US3330769A - Metal cleaning - Google Patents

Metal cleaning Download PDF

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Publication number
US3330769A
US3330769A US339606A US33960664A US3330769A US 3330769 A US3330769 A US 3330769A US 339606 A US339606 A US 339606A US 33960664 A US33960664 A US 33960664A US 3330769 A US3330769 A US 3330769A
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US
United States
Prior art keywords
parts
acid
hlb value
cleaning
metal
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
US339606A
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English (en)
Inventor
Golben Michael
John W Pearson
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.)
3M Co
Original Assignee
Minnesota Mining and Manufacturing Co
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 Minnesota Mining and Manufacturing Co filed Critical Minnesota Mining and Manufacturing Co
Priority to US339606A priority Critical patent/US3330769A/en
Priority to GB47240/64A priority patent/GB1092867A/en
Priority to GB20652/67A priority patent/GB1092868A/en
Priority to DE19641546161 priority patent/DE1546161B2/de
Priority to JP39070790A priority patent/JPS4930615B1/ja
Priority to FR1893A priority patent/FR1420885A/fr
Priority to CH59665A priority patent/CH485871A/de
Priority to BE658442D priority patent/BE658442A/xx
Priority to SE783/65A priority patent/SE319664B/xx
Priority to NL656500857A priority patent/NL149235B/xx
Application granted granted Critical
Publication of US3330769A publication Critical patent/US3330769A/en
Anticipated expiration legal-status Critical
Expired - Lifetime legal-status Critical Current

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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
    • C23G—CLEANING OR DE-GREASING OF METALLIC MATERIAL BY CHEMICAL METHODS OTHER THAN ELECTROLYSIS
    • C23G1/00—Cleaning or pickling metallic material with solutions or molten salts
    • C23G1/02—Cleaning or pickling metallic material with solutions or molten salts with acid solutions
    • C—CHEMISTRY; METALLURGY
    • C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • C11D2111/00—Cleaning compositions characterised by the objects to be cleaned; Cleaning compositions characterised by non-standard cleaning or washing processes
    • C11D2111/40—Specific cleaning or washing processes

Definitions

  • This invention relates to the cleaning of metal parts prior to the applicaton of an overcoating material. It particularly relates to the cleaning of metal parts prior to the application of a metal by mechanical plating.
  • inorganic pickling acids often leave a carbon smut on the metal surface, making it extremely difficult to obtain uniform coverage of an overcoating material.
  • acid pickling tends to trap hydrogen in the metal lattice, making the metal more brittle (i.e., hydrogen embrittlement), frequently resulting in breakage of a cleaned and subsequently electroplated part.
  • the present invention is believed to provide for the first time a unitary one-shot process for cleaning metal parts to be plated, thereby effecting a great economy in both cleaning time and requisite plant space.
  • the process is convenient, eliminating the need for the constant careful maintenance of several treating baths and the transfer of parts from one bath to another. It is simple and inexpensive, producing consistent and predictable results.
  • the metal parts to be cleaned are placed in a container (which may be the same barrel used in mechanical plating) and a relatively small amount of aqueous cleaning solution, and, preferably, impact media are added.
  • the parts and solution are agitated until the parts are cleaned, after which the cleaning solution is flushed away, leaving the cleaned, degreased, descaled, desmutted etched parts ready for plating.
  • the cleaning composition comprises a water-soluble mixture of metal oxide-removing acid, hydrogen embrittlement inhibitor, and surfactant having the combined properties of metal wetting, oxide scale and dirt detergency, and oil emulsification.
  • the scale-removing acid used in the cleaning solution may be either mineral or organic, the former being relatively inexpensive and the latter being both easier to control and less corrosive at room temperature. Descaling and etching 10,000 grams of typical metal parts requires enough acid to supply between 1 and 5 grams of available hydrogen ion. Either monobasic or polybasic acids may be employed, but for purposes of this invention a hydrogen ion is considered to be available if it has an dissociation constant of at least 10- In order to minimize hydrogen embrittlement, I also prefer to include a hydrogen embrittlement inhibitor. Whether or not an inhibitor works with the particular acid used can be determined empirically by known procedures, of the type described in the specific example following.
  • HLB hydrophilelipophile balance
  • Surfactants are molecules having a hydrophilic portion and a hydrophobic, or lipophilic, portion, so that in another sense the HLB number is related to the ratio between hydrophilic groups and lipophilic groups in the molecule.
  • Those surfactants in which the lipophilic groups are dominant tend to be oil-soluble and hence are extremely effective in wetting surfaces which may be contaminated with organic materials, e.g., oils; such surfactants tend to have an HLB value of 5 or less.
  • Surfactants in which the hydrophilic and lipophilic groups are roughly balanced have an HLB value in the proximate range of 12 to 17 and tend to function as detergents if their molecular weight is relatively low and as emulsifiers if their molecular Weight is relatively high.
  • Surfactants in which the lipophilic groups are dominant have and HLB value of more than 17 and function effectively as dispersants for carbonaceous or other materials.
  • a mixture of surfactants is employed.
  • One surfactanta wetting agent which loosens oil and dirt and aids the acid in uniformly contacting the metal oxide scale-has an HLB value in the range of 1 to 5.
  • Another surfactant-a detergent which aids in suspending dirt and scalehas an HLB value in the range of 12 to 17, and a third surfactantan emulsifier which emulsifies residual oils-has an HLB value in the range of 12 to 17.
  • a fourth surfactant-a dispersant which prevents particle agglomeration and redeposition and which has an HLB value greater than 17-is also present.
  • emulsifying ability is a requisite for the composition of this invention. Oftentimes parts to be cleaned are supplied in very oily condition; for example, 10,000 grams of metal articles may include 150 grams or more of oil.
  • the qb and therefrom the HLB is determined with an emulsifying machine substantially like that described on pages 378 et seq. of the Davies and Rideal book, previously mentioned. In this machine oil 1 and water are pumped through flow gauges from separate reservoirs at controlled rates and fed between two polymethyl methacrylate shearing plates.
  • a precise way of determining the inversion point involves measuring the electrical conductivity of the emulsion, which decreases sharply as the change from water-in-oil to oil-inwater occurs, and conversely increases sharply as the change from oil-in-water to water-in-oil occurs. Flow rates are adjusted to establish the oil:water ratio, at phase inversion.
  • EXAMPLE Hydrogen embrittlement inhibitor To 50.2 parts of de-ionized water is added 32.0 parts of a water-soluble high molecular weight polyoxyethylene glycol. The charge is heated to 120 F. and maintained at that temperature until all the polyoxyethylene glycol has been dissolved and a uniform solution has resulted. The temperature is then lowered to 75 F at which time the following ingredients are added: 4.8 parts of concentrated hydrochloric acid, 6.5 parts of o-toluidine, and 6.5 parts of 37% formaldehyde, and the reaction kettle sealed. When the exothermic reaction has ended, the charge is heated briefly to 120 F., cooled to 85 F. and drained from the container. This composition is hereinafter referred to as Composition A.
  • the Pluronics referred to in the preceding paragraph are heatand acid-stable, nontoxic non-ionic surfactants made by adding propylene oxide to propylene glycol in sufiicient amount to form a hydrophobic nucleus, and thereafter graft polymerizing ethylene oxide on each end of the polyoxypropylene nucleus to form two hydrophilic polyoxyethylene chains.
  • Pluronic L-64 is a liquid which has a polyoxypropylene nucleus having an average molecular weight of about 1,750, polyoxyethylene making up approximately 40% of the total weight of the molecule; this surfactant has an HLB value of 15 and is useful as a carbon soil remover.
  • Pluronic L-101 is a liquid having a polyoxypropylene nucleus with an average molecular weight of Mineral spirits, or ligroin, i.e., the fourth fraction of petroleum distillation product, having a density of 0.707 to 0.722 and a boiling range of 90120 C.
  • Pluronic P-l04 is a paste having a polyoxypropylene nucleus with an average molecular weight of approximately 3,250, polyoxyethylene making up approximately 40% of the total weight of the molecule; this surfactant has an HLB value of approximately 13 and is particularly useful as an emulsifying agent.
  • the cleaning composition just described is extremely useful for a wide range of metal cleaning operations.
  • metal parts vary in surface area and amount of scale, and although such parts are often not completely drenched with oil, this composition is suitable for cleaning operations in which the worst reasonably anticipated conditions might be encountered.
  • the novel one-shot method taught herein provides simultaneous mechanical and chemical cleaning of metal parts which are to be subsequently overcoated.
  • the parts are placed in an aqueous descaling and degreasing composition, which is then vigorously agitated while the parts are being mechanically cleaned to loosen the scale and oil; after cleaning has been completed, the parts are rinsed and then overcoated as desired.
  • the cleaning and rinsing operation is conveniently effected in an inclined rotary open end barrel, the impingement of the parts on each other and the walls of the barrel during rotation serving to loosen the scale, oil and dirt which contaminates the metal substrate.
  • the mechanical cleaning is rendered more efficient by including small particles, or impact media, in the charge.
  • the excess liquid is then decanted, and, if mechanical plating is to be carried on in the same barrel, a conventional anchoring solution (such as a coppering solution) and a mechanical plating charge are successively introduced. If, alternatively, the cleaned articles are to be painted, electroplated, or otherwise overcoated, they are screened from the impact media and transported to the next station.
  • a conventional anchoring solution such as a coppering solution
  • a standard high carbon steel spring wire hose clamp having a Rockwell C hardness of at least 53 is cleaned, plated, and, after a given lapse of time, spread with a standard instrument and slipped over a bar which is slightly greater in diameter than the normal ID. of the clamp. If the hose clamp has been hydrogen-embrittled, it will fail, i.e., break, either immediately, or within 24 hours; generally speaking, the shorter the time lapse before testing, the greater the probability of failure.
  • a total of 150 No. 15 hose clamps were cleaned as just described, given a copper anchor coat, and immediately mechanically plated with zinc. Four hours after plating, 50 of the clamps were mounted on a test bar having a diameter of 0.953 inch, no failures occurring within 24 hours. Twentyfour hours after plating, the other clamps were mounted on the test bar; again no failures occurred within 24 hours.
  • This condition may be alleviated by adding a small amount of one or more soluble salts, e.g., sulfates, of tin, lead, cadmium, mercury, etc. It is also desirable under such conditions to make certain that a carbon soil dispersant, i.e., a high- HLB surfactant, is present in the surfactant mixture.
  • a carbon soil dispersant i.e., a high- HLB surfactant
  • Phosphoric acid offers particular advantages when the surface to be cleaned is thereafter to be painted.
  • organic acids both monobasic and multibasic.
  • tartaric, citric, diglycolic, chlorosulfonic, formic, acetic, and mono-, dior tri-chloroacetic acid may be employed.
  • acids which might the considered too weak are rendered more effective by the preferred elevated cleaning temperature.
  • Glycolic acid possesses the advantage that it is a sequestering agent and hence aids in competing with the metal for the oxygen atoms which are in the oxide coating; similarly, where the available water supply contains an ion which interferes with cleaning action, glycolic acid aids in sequestering such ions.
  • other acid-stable sequestering agents may be added; thus, Versenex 80 (based on a diethylene triamide penta acetic acid adduct) or Clarotex may be used.
  • the Pluronics are attractive surfactants to work with because their stability, chemical similarity, and physical characteristics have been determined.
  • the surfactant mixture of the cleaning solution described herein may, however, be any acid-stable materials of suitable HLB having the following ionic nature: all anionic, a blend of anionic and non-ionic, all non-ionic, a blend of non-ionic and cationic, and all cationic.
  • the addition of these surfactants thus extends the usefulness of the cleaning compositions described herein.
  • Composition A contains a combination of materials which are individually effective in this regard, both the polyoxyethylene glycol and the o-toluidine being able to reduce or suppress hydrogen embrittlement, even at high temperatures. In Composition A some of these materials are reacted, resulting in an adduct of orthotoluidine and and formaldehyde having the characteristics of stability and excellent inhibition.
  • a wide variety of commercially available inhibitors such as Polyrad 1110A, Armohib 28, or hexynol, substituted thioureas, and most amines or proteins, can be employed with at least some degree of success. Inhibitors are at least somewhat selective, however, and a given inhibitor may be more effective with one acid than with another.
  • a balanced composition for preparing a wide variety of scaly, oily, dirty, or otherwise contaminated ferrous metal surfaces for subsequent overcoating consisting essentially of a water-soluble mixture of:
  • sufiicient strong acid having a dissociation constant greater than 10- to provide 1-5 parts by weight of hydrogen ion
  • an acid-stable surfactant system consisting essentially of substantially equal parts by weight of the following individually acid-stable components:
  • dispersant having an HLB value of at least 17, detergent having an HLB value in the range of 12-17, sufiicient emulsifier to emulsify parts by weight of mineral spirits, said emulsifier having a higher molecular weight than said detergent and an HLB value in the range of 1217, and wetting agent for ferrous metals, the lipophilic groups being dominant in said wetting agent, having an HLB value on the order of 5 or less.
  • composition of claim 1 wherein the wetting agent is a surfactant selected from the class consisting of coco amine N,N-substituted with ethylene oxide and bydrogenated tallow amine N,N-substituted with ethylene oxide.
  • composition of claim 3 wherein each of the components of the surfactant system has a hydrophobic polyoxypropylene nucleus with hydrophilic polyoxyethylene chains graft-polymerized thereon.
  • a one-shot method of preparing ferrous metal articles for subsequent overcoating comprising: (1) placing in a rotary container, impact media, water, on the order of 10,000 parts by weight of small ferrous articles to be cleaned, and the composition of claim 1, (2) rotating said container to both mechanically and chemically clean, descale, and desmut the metal articles, and (3) removing the cleaning solution.

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  • 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)
  • Cleaning And De-Greasing Of Metallic Materials By Chemical Methods (AREA)
  • Detergent Compositions (AREA)
US339606A 1964-01-23 1964-01-23 Metal cleaning Expired - Lifetime US3330769A (en)

Priority Applications (10)

Application Number Priority Date Filing Date Title
US339606A US3330769A (en) 1964-01-23 1964-01-23 Metal cleaning
GB47240/64A GB1092867A (en) 1964-01-23 1964-11-19 Metal cleaning
GB20652/67A GB1092868A (en) 1964-01-23 1964-11-19 Metal cleaning
DE19641546161 DE1546161B2 (de) 1964-01-23 1964-12-10 Verfahren zur reinigung von metallgegenstaenden und reinigungs masse
JP39070790A JPS4930615B1 (ja) 1964-01-23 1964-12-17
FR1893A FR1420885A (fr) 1964-01-23 1965-01-14 Perfectionnements au décapage des métaux
CH59665A CH485871A (de) 1964-01-23 1965-01-15 Wasserlösliche Masse zur Vorbereitung von Metallgegenständen für das nachfolgende Überziehen
BE658442D BE658442A (ja) 1964-01-23 1965-01-18
SE783/65A SE319664B (ja) 1964-01-23 1965-01-21
NL656500857A NL149235B (nl) 1964-01-23 1965-01-22 Werkwijze voor het bereiden van een reinigingsmiddel voor metalen voorwerpen.

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
US339606A US3330769A (en) 1964-01-23 1964-01-23 Metal cleaning

Publications (1)

Publication Number Publication Date
US3330769A true US3330769A (en) 1967-07-11

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Family Applications (1)

Application Number Title Priority Date Filing Date
US339606A Expired - Lifetime US3330769A (en) 1964-01-23 1964-01-23 Metal cleaning

Country Status (9)

Country Link
US (1) US3330769A (ja)
JP (1) JPS4930615B1 (ja)
BE (1) BE658442A (ja)
CH (1) CH485871A (ja)
DE (1) DE1546161B2 (ja)
FR (1) FR1420885A (ja)
GB (1) GB1092867A (ja)
NL (1) NL149235B (ja)
SE (1) SE319664B (ja)

Cited By (12)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3494795A (en) * 1967-08-07 1970-02-10 Fremont Ind Inc Spray cleaning method for removing oil,grease,dirt and embedded oxides from painted surfaces
US3909437A (en) * 1973-01-18 1975-09-30 Dow Chemical Co Noncorrosive acid, solvent and nonionic surfactant composition
US3979219A (en) * 1975-03-06 1976-09-07 Fremont Industries, Inc. Wood finish remover
US4100096A (en) * 1976-06-04 1978-07-11 Addressograph Multigraph Corp. Cleaner for hydrophilic metal surfaces of lithographic duplicators
DE2942934A1 (de) * 1978-10-27 1980-05-08 Centre Rech Metallurgique Verfahren zur kontinuierlichen behandlung von stahlblechen
US4541945A (en) * 1982-09-30 1985-09-17 Amchem Products Inhibitor-containing acid cleaning compositions and processes
US4608086A (en) * 1983-01-19 1986-08-26 Tennant Company Membrane remover/etchant
US5658869A (en) * 1995-10-16 1997-08-19 Singer; Barrie Metal finishing composition
US20090145427A1 (en) * 2007-12-07 2009-06-11 Groeger Joseph H Method for Applying a Polymer Coating to an Internal Surface of a Container
WO2009073012A1 (en) * 2007-12-07 2009-06-11 Presspart Gmbh & Co. Kg Method for applying a polymer coating to an internal surface of a container
CN104289468A (zh) * 2007-12-07 2015-01-21 普莱斯博有限两合公司 施加聚合物涂料于容器内表面的方法
US20190189312A1 (en) * 2017-12-19 2019-06-20 National Cheng Kung University Pretreatment of Thick-Film Aluminum Electrode for Metal Plating

Families Citing this family (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS60224818A (ja) * 1984-04-20 1985-11-09 Itochu Shoji Kk 原綿中の色物除去方法およびその装置
JPH0525713A (ja) * 1991-05-17 1993-02-02 Murata Mach Ltd 混打綿工程の異物検出装置
JP3673357B2 (ja) * 1997-01-27 2005-07-20 メルテックス株式会社 めっき用の前処理洗浄剤

Citations (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2261700A (en) * 1939-04-03 1941-11-04 Nat Aluminate Corp Cleaning composition
US2326837A (en) * 1940-01-13 1943-08-17 Nat Carbon Co Inc Cleaning composition and method for its use
US2399267A (en) * 1940-07-27 1946-04-30 Solventol Chemical Products In Cleaning method
US2571581A (en) * 1948-09-09 1951-10-16 Detrex Corp Degreasing machine
US2683343A (en) * 1952-11-15 1954-07-13 Gen Motors Corp Tumbling process
US2942956A (en) * 1958-10-13 1960-06-28 Wyandotte Chemicals Corp Aluminum brightener compositions
US3041285A (en) * 1955-05-27 1962-06-26 Purex Corp Ltd Composition for cleaning and polishing aluminum and aluminum alloys
US3162547A (en) * 1961-07-31 1964-12-22 Rohr Corp Secondary deoxidizer for aluminum and its alloys

Patent Citations (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2261700A (en) * 1939-04-03 1941-11-04 Nat Aluminate Corp Cleaning composition
US2326837A (en) * 1940-01-13 1943-08-17 Nat Carbon Co Inc Cleaning composition and method for its use
US2399267A (en) * 1940-07-27 1946-04-30 Solventol Chemical Products In Cleaning method
US2571581A (en) * 1948-09-09 1951-10-16 Detrex Corp Degreasing machine
US2683343A (en) * 1952-11-15 1954-07-13 Gen Motors Corp Tumbling process
US3041285A (en) * 1955-05-27 1962-06-26 Purex Corp Ltd Composition for cleaning and polishing aluminum and aluminum alloys
US2942956A (en) * 1958-10-13 1960-06-28 Wyandotte Chemicals Corp Aluminum brightener compositions
US3162547A (en) * 1961-07-31 1964-12-22 Rohr Corp Secondary deoxidizer for aluminum and its alloys

Cited By (16)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3494795A (en) * 1967-08-07 1970-02-10 Fremont Ind Inc Spray cleaning method for removing oil,grease,dirt and embedded oxides from painted surfaces
US3909437A (en) * 1973-01-18 1975-09-30 Dow Chemical Co Noncorrosive acid, solvent and nonionic surfactant composition
US3957529A (en) * 1973-01-18 1976-05-18 The Dow Chemical Company Method for cleaning and passivating a metal surface
US3979219A (en) * 1975-03-06 1976-09-07 Fremont Industries, Inc. Wood finish remover
US4100096A (en) * 1976-06-04 1978-07-11 Addressograph Multigraph Corp. Cleaner for hydrophilic metal surfaces of lithographic duplicators
DE2942934A1 (de) * 1978-10-27 1980-05-08 Centre Rech Metallurgique Verfahren zur kontinuierlichen behandlung von stahlblechen
US4389254A (en) * 1978-10-27 1983-06-21 Centre De Recherches Metallurgiques-Centrum Voor Research In De Metallurgie Continuous treatment of steel sheet
US4541945A (en) * 1982-09-30 1985-09-17 Amchem Products Inhibitor-containing acid cleaning compositions and processes
US4608086A (en) * 1983-01-19 1986-08-26 Tennant Company Membrane remover/etchant
US5658869A (en) * 1995-10-16 1997-08-19 Singer; Barrie Metal finishing composition
US20090145427A1 (en) * 2007-12-07 2009-06-11 Groeger Joseph H Method for Applying a Polymer Coating to an Internal Surface of a Container
WO2009073012A1 (en) * 2007-12-07 2009-06-11 Presspart Gmbh & Co. Kg Method for applying a polymer coating to an internal surface of a container
US8227027B2 (en) * 2007-12-07 2012-07-24 Presspart Gmbh & Co. Kg Method for applying a polymer coating to an internal surface of a container
US8703306B2 (en) 2007-12-07 2014-04-22 Presspart Gmbh & Co. Kg Method for applying a polymer coating to an internal surface of a container
CN104289468A (zh) * 2007-12-07 2015-01-21 普莱斯博有限两合公司 施加聚合物涂料于容器内表面的方法
US20190189312A1 (en) * 2017-12-19 2019-06-20 National Cheng Kung University Pretreatment of Thick-Film Aluminum Electrode for Metal Plating

Also Published As

Publication number Publication date
FR1420885A (fr) 1965-12-10
SE319664B (ja) 1970-01-19
NL6500857A (ja) 1965-07-26
GB1092867A (en) 1967-11-29
DE1546161A1 (de) 1969-07-17
NL149235B (nl) 1976-04-15
JPS4930615B1 (ja) 1974-08-14
DE1546161B2 (de) 1972-03-02
BE658442A (ja) 1965-05-17
CH485871A (de) 1970-02-15

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