EP0017302B1 - Procédé de rinçage durant la phosphatation de substrats métalliques - Google Patents
Procédé de rinçage durant la phosphatation de substrats métalliques Download PDFInfo
- Publication number
- EP0017302B1 EP0017302B1 EP80200302A EP80200302A EP0017302B1 EP 0017302 B1 EP0017302 B1 EP 0017302B1 EP 80200302 A EP80200302 A EP 80200302A EP 80200302 A EP80200302 A EP 80200302A EP 0017302 B1 EP0017302 B1 EP 0017302B1
- Authority
- EP
- European Patent Office
- Prior art keywords
- rinse
- stage
- rinsing
- post
- water
- 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
Links
- 238000000034 method Methods 0.000 title claims abstract description 21
- 229910052751 metal Inorganic materials 0.000 title claims abstract description 12
- 239000002184 metal Substances 0.000 title claims abstract description 12
- 150000002739 metals Chemical class 0.000 title claims abstract description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 14
- 239000010802 sludge Substances 0.000 claims abstract description 10
- 229910019142 PO4 Inorganic materials 0.000 claims abstract description 4
- 150000001450 anions Chemical class 0.000 claims abstract description 4
- 150000001768 cations Chemical class 0.000 claims abstract description 4
- 238000000576 coating method Methods 0.000 claims abstract description 3
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 claims abstract description 3
- 239000010452 phosphate Substances 0.000 claims abstract description 3
- 238000004140 cleaning Methods 0.000 description 8
- 239000013505 freshwater Substances 0.000 description 6
- 239000008237 rinsing water Substances 0.000 description 4
- 238000011010 flushing procedure Methods 0.000 description 3
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 description 2
- 229910001860 alkaline earth metal hydroxide Inorganic materials 0.000 description 2
- 238000005238 degreasing Methods 0.000 description 2
- 150000002500 ions Chemical class 0.000 description 2
- 238000006386 neutralization reaction Methods 0.000 description 2
- 238000002161 passivation Methods 0.000 description 2
- 235000021317 phosphate Nutrition 0.000 description 2
- 239000004094 surface-active agent Substances 0.000 description 2
- 238000009825 accumulation Methods 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 235000011116 calcium hydroxide Nutrition 0.000 description 1
- 239000000920 calcium hydroxide Substances 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 239000000356 contaminant Substances 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000009189 diving Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 238000009472 formulation Methods 0.000 description 1
- 229910001385 heavy metal Inorganic materials 0.000 description 1
- 230000002452 interceptive effect Effects 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 150000003013 phosphoric acid derivatives Chemical class 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 239000011541 reaction mixture Substances 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 238000004062 sedimentation Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
- 239000002562 thickening agent Substances 0.000 description 1
- 239000002351 wastewater Substances 0.000 description 1
- 238000004065 wastewater treatment Methods 0.000 description 1
Images
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
- C23C22/00—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
- C23C22/73—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals characterised by the process
Definitions
- the invention relates to a rinsing process in the application of phosphate coatings to metals, the metal surface passing through at least one pre-rinsing stage, a phosphating stage and at least two rinsing stages and rinsing water of the first rinsing stage being freed from annoying anions and cations and being used again for rinsing purposes after sludge removal .
- the typical process for phosphating processes consists in cleaning the metal surfaces, pre-rinsing before phosphating, phosphating itself and rinsing, which usually takes place in at least two stages.
- a disadvantage of the known methods is that either the fresh water savings are not satisfied or that considerable amounts of phosphating agent are introduced by the introduction of rinse water from the first rinse stage into the pre-rinse stage. These can cause a pre-passivation, which impairs the perfect layer formation in the phosphating stage.
- the object of the invention is to provide a rinsing process which avoids the disadvantages of the known processes, has a low fresh water requirement and rules out pre-passivation phenomena.
- the object is achieved in that the rinsing method mentioned at the outset is designed in accordance with the invention in such a way that practically all of the cleaned rinsing water after passing through the second rinsing stage NS2 is fed to the pre-rinsing stage VS and then returned to the first rinsing stage NS1.
- the water cleaned in the cleaning device is passed into the second rinse stage and from there into the pre-rinse stage.
- the rinse water from the pre-rinse stage is then led into the first rinse stage.
- This process which is a self-contained system, allows fresh water savings of around 90%. It is preferably suitable for phosphating processes that work with hydrogen peroxide accelerators.
- the pre-rinse stage When carrying out the method, it is possible to divide the pre-rinse stage into two treatment zones.
- the water that is fed to the pre-rinse stage is either divided between the two treatment zones or first to the second and then to the first rinse zone of the pre-rinse stage, as viewed in the direction of the flow of the metal surfaces.
- the rinse water is then returned to the first rinse stage.
- the second rinse stage can also be divided into two rinse zones.
- the rinse water from the last rinse zone is fed to the second rinse stage of the first rinse zone and from there to the pre-rinse stage.
- the metal surfaces emerging from the second rinse stage can be subjected to a further rinse treatment with fresh water, which then flows to the second rinse stage.
- the individual rinsing stages can be used for diving and / or spraying.
- the disruptive anions and cations are removed in a manner known per se.
- Phosphates and heavy metals can be precipitated, for example, by neutralization with alkaline earth metal hydroxide, especially milk of lime.
- the reaction mixture is brought to a pH of about 8.5.
- Dissolved alkali ions are not precipitated, but generally cause less interference, at least as long as there is no excessive accumulation in the rinsing baths.
- Such excessive enrichment can be avoided by e.g. B. in the formulation of degreasing and phosphating baths to the extent possible avoids the use of ions which result in soluble salts in the treatment with alkaline earth metal hydroxide.
- the precipitate resulting from the neutralization of the removed rinsing bath can be removed by the known methods of sludge separation, e.g. be removed from the solution by sedimentation and / or filtration.
- the separated sludge can be fed to a sludge thickener and a filter press for further concentration.
- the rinse water can be passed through a surfactant adsorber. This is recommended if a surfactant-containing solution is used in the degreasing stage.
- the sludge obtained in the phosphating stage is included in the method of cleaning the rinsing water.
- the sludge is separated off in the usual manner, but the thin sludge is also introduced into the treatment plant for reaction with suitable precipitants.
- the flushing method according to the invention is explained in more detail and, for example, using the figure. It represents a flow diagram for the rinse water.
- the initially degreased metal surfaces are passed through the pre-rinsing stage VS, the phosphating stage P, the first rinsing stage NS1 and the second rinsing stage NS2.
- the rinse water first passes from the cleaning device R into the second rinse stage NS2 and from there into the pre-rinse stage VS. After exiting the pre-rinse stage VS, it is returned to the first rinse stage NS1 and then fed to the cleaning device R.
- Losing water losses due to evaporation or mechanical discharge are compensated for by adding fresh water, which is expediently fed to the post-rinsing stage NS2.
- the arrow on the cleaning device R indicates the discharge of sludge.
Landscapes
- Chemical & Material Sciences (AREA)
- General Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Chemical Treatment Of Metals (AREA)
- Removal Of Specific Substances (AREA)
- Treatment Of Water By Ion Exchange (AREA)
- Manufacture And Refinement Of Metals (AREA)
Claims (1)
- Procédé de rinçage lors du dépôt le revêtements de phosphate sur des métaux, dans lequel la surface métallique parcourt au moins un stade de pré-rinçage, un stade de phosphatation, et au moins deux stades de post-rinçage et l'eau de rinçage du premier stade de post-rinçage est dé- barassée des anions et cation188 gênants par addition d'agents de précipitation et réutilisée pour des opérations de rinçage après séparation des boues, caractérisé en ce qu'on envoie au stade de pré-rinçage (Pré-R) pratiquement la totalité de l'eau de rinçage épurée après qu'elle ait traversé uniquement le deuxième stade de post-rinçage (PR-2) et ensuite, on la envoie au premier stade de post-rinçage (PR-1).
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| AT80200302T ATE5003T1 (de) | 1979-04-07 | 1980-04-01 | Spuelverfahren bei der aufbringung von phosphatueberzuegen auf metallen. |
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| GB7912299 | 1979-04-07 | ||
| GB7912299 | 1979-04-07 |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| EP0017302A1 EP0017302A1 (fr) | 1980-10-15 |
| EP0017302B1 true EP0017302B1 (fr) | 1983-10-12 |
Family
ID=10504422
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| EP80200302A Expired EP0017302B1 (fr) | 1979-04-07 | 1980-04-01 | Procédé de rinçage durant la phosphatation de substrats métalliques |
Country Status (3)
| Country | Link |
|---|---|
| EP (1) | EP0017302B1 (fr) |
| AT (1) | ATE5003T1 (fr) |
| DE (1) | DE3065238D1 (fr) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE4307591A1 (de) * | 1992-06-22 | 1994-09-15 | Eisenmann Kg Maschbau | Verfahren zur Nitritkonzentrationssenkung in Phosphatbad-Anlagen |
Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| AU591231B2 (en) * | 1986-02-18 | 1989-11-30 | Parker Chemical Company | Aluminum cleaning process |
| DE102008038653A1 (de) * | 2008-08-12 | 2010-03-25 | Henkel Ag & Co. Kgaa | Sukzessive korrosionsschützende Vorbehandlung von Metalloberflächen in einem Mehrstufenprozess |
| CN109989091B (zh) * | 2019-04-17 | 2024-09-03 | 镇江耐丝新型材料有限公司 | 一种钢丝用电解磷化系统 |
Family Cites Families (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB150475A (en) * | 1919-06-28 | 1920-09-09 | Frank Silson | Improved device for transmitting and magnifying sound |
| DE1805655C2 (de) * | 1968-10-28 | 1974-10-17 | Steuler Industriewerke Gmbh | Verfahren zur Fluessigkeitsspuelung von Gegenstaenden |
| GB1345716A (en) * | 1971-03-22 | 1974-02-06 | Oxy Effluent Control Ltd | Method and apparatus for rinsing contaminated articles |
| DE2729006A1 (de) * | 1977-06-28 | 1979-01-04 | Didier Werke Ag | Verfahren zur fluessigkeitsspuelung von gegenstaenden |
| GB1540308A (en) * | 1977-12-08 | 1979-02-07 | Pyrene Chemical Services Ltd | Process for the treatment of metal surfaces |
-
1980
- 1980-04-01 DE DE8080200302T patent/DE3065238D1/de not_active Expired
- 1980-04-01 EP EP80200302A patent/EP0017302B1/fr not_active Expired
- 1980-04-01 AT AT80200302T patent/ATE5003T1/de not_active IP Right Cessation
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE4307591A1 (de) * | 1992-06-22 | 1994-09-15 | Eisenmann Kg Maschbau | Verfahren zur Nitritkonzentrationssenkung in Phosphatbad-Anlagen |
Also Published As
| Publication number | Publication date |
|---|---|
| DE3065238D1 (en) | 1983-11-17 |
| ATE5003T1 (de) | 1983-10-15 |
| EP0017302A1 (fr) | 1980-10-15 |
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