EP1019565A1 - Procede pour la preparation de solutions d'attaque metalliferes alcalines - Google Patents

Procede pour la preparation de solutions d'attaque metalliferes alcalines

Info

Publication number
EP1019565A1
EP1019565A1 EP98954152A EP98954152A EP1019565A1 EP 1019565 A1 EP1019565 A1 EP 1019565A1 EP 98954152 A EP98954152 A EP 98954152A EP 98954152 A EP98954152 A EP 98954152A EP 1019565 A1 EP1019565 A1 EP 1019565A1
Authority
EP
European Patent Office
Prior art keywords
liquid
extraction
phase
alkaline
solution
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.)
Withdrawn
Application number
EP98954152A
Other languages
German (de)
English (en)
Inventor
Antonio Maria Celi
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.)
Grs Recycling & Co KG GmbH
Original Assignee
Grs Recycling & Co KG GmbH
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 Grs Recycling & Co KG GmbH filed Critical Grs Recycling & Co KG GmbH
Publication of EP1019565A1 publication Critical patent/EP1019565A1/fr
Withdrawn legal-status Critical Current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
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D11/00—Solvent extraction
    • B01D11/04—Solvent extraction of solutions which are liquid
    • B01D11/0446—Juxtaposition of mixers-settlers
    • B01D11/0457—Juxtaposition of mixers-settlers comprising rotating mechanisms, e.g. mixers, mixing pumps
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D11/00—Solvent extraction
    • B01D2011/002—Counter-current extraction

Definitions

  • the invention relates to a process for the preparation of alkaline metal-containing etching solutions, in which a flux g-liquid extraction is carried out, the etching solution forming the heavy phase and an organic solution forming the light phase and the metal ions being removed from the etching solution, the extract phase being washed and the alkaline component and the metal component can be recovered from the extract phase.
  • Alkaline etching solutions are used in the manufacture of printed circuit boards, for example. These etching solutions contain ammonia and one or more ammonia salts. If the ammonium chloride etching process is used, the copper concentration in the etching solution rises during the etching and at a copper concentration of 170 g / l, for example, the etching process generally stops.
  • the fumigated ammoniacal etching solution can be used again after a liquid-liquid extraction, in which the copper is extracted from the etching solution, and after the target parameters have been restored.
  • EP 0 638 662 A1 discloses a process for the preparation of ammacological metalloses, in which a menstrual extraction tower operating in countercurrent is used.
  • the starting material is an ammomacal metal solution (etching solution), which contains ammonium, copper, chloride, copper sulfate etc.
  • etching solution ammonium, copper, chloride, copper sulfate etc.
  • the known method provides a two-stage extraction of the metal ions from the aqueous consumed etchant (aqueous heavy phase) by mixing with a 30% by volume extraction agent solution with aldoxime and / or ketoxime complexing agent Kerosene-like liquid agent (organic light phase mixed solution).
  • the two phases are separated in the separation space and the organic light phase entrainment particles are coalized and removed from the demetallized etchant in a coalescence separator arranged behind the tower-shaped battery, and the etchant is then filtered with activated carbon.
  • This filtration is necessary because organic solvents that may still be present in the caustic solution make the etching process very difficult on the one hand and on the other hand significantly impair the quality of the etched circuit boards.
  • the metal-containing organic light-phase mixed solution is washed with water with a small proportion of hydrochloric acid, the two phases being separated in the corresponding separation space and then the detergent entrainment articles are then coaled and removed from the organic metal-containing light-phase mixed solution in a coalescence separator provided for this purpose.
  • the extract phase is followed by a re-extraction phase in which the complexing agents of the organic light phase mixed solution are regenerated by means of an aqueous sulfate-containing electrolyte solution.
  • a re-extraction phase in which the complexing agents of the organic light phase mixed solution are regenerated by means of an aqueous sulfate-containing electrolyte solution.
  • the copper sulfate is filtered with activated carbon in front of the electrolyte bath supply in order to remove organic light phase mixed solution entrainment articles, since otherwise the efficiency of the electrolyte bath is reduced and, if necessary, an anode / cathode short circuit can lead to surface ignition.
  • the low-metal organic light phase mixed solution is then washed out with wash water washed in the first washing process, again the mixing phases being separated in a separation space and the detergent entrainment articles being coalized and removed in a corresponding coalescence separator.
  • Separate coalescence cylinders are provided for each of the coalescence processes, as a result of which the apparatus volume and thus also the solution volumes to be used increase significantly. On the other hand, these are required to achieve a sufficient degree of separation.
  • the water used for the washing process in the re-extraction is subsequently sulphate-containing and is neutralized for reuse with milk of lime. Due to the circulation of the treated water, the system is filled with gypsum, and the phase separation of the mixed solutions is made more difficult due to the contamination and soaping of the phase separating surface. In addition, the gypsum is contaminated with chemicals and copper ions and must be disposed of as special waste.
  • the invention has for its object to provide a method for liquid-liquid extraction, which is energy-saving, inexpensive and less polluting.
  • a liquid-liquid extraction is carried out, the etching solution forming the heavy phase and an organic solution forming the light phase and the metal ions being removed from the etching solution.
  • the heavy and light phases are separated by coalescence.
  • the extract phase is washed and the alkaline load and the metal component are recovered from the extract phase.
  • the alkaline load is removed from the alkaline-loaded washing liquid by stripping.
  • An important advantage of the method according to the invention results from the fact that the heavy and light phases are separated by coalescence in each extraction stage. In this way, a common coalescence separation can be carried out for both phases, and even in the case of an emulsion of the solutions, the separation is practically complete and the separation time is shortened.
  • the alkaline component can be advantageously fed, after cooling of the regenerated etching solution to stop again to the Sollwertpa ⁇ parameters.
  • the stripping of the alkaline component of the wash water is advantageously carried out in vacuo.
  • a filling reaction can remove the alkaline load from the washing liquid used for the extract phase by means of a filling reaction. This makes it possible to completely circulate the washing liquid, which means that it can then be used to wash the extract phase.
  • free ammonia and one or more ammonium salt (s) are preferably used as the alkaline component of the etching solution, the ammonium salt advantageously being ammonium chloride, ammonium carbonate, ammonium bicarbonate and / or ammonium sulfate.
  • Water is advantageously used as the washing liquid.
  • An advantageous embodiment of the processing method according to the invention is characterized in that the metal component is recovered from the metal-containing extract phase in a liquid-liquid re-extraction using dilute acid as the electrolyte solution. After removal of the metal constituent, this can then advantageously be used again in the liquid-liquid re-extraction as the lead phase for the liquid-liquid extraction. This reduces the amount of extractant used and thus the process costs.
  • the metal component is preferably removed from the metal-containing electrolyte solution by means of electrolysis and the electrolyte solution is then reused for the liquid-liquid extraction.
  • a coalescence separation is carried out on the electrolyte solution after the re-extraction and / or the electrolyte solution is filtered using activated carbon.
  • activated carbon In this way, carry-along items from the light phase mixed solution removed, and thus a reduction in the electrolyte bath efficiency can be prevented. It also does not happen that these particles float on the electrolyte surface or can lead to surface ignition in the event of a possible anode / cathode short circuit.
  • each re-extraction stage carries out a coalescence separation of the heavy and light phases.
  • ammoniacal metal solutions in particular, can be processed without waste water and without the problems mentioned at the beginning.
  • the following steps are carried out in a preferred method variant: a) The metal ions are extracted from the used etching solution by means of a liquid ion exchanger; b) Traces of the organic phase are removed from the etching solution to be processed by means of a coalescence separator and activated carbon adsorber; c) the ammonia is washed out ⁇ exchanger by means of water from the liquid ion; d) the ammonia is recovered from the wash water by means of vacuum stripping; e) the chemicals which are used up during the etching process are metered into the regenerated etching solution in order to reset the setpoint parameters; f) the finished etching solution is filtered; g) the complexing agents of the organic light phase mixed solution which is preferably used as the extractant are re-extracted by means of dilute acid, ie electrolyte solution; h
  • a device for liquid-liquid extraction can advantageously be used to carry out this method, in which the solvent phase is the light phase and the raffinate phase is the heavy phase and which comprises a mixer-separator battery in tower form.
  • the solvent phase is the light phase
  • the raffinate phase is the heavy phase and which comprises a mixer-separator battery in tower form.
  • a plurality of separation spaces which are separate from one another are arranged one above the other in a tower, the separation spaces each having a mixing space and the mixing spaces being arranged one above the other.
  • An inlet of the light phase is essentially at the bottom in the mixing rooms and an outlet of the light phase is essentially at the top in the mixing rooms and the outlet of the solvent phase is provided at the top of the battery.
  • An inflow of the heavy phase is essentially provided at the top in the separation rooms, an inflow of the heavy phase in each case essentially at the bottom into the associated mixing rooms and an outlet of the heavy phase from the bottom of the separation rooms, the outflow of the raffinate phase being provided at the bottom of the battery.
  • a coalescence separation device is in each case at the inlet of the heavy phase into the respective separation room or at the outlet of the heavy phase provided from the respective mixing room.
  • This device has a compact structure with an integrated coalescer, which serves as a phase separation intensifier or separation accelerator. The method according to the invention can thus be carried out in a relatively limited phase separation time in a volume-limiting manner with comparatively little piping and little space requirement and thus also very economically.
  • the invention provides a device for processing alkaline metal-containing etching solutions, in which a liquid-liquid extraction is carried out and an organic solution is conducted in countercurrent to the etching solution and the metal ions are removed from the etching solution.
  • the device has a coalescence direction for the light and heavy phase in each extraction stage. It also includes a washing stage for the extract phase and a device for recovering the alkaline component and the metal component from the extract phase.
  • a tap device is provided for removing the alkaline component from the washing liquid loaded with the alkaline component. This device is preferably used to carry out the method according to the invention.
  • the mixer-separator battery according to the invention is described below using the example of a process for treating ammonium-copper chloride (heavy phase) loaded with up to 160 g / 1 copper as a result of an ammonium-chlorine etching process and with reference to the drawing.
  • An organic light-phase mixture for example with aldoxime and / or ketoxime complexing agents in kerosene-like flux, is used as the extracting agent.
  • arrows shown in bold in the figure have been chosen to show the transport of the aqueous heavy-phase solutions.
  • the transport of the organic light-phase mixed solution is shown with thinly drawn arrows, and the small, thin arrows show the continuation of the stripped ammonia.
  • the two mixer-separator batteries illustrated in the drawing are of identical design and comprise two extraction or re-extraction stages in their lower tower parts. Two washing stages are provided in the upper parts of the tower.
  • the extraction battery E comprises two stages two separating spaces 9, 10 filled with full cores. These separating spaces each contain a mixing space 3, 4, which are arranged one above the other. A countercurrent mixture of etching solution (heavy phase) and organic light phase solution is present in the mixing rooms. seen.
  • the upper mixing spaces 12, 13, which are also arranged one above the other in separation spaces 19, 20, are intended for mixing with water, ie for washing the metal-containing organic light-phase solution.
  • Ruhrer RW, RE in a conventional manner, the waves of which extend downwards from the cover of the extraction battery and bearings are carried out, at the same time ensuring a seal between adjacent steps. By means of a continuous tube, a tight bridging of the upper partitions 19, 20 is ensured.
  • the Ruhrers are each arranged at the height of the inflows and phase boundaries in order to achieve a good mixture of substances immediately.
  • the mixing rooms 3, 4 and 12, 13 are closed off from one another by partitions, the lower part 9 being provided with a bottom and the upper part 20 being provided with a cover.
  • the phase boundary n in the separating spaces is each indicated by a thin line T.
  • Aqueous, used or metal-loaded etching solution is introduced into the mixing chamber 4 through a feed pipe 1.
  • a drain pipe 6 is provided for guiding the heavy phase, ie the treated etching solution, from the separating chamber 10 into the lower mixing chamber 3, in which a return pipe 2, 2R with integrated addition container 34 is also merged.
  • a flow ⁇ pipe 21 the bottom of the separation space 9 is provided for the demetallized etchant (raffinate).
  • the drain pipe 21 opens into a coalescence separator 22 with a discharge pipe 32 and continues to an activated carbon adsorber 23. After the organic phase has been removed from the raffinate phase, the latter is passed through a pipe 24 to restore the setpoint.
  • Obliquely arranged drain pipes 8, 7 are used for guiding mixed organic solution / etching solution via coalescence separator - ⁇ chtept K in the corresponding separation spaces 10, 9.
  • the Kölesenzentrennemides K serve to coalize possible mixed-phase emulsions. Their gradual arrangement results in an extremely integrated structure and accordingly less expensive solution is required.
  • An ascending pipe 5 is provided between the separating spaces 9 and 10 for the ascending light phase.
  • Another riser pipe 11 leads from the upper separation chamber 10 into the lower mixing chamber 12 of the washing stages.
  • a further riser pipe 16 for the light phase solution extends upward from the associated separation chamber into the upper mixing chamber 13.
  • An overflow pipe 33 extends from the upper separation chamber 20 through the cover and leads to the re-extraction battery R.
  • a drain pipe 15 for the wash water / light phase mixture leads from the upper separation space 20 into the lower mixing space 12.
  • Diagonally arranged drain tubes 18, 17 are used to guide the wash water / light phase mixture via coalescence separation devices K m and the corresponding separation spaces 20, 19.
  • a wash water feed pipe 14 In the upper mixing chamber 13 there is a wash water feed pipe 14, and a wash water drain pipe 25 leads from the lower separation chamber 19 to a heat exchanger 27.
  • a feed 31 for additional wash water In the E feed pipe 14 there is a feed 31 for additional wash water, via which the amount of water in the circuit can be filled, as well as a return pipe 26 branched off from the drain pipe 25 for a partial washing water quantity.
  • the heat exchanger 27 is connected to a vacuum stripper 29.
  • this is of the reboiler type, ie the washing water is passed through a reboiler in which the volatile components parts (such as ammonia) are evaporated.
  • a tube 30 leads cooled ammonia from the vacuum stripper 29 to the line 24.
  • a tube 28 serves to transport the ammonia-free washing water from the vacuum stripper 29 through the heat exchanger 27 and at the other end takes on the task of feeding the washing water into the re-extraction battery R for sulfate washing.
  • the structure of the re-extraction battery R is identical to that of the extraction battery E.
  • the parts corresponding to those of the extraction battery are therefore identified by an added letter R, but otherwise have the same numbers. As far as the parts and functions are the same, they will not be described again.
  • an aqueous sulfate-containing electrolyte solution is fed through the feed pipe 1R.
  • the drain pipe 21R is provided for the discharge of copper sulfate through an additional coalescer 22R with a discharge pipe 32R and an activated carbon filter 23R into an electrolyte bath 36, from which copper-containing electrolyte solution reaches the feed pipe 1R via a filter 37.
  • the pipe 28 for washing water exiting from the first extraction battery and cleaned from the alkaline component leads into the upper mixing cylinder 13R of the re-extraction battery R.
  • a drain pipe 25R serves to discharge washing water / light phase mixture and leads to a filling bath 35 in which the ammonium sulfate is removed from the washing water becomes.
  • the already mentioned feed pipe 14 then leads the wash water from the filling bath 35 into the mixing chamber 13 of the extraction battery E.
  • Step a The processes of the method according to the invention are as follows: Step a:
  • the method consists in that the metal ions are removed from the used etching solution with the aid of a liquid ion exchanger in a two-stage extraction process. Due to the low weight compared to the aqueous solution, the light solution phase increases during the extraction from the lower rooms up to the overflow pipe and is increasingly exposed to metal. Because of its greater weight, the etching solution in turn passes down through the drain pipes and the coalescence separation devices and emerges as a metal-free etching solution (raffinate phase). In order to remove any emulsion, the aqueous heavy phase / organic light phase mixed solution is precoalized in the integrated coalescers.
  • Step b
  • the ammonia is obtained from the washing water of the first washing process, which is loaded with entraining articles with ammonia-ammonium chloride.
  • the stripped ammonia is again added to the regenerated etching solution before the setpoint parameters are restored. Further components used during the etching process are metered back into the etching solution in order to restore the setpoint parameters.
  • the etching solution is then filtered and is ready for the next use.
  • the washing water freed from the ammonia is fed through heat exchangers to the sulfate wash of the re-extraction battery R.
  • Step f
  • the re-extraction of the copper ions from the liquid ion exchanger is carried out in two stages using dilute acid, the complexing agents of the organic light-phase mixed solution being regenerated.
  • the copper-containing electrolyte solution / light-phase mixed solution is precolored in each case in the corresponding integrated coalescer in order to eliminate any emulsion.
  • the two mixture phases are separated in the corresponding separation room.
  • the etching solution comes down again due to the higher weight.
  • the mixed solution gets down and copper sulphate comes out at the lower outlet. Due to the lower weight in relation to the aqueous solution, the light-solution phase rises and emerges as a mixture of solutions after the re-extraction process.
  • Step g
  • the liquid ion exchanger is washed out with washing water from the first washing process after the ammonia stripping process, but is not completely free of ammonia.
  • the copper-containing electrolyte solution / copper-free light-phase mixed solution is precoalized in appropriate integrated coalescers. This eliminates any emulsion.
  • the two mixture phases are separated in the corresponding separation room.
  • the wash water is treated before reuse to remove the chemicals still present.
  • the copper is recovered in the electrolyte bath.
  • Electrolyte is passed on for reuse.
  • the ammonium sulfate is removed from the wash water of the second wash before being reused in the replenishing bath.

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  • 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)
  • Physical Water Treatments (AREA)
  • Extraction Or Liquid Replacement (AREA)
  • ing And Chemical Polishing (AREA)
  • Weting (AREA)

Abstract

L'invention concerne un procédé pour la préparation de solutions d'attaque métallifères alcalines, dans lequel s'effectue une extraction liquide-liquide, la solution d'attaque formant la phase lourde et une solution organique formant la phase légère, et les ions métalliques étant éliminés de la solution d'attaque. Une séparation par coalescence est réalisée au cours de chaque étape d'extraction. La phase d'extraction est lavée et le constituant alcalin ainsi que le constituant métallique sont récupérés dans cette phase d'extraction. Le constituant alcalin est éliminé, par épuration, du liquide de lavage chargé de ce dernier.
EP98954152A 1997-09-10 1998-09-05 Procede pour la preparation de solutions d'attaque metalliferes alcalines Withdrawn EP1019565A1 (fr)

Applications Claiming Priority (3)

Application Number Priority Date Filing Date Title
DE19739568 1997-09-10
DE19739568 1997-09-10
PCT/DE1998/002669 WO1999013130A1 (fr) 1997-09-10 1998-09-05 Procede pour la preparation de solutions d'attaque metalliferes alcalines

Publications (1)

Publication Number Publication Date
EP1019565A1 true EP1019565A1 (fr) 2000-07-19

Family

ID=7841767

Family Applications (1)

Application Number Title Priority Date Filing Date
EP98954152A Withdrawn EP1019565A1 (fr) 1997-09-10 1998-09-05 Procede pour la preparation de solutions d'attaque metalliferes alcalines

Country Status (3)

Country Link
EP (1) EP1019565A1 (fr)
AU (1) AU1141399A (fr)
WO (1) WO1999013130A1 (fr)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108014516A (zh) * 2017-11-14 2018-05-11 中国核电工程有限公司 一种混合澄清槽

Families Citing this family (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE19815287A1 (de) * 1998-04-06 1999-10-07 Celi Ivo Letterio Mehrstufen Gegenstrom Extraktionsturm mit statischem Mischer und integriertem Koaleszenzer
DE19815288A1 (de) * 1998-04-06 1999-10-07 Celi Ivo Letterio Verfahren zur energiesparenden und abwasserfreien Aufbereitung ammoniakalischer Metallösung aus dem Ätzvorgang zur Herstellung der Leiterplatten

Family Cites Families (11)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
NL72682C (fr) * 1950-09-20
US2714056A (en) * 1952-10-20 1955-07-26 Dow Chemical Co Method of operating mixer-settler extractors
US4083758A (en) * 1976-09-27 1978-04-11 Criterion Process for regenerating and for recovering metallic copper from chloride-containing etching solutions
SE411231B (sv) * 1978-05-02 1979-12-10 Mx Processer Reinhardt Forfarande for atervinning av ett ammonialkaliskt etsbad
JPS5591979A (en) * 1978-12-29 1980-07-11 Yamatoya Shokai:Kk Recovering and circulating apparatus for alkaline etching waste solution
JPS55145177A (en) * 1979-04-28 1980-11-12 Kagaku Gijutsu Shinkoukai Treating method of alkali etchant waste solution
JPS55162307A (en) * 1979-06-05 1980-12-17 Steiner Ladislav Liquiddliquid extracting tower
AT376377B (de) * 1980-09-11 1984-11-12 Voest Alpine Ag Zweiphasengegenstromapparat
IT1261515B (it) * 1993-08-13 1996-05-23 In Tec Italia Int Env Tech Srl Procedimento per il recupero delle soluzioni di incisione dei metalli spente.
DE4334696A1 (de) * 1993-10-12 1995-04-13 Vulkan Eng Gmbh Verfahren zum Regenerieren von Ätzlösungen
DE19521352A1 (de) * 1995-06-12 1996-12-19 Henkel Kgaa Verfahren zur Aufarbeitung ammoniakalischer Metallösungen

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
See references of WO9913130A1 *

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108014516A (zh) * 2017-11-14 2018-05-11 中国核电工程有限公司 一种混合澄清槽

Also Published As

Publication number Publication date
AU1141399A (en) 1999-03-29
WO1999013130A1 (fr) 1999-03-18

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