EP0157190A1 - Procédé de décapage d'aluminium - Google Patents
Procédé de décapage d'aluminium Download PDFInfo
- Publication number
- EP0157190A1 EP0157190A1 EP85102400A EP85102400A EP0157190A1 EP 0157190 A1 EP0157190 A1 EP 0157190A1 EP 85102400 A EP85102400 A EP 85102400A EP 85102400 A EP85102400 A EP 85102400A EP 0157190 A1 EP0157190 A1 EP 0157190A1
- Authority
- EP
- European Patent Office
- Prior art keywords
- bath
- pickling
- aluminum
- pickling bath
- aluminum hydroxide
- 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
Links
- 229910052782 aluminium Inorganic materials 0.000 title claims abstract description 26
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 title claims abstract description 26
- 238000000034 method Methods 0.000 title claims abstract description 23
- 239000004411 aluminium Substances 0.000 title abstract 2
- 238000005530 etching Methods 0.000 title 1
- HEMHJVSKTPXQMS-UHFFFAOYSA-M sodium hydroxide Inorganic materials [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 57
- 238000005554 pickling Methods 0.000 claims abstract description 52
- WNROFYMDJYEPJX-UHFFFAOYSA-K aluminium hydroxide Chemical compound [OH-].[OH-].[OH-].[Al+3] WNROFYMDJYEPJX-UHFFFAOYSA-K 0.000 claims abstract description 24
- 235000011121 sodium hydroxide Nutrition 0.000 claims abstract description 19
- 239000003513 alkali Substances 0.000 claims abstract description 8
- AEQDJSLRWYMAQI-UHFFFAOYSA-N 2,3,9,10-tetramethoxy-6,8,13,13a-tetrahydro-5H-isoquinolino[2,1-b]isoquinoline Chemical compound C1CN2CC(C(=C(OC)C=C3)OC)=C3CC2C2=C1C=C(OC)C(OC)=C2 AEQDJSLRWYMAQI-UHFFFAOYSA-N 0.000 claims abstract description 7
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims abstract description 7
- 239000008139 complexing agent Substances 0.000 claims abstract description 7
- 238000001556 precipitation Methods 0.000 claims abstract description 7
- 239000000176 sodium gluconate Substances 0.000 claims abstract description 7
- 235000012207 sodium gluconate Nutrition 0.000 claims abstract description 7
- 229940005574 sodium gluconate Drugs 0.000 claims abstract description 7
- 238000011065 in-situ storage Methods 0.000 claims abstract description 3
- 230000008929 regeneration Effects 0.000 claims abstract description 3
- 238000011069 regeneration method Methods 0.000 claims abstract description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 12
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 10
- 238000001914 filtration Methods 0.000 claims description 10
- 239000000126 substance Substances 0.000 claims description 9
- 239000007787 solid Substances 0.000 claims description 8
- 229910000029 sodium carbonate Inorganic materials 0.000 claims description 5
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims description 3
- 150000001447 alkali salts Chemical class 0.000 claims description 3
- 239000000706 filtrate Substances 0.000 claims description 3
- 238000000926 separation method Methods 0.000 claims description 2
- 229910021502 aluminium hydroxide Inorganic materials 0.000 abstract 2
- 229910019142 PO4 Inorganic materials 0.000 abstract 1
- 230000004075 alteration Effects 0.000 abstract 1
- 235000021317 phosphate Nutrition 0.000 abstract 1
- 150000003013 phosphoric acid derivatives Chemical class 0.000 abstract 1
- 235000011118 potassium hydroxide Nutrition 0.000 abstract 1
- 150000004763 sulfides Chemical class 0.000 abstract 1
- 150000003467 sulfuric acid derivatives Chemical class 0.000 abstract 1
- 150000004764 thiosulfuric acid derivatives Chemical class 0.000 abstract 1
- 239000000243 solution Substances 0.000 description 11
- 230000015572 biosynthetic process Effects 0.000 description 5
- 239000008237 rinsing water Substances 0.000 description 4
- 238000005406 washing Methods 0.000 description 4
- ANBBXQWFNXMHLD-UHFFFAOYSA-N aluminum;sodium;oxygen(2-) Chemical compound [O-2].[O-2].[Na+].[Al+3] ANBBXQWFNXMHLD-UHFFFAOYSA-N 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 230000000737 periodic effect Effects 0.000 description 3
- 229910001388 sodium aluminate Inorganic materials 0.000 description 3
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000001704 evaporation Methods 0.000 description 2
- 230000008020 evaporation Effects 0.000 description 2
- 229910052739 hydrogen Inorganic materials 0.000 description 2
- 239000001257 hydrogen Substances 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 238000007747 plating Methods 0.000 description 2
- 239000002351 wastewater Substances 0.000 description 2
- -1 B. the anodization Chemical compound 0.000 description 1
- 206010039509 Scab Diseases 0.000 description 1
- 230000001464 adherent effect Effects 0.000 description 1
- 229910001854 alkali hydroxide Inorganic materials 0.000 description 1
- 150000008044 alkali metal hydroxides Chemical class 0.000 description 1
- 239000012670 alkaline solution Substances 0.000 description 1
- 238000002048 anodisation reaction Methods 0.000 description 1
- 239000012065 filter cake Substances 0.000 description 1
- 238000007730 finishing process Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 239000002054 inoculum Substances 0.000 description 1
- 230000001788 irregular Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 239000013589 supplement Substances 0.000 description 1
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
- C23F1/10—Etching compositions
- C23F1/14—Aqueous compositions
- C23F1/32—Alkaline compositions
- C23F1/36—Alkaline compositions for etching aluminium or alloys thereof
-
- 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
-
- 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
- C23G—CLEANING OR DE-GREASING OF METALLIC MATERIAL BY CHEMICAL METHODS OTHER THAN ELECTROLYSIS
- C23G1/00—Cleaning or pickling metallic material with solutions or molten salts
- C23G1/14—Cleaning or pickling metallic material with solutions or molten salts with alkaline solutions
- C23G1/22—Light metals
-
- 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
- C23G—CLEANING OR DE-GREASING OF METALLIC MATERIAL BY CHEMICAL METHODS OTHER THAN ELECTROLYSIS
- C23G1/00—Cleaning or pickling metallic material with solutions or molten salts
- C23G1/36—Regeneration of waste pickling liquors
Definitions
- the invention relates to a pickling process for aluminum in an alkali bath.
- Dissolving 27 g of aluminum (1 mol) consumes 40 g of sodium hydroxide solution (1 mol) and 18 g of water (1 mol) to form 82 g of dissolved sodium aluminate (1 mol) and 3 g of hydrogen (1.5 mol).
- the bath concentration of sodium aluminate increases, the sodium hydroxide solution and the corresponding pickling power decrease.
- the bath activity can be maintained by periodically adding additional sodium hydroxide solution.
- a complexing agent is added to avoid the formation of solid adherent crusts from aluminum hydroxide.
- the periodic removal of the worn pickling baths can be avoided by letting the concentration of dissolved aluminum rise to about 110 g / l. At this concentration, the bath liquid carried along with the treated pieces contains as much dissolved aluminum as was produced by pickling the corresponding pieces in the bath. A steady state is reached; the sodium hydroxide and complexing agent consumption must be supplemented by adding appropriate fresh chemicals; the total amount of dissolved aluminum gets into the wastewater with the rinse water and must be removed from a dilute solution.
- the practically constant pickling bath composition ensures a constant quality of the treated pieces, but the high salt concentration often leads to the formation of stains on the pickled pieces during their transport from the pickling to the rinsing bath (see JH Dailey, Plating and surfaces finishing, July 1982 p 44)
- Another way to solve the problem of worn pickling baths is to transfer part of the pickling bath into a separate container and to cause the precipitation of the aluminum hydroxide from the sodium hydroxide solution by changing the temperature and adding considerable amounts of aluminum hydroxide as inoculants according to the equation :
- the object of the present invention was therefore to provide a pickling process for aluminum which largely avoids the disadvantages outlined above and leads in a simple and economical manner to a pickled aluminum of as constant a quality as possible.
- the invention relates to a pickling process for aluminum in an alkali lye bath, which is characterized in that the aluminum hydroxide formed is precipitated in the bath in situ with simultaneous regeneration of the used alkali.
- Sodium or potassium hydroxide solution is preferably used as the alkali hydroxide solution. It is expedient to work with a dilute pickling bath, and the pickling bath used according to the invention preferably contains less than 10 g / l, particularly preferably 1 to 10 g / 1 and in particular 3 to 6 g / 1 sodium or potassium hydroxide solution; the concentration of dissolved aluminum is less than 20 g / l, preferably less than 15 g / l, in particular 2 to 20 g / l, preferably 2 to 15 g / l, particularly preferably 4 to 8 g / l. These low alkali concentrations enable the precipitation of an easily filterable aluminum hydroxide and an easy generation of lye directly in the pickling bath.
- he low concentration of the pickling bath in dissolved material fen also helps to keep the chemical loss caused by entrainment at a low level. The loss is further reduced if the pickled pieces are drained properly and the rinsing water is recycled.
- the temperature of the pickling bath is preferably between 50 and 75 ° C.
- the concentration of dissolved substances remains essentially constant during the pickling of the aluminum, because the aluminum hydroxide continuously fails, and should preferably be in the concentration range given above as preferred. This enables a regular pickling rate of 3 to 7 g aluminum per m 2 and minute at a bath temperature of 50 to 75 ° C. The quality of the treated pieces is consistently good.
- the aluminum hydroxide formed during pickling accumulates in the pickling bath without disturbing the pickling. But it is desirable to keep the solids content of the bath between 10 and 30 g / 1 by the solid z. B. is separated by decanting and / or filtering.
- the solids separation can be carried out batchwise or continuously, and is expediently carried out in part of the pickling bath.
- the filtration form (filtration residue) obtained by the process according to the invention is good;
- the filtration cake is easy to wash and contains more than 50% solids, which makes it easier to evaluate the aluminum hydroxide.
- the precipitation of aluminum hydroxide can be done by adding alkali salts, e.g. B. of sodium carbonate, preferably in an amount of 5 to 100 g / 1, in particular 20 to 60 g / 1.
- alkali salts e.g. B. of sodium carbonate
- the state of matter and thus the filterability of the precipitated aluminum hydroxide is also affected by the presence of complexing agents, e.g. B. influenced by sodium gluconate. It is therefore advisable to add such complexing agents, e.g. B. sodium gluconate in an amount such that its concentration in the bath is between 0.01 to 1.0 g / 1, in particular 0.1 to 0.5 g / 1.
- the lifetime of the pickling bath according to the invention is practical - table indefinitely if the losses caused by entrainment be supplemented by adding the appropriate amounts of fresh chemicals. These losses and the corresponding chemical costs can be kept to a minimum if the filtrate and washing water from the aluminum hydroxide filtration and the rinsing water of the pickled pieces are returned in whole or in part to the pickling bath. This return of the washing and rinsing water also serves to supplement the water loss caused by the formation of the aluminum hydroxide and the evaporation.
- the replacement and removal of the worn pickling baths is no longer necessary, which means that a considerable saving in pickling costs can be achieved.
- the necessary for carrying out the pickling process according to the invention Z usatzinvestitionen are small and consist essentially of the cost of a filtration plant.
- the bath is loaded with about 120 kg of dissolved aluminum.
- the precipitation of the aluminum hydroxide begins and is continued in accordance with the treatment of further pieces of aluminum.
- the solids content is allowed to rise to about 350 kg (corresponding to the treatment of a further 5000 m 2 of aluminum) and is kept between 250 and 500 kg by continuous or batchwise filtration of part of the bath.
- the filter cake is washed with 2 to 4 times its weight of water. The solids content depends on the filter type, but is at least 50%.
- the filtrate and wash water are returned to the pickling bath.
- the losses that occur during operation are supplemented by periodic addition of water, 100 kg sodium carbonate, 50 kg caustic soda (or equivalent amounts of sodium hydroxide solution) and 2 kg sodium gluconate.
- the above consumption relates to the pickling of approximately 5000 m 2 of aluminum, corresponding to the formation of 350 kg of aluminum hydroxide. These are maximum values that were measured in a system without returning the washing and rinsing water.
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)
- Cleaning And De-Greasing Of Metallic Materials By Chemical Methods (AREA)
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| AT85102400T ATE54679T1 (de) | 1984-03-16 | 1985-03-04 | Beizverfahren fuer aluminium. |
Applications Claiming Priority (4)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CH1325/84A CH660201A5 (fr) | 1984-03-16 | 1984-03-16 | Procede de decapage de l'aluminium dans un bain de lessive alcaline. |
| CH1325/84 | 1984-03-16 | ||
| DE3426114 | 1984-07-16 | ||
| DE19843426114 DE3426114A1 (de) | 1984-03-16 | 1984-07-16 | Beizverfahren fuer aluminium |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| EP0157190A1 true EP0157190A1 (fr) | 1985-10-09 |
| EP0157190B1 EP0157190B1 (fr) | 1990-07-18 |
Family
ID=25687339
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| EP19850102400 Expired - Lifetime EP0157190B1 (fr) | 1984-03-16 | 1985-03-04 | Procédé de décapage d'aluminium |
Country Status (1)
| Country | Link |
|---|---|
| EP (1) | EP0157190B1 (fr) |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE4008379A1 (de) * | 1990-03-15 | 1991-09-19 | Gartner & Co J | Verfahren und anlage zum regenerieren von alkalihaltigen aluminiumbeizloesungen |
| US5512129A (en) * | 1990-03-15 | 1996-04-30 | Josef Gartner & Co. | Method for regenerating alkaline solutions for pickling aluminum |
| DE102013108375A1 (de) * | 2013-01-31 | 2014-07-31 | Thomas König | Verfahren zum Aufbereiten eines Beiz- und/oder Eloxalbades und Eloxieranordnung |
| CN112921316A (zh) * | 2021-01-20 | 2021-06-08 | 福建省闽发铝业股份有限公司 | 一种绿色环保铝型材喷涂前处理工艺 |
Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| ITMO20060401A1 (it) * | 2006-12-07 | 2008-06-08 | Italtecno S R L | Impianto per il recupero di soda caustica da soluzioni caustiche e relativo procedimento. |
| EP2352859B1 (fr) | 2008-11-03 | 2018-06-27 | Thomas König | Procédé et installation de décapage |
| DE102008063729A1 (de) * | 2008-11-03 | 2010-05-06 | König, Thomas | Beizverfahren und Beizanlage |
Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US2653861A (en) * | 1953-03-09 | 1953-09-29 | Enthone | Etching aluminum using hexahydroxyheptanoic acid as a modifier |
| US2884728A (en) * | 1954-08-16 | 1959-05-05 | Turco Products Inc | Apparatus and method for removing metal from the surface of a metal object |
| DE1073272B (de) * | 1960-01-14 | Amchem Products Ine Ambler Pa (V St A) | andsdale Mounted Route Pa (V St A ) I Losung und Mittel zum Ätzen von Aluminium | |
| FR1582144A (fr) * | 1968-06-24 | 1969-09-26 | ||
| FR2169883A1 (fr) * | 1971-12-30 | 1973-09-14 | Diversey France | |
| DE2439202A1 (de) * | 1974-08-16 | 1976-02-26 | Blasberg Gmbh & Co Kg Friedr | Bad und badzusammensetzung zum aetzen von aluminium und aluminiumlegierungen |
| EP0143715A1 (fr) * | 1983-11-24 | 1985-06-05 | DIVERSEY FRANCE S.A. Société anonyme dite: | Bain de traitement de l'aluminium et procédé mettant en oeuvre ce bain notamment dans le domaine du satinage et de l'usinage chimique |
-
1985
- 1985-03-04 EP EP19850102400 patent/EP0157190B1/fr not_active Expired - Lifetime
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE1073272B (de) * | 1960-01-14 | Amchem Products Ine Ambler Pa (V St A) | andsdale Mounted Route Pa (V St A ) I Losung und Mittel zum Ätzen von Aluminium | |
| US2653861A (en) * | 1953-03-09 | 1953-09-29 | Enthone | Etching aluminum using hexahydroxyheptanoic acid as a modifier |
| US2884728A (en) * | 1954-08-16 | 1959-05-05 | Turco Products Inc | Apparatus and method for removing metal from the surface of a metal object |
| FR1582144A (fr) * | 1968-06-24 | 1969-09-26 | ||
| FR2169883A1 (fr) * | 1971-12-30 | 1973-09-14 | Diversey France | |
| DE2439202A1 (de) * | 1974-08-16 | 1976-02-26 | Blasberg Gmbh & Co Kg Friedr | Bad und badzusammensetzung zum aetzen von aluminium und aluminiumlegierungen |
| EP0143715A1 (fr) * | 1983-11-24 | 1985-06-05 | DIVERSEY FRANCE S.A. Société anonyme dite: | Bain de traitement de l'aluminium et procédé mettant en oeuvre ce bain notamment dans le domaine du satinage et de l'usinage chimique |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE4008379A1 (de) * | 1990-03-15 | 1991-09-19 | Gartner & Co J | Verfahren und anlage zum regenerieren von alkalihaltigen aluminiumbeizloesungen |
| US5512129A (en) * | 1990-03-15 | 1996-04-30 | Josef Gartner & Co. | Method for regenerating alkaline solutions for pickling aluminum |
| DE102013108375A1 (de) * | 2013-01-31 | 2014-07-31 | Thomas König | Verfahren zum Aufbereiten eines Beiz- und/oder Eloxalbades und Eloxieranordnung |
| CN112921316A (zh) * | 2021-01-20 | 2021-06-08 | 福建省闽发铝业股份有限公司 | 一种绿色环保铝型材喷涂前处理工艺 |
Also Published As
| Publication number | Publication date |
|---|---|
| EP0157190B1 (fr) | 1990-07-18 |
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