WO1996012832A1 - Solution aqueuse et acide servant a nettoyer de l'aluminium et methode de nettoyage afferente - Google Patents

Solution aqueuse et acide servant a nettoyer de l'aluminium et methode de nettoyage afferente Download PDF

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Publication number
WO1996012832A1
WO1996012832A1 PCT/JP1995/001171 JP9501171W WO9612832A1 WO 1996012832 A1 WO1996012832 A1 WO 1996012832A1 JP 9501171 W JP9501171 W JP 9501171W WO 9612832 A1 WO9612832 A1 WO 9612832A1
Authority
WO
WIPO (PCT)
Prior art keywords
acidic
aqueous solution
aluminum
acid
cleaning
Prior art date
Application number
PCT/JP1995/001171
Other languages
English (en)
Japanese (ja)
Inventor
Satoshi Ikeda
Masayuki Kamimura
Original Assignee
Nippon Paint Co., Ltd.
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
Priority claimed from JP25634694A external-priority patent/JP3192562B2/ja
Application filed by Nippon Paint Co., Ltd. filed Critical Nippon Paint Co., Ltd.
Priority to KR1019970702506A priority Critical patent/KR100231390B1/ko
Priority to EP95921156A priority patent/EP0789094A4/fr
Publication of WO1996012832A1 publication Critical patent/WO1996012832A1/fr

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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
    • C23G1/12—Light metals
    • 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
    • C23G1/12—Light metals
    • C23G1/125—Light metals aluminium
    • 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
    • C23F1/00—Etching metallic material by chemical means
    • C23F1/10—Etching compositions
    • C23F1/14—Aqueous compositions
    • C23F1/16—Acidic compositions
    • C23F1/20—Acidic compositions for etching aluminium or alloys thereof

Definitions

  • the present invention relates to an acidic cleaning aqueous solution of an aluminum-based metal and a cleaning method thereof.
  • the present invention relates to an aqueous cleaning solution of an aluminum-based metal and a cleaning method thereof, and more particularly to a cleaning aqueous solution capable of satisfactorily removing lubricating oil and aluminum powder adhered to an aluminum surface by molding and a cleaning method thereof.
  • Products with an aluminum surface such as aluminum containers for beverages, made of aluminum-based metal, ie aluminum or aluminum alloy, are usually manufactured by a forming operation called drawing and ironing (hereinafter referred to as DI processing). .
  • DI processing drawing and ironing
  • lubricating oil force is applied to the metal surface, and aluminum powder (smut) adheres to the inner wall of the obtained container, especially.
  • the surface of this type of container is generally protected thereafter by, for example, a tanning treatment or painting. Therefore, it is necessary to remove the lubricating oil or the smut from the metal surface and clean it before the ib treatment.
  • an acidic cleaning agent is generally used to clean the metal surface by etching it appropriately.
  • a chromic acid-based hydrofluoric acid-based cleaning agent has been often used as such an acidic cleaning agent.
  • hydrofluoric acid-based cleaning agents excel at being able to perform low-temperature acidic cleaning (up to 50 ° C).
  • since the above detergents are harmful substances and strict wastewater regulations, in recent years, it has been desired to establish a low-temperature acidic cleaning technology of chromium-free and fluorine-free.
  • Japanese Patent Publication No. 3-50838, "Aluminum Surface Cleaner” and Japanese Patent Publication No. 3-6, 5436, "Aluminum Surface Cleaner Management Method” contain no or small amounts of fluorine ions, A cleaning agent containing ferric ion instead of fluorine ion as an accelerating agent in an acid cleaning agent with a pH of 2 or less adjusted with Z or nitric acid, and an iS element in the cleaning bath There is disclosed a management method for managing a ferric ion in a bath by controlling an electric potential.
  • the etching reaction of aluminum in an acidic wash ⁇ includes ⁇ Roh once reaction of aluminum becomes ⁇ Ruminiumuion (A 1 3+), H + force in the cleaning liquid, 'it reduced the 1Z2H 2 by force Sword Reaction. Therefore, the addition of ferric in an acidic wash ⁇ (Fe 3+), the anode reaction to the F e 3+ is reduced to F e 2+, since the place the H + reducing at the same time, aluminum etching reaction Is promoted. Further, by controlling the acid potential of the washing bath by the oxidizing agent and controlling the concentration of the second ion in the bath, the F e 2+ igJ increases as the etching reaction of aluminum proceeds. Can suppress ⁇ and oxidize F e 2+ to F e 3+
  • the present invention has been made to solve such problems, and an acid washing aqueous solution containing an acid metal ion as an etching accelerator does not have harmful fluorine and chromium.
  • Aluminum-based metal with acid cleaning
  • the aqueous acidic washing solution of the aluminum-based metal according to the present invention contains an inorganic acid in an amount of pH 2 or less, an oxidized metal ion, and a chelate dispersant. It is characterized by.
  • the acidic cleaning aqueous solution of another aluminum-based metal according to the present invention contains an inorganic acid in an amount of pH 2 or less, an acid ib metal ion, a surfactant, and a chelate dispersant. I do.
  • the method for washing comprises: at least one selected from inorganic acids having an pH of 2 or less; an oxidized metal ion; a chelate dispersant; Accordingly, a surfactant and an aqueous cleaning solution of an aluminum-based metal containing are used, and “acid ikS! Metal ion and oxidizing agent” or “oxidizing agent” is replenished into the acidic cleaning acid aqueous solution, and the acid of the aqueous solution is added.
  • a method for acid-washing an aluminum-based metal characterized by maintaining and controlling metal oxide ions in the aqueous solution by measuring a bit source potential.
  • the acidic cleaning aqueous solution is obtained by diluting the concentrated aqueous solution of the acidic cleaning aqueous solution to a concentration within the range of use with an appropriate amount of water, which is used as a washing bath for cleaning aluminum-based metal materials.
  • examples of the inorganic acids include sulfuric acid and sulfuric acid.
  • the oxidized gold ⁇ ion, ferric ion (F e 3+), metavanadate ion (V0 3 "), ceric ion (Ce 4+), cobalt ions (Co 5+), tin (Sn 4 +), and the like preferably, ⁇ ferric ions (F e 3+), Metabanaji phosphate ion (V0 3 -.. a)
  • the oxidized metal ions, metal plurality have a valence
  • the platform stands for the higher valence gold ion.
  • the source of the ferric ion includes a water-soluble ferric salt such as ferric sulfate, ferric nitrate, and ferric perchlorate.
  • the source of metavanadate ions includes sodium metavanadate, potassium metavanadate, and ammonium metavanadate. ⁇ 2
  • the source of cerium ions is cerium sulfate ammonium, etc.
  • Can be Sources of cobalt ions include sulfur cobalt 2 cobalt and sulfur island 2 cobalt ammonium.
  • Sources of tin ions include stannic sulfate, stannic nitrate, and the like.
  • the chelate dispersant used in the present invention is a chelate which forms a chelate with an oxidizing agent metal ion, and stabilizes an acid metal ion in an aqueous solution under a strong acid. Any compound that improves dispersibility may be used. Preferably, a oxidized phosphonate is used.
  • Preferred examples of the phosphonic acid compound include 1-hydroxyethylidene-1,1-diphosphonic acid, aminotri (methylenephosphonic acid), and ethylenediaminetetra (methylenephosphonic acid).
  • nonionic, cationic, anionic and amphoteric surfactants can be used as before.
  • nonionics such as ethoxylated alkylphenols, hydrocarbon derivatives, abietic acid derivatives, primary ethoxylated alcohols and modified polyethoxylated alcohols are particularly preferred.
  • bromine ion and / or polyhydric alcohol as a surfactant decomposition inhibitor.
  • Sources of bromine ions include a 47% aqueous HBr solution, potassium bromide, sodium bromide, aluminum bromide, iron bromide and the like.
  • the polyhydric alcohol those having at least two hydroxyl groups per molecule in adjacent carbon atoms in the main chain are preferable, and the dihydric alcohols 1,2-ethanediol (ethylene glycol), 1,2- Propanediol (propylene glycol), 1,2-pentanediol, 1,2-butanediol, and trivalent alcohol 1,2,3-propanetriol (glycerin), 1,2,4-butantriol And tetrahydric alcohols such as 1,2,3,4-butanetetralaol.
  • the dihydric alcohols 1,2-ethanediol (ethylene glycol), 1,2- Propanediol (propylene glycol), 1,2-pentanediol, 1,2-butanediol, and trivalent alcohol 1,2,3-propanetriol (glycerin), 1,2,4-butantriol And tetrahydric alcohols such as 1,2,3,4-butanetetralaol.
  • the OR P control oxidizing agent in this case, hydrogen peroxide (H 2 0 2), persulfates (e.g., Na S 2 0 8 2 - ), ozone (0 3), cerium compounds (e.g., sulfuric acid Seriumua Nmoniu ⁇ : (NH 4) 4 Ce ( S0 4) 4)), nitrites (e.g. NaN0 2, KN0 2), metavanadate ion (V0 3 -) Ru mentioned compounds force "that generates.
  • H 2 0 2 hydrogen peroxide
  • persulfates e.g., Na S 2 0 8 2 -
  • cerium compounds e.g., sulfuric acid Seriumua Nmoniu ⁇ : (NH 4) 4 Ce ( S0 4)
  • nitrites e.g. NaN0 2, KN0 2
  • V0 3 - metavanadate ion
  • the acidic cleaning aqueous solution of the present invention is adjusted to pH 2 or less with an inorganic acid. More preferably, the aqueous acidic washing solution has a pH of 6.2 to 2. If the pH force exceeds 2, the etching rate on the aluminum surface will be extremely reduced, and it will be difficult to demonstrate its effectiveness as a cleaning bath. On the other hand, when the pH is lower than 6, the economic efficiency is poor, and the carry-in capacity to the next it ⁇ process is increased, leading to poor formation.
  • the oxidized metal ion is preferably contained in the acidic washing aqueous solution in an amount of 0.05 to 4 gZ1, more preferably 0.2 to 2 gZl. If the content of oxidized gold ion is less than 0.05 gZl, the amount of etching tends to be insufficient, and the desmutability tends to decrease. On the other hand, if the content exceeds 4% / 1, there is no difference in the cleaning properties, and it is uneconomical.
  • the chelate dispersant is preferably strongly contained in the acidic aqueous solution at 0.05 to 5 gZl, and more preferably 0.1 to 2 gZl. If the amount is not 0.05 gZl, chelation is not sufficient, and oxidized metal hydroxide is formed, and a sediment (sludge) force is generated in the aqueous solution. Further, in the heater section in the pre-cleaning step, the hydroxide of the acid it ⁇ metal ion may adhere. When the washing method of the present invention is performed by spraying In the case, the spray riser and the spray nozzle are clogged. If it exceeds 5 g /, there is no difference in chelate dispersibility, and it is uneconomical.
  • the surfactant is preferably contained in the aqueous acidic washing solution in an amount of 0.1 to 10 g / l, more preferably 0.5 to 2 g / l. If the surfactant content is less than 0.11, the detergency, especially the degreasing property, tends to decrease. If the content exceeds 10 1, there is no difference in detergency and it is uneconomical.
  • bromine ions are contained in the washing aqueous solution in an amount of 0.002 to 0.1 lg / 1. If the bromine ion content is less than 0.002 g / l, the effect of suppressing the oxidative decomposition reaction of the surfactant tends to decrease. If the content exceeds 0.1 lgZl, the oxidative decomposition reaction of the surfactant L, which can not have the effect of Oil.
  • Polyhydric alcohols having at least two hydroxyl groups in one molecule directly linked to adjacent carbon atoms in the main chain are preferably contained in an acidic washing aqueous solution in an amount of 0.1 to 5 gZl, preferably 0.2 to 5 gZl. More preferably, it contains 3 gZl.
  • the content of the polyhydric alcohol having the above structure is less than 0.1 / 1, the effect of suppressing the decomposition reaction tends to be insufficient.
  • the content is more than 5 g / 1, the difference in washing performance is not recognized and it is uneconomical, and the polyhydric alcohol power is high, so that the load on wastewater treatment increases.
  • the acidic cleaning bath has a redox potential of 0.5 to 0.8 V (vs. Ag / AgC1).
  • ferrous ion (Fe 2+ ) power can be increased by newly replenishing only ferric ion (Fe 3+ ).
  • Fe 2+ ferrous ion
  • Fe 3+ ferric ion
  • take it out of the acidic cleaning bath O / 12832 treated objects, such as aluminum cans carry iron ions into the next step, and may precipitate in the next step or adversely affect the ibfiJ process. Therefore, if the “oxidized metal ion and oxidizing agent” or “oxidizing agent” is captured and the acid ibii original potential (ORP) is maintained in the above range, the above-mentioned problems can be solved.
  • the acidic cleaning method for the aluminum surface according to the present invention may use either a spray method or a dipping method.
  • the treatment iSJ is preferably 35 to 80, more preferably 50 to 70. If the treatment exceeds 80, excess etching occurs and the aging of the treatment bath is accelerated. If the treatment is less than 35, the amount of etching is insufficient, and the de-smutting property decreases.
  • the acid washing treatment time is preferably 30 to 300 seconds. If the processing time exceeds 300 seconds, excessive etching will occur and the aging of the processing bath will be accelerated. If the processing time is less than 30 seconds, the etching amount will be insufficient, and the de-smuttability will decrease. More preferably, it is 45 to: L 20 seconds.
  • the aluminum surface cleaned by the acidic cleaning agent of the present invention may be washed with water and then subjected to, for example, a phosphate chemical treatment according to a conventional method.
  • a chelate is formed in an acidic aqueous solution between an oxidized metal ion and a chelate salt, particularly by using a chelate dispersant, and the oxidized metal ion is dispersed in an acidic aqueous solution.
  • the whiteness in the dried container is visually determined. It is considered good if the degreasing and de-smutting has a complete and fully etched white appearance, and the following 5 grades are evaluated according to the whitening 3 ⁇ 4 ⁇ .
  • the detergent used for the evaluation of detergency was diluted 20 times with water, heated with an electric heater (60.C, 1 day), and the state of sludge fixation in the electric heater was evaluated in three steps.
  • Example 14 of Table 1 two types of chelating dispersants are used. Table 2 Evaluation results
  • Example 3 The same procedure as in Example 3 was carried out using the cleaning agent of Example 3 with the addition of 0.04 g Z1 of bromine ion. The results were the same as in Example 3, and each evaluation item was good.
  • ORP is 0.60 by changing the addition S of H 2 0 2 in the aqueous solution (water temperature 70 ° C), 0. 50, was used to evaluate the performance of the time 0. 45V (V s. AgZAg C 1). Table 4
  • the above containers were sprayed with each cleaning agent at 70 ° C for 60 seconds, then washed with water for 15 seconds, followed by deionized water for 5 seconds, and dried at 95 ° C.
  • the acidic cleaning aqueous solution composed of the addition amounts described in the examples shown in Table 5 below was heated to 70 liters, and hydrogen peroxide was added dropwise with stirring.
  • the amount of hydrogen peroxide theoretically required is a, and the amount The oxidation efficiency was calculated by the following equation.
  • Table 6 shows the beams.
  • the appearance, water wettability and de-smuttability are based on the evaluation criteria used in the evaluations of the above Examples 1 to 16 and Comparative Examples 1 to 4.
  • a product having an aluminum surface for example, an aluminum-based metal, that is, an aluminum container for beverages made of aluminum or an aluminum alloy is manufactured by a forming operation called drawing and ironing (hereinafter, referred to as DI processing).
  • DI processing drawing and ironing
  • the present invention can be applied to a cleaning aqueous solution and a cleaning method for removing lubricating oil and aluminum powder (smart) attached to a metal surface.

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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)

Abstract

L'invention concerne une solution aqueuse et acide servant à nettoyer de l'aluminium. Cette solution contient des ions métal oxydés comme accélérateur d'attaque, mais sans ions fluor ni chrome présentant un danger. Elle contient également un acide inorganique, des ions métalliques oxydés, un dispersant chélaté ains qu'un agent tensioactif, le cas échéant, et, de surcroît, un agent oxydant pour les ions métalliques réduits par nettoyage. La présence du dispersant a pour effet d'empêcher la formation d'un dépôt à partir du métal oxydé, ce qui permet d'élaborer une solution aqueuse et acide n'en comportant pas.
PCT/JP1995/001171 1994-10-21 1995-06-12 Solution aqueuse et acide servant a nettoyer de l'aluminium et methode de nettoyage afferente WO1996012832A1 (fr)

Priority Applications (2)

Application Number Priority Date Filing Date Title
KR1019970702506A KR100231390B1 (ko) 1994-10-21 1995-06-12 알루미늄계 금속의 산성 세정수용액 및 그 세정방법
EP95921156A EP0789094A4 (fr) 1994-10-21 1995-06-12 Solution aqueuse et acide servant a nettoyer de l'aluminium et methode de nettoyage afferente

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
JP6/256346 1994-10-21
JP25634694A JP3192562B2 (ja) 1993-11-05 1994-10-21 アルミニウム系金属の酸性洗浄水溶液及びその洗浄方法

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Publication Number Publication Date
WO1996012832A1 true WO1996012832A1 (fr) 1996-05-02

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Country Link
EP (1) EP0789094A4 (fr)
KR (1) KR100231390B1 (fr)
CN (1) CN1063236C (fr)
WO (1) WO1996012832A1 (fr)

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Publication number Priority date Publication date Assignee Title
JP4303365B2 (ja) * 1998-07-30 2009-07-29 日本ペイント株式会社 アルミニウム系金属の洗浄水溶液およびその洗浄方法
JP2001226790A (ja) * 2000-02-15 2001-08-21 Nippon Paint Co Ltd アルミニウム材用酸性洗浄液およびその洗浄方法
GB0314900D0 (en) * 2003-06-26 2003-07-30 Natech Ltd Cleaning material
GB0500071D0 (en) * 2005-01-05 2005-02-09 Houghton Australia Pty Ltd Cleaning formulation
CN101205609B (zh) * 2006-12-18 2010-08-11 比亚迪股份有限公司 一种镁合金表面活化用组合物
CN101381877B (zh) * 2007-09-04 2010-12-01 北京北方微电子基地设备工艺研究中心有限责任公司 精密零件的清洗方法
FR2941241B1 (fr) * 2009-01-22 2011-05-27 Airbus France Procede et solution de decapage sans chrome hexavalent d'une surface en aluminium ou en alliage d'aluminium et procede de traitement comprenant au moins une etape de decapage par ce procede.
CN102373340A (zh) * 2010-08-23 2012-03-14 北京化工大学 一种从复合推进剂中回收铝粉方法
DE102012104951A1 (de) * 2012-06-08 2013-12-12 Stockmeier Chemie GmbH & Co.KG Verwendung einer phosphonsäure- und/oder phosphonsäurederivathaltigen Lösung bei der Entfettung von Metalloberflächen, entfettende Lösung und Verfahren zur Entfettung einer Metalloberfläche
JP5580948B1 (ja) * 2013-09-27 2014-08-27 日本ペイント株式会社 アルミニウム缶の表面処理方法
CN104593793B (zh) * 2015-02-12 2018-08-28 佛山市仁昌科技有限公司 一种铝和铝合金表面预处理中和液
KR101629336B1 (ko) * 2015-09-02 2016-06-10 (주)아인스 알루미늄 부재의 세정 방법
CN105908239A (zh) * 2016-05-31 2016-08-31 刘洪建 一种提高铝及铝合金表面强度的处理方法
KR101709303B1 (ko) * 2016-11-10 2017-02-22 우지훈 산세정 효과를 증진시키는 용액조성물
CN106835165A (zh) * 2017-03-06 2017-06-13 上海赛敏环保科技有限公司 铝合金除霉斑清洗剂及清洗应用方法
EP3620502A1 (fr) * 2018-09-10 2020-03-11 Carl Bechem Gmbh Composition destiné à la production d'une composition lubrifiante
CN110512210A (zh) * 2019-09-28 2019-11-29 立邦涂料（重庆）化工有限公司 一种无氟低温腐蚀剂及制备方法

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Also Published As

Publication number Publication date
KR100231390B1 (ko) 1999-12-01
CN1170443A (zh) 1998-01-14
EP0789094A1 (fr) 1997-08-13
CN1063236C (zh) 2001-03-14
KR970707324A (ko) 1997-12-01
EP0789094A4 (fr) 1998-01-14

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