EP0516652B1 - Bäder und verfahren zum chemischen polieren von rostfreien stahloberflächen - Google Patents

Bäder und verfahren zum chemischen polieren von rostfreien stahloberflächen Download PDF

Info

Publication number
EP0516652B1
EP0516652B1 EP91903564A EP91903564A EP0516652B1 EP 0516652 B1 EP0516652 B1 EP 0516652B1 EP 91903564 A EP91903564 A EP 91903564A EP 91903564 A EP91903564 A EP 91903564A EP 0516652 B1 EP0516652 B1 EP 0516652B1
Authority
EP
European Patent Office
Prior art keywords
acid
baths
mole
polishing
baths according
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 - Lifetime
Application number
EP91903564A
Other languages
English (en)
French (fr)
Other versions
EP0516652A1 (de
Inventor
Marianne Reignier
François Dujardin
Léopold DIMARTINELLY
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.)
Solvay SA
Original Assignee
Solvay SA
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 Solvay SA filed Critical Solvay SA
Publication of EP0516652A1 publication Critical patent/EP0516652A1/de
Application granted granted Critical
Publication of EP0516652B1 publication Critical patent/EP0516652B1/de
Anticipated expiration legal-status Critical
Expired - Lifetime legal-status Critical Current

Links

Classifications

    • CCHEMISTRY; METALLURGY
    • C23COATING 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
    • C23FNON-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
    • C23F3/00Brightening metals by chemical means
    • C23F3/04Heavy metals
    • C23F3/06Heavy metals with acidic solutions

Definitions

  • the present invention relates to the composition of baths for the chemical polishing of stainless steel surfaces.
  • Chemical polishing of metal surfaces is a well-known technique (electrolytic and chemical polishing of metals - W.J. Mc G. TEGART - Dunod - 1960 - p. 122 et seq.); it consists in treating the metal surfaces to be polished with oxidizing baths.
  • baths are generally used comprising a mixture, in aqueous solution, of hydrochloric, phosphoric and nitric acids (patent US-A-2662814).
  • suitable additives such as surfactants, viscosity regulators and brighteners.
  • a composition of a bath for the chemical polishing of stainless steel surfaces comprising, in aqueous solution, a mixture of phosphoric acid, nitric acid and acid. hydrochloric acid, a viscosity regulator chosen from water-soluble polymers, a surfactant and sulfosalicylic acid as a brightening agent.
  • the invention aims to provide baths designed to carry out slow and effective chemical polishing of stainless steel surfaces, at working temperatures below 50 ° C.
  • the invention relates to baths for the chemical polishing of stainless steel surfaces, comprising, in aqueous solution, a mixture of hydrochloric acid, nitric acid and phosphoric acid, an optionally substituted hydroxybenzoic acid, a compound abietic and an additive selected from perchloric acid and the water-soluble salts of perchloric acid.
  • hydroxybenzoic acid serves as a brightening agent. It can be unsubstituted such as salicylic acid or substituted such as sulfosalicylic acid. Salicylic acid is preferred.
  • abietic compounds are chemical compounds comprising an abietyl radical of general formula: or a hydroabietyl or dehydroabietyl radical.
  • the abietic compound must be soluble in the aqueous solution.
  • Abietic compounds which can be used in the baths according to the invention are abietamines.
  • abietamines which are very suitable in the baths according to the invention, are those in which at least one of the radicals X1 and X2 is a radical of general formula: -CH2-R2 in which R2 denotes a linear or cyclic alkyl radical, substituted or unsubstituted, saturated or unsaturated, comprising at least one carbonyl group.
  • R2 denotes a linear or cyclic alkyl radical, substituted or unsubstituted, saturated or unsaturated, comprising at least one carbonyl group.
  • substituted abietamines and the means of obtaining them are described in GB-A-734665.
  • abietamines of this type which can be used in the baths according to the invention, are those in which the alkyl residue R2 is selected from acetonyl, 2-keto butyl, 4-methyl 2-keto-pentenyl-3, 4-hydroxy 4 radicals -methyl 2-keto pentyl, 2-keto cyclopentyl, 4-hydroxy 2-keto pentenyl-3, 2-keto cyclohexyl, 2,5-diketo hexyl and 2-phenyl 2-keto ethyl.
  • the respective amounts of additive selected from perchloric acid and its water-soluble salts, on the one hand, and of abietic compound, on the other hand, should be adjusted to make coadsorption possible. on the surface of the steel to be polished, while avoiding exceeding their solubility product.
  • the baths according to the invention contain, per liter, between 0.001 and 0.5 mole of the additive selected from perchloric acid and its water-soluble salts and between 0.005 and 1 g of the abietic compound.
  • the polishing baths according to the invention may optionally contain additives usually present in baths known for the chemical polishing of metals, for example surfactants, alcohols and viscosity regulators. They may in particular include products of the DEHYQUART brand (Henkel), which are surfactants selected from alkylpyridinium salts and quaternary ammonium salts, comprising substituted or unsubstituted alkyl, phenyl or benzyl radicals.
  • additives usually present in baths known for the chemical polishing of metals for example surfactants, alcohols and viscosity regulators. They may in particular include products of the DEHYQUART brand (Henkel), which are surfactants selected from alkylpyridinium salts and quaternary ammonium salts, comprising substituted or unsubstituted alkyl, phenyl or benzyl radicals.
  • the baths according to the invention are suitable for the chemical polishing of all austenitic stainless steel surfaces. They are specially adapted for polishing austenitic steels containing between 16 and 26% by weight of chromium and between 6 and 22% by weight of nickel, such as steels of grade 18/8 and 18/10, free of molybdenum (AISI standard -304 and 304L).
  • the baths according to the invention have the particularity of polishing such steels at low speed, generally requiring a contact time of between 2 and 20 hours, generally between 5 and 12 hours. They can be used at all temperatures between 20 ° C and the boiling temperature.
  • the baths according to the invention have the additional advantage of performing good quality polishing of welded assemblies according to the rules of the art.
  • the invention also relates to a method for polishing a stainless steel surface, according to which the surface is placed in contact with a chemical polishing bath according to the invention.
  • the contacting of the metal surface with the bath can be carried out in any suitable manner, for example by immersion.
  • the contact time of the surface to be polished with the bath must be sufficient to achieve effective polishing of the surface. However, it cannot exceed a critical value beyond which the bath loses its polishing properties.
  • the optimum contact time depends on many parameters such as the grade of the steel, the configuration and the initial roughness of the surface to be polished, the composition of the bath, the working temperature, the possible agitation of the bath in contact with the surface, the ratio between the area of the surface to be polished and the volume of the bath; it must be determined in each particular case by routine laboratory work.
  • the bath is carried out at a temperature between 20 and 50 ° C, preferably between 35 and 45 ° C, at normal atmospheric pressure, and the surface to be polished in contact with the bath for a time between 5 and 12 hours.
  • the operating conditions were as follows: . bath volume 1940 cm3, . surface area subject to polishing 87 cm2, . temperature 35 ° C, . duration of immersion 11:00.
  • the appearance of the surface is satin.
  • the operating conditions were as follows: . bath volume 970 cc, . surface area subject to polishing 43 cm2, . temperature 35 ° C, . duration of immersion 12 hours.
  • the operating conditions were as follows: . bath volume 970 cc, . surface area subject to polishing 43 cm2, . temperature 35 ° C, . duration of immersion 9 hours, 30 minutes.

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)
  • ing And Chemical Polishing (AREA)
  • Cleaning And De-Greasing Of Metallic Materials By Chemical Methods (AREA)
  • Finish Polishing, Edge Sharpening, And Grinding By Specific Grinding Devices (AREA)
  • Chemical Treatment Of Metals (AREA)

Claims (10)

  1. Bäder zum chemischen Polieren von rostfreien Stahloberflächen, die in wässriger Lösung eine Mischung aus Salzsäure, Salpetersäure und Phosphorsäure, ein Glanzmittel, ausgewählt unter den gegebenenfalls substituierten Hydroxybenzoesäuren, und eine Abietin-Verbindung umfassen, dadurch gekennzeichnet, daß sie ein Zusatzmittel, ausgewählt unter Perchlorsäure und den wasserlöslichen Salzen der Perchlorsäure, in einer Menge zwischen 0,001 und 0,5 Mol pro Liter Lösung umfassen, wobei die Abietin-Verbindung in einer Menge zwischen 0,005 und 1 g pro Liter Lösung vorhanden ist.
  2. Bäder nach Anspruch 1, dadurch gekennzeichnet, daß die Hydroxybenzoesäure Salicylsäure ist.
  3. Bäder nach Anspruch 1, dadurch gekennzeichnet, daß die substituierte Hydroxybenzoesäure Sulfosalicylsäure ist.
  4. Bäder nach einem der Ansprüche 1 bis 3, dadurch gekennzeichnet, daß die Abietin-Verbindung ein substituiertes Abietamin der allgemeinen Formel:
    Figure imgb0007
    ist, in der
    - R₁ einen Abietyl-, Hydroabietyl- oder Dehydroabietylrest darstellt,
    - X₁ einen wenigstens eine Carbonylgruppe umfassenden Rest darstellt, und
    - X₂ ein Wasserstoffatom oder einen wenigstens eine Carbonylgruppe umfassenden Rest darstellt.
  5. Bäder nach Anspruch 4, dadurch gekennzeichnet, daß wenigstens einer der Reste X₁ und X₂ ein Rest der allgemeinen Formel:



            - CH₂-R₂



    ist, in der R₂ einen linearen oder zyklischen, substituierten oder nicht substituierten, gesättigten oder ungesättigten Alkylrest mit wenigstens einer Carbonylgruppe darstellt.
  6. Bäder nach Anspruch 5, dadurch gekennzeichnet, daß der Alkylrest R₂ ausgewählt ist unter den Acetonyl-, 2-Ketobutyl-, 4-Methyl-2-keto-pentenyl-3-, 4-Hydroxy-4-methyl-2-keto-pentyl-, 2-Keto-cyclopentyl-, 4-Hydroxy-2-keto-pentenyl-3-, 2-Keto-cyclohexyl-, 2,5-Diketo-hexyl- und 2-Phenyl-2-keto-ethylresten.
  7. Bäder nach einem der Ansprüche 1 bis 6, dadurch gekennzeichnet, daß sie pro Liter wässriger Lösung:
    - zwischen 0,5 und 5 Mol Salzsäure,
    - zwischen 0,005 und 1 Mol Salpetersäure
    - zwischen 0,005 und 1 Mol Phosphorsäure,
    - zwischen 0,0005 und 0,5 Mol des Zusatzstoffes, ausgewählt unter Perchlorsäure und ihren wasserlöslichen Salzen,
    - zwischen 0,005 und 1 g Abietin-Verbindung,
    - zwischen 0,001 und 5 g substituierter oder nicht substituierter Hydroxybenzoesäure.
    umfassen.
  8. Bäder nach einem der Ansprüche 1 bis 7 zum chemischen Polieren von Oberflächen aus Austenitstahl.
  9. Bäder nach Anspruch 8 zum chemischen Polieren von Oberflächen aus Austenitstählen und molybdänfreien Chrom- und Nickellegierungen.
  10. Verfahren zum chemischen Polieren einer Oberfläche aus rostfreiem Stahl, gemäß dem man die Oberfläche mit einem chemischen Polierbad in Verbindung bringt, dadurch gekennzeichnet, daß man ein Bad gemäß einem der Ansprüche 1 bis 9 einsetzt, das man bei einer Temperatur zwischen 20 und 50°C hält.
EP91903564A 1990-02-23 1991-02-18 Bäder und verfahren zum chemischen polieren von rostfreien stahloberflächen Expired - Lifetime EP0516652B1 (de)

Applications Claiming Priority (3)

Application Number Priority Date Filing Date Title
BE9000212A BE1003671A3 (fr) 1990-02-23 1990-02-23 Bains et procede pour le polissage chimique de surfaces en acier inoxydable.
BE9000212 1990-02-23
PCT/BE1991/000011 WO1991013188A1 (fr) 1990-02-23 1991-02-18 Bains et procede pour le polissage chimique de surfaces en acier inoxydable

Publications (2)

Publication Number Publication Date
EP0516652A1 EP0516652A1 (de) 1992-12-09
EP0516652B1 true EP0516652B1 (de) 1994-09-21

Family

ID=3884688

Family Applications (1)

Application Number Title Priority Date Filing Date
EP91903564A Expired - Lifetime EP0516652B1 (de) 1990-02-23 1991-02-18 Bäder und verfahren zum chemischen polieren von rostfreien stahloberflächen

Country Status (20)

Country Link
EP (1) EP0516652B1 (de)
JP (1) JPH05504171A (de)
KR (1) KR920703875A (de)
CN (1) CN1054277A (de)
AT (1) ATE111972T1 (de)
BE (1) BE1003671A3 (de)
BG (1) BG60923B1 (de)
BR (1) BR9106053A (de)
CA (1) CA2076398A1 (de)
CS (1) CS47991A2 (de)
DE (1) DE69104188T2 (de)
ES (1) ES2065000T3 (de)
HU (1) HU212489B (de)
MY (1) MY106554A (de)
PL (1) PL166062B1 (de)
PT (1) PT96850A (de)
RU (1) RU2060302C1 (de)
SG (1) SG20095G (de)
WO (1) WO1991013188A1 (de)
YU (1) YU47807B (de)

Families Citing this family (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
BE1012670A3 (fr) * 1999-05-07 2001-02-06 Solvay Bains et procede pour le polissage chimique de surfaces en acier inoxydable.
CN104911686A (zh) * 2015-06-04 2015-09-16 上海大学兴化特种不锈钢研究院 提高304l不锈钢耐点蚀性能的磁调控表面处理方法
CN107460484B (zh) * 2017-07-13 2019-10-11 飞而康快速制造科技有限责任公司 用于抛光镍基合金工件内流道的抛光试剂、方法及系统

Family Cites Families (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS4829455B1 (de) * 1967-03-23 1973-09-10
SU1105292A1 (ru) * 1982-07-30 1984-07-30 Московский ордена Ленина и ордена Трудового Красного Знамени химико-технологический институт им.Д.И.Менделеева Раствор дл удалени никелевых покрытий,нанесенных химическим способом
SU1239172A1 (ru) * 1984-06-29 1986-06-23 Предприятие П/Я Г-4517 Раствор дл химического травлени нержавеющих сталей
FR2608173B1 (fr) * 1986-12-15 1993-07-16 Solvay Bains et procede pour le polissage chimique de surfaces en acier inoxydable

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
Chemical Abstracts, vol. 80, No. 14, 8 April 1979, Columbus, Ohio, US, see page 157, abstract 73166y; & JP-B-73 029 455 *

Also Published As

Publication number Publication date
PL166062B1 (pl) 1995-03-31
BE1003671A3 (fr) 1992-05-19
RU2060302C1 (ru) 1996-05-20
MY106554A (en) 1995-06-30
YU29891A (sh) 1993-11-16
ATE111972T1 (de) 1994-10-15
SG20095G (en) 1995-08-18
YU47807B (sr) 1996-01-09
PT96850A (pt) 1991-10-31
EP0516652A1 (de) 1992-12-09
BG96809A (bg) 1993-12-24
HU212489B (en) 1996-07-29
KR920703875A (ko) 1992-12-18
WO1991013188A1 (fr) 1991-09-05
BG60923B1 (bg) 1996-06-28
DE69104188D1 (de) 1994-10-27
JPH05504171A (ja) 1993-07-01
DE69104188T2 (de) 1995-05-04
CN1054277A (zh) 1991-09-04
HUT63468A (en) 1993-08-30
CA2076398A1 (fr) 1991-08-24
BR9106053A (pt) 1992-11-24
ES2065000T3 (es) 1995-02-01
CS47991A2 (en) 1991-11-12

Similar Documents

Publication Publication Date Title
EP0462646B1 (de) Bäder und Verfahren zum chemischen Polieren von Oberflächen aus rostfreiem Stahl
EP0516653B1 (de) Bäder und verfahren zum chemischen polieren von rostfreien stahloberflächen
EP0425012B1 (de) Bäder und Verfahren zum chemischen Polieren von Kupfer- oder Kupferlegierung-Oberflächen
EP0516652B1 (de) Bäder und verfahren zum chemischen polieren von rostfreien stahloberflächen
EP0206386B1 (de) Lösungen und Verfahren zum chemischen Polieren von Oberflächen von rostfreien Stahlen
EP0274776B1 (de) Bäder und Verfahren zum chemischen Polieren von rostfreien Stahloberflächen
EP0193239B1 (de) Zusammensetzungen und Verfahren zum chemischen Polieren von Stahloberflächen
EP0753083B1 (de) Bäder und verfahren zum chemischen polieren von rostfreien stahloberflächen
EP0309031A1 (de) Bäden und Verfahren zum chemischen Polieren von Oberflächen aus Kupfer oder Kupferlegierungen
BE1012670A3 (fr) Bains et procede pour le polissage chimique de surfaces en acier inoxydable.
US5135610A (en) Baths and process for chemical polishing of stainless steel surfaces
BE1003579A3 (fr) Bains et procede pour le polissage chimique de surfaces en acier inxoydable.

Legal Events

Date Code Title Description
PUAI Public reference made under article 153(3) epc to a published international application that has entered the european phase

Free format text: ORIGINAL CODE: 0009012

17P Request for examination filed

Effective date: 19920814

AK Designated contracting states

Kind code of ref document: A1

Designated state(s): AT BE CH DE DK ES FR GB GR IT LI LU NL SE

17Q First examination report despatched

Effective date: 19931015

RAP1 Party data changed (applicant data changed or rights of an application transferred)

Owner name: SOLVAY (SOCIETE ANONYME)

GRAA (expected) grant

Free format text: ORIGINAL CODE: 0009210

AK Designated contracting states

Kind code of ref document: B1

Designated state(s): AT BE CH DE DK ES FR GB GR IT LI LU NL SE

PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: DK

Effective date: 19940921

Ref country code: AT

Effective date: 19940921

REF Corresponds to:

Ref document number: 111972

Country of ref document: AT

Date of ref document: 19941015

Kind code of ref document: T

REF Corresponds to:

Ref document number: 69104188

Country of ref document: DE

Date of ref document: 19941027

ITF It: translation for a ep patent filed
GBT Gb: translation of ep patent filed (gb section 77(6)(a)/1977)

Effective date: 19941213

EAL Se: european patent in force in sweden

Ref document number: 91903564.2

REG Reference to a national code

Ref country code: ES

Ref legal event code: FG2A

Ref document number: 2065000

Country of ref document: ES

Kind code of ref document: T3

PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: LU

Free format text: LAPSE BECAUSE OF NON-PAYMENT OF DUE FEES

Effective date: 19950228

Ref country code: LI

Effective date: 19950228

Ref country code: CH

Effective date: 19950228

REG Reference to a national code

Ref country code: GR

Ref legal event code: FG4A

Free format text: 3014416

PLBE No opposition filed within time limit

Free format text: ORIGINAL CODE: 0009261

STAA Information on the status of an ep patent application or granted ep patent

Free format text: STATUS: NO OPPOSITION FILED WITHIN TIME LIMIT

26N No opposition filed
PGFP Annual fee paid to national office [announced via postgrant information from national office to epo]

Ref country code: SE

Payment date: 19960124

Year of fee payment: 6

PGFP Annual fee paid to national office [announced via postgrant information from national office to epo]

Ref country code: FR

Payment date: 19960125

Year of fee payment: 6

PGFP Annual fee paid to national office [announced via postgrant information from national office to epo]

Ref country code: BE

Payment date: 19960129

Year of fee payment: 6

PGFP Annual fee paid to national office [announced via postgrant information from national office to epo]

Ref country code: GR

Payment date: 19960130

Year of fee payment: 6

PGFP Annual fee paid to national office [announced via postgrant information from national office to epo]

Ref country code: GB

Payment date: 19960209

Year of fee payment: 6

PGFP Annual fee paid to national office [announced via postgrant information from national office to epo]

Ref country code: ES

Payment date: 19960219

Year of fee payment: 6

PGFP Annual fee paid to national office [announced via postgrant information from national office to epo]

Ref country code: DE

Payment date: 19960227

Year of fee payment: 6

PGFP Annual fee paid to national office [announced via postgrant information from national office to epo]

Ref country code: NL

Payment date: 19960229

Year of fee payment: 6

PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: GB

Effective date: 19970218

PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: SE

Effective date: 19970219

Ref country code: ES

Free format text: LAPSE BECAUSE OF NON-PAYMENT OF DUE FEES

Effective date: 19970219

PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: BE

Effective date: 19970228

BERE Be: lapsed

Owner name: S.A. SOLVAY

Effective date: 19970228

PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: GR

Free format text: THE PATENT HAS BEEN ANNULLED BY A DECISION OF A NATIONAL AUTHORITY

Effective date: 19970831

PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: NL

Effective date: 19970901

REG Reference to a national code

Ref country code: GR

Ref legal event code: MM2A

Free format text: 3014416

GBPC Gb: european patent ceased through non-payment of renewal fee

Effective date: 19970218

PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: FR

Effective date: 19971030

PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: DE

Effective date: 19971101

EUG Se: european patent has lapsed

Ref document number: 91903564.2

NLV4 Nl: lapsed or anulled due to non-payment of the annual fee

Effective date: 19970901

REG Reference to a national code

Ref country code: FR

Ref legal event code: ST

REG Reference to a national code

Ref country code: ES

Ref legal event code: FD2A

Effective date: 19990301

PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: IT

Free format text: LAPSE BECAUSE OF NON-PAYMENT OF DUE FEES;WARNING: LAPSES OF ITALIAN PATENTS WITH EFFECTIVE DATE BEFORE 2007 MAY HAVE OCCURRED AT ANY TIME BEFORE 2007. THE CORRECT EFFECTIVE DATE MAY BE DIFFERENT FROM THE ONE RECORDED.

Effective date: 20050218