EP0193239B1 - Bains et procédé pour le polissage chimique de surfaces en acier - Google Patents
Bains et procédé pour le polissage chimique de surfaces en acier Download PDFInfo
- Publication number
- EP0193239B1 EP0193239B1 EP86200262A EP86200262A EP0193239B1 EP 0193239 B1 EP0193239 B1 EP 0193239B1 EP 86200262 A EP86200262 A EP 86200262A EP 86200262 A EP86200262 A EP 86200262A EP 0193239 B1 EP0193239 B1 EP 0193239B1
- Authority
- EP
- European Patent Office
- Prior art keywords
- baths
- mol
- aqueous solution
- ferricyanide
- bath
- 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
- 238000005498 polishing Methods 0.000 title claims abstract description 47
- 229910000831 Steel Inorganic materials 0.000 title claims abstract description 13
- 239000010959 steel Substances 0.000 title claims abstract description 13
- 239000000203 mixture Substances 0.000 title claims description 18
- 238000000034 method Methods 0.000 title claims description 15
- 230000008569 process Effects 0.000 title claims description 6
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 26
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims abstract description 26
- 239000007864 aqueous solution Substances 0.000 claims abstract description 21
- 239000000126 substance Substances 0.000 claims abstract description 19
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims abstract description 15
- 150000002500 ions Chemical class 0.000 claims abstract description 15
- YAGKRVSRTSUGEY-UHFFFAOYSA-N ferricyanide Chemical compound [Fe+3].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-] YAGKRVSRTSUGEY-UHFFFAOYSA-N 0.000 claims abstract description 14
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims abstract description 13
- 229910017604 nitric acid Inorganic materials 0.000 claims abstract description 13
- -1 potassium ferricyanide Chemical compound 0.000 claims description 13
- 239000000243 solution Substances 0.000 claims description 13
- 239000002253 acid Substances 0.000 claims description 9
- 239000004094 surface-active agent Substances 0.000 claims description 8
- 150000007513 acids Chemical class 0.000 claims description 5
- XMBWDFGMSWQBCA-UHFFFAOYSA-N hydrogen iodide Chemical compound I XMBWDFGMSWQBCA-UHFFFAOYSA-N 0.000 claims description 4
- ZMZDMBWJUHKJPS-UHFFFAOYSA-N hydrogen thiocyanate Natural products SC#N ZMZDMBWJUHKJPS-UHFFFAOYSA-N 0.000 claims description 4
- CPELXLSAUQHCOX-UHFFFAOYSA-M Bromide Chemical compound [Br-] CPELXLSAUQHCOX-UHFFFAOYSA-M 0.000 claims description 3
- 150000001450 anions Chemical class 0.000 claims description 3
- XFXPMWWXUTWYJX-UHFFFAOYSA-N Cyanide Chemical compound N#[C-] XFXPMWWXUTWYJX-UHFFFAOYSA-N 0.000 claims description 2
- 229920003086 cellulose ether Polymers 0.000 claims description 2
- 150000001805 chlorine compounds Chemical class 0.000 claims description 2
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 abstract description 14
- 229910001220 stainless steel Inorganic materials 0.000 abstract description 9
- 239000010935 stainless steel Substances 0.000 abstract description 8
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 abstract description 7
- 229910052804 chromium Inorganic materials 0.000 abstract description 7
- 239000011651 chromium Substances 0.000 abstract description 7
- 229910052759 nickel Inorganic materials 0.000 abstract description 7
- 229910052751 metal Inorganic materials 0.000 description 14
- 239000002184 metal Substances 0.000 description 14
- 239000000654 additive Substances 0.000 description 7
- 230000009471 action Effects 0.000 description 3
- 239000003795 chemical substances by application Substances 0.000 description 3
- 238000005260 corrosion Methods 0.000 description 3
- 230000007797 corrosion Effects 0.000 description 3
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 2
- ZMZDMBWJUHKJPS-UHFFFAOYSA-M Thiocyanate anion Chemical compound [S-]C#N ZMZDMBWJUHKJPS-UHFFFAOYSA-M 0.000 description 2
- 230000000996 additive effect Effects 0.000 description 2
- 229910052784 alkaline earth metal Inorganic materials 0.000 description 2
- 229910000963 austenitic stainless steel Inorganic materials 0.000 description 2
- 230000008901 benefit Effects 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 150000002739 metals Chemical class 0.000 description 2
- 229910052700 potassium Inorganic materials 0.000 description 2
- 239000011591 potassium Substances 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- WXHLLJAMBQLULT-UHFFFAOYSA-N 2-[[6-[4-(2-hydroxyethyl)piperazin-1-yl]-2-methylpyrimidin-4-yl]amino]-n-(2-methyl-6-sulfanylphenyl)-1,3-thiazole-5-carboxamide;hydrate Chemical compound O.C=1C(N2CCN(CCO)CC2)=NC(C)=NC=1NC(S1)=NC=C1C(=O)NC1=C(C)C=CC=C1S WXHLLJAMBQLULT-UHFFFAOYSA-N 0.000 description 1
- 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 description 1
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 description 1
- 230000006978 adaptation Effects 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 229910052783 alkali metal Inorganic materials 0.000 description 1
- 229910001513 alkali metal bromide Inorganic materials 0.000 description 1
- 229910001516 alkali metal iodide Inorganic materials 0.000 description 1
- 150000001340 alkali metals Chemical class 0.000 description 1
- 150000001342 alkaline earth metals Chemical class 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 239000011260 aqueous acid Substances 0.000 description 1
- 230000000712 assembly Effects 0.000 description 1
- 238000000429 assembly Methods 0.000 description 1
- 239000011324 bead Substances 0.000 description 1
- 238000005282 brightening Methods 0.000 description 1
- 239000001913 cellulose Substances 0.000 description 1
- 229920002678 cellulose Polymers 0.000 description 1
- 239000000470 constituent Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 238000011065 in-situ storage Methods 0.000 description 1
- 239000003112 inhibitor Substances 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 238000012423 maintenance Methods 0.000 description 1
- 238000005272 metallurgy Methods 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229910052750 molybdenum Inorganic materials 0.000 description 1
- 239000011733 molybdenum Substances 0.000 description 1
- 150000002825 nitriles Chemical class 0.000 description 1
- 239000002736 nonionic surfactant Substances 0.000 description 1
- 239000006259 organic additive Substances 0.000 description 1
- 239000000276 potassium ferrocyanide Substances 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- XOGGUFAVLNCTRS-UHFFFAOYSA-N tetrapotassium;iron(2+);hexacyanide Chemical compound [K+].[K+].[K+].[K+].[Fe+2].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-] XOGGUFAVLNCTRS-UHFFFAOYSA-N 0.000 description 1
- 239000002562 thickening agent Substances 0.000 description 1
- YARHBRUWMYJLHY-UHFFFAOYSA-Q triazanium;iron(3+);hexacyanide Chemical compound [NH4+].[NH4+].[NH4+].[Fe+3].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-] YARHBRUWMYJLHY-UHFFFAOYSA-Q 0.000 description 1
- 229920003169 water-soluble polymer Polymers 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
- C23F3/00—Brightening metals by chemical means
- C23F3/04—Heavy metals
- C23F3/06—Heavy metals with acidic solutions
Definitions
- the present invention relates to the composition of baths for the chemical polishing of steel surfaces, in particular stainless steel.
- 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 d hydrochloric acid, a viscosity regulator chosen from water-soluble polymers, a surfactant and sulfosalicylic acid as a brightening agent.
- This known polishing bath has proven to be very effective. However, it has the disadvantage of containing several organic additives, which add to the cost, complicate its implementation and constitute a source of pollution during the rejection of the spent bath.
- a bath of simpler composition for the chemical polishing of steels, this bath comprising, in aqueous solution, a mixture of hydrochloric acid, phosphoric acid and nitric acid, potassium ferrocyanide and the surfactant OP- 7 which is a nonionic surfactant from the family of alkylphenols (Central Patents Index, Basic Abstracts Journal, section E, Derwent Publications Ltd, London, abbreviated 13581 U-EM: Soviet author's certificate SU-344 035).
- this known bath has however proved powerless to achieve uniform polishing, of good quality.
- the known polishing baths which have just been described have the common characteristic of attacking the metal at very high speed.
- a polishing treatment of a steel surface with such baths can generally not exceed a few minutes, at the risk of causing local corrosion.
- This high speed of action of known polishing baths is a drawback, because it makes them unusable for certain applications, in particular for polishing the internal face of the walls of large tanks, such as boilers, autoclaves or crystallizers .
- the time required for filling and emptying such tanks being generally much greater than the duration of the optimum chemical polishing treatment, it indeed becomes impossible to obtain a uniform polish of the wall, certain areas of the latter being insufficiently others are deeply corroded.
- the high speed of action of known chemical polishing baths also makes polishing control difficult. These known baths are also ineffective for polishing surfaces in contact with which the renewal of the bath is difficult, since this results in abrupt modifications to the local compositions of the bath.
- the object of the present invention is to remedy the aforementioned drawbacks of known polishing baths, by providing bath compositions for the chemical polishing of austenitic stainless steel surfaces, in particular steel alloyed with chromium and nickel, which make it possible to avoid the use of multiple additives, which are effective in all types of application including the polishing of large surfaces or surfaces that are difficult to access and which make it possible to produce polishes of excellent quality.
- the invention therefore relates to baths for the chemical polishing of steel surfaces, comprising, in aqueous solution, a mixture of hydrochloric acid, phosphoric acid and nitric acid; according to the invention, the baths comprise, in the aqueous solution, ferricyanide complex ions.
- the ferricyanide complex ions are complex cyanides of general formula [Fe lil (CN) 6] 3- , also called hexacyanoferrates (III) (Encyclopedia of Chemical Technology - Kirk-Othmer - John Wiley & Sons , Inc. - 1967 - Vol. 12 - pages 25, 26, 31, 32). They can be present in the aqueous solution in the form of any dissolved compounds such as, for example, hexacyanoferric acid (III), ammonium ferricyanide and ferricyanides of alkali and alkaline earth metals. Preferred compounds are the alkali metal ferricyanides, potassium ferricyanide being especially recommended.
- Preferred baths are those which are essentially free of such additives.
- these contain anions selected from the bromide, iodide and thiocyanate ions.
- These anions can generally be used in the state of alkali metal bromide, iodide or thiocyanate, the latter advantageously being sodium.
- the baths according to this embodiment of the invention have proved to be particularly advantageous for the polishing of welded assemblies, at the level of the weld beads. The best results are obtained for contents of bromide anion, iodide or thiocyanate comprised between 10-5 and 1 gram-ion per liter, the contents of between 10- 4 and 10- 2 gram-ion per liter being preferred.
- the baths according to the invention are suitable for polishing all austenitic stainless steel surfaces. They find a particularly advantageous application in the polishing of austenitic stainless steels alloyed with chromium and nickel, in particular those containing between 12 and 26% of chromium and between 6 and 22% of nickel, such as steels 18/8 and 18/10 , for example.
- the invention therefore also relates to a method for polishing a steel surface, according to which the surface is brought into contact with a chemical polishing bath according to the invention.
- a prefabricated bath can be used, in contact with which the metal surface to be polished is then placed.
- the metal surface is first brought into contact with an aqueous solution of hydrochloric acid, phosphoric acid and nitric acid, then added complex ferricyanide ions to the solution, while it is in contact with the metal surface.
- 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 local corrosions may appear on the surface.
- the optimum contact time depends on many parameters such as the metal or alloy constituting the surface to be polished, the configuration and initial roughness thereof, the composition of the bath, the working temperature, the possible turbulence of the bath in contact with the surface, the ratio between the area of the metal surface to be polished and the volume of the bath used; it must be determined in each particular case by routine laboratory work.
- the surface to be polished is brought into contact with the aqueous acid solution at a temperature between 15 and 70 ° C. preferably 20 and 55 ° C., the ferricyanide complex ions are added to said solution after having maintained the surface in contact for at least 15 minutes, and then the maintenance of the surface in contact with the resulting bath is continued for a time at least equal 1 hour.
- the addition of the ferricyanide complex ions to the acid solution can for example be carried out after the surface to be polished has been kept in contact with said solution for a time between 30 and 60 minutes and the resulting bath can then be kept in contact with the surface for a time between 6 and 24 hours.
- a chemical polishing bath in accordance with the invention was used to polish the internal face of a spherical stainless steel tank with a capacity of 6 m 3 and a diameter of 2.4 m, made of stainless steel of grade ASTM-316L , which is a steel alloyed with chromium (16.0 to 18.0% nickel (10.0 to 14.0% and molybdenum (2.0 to 3.0% (Engineering techniques - Metallurgy -M 323A-8 (Table G) - July 1983).
- the bath used had the following composition: Mixture of acids:
- the bath was introduced into the tank, at a rate of 3.9 per dm 2 of surface to be polished, and it was subjected to a stirring movement therein by means of a three-blade agitator, while maintaining its temperature between 45 and 50 ° C.
- the tank was drained and rinsed with demineralized water.
- a chemical polishing bath in accordance with the invention was used to polish the external surface of the tubes of a tubular heat exchanger made of stainless steel 1.9 m in diameter and 6 m in length.
- This exchanger was equipped with 455 tubes of 50 mm in diameter and 9 baffles made, like the ferrule, in stainless steel grade ASTM-304L, which is a steel alloyed with chromium (18.0 to 20.0%) and Nickel (8.0 to 12.0%) (Techniques de l'In distributedur Métallurgie-M.323A - 8 (Table G) July 1983).
- the bath used had the following composition: Mixture of acids in aqueous solution
- This bath was introduced into a shuttle circuit at the rate of 1.3 per dm 2 of surface to be polished and it was subjected to a linear passage movement over the surfaces to be treated by means of a circulation pump, while maintaining its temperature between 45 and 50 C by injecting steam inside the tubes.
- This bath made it possible to chemically polish, almost perfectly, the outside surface of the tube bundle.
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)
- Macromolecular Compounds Obtained By Forming Nitrogen-Containing Linkages In General (AREA)
- Polyethers (AREA)
- Artificial Filaments (AREA)
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
AT86200262T ATE44553T1 (de) | 1985-03-04 | 1986-02-20 | Zusammensetzungen und verfahren zum chemischen polieren von stahloberflaechen. |
Applications Claiming Priority (2)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
FR8503263 | 1985-03-04 | ||
FR8503263A FR2578271A1 (fr) | 1985-03-04 | 1985-03-04 | Bains et procede pour le polissage chimique de surfaces en acier. |
Publications (2)
Publication Number | Publication Date |
---|---|
EP0193239A1 EP0193239A1 (fr) | 1986-09-03 |
EP0193239B1 true EP0193239B1 (fr) | 1989-07-12 |
Family
ID=9316903
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
EP86200262A Expired EP0193239B1 (fr) | 1985-03-04 | 1986-02-20 | Bains et procédé pour le polissage chimique de surfaces en acier |
Country Status (8)
Country | Link |
---|---|
US (1) | US4652340A (es) |
EP (1) | EP0193239B1 (es) |
JP (1) | JPS61217600A (es) |
AT (1) | ATE44553T1 (es) |
DE (1) | DE3664339D1 (es) |
ES (1) | ES8705930A1 (es) |
FR (1) | FR2578271A1 (es) |
PT (1) | PT82125B (es) |
Families Citing this family (7)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
BE1003579A3 (fr) * | 1989-10-26 | 1992-04-28 | Solvay | Bains et procede pour le polissage chimique de surfaces en acier inxoydable. |
US5279707A (en) * | 1992-10-23 | 1994-01-18 | Time Savers | Die discoloration remover solution and method |
US5338375A (en) * | 1993-10-18 | 1994-08-16 | Rohm And Haas Company | Use of iron salts as corrosion inhibitors in titanium vessels |
FR2717829B1 (fr) * | 1994-03-28 | 1996-05-24 | Solvay | Bains et procédé pour le polissage chimique de surfaces en acier inoxydable. |
CN108570699A (zh) * | 2018-05-16 | 2018-09-25 | 扬州虹扬科技发展有限公司 | 一种电镀前处理药剂及处理工艺 |
CN110724999B (zh) * | 2019-10-23 | 2021-09-28 | 沈阳航空航天大学 | 一种用于高Cr含量的CoCrNi多主元合金的电解液及腐蚀工艺 |
CN111876783A (zh) * | 2020-07-10 | 2020-11-03 | 山东电力工业锅炉压力容器检验中心有限公司 | 一种金相化学抛光液及在奥氏体不锈钢金相检测领域的应用 |
Family Cites Families (10)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US1809041A (en) * | 1930-02-03 | 1931-06-09 | Swann Res Inc | Inhibitor |
US2502621A (en) * | 1945-10-08 | 1950-04-04 | Menasco Mfg Company | Method of determining oxygen concentration in steel |
US2662814A (en) * | 1949-08-27 | 1953-12-15 | Diversey Corp | Method and composition for chemically polishing metals |
LU30914A1 (es) * | 1950-10-27 | |||
LU38281A1 (es) * | 1959-03-09 | |||
US3457107A (en) * | 1965-07-20 | 1969-07-22 | Diversey Corp | Method and composition for chemically polishing metals |
FR2457315A1 (fr) * | 1979-05-25 | 1980-12-19 | Solvay | Bain pour le polissage chimique de surfaces en acier |
FR2465010A1 (fr) * | 1979-09-17 | 1981-03-20 | Solvay | Procede pour inhiber la corrosion d'une installation metallique au contact d'un bain acide |
FR2476146A1 (fr) * | 1980-02-20 | 1981-08-21 | Solvay | Bain pour l'elimination d'une pellicule de magnetite d'une surface metallique |
US4289576A (en) * | 1980-05-27 | 1981-09-15 | Halliburton Company | Method for removing cobalt-containing deposits from surfaces |
-
1985
- 1985-03-04 FR FR8503263A patent/FR2578271A1/fr not_active Withdrawn
-
1986
- 1986-02-20 AT AT86200262T patent/ATE44553T1/de not_active IP Right Cessation
- 1986-02-20 DE DE8686200262T patent/DE3664339D1/de not_active Expired
- 1986-02-20 EP EP86200262A patent/EP0193239B1/fr not_active Expired
- 1986-03-03 PT PT82125A patent/PT82125B/pt unknown
- 1986-03-03 US US06/840,749 patent/US4652340A/en not_active Expired - Lifetime
- 1986-03-03 ES ES552595A patent/ES8705930A1/es not_active Expired
- 1986-03-04 JP JP61047164A patent/JPS61217600A/ja active Granted
Also Published As
Publication number | Publication date |
---|---|
ES552595A0 (es) | 1987-05-16 |
EP0193239A1 (fr) | 1986-09-03 |
FR2578271A1 (fr) | 1986-09-05 |
ES8705930A1 (es) | 1987-05-16 |
PT82125B (pt) | 1988-04-21 |
JPS61217600A (ja) | 1986-09-27 |
PT82125A (fr) | 1986-04-01 |
DE3664339D1 (en) | 1989-08-17 |
US4652340A (en) | 1987-03-24 |
ATE44553T1 (de) | 1989-07-15 |
JPH0577751B2 (es) | 1993-10-27 |
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