US3342709A - Electrodeposition of chromium and anti-misting agents therefor - Google Patents

Electrodeposition of chromium and anti-misting agents therefor Download PDF

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Publication number
US3342709A
US3342709A US311243A US31124363A US3342709A US 3342709 A US3342709 A US 3342709A US 311243 A US311243 A US 311243A US 31124363 A US31124363 A US 31124363A US 3342709 A US3342709 A US 3342709A
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group
sulfonated
bath
chromium
alkyl
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US311243A
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Johnson Andy Albert
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M&T Chemicals Inc
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M&T Chemicals Inc
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Priority to US311243A priority Critical patent/US3342709A/en
Priority to IL22129A priority patent/IL22129A/en
Priority to FR989012A priority patent/FR1408622A/fr
Priority to GB38868/64A priority patent/GB1079647A/en
Priority to NL646411160A priority patent/NL148361B/xx
Priority to CH1238764A priority patent/CH463902A/de
Priority to DE1496904A priority patent/DE1496904C3/de
Application granted granted Critical
Publication of US3342709A publication Critical patent/US3342709A/en
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    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D3/00—Electroplating: Baths therefor
    • C25D3/02—Electroplating: Baths therefor from solutions
    • C25D3/04—Electroplating: Baths therefor from solutions of chromium
    • C25D3/10—Electroplating: Baths therefor from solutions of chromium characterised by the organic bath constituents used
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10S—TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10S516/00—Colloid systems and wetting agents; subcombinations thereof; processes of
    • Y10S516/01—Wetting, emulsifying, dispersing, or stabilizing agents
    • Y10S516/03—Organic sulfoxy compound containing
    • Y10S516/05—Organic amine, amide, or n-base containing

Definitions

  • This invention relates to chromium plating. More particularly it relates to a novel technique for suppressing the evolution of fumes from chromium plating baths.
  • chromium plating may be effected from baths which contain chromic acid and sulfate (typically introduced as sulfuric acid) together with other ingredients or additives including those which may control or regulate the plating characteristics of the bath.
  • Typical of such regulating additives may be strontium sulfate and potassium silicofluoride with or without additions of excess strontium ion (introduced as SrCO SrCrO,, etc.) of excess potassium ion (introduced as K CrO K Cr O- etc.) which may make the bath a high speed bath which is self-regulating with respect to catalyst anion.
  • the novel composition of this invention which is characterized by its ability to controllably develop and maintain over an extended period of time a fixed predetermined optimum thickness of foam may comprise an anti-misting amount of a mixture of a sulfonated 2-alkylbenzimidazole and a disulfonated alkyl diphenyl oxide.
  • chromium plating in a bath containing chromic acid and sulfate wherein substantial quantities of gas may be liberated from the electrodes by the process which comprises maintaining a chromium plating bath containing chromic acid and sulfate, maintaining therein an anti-misting amount of a mixture of a sulfonated Z-alkylbenzimidazole and a disulfonated alkyl diphenyl oxide, and plating chromium onto a cathode in said bath.
  • chromium plating baths with which this invention may be employed may commonly have the following illustrative composition.
  • novel fume suppressant or anti-misting agent of this invention may include a disulfonated alkyl diphenyl oxide, typically having the following formula:
  • R is a hydrocarbon radical having 6-18 carbon atoms
  • n is 0-1
  • X is a cation selected from the group consisting of hydrogen, ammonium and metals.
  • R radicals which may be employed may be alkyl radicals including hexyl, octyl, nonyl, dodecyl, and octadecyl radicals. preferably octyl, nonyl, and dodecyl radicals.
  • the R radicals may preferably be the same.
  • X may typically include sodium, ammonium, hydrogen, potassium, lithium, trivalent chromium, calcium, strontium, barium, magnesium, nickel, iron. and copper.
  • X may preferably be ammonium or alkali metal eg sodium, potassium, and lithium.
  • the sulfonated alkyl diphenyl oxide in the highly acid and strongly oxidizing bath is believed to exist in the form of the acid radical having the formula a. sor
  • the sulfonated alkyl diphenyl oxide as produced and utilized may be a mixture of compounds containing the noted substituents.
  • the sulfonic acid groups may be primarily substituted in the position ortho to the etherbearing carbon, and the alkyl chain may be primarily substituted in the position para to that carbon.
  • the commercial product may be a mixture of monoand dialkyl substituted products.
  • a preferred composition may be a mixture of the disulfonated salts of monododecyl diphenyl oxide and didocecyl diphenyl oxide. The disodium and dipotassium salts may be preferred.
  • the novel fume-suppressant or anti-misting agent of this invention may include a compound which may typically have the structure wherein Ar is selected from the group consisting of phenyl and naphthyl rings, said ring being incorporated into the imidazole structure through vicinal carbon atoms of said ring; M is a cation selected from the group consisting of hydrogen, ammonium and metals; R is a non-aromatic hydrocarbon radical containing at least 3 carbon atoms; R" is selected from the group consisting of hydrogen, alkyl, aryl, aralkyl, omega-sulfonated alkyl, sulfonated 20 aryl, and sulfonated aralkyl; R' is selected from the group consisting of hydrogen, alkyl and aralkyl; Y is a water-soluble anion; and a is 0-1.
  • the group Ar may be phenyl or naphthyl, and preferably it may be phenyl. 3
  • the cation M may be hydrogen, ammonium, or a metal.
  • M may be selected from the group consisting of hydrogen, ammonium, sodium, potassium, lithium, trivalent chromium, calcium, strontium, barium, magnesium, nickel, iron, and copper.
  • M may 35 be ammonium or an alkali metal e.g. sodium, potassium and lithium.
  • the group R may be a non-aromatic hydrocarbon containing at least 3 carbon atoms.
  • R may be selected from the group consisting of alkyl, cycloalkyl, alkenyl, and cycloalkenyl radicals.
  • R may contain at least 8, say 8-18 carbon atoms.
  • Preferred R groups may include n-octyl, isooctyl, nonyl, decyl, undecyl, tridecyl, pentadecyl, heptadecyl octadecyl, 4-ethylcyclohexyl, octenyl, nonenyl, undecenyl, tridecenyl, pentadecenyl, heptadecenyl, 4-amylcyclohexenyl, etc.
  • the group R may be hydrogen, alkyl, aryl, aralkyl, omega-sulfonated alkyl, sulfonated aryl or sulfonated aralkyl.
  • R may be omega-sulfonated alkyl, sulfonated aryl or sulfonated aralkyl and most preferably 5 R" may be selected from the group consisting of omegasulfonated lower alkyl (i.e. an alkyl containing less than about 6 carbon atoms), sulfonated phenyl and sulfonated benzyl.
  • the sulfonated group contained in the R" group may typically be of the form MO S wherein M is as defined supra and preferably wherein M is alkali metal, e.g. sodium, potassium, ammonium or lithium.
  • R' may be hydrogen, alkyl or aralkyl.
  • R may be selected from the group consisting of hydrogen, lower alkyl (i.e. an alkyl containing less than about 6 carbon atoms) and benzyl. Most preferably, R' may be benzyl.
  • the group Y may be a solubilizing anion, typically a water-soluble anion.
  • Y may be selected from the group consisting of bromide, iodide, sulfate, acetate, methosulfate, ethosulfate, citrate, and perchlorate.
  • the sulfonated Z-alkylbenzimidazoles which may be present in the novel compositions of this invention may contain a quaternary nitrogen atom.
  • a may be 1 and the compound may be a quaternized sulfonated Z-alkylbenzimidazole.
  • the compound as added may contain no quaternized nitrogen atom.
  • the sulfonated 2-alkylbenzimidazole is added to the plating bath as an unquaternized compound, it may be converted in the acid bath to a quaternary compound. 7
  • R also contains a sulfonate group
  • this group may also be present in the ionized 0 5 form.
  • the nitrogen atoms of the imidazole ring may also be present as ionized quaternary nitrogens in the highly acidic plating bath.
  • These materials may be readily mixed together in powdered form or in aqueous solution; and stored or used as such.
  • the solutions may contain stabilizing amounts of a chromate or dichromate, of e.g., sodium or potassium to inhibit growth of fungi or mold.
  • the two components of the novel fume-suppressant composition may be preblended prior to their addition to the bath, or they may be added thereto individually. When added individually, they may be added as a solid or in separate aqueous solutions. Preferably, they may be preblended prior to the addition. Preblending may be accomplished by physically mixing the solid materials or by dissolving both of them in the same aqueous solution. This solution may typically contain about 120%, say 10%, by weight of the fume-suppressant composition.
  • the dry materials may also be blended and compressed, i.e. pelletized, preferably together with a release agent, say sodium bicarbonate.
  • this blanket should be stable and of substantial, yet not too great, thickness, which could be dangerous because of the large amount of entrapped oxygen and hydrogen.
  • the geometry of the plating system affects the desired concentration of additive as it will affect the thickness of the foam blanket for a given volume of bath. It is not contemplated that more than about 5 g./l. of the additive will be present in the bath at any one time.
  • the bath may contain about 0.001 g./l. to 1.0 g./l. Larger amounts may be used but no apparent advantage may be realized thereby.
  • the novel fume-suppressant composition may be present in chromium plating baths in the amount of 0.001 to 1.0 g./l. of bath.
  • the composition may be present in the amount of 0.002 to 0.05, say 0.01 g./1. of bath.
  • the anti-misting properties of the novel composition of this invention may endure over an extended period of time. This may be due in part to the unexpected synergistic action between the two components of the composition, thereby maintaining a substantially constant foam level for an indefinitely long period of time. It is a particular feature of this composition that presence of considerable excesses of this material (as by inadvertent overdosage) do not cause build up of any substantially excessive amount of foam.
  • This agent was the Ultrav-on WC brand of the sodium salt of Z-n-heptadecyl, 3-sulfobenzyl benzimidazole sulfonate.
  • This agent was the Dowfax 2A1 brand of the mixture of disodium salts of monododecyl diphenyl oxide disulfonate and didodecyl diphenyl oxide disulfonate;
  • This agent was a mixtureof 50%-50% of each of the agents of Examples I and II.
  • compositions were added in amount of l g./l. to one liter of a chromium plating solution having the following composition:
  • composition III of this invention permitted attainment of a desirable moderate foam blanket to about 75 hours while the composition II gave a satisfactory blanket for only 5 hours.
  • the composition I gave undesirably high foam at the controlled concentrations of the test. It is particularly noteworthy that composition III gave a foam of substantially uniform thickness over a long period of time, while the foams produced by I and II varied widely or were excessive over the same period of time.
  • compositions of this invention may produce less sulfate build-up in a commercial bath than fume-suppressants previously used. Sulfate ion is produced when the fume-suppressant breaks down in the plate bath. Since the compositions of this invention (e.g. composition III) may be effective for 68 times as long as previously used agents, they need not be added as frequently, and sulfate build-up may be thereby reduced.
  • a novel composition characterized by its ability to controllably develop and maintain over an extended period of time a fixed predetermined blanket of foam which consists essentially of a mixture of 5-95 parts by weight of a sulfonated 2-alkyl benzimidazole and 5-95 parts by weight of a disulfonated alkyl diphenyl oxide.
  • a novel composition characterized by its ability to controllably develop and maintain over an extended pe riod of time a fixed predetermined blanket of foam which consists essentially of (a) 5-95 parts of a disulfonated alkyl diphenyl oxide having the formula Q Q R.
  • R is an alkyl group containing 6-18 carbon atoms
  • X is a cation selected from the group consisting of hydrogen, ammonium and metals
  • n is 0l
  • M is a cation selected from the group consisting of hyrogen, ammonium and metals
  • R is a non-aromatic hydrocarbon containing 3-18 carbon atoms
  • R" is selected from the group consisting of omega-sulfonated lower alkyl, sulfonated phenyl and sulfonated benzyl
  • R' is selected from the group consisting of hydrogen, lower alkyl and benzyl
  • Y is a water-soluble anion
  • a is 0-1.
  • a novel composition characterized by its ability to controllably develop and maintain over an extended period of time a fixed predetermined blanket of foam which consists essentially of (a) 30-90 parts of a disulfonated alkyl diphenyl oxide having the formula Q Rn SOQX R SOaX wherein Ar is selected from the group consisting of phenyl and naphthyl rings, said ring being incorporated into the imidazole structure through vicinal carbon atoms of said ring; M is a cation selected from the group consisting of hydrogen, ammonium and metals; R is a non-aromatic hydrocarbon containing 3-18 carbon atoms; R" is selected from the group consisting of omega-sulfonated lower alkyl, sulfonated phenyl and sulfonated benzyl; R'" is selected from the group consisting of hydrogen, lower alkyl and benzyl; Y is a water-soluble anion; and a is -1.
  • a novel composition as claimed in claim 3 wherein said compound is sodium 2-n-heptadecyl, 3-sulfophenyl benzimidazole sulfonate.
  • a novel composition as claimed in claim 3 wherein said compound is sodium Z-n-heptadecyl, 3-sulfobenzyl benzimidazole sulfonate.
  • a novel composition as claimed in claim 3 wherein said compound is sodium Z-n-heptadecyl, 3-omega-sulfon-butyl benzimidazole sulfonate.
  • disulfonated alkyl diphenyl oxide is a mixture of disodium monododecyl diphenyl oxide disulfonate and disodium didodecyl diphenyl oxide disulfonate.
  • Ar is selected from the group consisting of phenyl and naphthyl rings, said ring being incorporated into the imidazole structure through vicinal carbon atoms of said ring;
  • M is a cation selected from the group consisting of hydrogen, ammonium and metals;
  • R is a non-aromatic hydrocarbon containing 3-18 carbon atoms;
  • R" is selected from the group consisting of omega-sulfonated lower alkyl, sulfonated phenyl and sulfonated benzyl;
  • R' is selected from the group consisting of hydrogen, lower alkyl and benzyl;
  • Y is a water-soluble anion; and a is 0-1.
  • disulfonated alkyl diphenyl oxide is a mixture of disodium monodidodecyl diphenyl oxide disulfonate.
  • a novel bath for the electrodeposition of chromium comprising an aqueous acid chromium plating solution and, as an anti-misting agent, a composition consisting essentially of 5-95 parts by weight of a sulfonated Z-alkyl benzimidazole and 5-95 parts by weight of a disulfonated alkyl diphenyl oxide, said composition being present in said bath in the amount of about 0.0011.0 g./l.
  • a novel bath for the electrodeposition of chromium comprising an aqueous acid chromium plating solution and, as an anti-misting agent, 0.00l-1.0 g./l. of a composition consisting essentially of (a) 5-95 parts of a disulfonated alkyl diphenyl oxide having the formula Rn 803 R SOsX wherein R is an alkyl group containing 6-18 carbon atoms; X is a cation selected from the group consisting of hydrogen, ammonium and metals; and n is 0-1 and (b) 5-95 parts of a compound having the formula wherein Ar is selected from the group consisting of phenyl and naphthyl rings, said ring being incorporated into the imidazole structure through vicinal carbon atoms of said ring; M is a cation selected from the group consisting of hydrogen, ammonium and metals; R is a non-aromatic hydrocarbon containing 3-18 carbon atoms; R" is selected from the group consist
  • a novel bath for the electrodeposition of chromium comprising an aqueous acid chromium plating solution and, as an anti-misting agent, 0002-005 g./l. of a composition consisting essentially of (a) 30-90 parts of a disulfonated alkyl diphenyl oxide having the formula Rn SO3X R wherein R is an alkyl group containing 6-18 carbon atoms; X is a cation selected from the group consisting of hydrogen, ammonium and metals; and n is -1 and (b) 10-70 parts of a compound having the formula wherein Ar is selected from the group consisting of phenyl and naphthyl rings, said ring being incorporated into the imidazole structure through vicinal carbon atoms of said ring; M is a cation selected from the group consisting of hydrogen, ammonium and metals; R is a non-aromatic hydrocarbon containing 3-18 carbon atoms; R is selected from the group consisting of omega-sul
  • a novel bath as claimed in claim 17 wherein said compound is sodium Z-n-heptadecyl, 3-sulfophenyl benzimidazole sulfonate.
  • a novel bath as claimed in claim 17 wherein said compound is sodium 2-n-heptadecyl, 3-su1f0benzyl benzimidazole sulfonate.
  • a novel bath as claimed in claim 17 wherein said compound is sodium 2-n-heptadecyl, 3-omega-sulf0-nbutyl benzimidazole sulfonate.
  • a novel bath as claimed in claim 17 wherein the disulfonated alkyl diphenyl oxide is a mixture of disodium monododecyl diphenyl oxide disulfonate and disodium didodecyl diphenyl oxide disulfonate.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Electroplating And Plating Baths Therefor (AREA)
  • Agricultural Chemicals And Associated Chemicals (AREA)
  • Indole Compounds (AREA)
US311243A 1963-09-24 1963-09-24 Electrodeposition of chromium and anti-misting agents therefor Expired - Lifetime US3342709A (en)

Priority Applications (7)

Application Number Priority Date Filing Date Title
US311243A US3342709A (en) 1963-09-24 1963-09-24 Electrodeposition of chromium and anti-misting agents therefor
IL22129A IL22129A (en) 1963-09-24 1964-09-23 Plating with chromium
FR989012A FR1408622A (fr) 1963-09-24 1964-09-23 Composition et procédé pour le dépôt électrolytique du chrome
GB38868/64A GB1079647A (en) 1963-09-24 1964-09-23 Improvemets in or relating to chromium plating
NL646411160A NL148361B (nl) 1963-09-24 1964-09-24 Werkwijze ter bereiding van een nevelonderdrukkend middel, werkwijze ter bereiding van een zuur, waterig chroombad, en werkwijze voor het elektrolytisch bekleden met chroom.
CH1238764A CH463902A (de) 1963-09-24 1964-09-24 Verfahren zum elektrolytischen Abscheiden von Chrom
DE1496904A DE1496904C3 (de) 1963-09-24 1964-09-24 Verfahren zur Verhinderung einer Nebelbildung beim Betrieb von galvanischen Chrombadern

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US311243A US3342709A (en) 1963-09-24 1963-09-24 Electrodeposition of chromium and anti-misting agents therefor

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US (1) US3342709A (enrdf_load_stackoverflow)
CH (1) CH463902A (enrdf_load_stackoverflow)
DE (1) DE1496904C3 (enrdf_load_stackoverflow)
GB (1) GB1079647A (enrdf_load_stackoverflow)
IL (1) IL22129A (enrdf_load_stackoverflow)
NL (1) NL148361B (enrdf_load_stackoverflow)

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3432408A (en) * 1966-08-03 1969-03-11 Udylite Corp Chromium plating electrolyte and method for preventing mist therein
US3489662A (en) * 1966-03-28 1970-01-13 Reuven Merker Chromium plating using fume- and mist-depressant
EP3431634A1 (en) * 2017-06-15 2019-01-23 Rohm and Haas Electronic Materials LLC Environmentally friendly nickel electroplating compositions and methods

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2036525A (en) * 1932-04-27 1936-04-07 Soc Of Chemical Ind Imidazole sulphonic acids useful as textile assisting agents and process of making same
US2053822A (en) * 1933-12-15 1936-09-08 Soc Of Chemical Ind Alkylated imidazoles of high molecular weight and process of making same
US2854477A (en) * 1956-11-20 1958-09-30 Dow Chemical Co Method of making alkyl diphenyl ether sulfonates
US2956935A (en) * 1957-10-08 1960-10-18 Metal & Thermit Corp Chromium plating

Family Cites Families (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2750334A (en) * 1953-01-29 1956-06-12 Udylite Res Corp Electrodeposition of chromium
US2846380A (en) * 1956-05-07 1958-08-05 Udylite Res Corp Chromium electroplating

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2036525A (en) * 1932-04-27 1936-04-07 Soc Of Chemical Ind Imidazole sulphonic acids useful as textile assisting agents and process of making same
US2053822A (en) * 1933-12-15 1936-09-08 Soc Of Chemical Ind Alkylated imidazoles of high molecular weight and process of making same
US2854477A (en) * 1956-11-20 1958-09-30 Dow Chemical Co Method of making alkyl diphenyl ether sulfonates
US2956935A (en) * 1957-10-08 1960-10-18 Metal & Thermit Corp Chromium plating

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3489662A (en) * 1966-03-28 1970-01-13 Reuven Merker Chromium plating using fume- and mist-depressant
US3432408A (en) * 1966-08-03 1969-03-11 Udylite Corp Chromium plating electrolyte and method for preventing mist therein
EP3431634A1 (en) * 2017-06-15 2019-01-23 Rohm and Haas Electronic Materials LLC Environmentally friendly nickel electroplating compositions and methods
US10508348B2 (en) 2017-06-15 2019-12-17 Rohm And Haas Electronic Materials Llc Environmentally friendly nickel electroplating compositions and methods

Also Published As

Publication number Publication date
CH463902A (de) 1968-10-15
GB1079647A (en) 1967-08-16
NL6411160A (enrdf_load_stackoverflow) 1965-03-25
DE1496904B2 (de) 1973-04-12
IL22129A (en) 1968-03-28
DE1496904A1 (de) 1969-08-14
DE1496904C3 (de) 1973-11-08
NL148361B (nl) 1976-01-15

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