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US4851148A Expired / Lapsed US ⏱️ 0.0 years remaining

Method of controlling an aluminum surface cleaning composition

Assignee: Henkel Corp
•
Filing: 1986-04-03
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Granted: 1989-07-25
•
Expires: 2006-04-03
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Abstract

Abstract In chromium-free aqueous acidic washing solutions for cleaning the surfaces of aluminum and aluminum-alloy particles, so as to remove therefrom smut and lubricating oil left on the surfaces thereof after metal forming operations, which solutions contain from 0.2 to 4 g/l ferric ion and sufficient sulfuric and/or nitric acid to impart a pH of 2 or less to the solutionh (and which optionally may also contain fluoride ions up to a concentration of 0.5 g/l) there is provided a method of controlling the effectiveness of the washing solution in which the ferric ion concentration therein is monitored, conveniently by the oxidation-reduction potential of the washing solution, as shown in FIG. 3, and is controlled within the desired limits by adding when appropriate suitable amounts of oxidant capable of oxidizing ferrous ions to ferric ions and, separately or in conjunction therewith, a replenisher containing a source of iron ions.

Inventors

  • 👤 Katsuyoshi Yamasoe
  • 👤 Satoshi Ikeda
  • 👤 Kiyotada Yasuhara

Bibliographic Details

Application Number —
Jurisdiction US
Data Source google_patents
Last Synchronized 2026-10-28 14:59
CPC Classifications
C; C23; C23G; C23G1/00; C23G1/02; C23G1/12; C23G1/125

Claims Analysis

Total Claims: 30
Claim 1
Independent Claim 152 words
In a process for cleaning an aluminum surface comprising the steps of a. contacting said aluminum surface with a chromium-free acidic aqueous cleaning solution consisting of from about 0.2 to about 4 g/l of ferric ions, a quantity of sulfuric and/or nitric acid to provide a pH for the cleaning solution of 2.0 or less, and up to 0.5 g/l of fluoride ions; the improvement comprising: b. monitoring the ferric ion concentration in the cleaning solution; c. when the ferric ion concentration falls below a predetermined level, restoring the ferric ion concentration to at least said predetermined level by adding to the cleaning solution an oxidant compatible with a clean aluminum surface in an amount sufficient to oxidize ferrous ions present in the cleaning solution to ferric ions; and d. replenishing the iron ion concentration in the cleaning solution as needed by the addition thereto of at least one water-soluble iron compound.
Claim 2
Dependent Claim 152 words
In a process for cleaning an aluminum surface comprising the steps of a. contacting said aluminum surface with a chromium-free acidic aqueous cleaning solution consisting of from about 0.2 to about 4 g/l of ferric ions, a quantity of sulfuric and/or nitric acid to provide a pH for the cleaning solution of 2.0 or less, and up to 0.5 g/l of fluoride ions; the improvement comprising: b. monitoring the ferric ion concentration in the cleaning solution; c. when the ferric ion concentration falls below a predetermined level, restoring the ferric ion concentration to at least said predetermined level by adding to the cleaning solution an oxidant compatible with a clean aluminum surface in an amount sufficient to oxidize ferrous ions present in the cleaning solution to ferric ions; and d. replenishing the iron ion concentration in the cleaning solution as needed by the addition thereto of at least one water-soluble iron compound.
Claim 3
Dependent Claim 14 words
In a process according to claim 1 wherein the cleaning solution is substantially fluoride-free.
Claim 4
Dependent Claim 28 words
In a process according to claim 1 wherein in step b. the ferric ion concentration is monitored by a measurement of the oxidation-reduction potential of the cleaning solution.
Claim 5
Dependent Claim 26 words
In a process according to claim 1 wherein in step c. the oxidant is one or more of a peroxide, nitrite, peroxosulfate, metavanadate or cerium compound.
Claim 6
Dependent Claim 27 words
In a process according to claim 4 wherein the oxidant is one or more of hydrogen peroxide, sodium nitrite, sodium peroxosulfate, ammonium metavanadate, and cerium ammonium sulfate.
Claim 7
Dependent Claim 23 words
In a process according to claim 1 wherein in step d. the water-soluble iron compound is selected from ferric sulfate and ferric nitrate.
Claim 8
Dependent Claim 31 words
In a process according to claim 1 wherein in step a. the ferric ions are present in the form of one or more of ferric sulfate, ferric nitrate, and ferric chlorate.
Claim 9
Dependent Claim 28 words
In a process according to claim 1 wherein in step a. the cleaning solution also contains from about 0.5 to about 4 g/l of a surface active agent.
Claim 10
Dependent Claim 19 words
In a process according to claim 1 wherein in step a. the cleaning solution also contains a chelating agent.
Claim 11
Dependent Claim 23 words
In a process according to claim 9 wherein the chelating agent is one or more of citric acid, oxalic acid, and tartaric acid.
Claim 12
Dependent Claim 34 words
In a process according to claim 1 wherein in step a. said contacting is carried out by immersion or spray at a temperature within the range of about 20° C. to about 80° C.
Claim 13
Dependent Claim 31 words
In a process according to claim 1 wherein in step c. the predetermined level of ferric ion is a quantity within the range of from about 0.2 to about 4 g/l.
Claim 14
Dependent Claim 46 words
In a process according to claim 1 including monitoring the pH of the solution and when the pH is greater than about 2.0, a quantity of sulfuric and/or nitric acid is added to the bath to lower the pH to between about 0.6 and about 2.0.
Claim 15
Dependent Claim 34 words
In a process according to claim 1 wherein in step d. the water-soluble iron compound is a ferrous compound which is added together with sufficient oxidant to oxidize the ferrous ions to ferric ions.
Claim 16
Dependent Claim 50 words
In a process according to claim 1 including monitoring the pH of the solution and when the pH is greater than a predeterminal pH level below 2.0, a quantity of sulfuric and/or nitric acid is added to the bath to lower the pH to between about 0.6 and about 2.0.
Claim 17
Dependent Claim 120 words
In a process for cleaning an aluminum surface comprising the steps of a. contacting said aluminum surface with a chromium-free acidic aqueous cleaning solution consisting of from about 0.2 to about 4 g/l of ferric ions, a quantity of sulfuric and/or nitric acid to provide a pH for the cleaning solution of 2.0 or less, and up to 0.5 g/l of fluoride ions; the improvement comprising: b. maintaining in the cleaning solution an oxidant compatible with a clean aluminum surface in an amount sufficient to oxidize ferrous ions present in the cleaning solution to ferric ions; and c. replenishing the iron ion concentration in the cleaning solution as needed by the addition thereto of at least one water-soluble iron compound.
Claim 18
Dependent Claim 120 words
In a process for cleaning an aluminum surface comprising the steps of a. contacting said aluminum surface with a chromium-free acidic aqueous cleaning solution consisting of from about 0.2 to about 4 g/l of ferric ions, a quantity of sulfuric and/or nitric acid to provide a pH for the cleaning solution of 2.0 or less, and up to 0.5 g/l of fluoride ions; the improvement comprising: b. maintaining in the cleaning solution an oxidant compatible with a clean aluminum surface in an amount sufficient to oxidize ferrous ions present in the cleaning solution to ferric ions; and c. replenishing the iron ion concentration in the cleaning solution as needed by the addition thereto of at least one water-soluble iron compound.
Claim 19
Dependent Claim 14 words
In a process according to claim 16 wherein the cleaning solution is substantially fluoride-free.
Claim 20
Dependent Claim 26 words
In a process according to claim 16 wherein in step b. the oxidant is one or more of a peroxide, nitrite, peroxosulfate, metavanadate or cerium compound.
Claim 21
Dependent Claim 27 words
In a process according to claim 18 wherein the oxidant is one or more of hydrogen peroxide, sodium nitrite, sodium peroxosulfate, ammonium metavanadate, and cerium ammonium sulfate.
Claim 22
Dependent Claim 23 words
In a process according to claim 16 wherein in step c. the water-soluble iron compound is selected from ferric sulfate and ferric nitrate.
Claim 23
Dependent Claim 31 words
In a process according to claim 16 wherein in step a. the ferric ions are present in the form of one or more of ferric sulfate, ferric nitrate, and ferric chlorate.
Claim 24
Dependent Claim 28 words
In a process according to claim 16 wherein in step a. the cleaning solution also contains from about 0.5 to about 4 g/l of a surface active agent.
Claim 25
Dependent Claim 19 words
In a process according to claim 16 wherein in step a. the cleaning solution also contains a chelating agent.
Claim 26
Dependent Claim 23 words
In a process according to claim 23 wherein the chelating agent is one or more of citric acid, oxalic acid, and tartaric acid.
Claim 27
Dependent Claim 34 words
In a process according to claim 16 wherein in step a. said contacting is carried out by immersion or spray at a temperature within the range of about 20° C. to about 80° C.
Claim 28
Dependent Claim 46 words
In a process according to claim 16 including monitoring the pH of the solution and when the pH is greater than about 2.0, a quantity of sulfuric acid/or nitric acid is added to the bath to lower the pH to between about 0.6 and about 2.0.
Claim 29
Dependent Claim 34 words
In a process according to claim 16 wherein in step c. the water-soluble iron compound is a ferrous compound which is added together with sufficient oxidant to oxidize the ferrous ions to ferric ions.
Claim 30
Dependent Claim 50 words
In a process according to claim 16 including monitoring the pH of the solution and when the pH is greater than a predetermined pH level below 2.0, a quantity of sulfuric and/or nitric acid is added to the bath to lower the pH to between about 0.6 and about 2.0.

References Cited (Backward Citations)

US3728188A Cited
US3993575A Cited
US4435223A Cited

USPTO Annuity & Maintenance Windows

Annuity Stage Window Opens Payment Deadline Surcharge Period Until Estimated Fee Status
3.5 Years (Year 4) 1992-07-24 1993-01-23 1993-07-25 $2000.00 Window Closed / Lapsed
7.5 Years (Year 8) 1996-07-24 1997-01-23 1997-07-25 $3760.00 Window Closed / Lapsed
11.5 Years (Year 12) 2000-07-24 2001-01-23 2001-07-25 $7700.00 Window Closed / Lapsed

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