DE2202457A1 - PROCESS FOR CHROMATING OBJECTS COATED WITH GALVANIC ZINC COATING - Google Patents
PROCESS FOR CHROMATING OBJECTS COATED WITH GALVANIC ZINC COATINGInfo
- Publication number
- DE2202457A1 DE2202457A1 DE19722202457 DE2202457A DE2202457A1 DE 2202457 A1 DE2202457 A1 DE 2202457A1 DE 19722202457 DE19722202457 DE 19722202457 DE 2202457 A DE2202457 A DE 2202457A DE 2202457 A1 DE2202457 A1 DE 2202457A1
- Authority
- DE
- Germany
- Prior art keywords
- solution
- liters
- acid
- acetic acid
- chromating
- 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
- 238000000034 method Methods 0.000 title claims description 10
- 238000004532 chromating Methods 0.000 title claims description 6
- 238000000576 coating method Methods 0.000 title description 11
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 title description 10
- 239000011701 zinc Substances 0.000 title description 10
- 229910052725 zinc Inorganic materials 0.000 title description 10
- 239000011248 coating agent Substances 0.000 title description 4
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 24
- 239000000243 solution Substances 0.000 claims description 24
- 229960000583 acetic acid Drugs 0.000 claims description 10
- BDAGIHXWWSANSR-UHFFFAOYSA-N methanoic acid Natural products OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 0.000 claims description 10
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 8
- 239000012362 glacial acetic acid Substances 0.000 claims description 6
- VWDWKYIASSYTQR-UHFFFAOYSA-N sodium nitrate Chemical compound [Na+].[O-][N+]([O-])=O VWDWKYIASSYTQR-UHFFFAOYSA-N 0.000 claims description 6
- OSWFIVFLDKOXQC-UHFFFAOYSA-N 4-(3-methoxyphenyl)aniline Chemical compound COC1=CC=CC(C=2C=CC(N)=CC=2)=C1 OSWFIVFLDKOXQC-UHFFFAOYSA-N 0.000 claims description 5
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 5
- 235000019253 formic acid Nutrition 0.000 claims description 5
- 229910017604 nitric acid Inorganic materials 0.000 claims description 5
- 230000002378 acidificating effect Effects 0.000 claims description 3
- 239000004317 sodium nitrate Substances 0.000 claims description 3
- 235000010344 sodium nitrate Nutrition 0.000 claims description 3
- JHWIEAWILPSRMU-UHFFFAOYSA-N 2-methyl-3-pyrimidin-4-ylpropanoic acid Chemical compound OC(=O)C(C)CC1=CC=NC=N1 JHWIEAWILPSRMU-UHFFFAOYSA-N 0.000 claims description 2
- 239000002253 acid Substances 0.000 claims description 2
- 241000252073 Anguilliformes Species 0.000 claims 1
- 101100039010 Caenorhabditis elegans dis-3 gene Proteins 0.000 claims 1
- 238000007598 dipping method Methods 0.000 claims 1
- 150000002500 ions Chemical class 0.000 claims 1
- 150000003752 zinc compounds Chemical class 0.000 claims 1
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 description 3
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- 240000007817 Olea europaea Species 0.000 description 2
- ZCDOYSPFYFSLEW-UHFFFAOYSA-N chromate(2-) Chemical compound [O-][Cr]([O-])(=O)=O ZCDOYSPFYFSLEW-UHFFFAOYSA-N 0.000 description 2
- 238000007747 plating Methods 0.000 description 2
- 241000132028 Bellis Species 0.000 description 1
- WGLPBDUCMAPZCE-UHFFFAOYSA-N Trioxochromium Chemical compound O=[Cr](=O)=O WGLPBDUCMAPZCE-UHFFFAOYSA-N 0.000 description 1
- 230000001464 adherent effect Effects 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- KRVSOGSZCMJSLX-UHFFFAOYSA-L chromic acid Substances O[Cr](O)(=O)=O KRVSOGSZCMJSLX-UHFFFAOYSA-L 0.000 description 1
- 229910000423 chromium oxide Inorganic materials 0.000 description 1
- 239000003792 electrolyte Substances 0.000 description 1
- AWJWCTOOIBYHON-UHFFFAOYSA-N furo[3,4-b]pyrazine-5,7-dione Chemical compound C1=CN=C2C(=O)OC(=O)C2=N1 AWJWCTOOIBYHON-UHFFFAOYSA-N 0.000 description 1
- 238000007654 immersion Methods 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 230000003678 scratch resistant effect Effects 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 208000006379 syphilis Diseases 0.000 description 1
- 238000004448 titration Methods 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
- 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
- C23C22/05—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 using aqueous solutions
- C23C22/06—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 using aqueous solutions using aqueous acidic solutions with pH less than 6
- C23C22/24—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 using aqueous solutions using aqueous acidic solutions with pH less than 6 containing hexavalent chromium compounds
- C23C22/26—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 using aqueous solutions using aqueous acidic solutions with pH less than 6 containing hexavalent chromium compounds containing also organic compounds
- C23C22/27—Acids
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)
- Chemically Coating (AREA)
- Chemical Treatment Of Metals (AREA)
Description
Verfahren zum Chromatieren von mit galvanischen Z1nküberzügen versehenen GegenstandenProcess for chromating objects provided with galvanic zinc coatings
Lie Erfindung betriff L ein verfahren zum Chromatieren von Gegenständen, die mit galvanischen ZiiiKüberzügen, insoesondere aas sauren, vorzugsweise schwefelsauren Bädern , versehen sind.Lie invention relates to a process for chromating Objects with galvanic zinc coatings, in particular aas acidic, preferably sulfuric acid, baths are provided.
Es ist bekannt, Zink oder galvaniscn verzinkte Gegenstände mit einem passivierenden · Chromüberzug zu verseilen. Eine sogenannte Schwarzverchromung von Zink und ZinküDerzügen kann mittels irendanioneni'reier Elektrolyten, die etwa 350 g/l OrO,, 5 g/l ßariumcaroonat und 5 g/l Eisessig enthalten, uei hohen Stromdichten von 100 bis 200 A/dm und niedrigen Temperaturen von 12 uis 1 J0J durchgeführt werden, liie Cxiromüberzüge enthalten zu uic JO/ό Chromoxyd. i»as Verfahren ist jedoch aufwendig und nicht allgemein anwendbar. Weiterhin Können Zinküberzüge durch liintaucnen in eine Lösung aus 100 g/l Chromsäure, 10 g/l Schwefelsäure und 3 g/l Salpetersäure geglänzt werden, wobei sicri ein brauner Chromatfilm abscheidet, hierbei wird jedoch häufig der Zinküberzug angegriffen und es lassen sich keine v/isch- und kratzfesten sowie ausreichend haftfeste Chromierungen insbesondere auf mittels saurer Bäder verzinkten Gegenständen erzielen.It is known to strand zinc or electro-galvanized objects with a passivating chrome coating. A so-called black chrome plating of zinc and zinc coatings can be carried out using irendanionic electrolytes, which contain about 350 g / l OrO ,, 5 g / l ßariumcaroonat and 5 g / l glacial acetic acid, at high current densities of 100 to 200 A / dm and low temperatures of 12 uis 1 J 0 J are carried out, liie cxirom coatings contain to uic JO / ό chromium oxide. However, this procedure is complex and not generally applicable. Can continue to zinc coatings by liintaucnen in a solution of 100 g / l of chromic acid, 10 g / l sulfuric acid and 3 g / l of nitric acid are polished, wherein SICRI a brown chromate film deposited, but in this case the zinc coating is frequently attacked and it can be no v / Achieve isch- and scratch-resistant as well as sufficiently adhesive chrome plating, especially on objects galvanized by means of acid baths.
309830/1018309830/1018
-D--D-
Es wurde gefanden, dai3 eine Ohromierung von galvanischen Zinküberzügen durcn Anwendung einer oesciauaten Lösung unter Einhaltung bestimmter .bedingungen, insbesondere Eins teilung eines bestimmten pH-Wertes ,derart durchgefünrt werden kann, daß innerhalb sehr Kurzer Verweilzeiten feste und anhaftende, oliv bis braun gefärote passivierende Überzüge erhalten werden.It has been found that galvanic ortomy Zinc coatings through the application of an oily solution Compliance with certain conditions, in particular classification a certain pH value, can be carried out in such a way that solid and adherent, olive to brown colored passivating coatings are obtained.
Das erfindungsgemäße Verfahren zum Chromatieren von mit galvanischen Zinküuerzügen versehenen Gegenständen durch Eintaucnen in eine saure, Chromationen und Titrationen entnaltende Lösung ist dadurch gekennzeichnet, dato man den Gegenstand in eine wässrige Lösung eintaucnt, dxe auf 100 LiterThe inventive method for chromating with galvanic Zinc coated objects by immersion in an acidic, chromate ions and titrations Solution is characterized by the fact that the object is immersed in an aqueous solution, dxe to 100 liters
a) 3 bis 15 Liter einer Lösung von 250 ois 330 g/l iMatriumdicnroraat und 200 bis JCO g/l Natriumnitrat, die auf den pH-Wert 0,3 mit Salpetersäure eingestellt ist,a) 3 to 15 liters of a solution of 250 to 330 g / l iMatriumdicnroraat and 200 to JCO g / l sodium nitrate added to the pH 0.3 is adjusted with nitric acid,
b) 3 bis 3 Liter einer Lösung von 500 bis 700 g/l 35 prozentiger Ameisensäure undb) 3 to 3 liters of a solution of 500 to 700 g / l 35 percent Formic acid and
c) 0,5 bis 3 Liter Eisessig bzw. konzentrierte Essigsäure enthält, und die Lösung auf einem pH-Wert von 2,1 bis 2,7 hält.c) contains 0.5 to 3 liters of glacial acetic acid or concentrated acetic acid, and maintaining the solution at pH 2.1 to 2.7.
Besonders bevorzugt ist eine Lösung, die auf 100 LiterA solution that is 100 liters is particularly preferred
a) 11 bis 11,5 Liter einer Lösung von 300 g/l Natriumdichromat und 250 g/l Natriumnitrat, die mit Salpetersäure auf einen pH-Wert von 0,3 eingestellt wurde,a) 11 to 11.5 liters of a solution of 300 g / l sodium dichromate and 250 g / l sodium nitrate, which with nitric acid on one pH value of 0.3 has been set,
o) 5 Liter Ameisensäurelösung der Dichte 1,133 (200O) und c) 6 bis 12 g/l Eisessig enthält.o) 5 liters of formic acid solution with a density of 1.133 (20 0 O) and c) 6 to 12 g / l glacial acetic acid.
Es. wurde gefunden, daß die Verwendung einer derartigen Lösung zusammen mit der sorgfältigen Einhaltung des genannten pH-Wertbereichs, die durch kontinuierliche lues sung und gegebenenfalls Zugabe von frischer Lösung erfolgt, eine Onromatierung insbesondere von aus schwefelsaurer Lösung galvanisch verzinkten Gegenständen erlauüt, wobei nicht nur eine im wesentlichen durch die Essigsäuremenge bestimmte, reproduzierbare Färbung von oliv bis braun gefärbten Tönungen erzielt wird, sondernIt. it has been found that the use of such a solution together with careful compliance with the specified pH value range, which is carried out by continuous lues solution and, if necessary, addition of fresh solution, in particular an onromatization from objects galvanized from sulfuric acid solution, whereby not only one essentially reproducible color determined by the amount of acetic acid from olive to brown tints, but rather
309830/1018309830/1018
gegenüber bekannten Chromatierun^sverfanren near icurze Verweilzeiten, die unter 60 bekunden Ue^er. u:xi uj.3 zu etwa 10 Sekunden oetra/ven Kennen, errexent werue;:, nouei axe passivxerende Chroiiic-enicut im feucnten Luutand völlig wxecii- und Kratzfest und. l.u trockenen Zaetanc uj.eoe- unu ^aftfest xst. ineuesondere uritt an oectnuc;1Lex. ,ionen derart enro.nati.erler verzinKter Jei_ejiu Cu,nue ^.exn kopu.xvern vier Jm^o-a^CiiicLL· aal'. Liies ΐΰΐ z.i5. bex ^&lvaiiisc^ ver^xiiklen una cixroua. tier ten Gegen stände^ , liie necnträßiicn ^euojen werden, von behenderer ^e-Compared to known chromating processes, the dwell times are short, which are less than 60 years. u: xi uj.3 to about 10 seconds oetra / ven kennen, erexent werue;:, nouei ax passivxerende Chroiiic-enicut in the feucnten Luutand completely wxecii- and scratch-proof and. lu dry Zaetanc uj.e o e- unu ^ aftfest xst. inewes special uritt an o ectnuc; 1 Lex., Ionen such enro.nati.erler galvanized Jei_ejiu Cu, nue ^ .exn kopu.xvern four Jm ^ oa ^ CiiicLL · aal '. Liies ΐΰΐ z.i5. bex ^ & lvaiiisc ^ ver ^ xiiklen una cixroua. animal objects ^, which can be neglected, from more agile ^ e-
Bei de;n erfindun^sgeiiiäiien Verfahren ole^ut aas JLroniatierungsveriiältiiiii, d.h. dc.1^ Vernal uIjxe von areiv/er nte,ii Jnron zu secnc wertige»a Gnro.u, pr^i-LbCn ^on^^t^i u, was mr ^r^xelan^ üöerlej^ener ^rjetmisse oextr:.it>. i.ie sxe nt.Cx: deja Vei-i&nren erLalten werden.In de; n inventions methods ole ^ ut aas JLroniatierungsveriiältiiiii, ie dc. 1 ^ Vernal uIjxe of areiv / er n t e, ii Jnron zu secnc valued »a Gnro.u, pr ^ i-LbCn ^ on ^^ t ^ iu, what mr ^ r ^ xelan ^ üöerlej ^ ener ^ rjetmisse oextr : .i t >. i.ie sxe nt.Cx: deja Vei-i & nren to be obtained.
J^e £γΓ in a LAn^-, wi ra uarcr aas lol^e-näe ^.exöpiei naiver erläutert.J ^ e £ γΓ in a LAn ^ -, wi ra uarcr aas lol ^ e-Nae ^ .exöpiei naively explained.
j3eispielj3example
LB wurde eine Lrisun^, sue a 30 Kt .■jatr^.L.uidicnrchiat und i ^atrx'oiiuiLxriM, auf 1tC Lioer cn ^oaicierte.i waoser ner^reG die iüi t Ga.ljje lersaurc auf einen pn-.Veri ^, 3 eingestellt i-'ie jiciite dei- i,osunu, ceuru^ 1,3^-° (^^ ·->) ·LB became a Lrisun ^, sue a 30 K t . ■ jatr ^ .L.uidicnrchiat and i ^ atrx'oiiuiLxriM, on 1tC Lioer cn ^ oaicierte.i waoser ner ^ reG the iüi t Ga.ljje lersaurc on a pn-. Veri ^, 3 set i-'ie jiciite dei- i, osun u , ceuru ^ 1,3 ^ - ° (^^ · ->) ·
iiis wurde weiter e ..ne ιοΰαυ^. - aus υ ■;·,■: itt3 (:-j,: Liter) :·^ 5fe-^ A.iieisens'.-iure ,auf 1CO Liter GnUiOnISXeI1IeHi /ascer ner/j,estellt, deren Diente 1,1 jj (^0Aj) oetruj,.iiis became further e ..ne ιοΰαυ ^. - from υ ■ ·, ■: i tt3 (: j ,: liter): · ^ ^ 5fe- A.iieisens' .- iure at 1CO liter GnUiOnISXeI 1 IeHi / ASCER ner / j, estellt whose Served 1 , 1 jj (^ 0 A j) oetruj ,.
ßs wurden 11,^ Liter der Lösung A, ;■■ iii üer der ^öü<xr^ L cowic 6--C cca - ;· ;o-i6cr icsusaure ai t entionicierucn 7asser auf 1GC Liter aufgefüllt.11, ^ liters of solution A,; ■■ iii over the ^ öü <xr ^ L cowic 6 - C cca -; ·; o- i6 cr icsusaure ai t deionicierucn 7asser made up to 1GC liter.
jj aiesec ^εα, das einen p;--Vert von <_, 1 i.aoie, v.urden aus üCw.vefel'^aurer Losoni, oalvö:xiöt;n verzinnte iice.-roare em^e-.l.'iJCn 1; see v'er.veilr:ext wurde c-^e .icre ^erausgenoirujj aiesec ^ εα, the one p; - vert of <_, 1 i.aoie, v. were from üCw.vefel '^ aurer Losoni, o alvö: xiöt; n tinned iice.-roare em ^ e-.l .'iJCn 1; see v'er.veilr: ext was c- ^ e .icre ^ erausgenoiru
309830/ 1018
BAD ORIGINAL309830/1018
BATH ORIGINAL
i/er erhaltene olivi'arbene ÜDerzu^ erwj.ec sicn alL· belli· ι'ε^π-kris ualliri, in ieuenteiu Zustand wisch- und iiraL^IeaL one iu XToc^eneii Zus uaiid als senr iesi hai'Lejid, sjo da;.;. die ;.:ol,rfc" cebo^en werden konnten, ohne α au ar: der uie^emelle der überzug aopulverle.i / he received olivi'arbene ÜDerzu ^ erwj.ec sicn alL · belli · ι'ε ^ π-kris ualliri, in ieuenteiu state wisch- and iiraL ^ IeaL one iu XToc ^ eneii Zus uaiid as senr iesi hai'Lejid, sjo there;. ; . the;.: ol, rfc " c ebo ^ en could be without α au ar: the uie ^ emelle the coating aopulverle.
Luc ;iad wuroe mi L euieiii j;igi tal-pli-ikieu^ei'ü. l KO üuerwael.L. i.achdeai der pH-.Verl aui" ^,7 angestiegen war, wurde erneut i'nscue Lccun^ zu^e^eben. Aiι L diese.α üad konnten kon-, Linuierlicii iloer längere Zeit Eisenrohre cnromutiert werden, ohne daU sich eine Qualitäts- oder i'aruanuerun,^ ueun üuerzaf;Luc; iad wuroe mi L euieiii j; igi tal-pli-ikieu ^ ei'ü. l KO üuerwael.L. After the pH-loss had risen to 7, it again became e. As a result, iron pipes could be chromated for a longer period of time without disrupting themselves a quality or i'aruanuerun, ^ ueun üuerza f ;
-Ja beil ua-Yes, among other things
309830/ 1018309830/1018
;AD; AD
Claims (1)
Priority Applications (6)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| DE19722202457 DE2202457C3 (en) | 1972-01-19 | Process for the chromating of objects provided with galvanic zinc coatings | |
| JP4170572A JPS5427300B2 (en) | 1972-01-19 | 1972-04-25 | |
| GB1917972A GB1328938A (en) | 1972-01-19 | 1972-04-25 | Electroless chromium plating process |
| IT2426572A IT955451B (en) | 1972-01-19 | 1972-05-12 | PROCEDURE FOR THE CHROME PLATING OF OBJECTS EQUIPPED WITH ZINC GALVANIC COATINGS |
| CA144,852A CA956056A (en) | 1972-01-19 | 1972-06-15 | Electroless chromium plating process |
| FR7221699A FR2168273B1 (en) | 1972-01-19 | 1972-06-16 |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| DE19722202457 DE2202457C3 (en) | 1972-01-19 | Process for the chromating of objects provided with galvanic zinc coatings |
Publications (3)
| Publication Number | Publication Date |
|---|---|
| DE2202457A1 true DE2202457A1 (en) | 1973-07-26 |
| DE2202457B2 DE2202457B2 (en) | 1977-04-21 |
| DE2202457C3 DE2202457C3 (en) | 1977-12-08 |
Family
ID=
Also Published As
| Publication number | Publication date |
|---|---|
| DE2202457B2 (en) | 1977-04-21 |
| FR2168273B1 (en) | 1976-08-06 |
| CA956056A (en) | 1974-10-15 |
| JPS5427300B2 (en) | 1979-09-08 |
| FR2168273A1 (en) | 1973-08-31 |
| GB1328938A (en) | 1973-09-05 |
| JPS4890938A (en) | 1973-11-27 |
| IT955451B (en) | 1973-09-29 |
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Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C3 | Grant after two publication steps (3rd publication) | ||
| E77 | Valid patent as to the heymanns-index 1977 | ||
| 8339 | Ceased/non-payment of the annual fee |