in such a way that the concentration is maintained in these favorable ranges, so that an optimal and defined, and thus easily controllable milling result can be achieved.
  • the nanofiltration is carried out in such a way that the aluminum is concentrated up to 100 g / l.
  • alkaline milling baths for dissolving aluminum have essentially been described in order to explain aluminum, it goes without saying that other metals can also be milled that dissolve with alkaline media and form corresponding complexes, such as zinc.
  • Fig. 1 shows schematically a system with which the inventive method is operated
  • Fig. 2 is a diagram in which the concentration of milling medium compared to the
  • the milling bath has a volume of about 60 m 3 and is operated at a temperature of 75-80 ° C., so that considerable amounts of water vapor 12 already escape.
  • Metallic workpieces made of aluminum are immersed in the milling bath 10, for example large-area curved aircraft trim elements with a dimension of several meters.
  • the aluminum of the workpiece reacts with the sodium hydroxide solution to form hydrogen and a soluble sodium aluminate complex, NaAI (OH) 4 .
  • a bath concentration of approximately 10 g aluminum per liter of bath liquid is removed and fed to a nanofilter 14, in which a nanofiltration is carried out.
  • the nanofilter 14 is constructed such that an inner tube has a tubular support structure in which a membrane is placed. This tube is surrounded by another tube.
  • Such nanofilters are used as module units, such as those offered by Membrane Products Kiryat Weizmann Ltd., Rehovot / Israel under the name SeIRO Tubula Modul TM 1228.
  • the membrane used has the specification MPT-34.
  • the membrane tube of a tube module has a diameter of approximately 10 mm
  • the support body consists of a perforated, porous tubular support body on which the membrane film MPT-34 is placed.
  • Such a module is based on the cross flow principle, i.e. the milling bath solution is pressurized with a pressure of 1-6 MPa by a pump (not shown here) and passed in one direction through the inner tube at a speed of 1-2 m / s. Under these conditions, sodium hydroxide and water molecules pass through the membrane in the radial direction and are converted into the so-called NaOH permeate, which is returned to the milling bath 10.
  • the milling bath solution which is depleted in water and sodium hydroxide, is concentrated in aluminate complex after leaving the nanofilter 14. The conditions are chosen so that a concentration in the range of about 50-100 g / l aluminum takes place.
  • This liquid which is referred to as Al concentrate, can now be fed to a preparation process, which can be carried out either on site or at a company that produces aluminum.
  • the Al concentrate is diluted with water according to the known Bayer process, and the aluminum hydroxide Al (OH) 3 formed is precipitated and centrifuged, if appropriate with the addition of appropriate germs, and fed as an Al product, for example to aluminum production.
  • the filtrate which remains when the precipitated Al (OH) 3 is separated off by filtration or centrifugation contains the sodium hydroxide solution formed when the sodium aluminate complex is split up and any undissolved sodium aluminate complex which is still dissolved. This filtrate can be fed again to the nanofilter 14, transferred there into the NaOH permeate and returned to the milling bath 10.
  • sodium hydroxide NaOH
  • the advantageous process control can be seen more clearly on the basis of the diagram in FIG. 2.
  • the milling bath 10 of FIG. 1 is operated in such a way that the concentration of sodium hydroxide solution is approximately 120 g / l, the concentration of dissolved aluminum is approximately in the range of 10 g / l.
  • These bath conditions can be maintained continuously through the nanofiltration and the constant recycling of the NaOH permeate formed.
  • Optimal etching or milling results can be achieved in this area, i.e. the milling speed is not so high that large parts are milled differently during the immersion process, but the milling speed is still sufficient and desirably high.
  • the concentration of aluminum is increased during nanofiltration, as indicated by the horizontal arrow pointing to the right.
  • approximately 70-80% of the sodium hydroxide solution contained in the milling bath has already been removed and converted into the NaOH permeate.
  • a dilution step with water is first carried out, so that this solution is relatively poor in sodium and aluminum (in the form of the dissolved aluminate complex).
  • the aluminum hydroxide is then precipitated by adding germs and the precipitated aluminum hydroxide is filtered off or, for example, centrifuged off. That arose
  • the filtrate contains, in addition to residual amounts of the still undissolved sodium aluminate complex, sodium hydroxide solution which has arisen during the cleavage of the complex, that is to say that previously bound sodium hydroxide solution is released again.
  • This filtrate is returned to the nanofiltration, it is controlled so that the sodium hydroxide permeate is diluted to such an extent that the evaporation losses of the milling bath are compensated for.
  • the dilution step described is first carried out because a direct splitting of the highly concentrated aluminate solution would lead to a sodium hydroxide concentration in the filtrate which is significantly higher than the solution desired in the bath.
  • the remaining 20-30% of the sodium hydroxide solution contained in the milling bath can be recovered and returned to the circuit so that ultimately no sodium hydroxide solution is used.
  • bath concentrations start with about 150 g of sodium hydroxide per liter of solution.
  • concentration of sodium hydroxide solution decreases and the concentration of dissolved aluminum increases, for example to a value in the range of 20 g / l aluminum.
  • the external addition of sodium hydroxide to the milling bath increases its concentration again suddenly and the milling process continues, whereby sodium hydroxide solution is used again and the concentration of aluminum in the milling bath increases continuously.
  • sodium hydroxide solution is again added, in this state such a bath is already referred to as a bad bath.

Landscapes

  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Separation Using Semi-Permeable Membranes (AREA)
  • ing And Chemical Polishing (AREA)
  • Manufacture And Refinement Of Metals (AREA)

Abstract

L'invention concerne un procédé d'exploitation d'un bain de fraisage (10) dans lequel une pièce métallique à fraiser est plongée dans un bain de fraisage (10) contenant un milieu de fraisage, le métal étant oxydé par réaction chimique entre lui et le milieu de fraisage et étant transformé en un complexe soluble. Le mélange obtenu est soumis à une séparation par laquelle le milieu de fraisage en excès est séparé du complexe, le milieu de fraisage ainsi récupéré étant à nouveau utilisé pour l'exploitation de bains de fraisage et le complexe étant soumis à un processus de préparation. Selon l'invention, un mélange d'ions métalliques complexes dissous et de milieu de fraisage est enlevé du bain de fraisage en cas de concentration d'ions métalliques complexes dissous qui soit très en dessous de la limite de saturation du bain. Le processus de séparation est une nanofiltration dans laquelle le milieu de fraisage est séparé du mélange selon le principe de l'osmose inversée, le résidu étant simultanément concentré en ions métalliques complexes.
EP98916915A 1997-03-14 1998-03-11 Procede et dispositif pour l'exploitation de bains de fraisage Expired - Lifetime EP0968322B1 (fr)

Applications Claiming Priority (3)

Application Number Priority Date Filing Date Title
DE19710563A DE19710563C2 (de) 1997-03-14 1997-03-14 Verfahren und Vorrichtung zum Betreiben von Aluminium-Fräsbädern
DE19710563 1997-03-14
PCT/EP1998/001388 WO1998041672A1 (fr) 1997-03-14 1998-03-11 Procede et dispositif pour l'exploitation de bains de fraisage

Publications (2)

Publication Number Publication Date
EP0968322A1 true EP0968322A1 (fr) 2000-01-05
EP0968322B1 EP0968322B1 (fr) 2003-12-10

Family

ID=7823351

Family Applications (1)

Application Number Title Priority Date Filing Date
EP98916915A Expired - Lifetime EP0968322B1 (fr) 1997-03-14 1998-03-11 Procede et dispositif pour l'exploitation de bains de fraisage

Country Status (4)

Country Link
US (1) US6454958B1 (fr)
EP (1) EP0968322B1 (fr)
DE (2) DE19710563C2 (fr)
WO (1) WO1998041672A1 (fr)

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DE19844227C2 (de) * 1998-09-26 2002-04-18 Daimler Chrysler Ag Verfahren und Vorrichtung zur Herstellung von Kristallen aus übersättigten Lösungen
JP3434750B2 (ja) * 1999-09-30 2003-08-11 Ｎｅｃエレクトロニクス株式会社 洗浄装置のライン構成及びその設計方法
AT409350B (de) * 2000-06-28 2002-07-25 Kostjak Michael Dipl Ing Dr Te Verfahren zum herauslösen von metallischem aluminium aus aluminiumhaltigen, festen abfällen
US7575687B2 (en) * 2005-08-16 2009-08-18 Ge Osmonics, Inc. Membranes and methods useful for caustic applications
US7909179B2 (en) * 2005-08-16 2011-03-22 Ge Osmonics, Inc. Modified polyamide matrices and methods for their preparation
ES2299317A1 (es) * 2005-11-08 2008-05-16 Corporacion Alimentaria Peñasanta, S.A. Procedimiento para la recuperacion de detergentes alcalinos de fase unica utilizados en instalaciones industriales de limpieza in situ.
JP5016973B2 (ja) 2007-05-21 2012-09-05 株式会社野坂電機 アルカリエッチング液のアルカリ回収方法及び装置
US20090000884A1 (en) 2007-06-26 2009-01-01 Akebono Corporation (North America) Brake rotor
WO2010060408A2 (fr) * 2008-11-03 2010-06-03 Koenig Thomas Procédé et installation de décapage
US20120006790A1 (en) * 2009-03-31 2012-01-12 Kurita Water Industries Ltd. Apparatus and method for treating etching solution
DE102012019731A1 (de) * 2012-10-09 2014-04-10 Overlack GmbH Verfahren zur Beschichtung von Metalloberflächen mit einer Konversionsschicht und Vorrichtung zur Durchführung des Verfahrens
DE102013108375A1 (de) * 2013-01-31 2014-07-31 Thomas König Verfahren zum Aufbereiten eines Beiz- und/oder Eloxalbades und Eloxieranordnung
US11545307B2 (en) * 2019-02-11 2023-01-03 Pacesetter, Inc. Fabrication of capacitors and recovery of capacitor fabrication matertials

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US4655928A (en) 1983-10-18 1987-04-07 Gnb Incorporated Membrane processes for metal recovery and pollution control in metal process industries
US5141610A (en) 1988-04-19 1992-08-25 Vaughan Daniel J Electrodialytic process for restoring sodium hydroxide etchants for aluminum
US5118399A (en) 1988-04-19 1992-06-02 Vaughan Daniel J Electrodialytic recovery process
DE3815271A1 (de) * 1988-05-05 1989-11-16 Sandoz Ag Verfahren zur reinigung von industrieabwaessern
US5198085A (en) * 1990-04-12 1993-03-30 Vaughan Daniel J Restoration of alkali hydroxide etchants of aluminum
CA2043717A1 (fr) 1990-07-06 1992-01-07 Thomas A. Davis Procede de recuperation des hydroxides de sodium et d'aluminium presents dans les residus de procedes d'attaque a l'acide
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Also Published As

Publication number Publication date
DE19710563A1 (de) 1998-09-17
US6454958B1 (en) 2002-09-24
WO1998041672A1 (fr) 1998-09-24
DE59810404D1 (de) 2004-01-22
EP0968322B1 (fr) 2003-12-10
DE19710563C2 (de) 2003-10-02

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