Source: http://www.google.com/patents/US4828615
Timestamp: 2018-01-20 11:33:11
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Patent US4828615 - Process and composition for sealing a conversion coated surface with a ... - Google Patents
A solution containing pentavalent vanadium is applied to a metal surface subsequent to conversion coating. The solution contains pentavalent vanadium ions which may be obtained from a sodium metavanadate or sodium metavanadate/orthovanadate solution that is acidified with an acid. Vanadium pentoxide...http://www.google.com/patents/US4828615?utm_source=gb-gplus-sharePatent US4828615 - Process and composition for sealing a conversion coated surface with a solution containing vanadium
Publication number US4828615 A
Application number US 07/028,922
Publication number 028922, 07028922, US 4828615 A, US 4828615A, US-A-4828615, US4828615 A, US4828615A
Inventors Thomas W. Cape
Patent Citations (8), Referenced by (35), Classifications (7), Legal Events (6)
Process and composition for sealing a conversion coated surface with a solution containing vanadium
US 4828615 A
1. An aqueous solution for rinsing metal surfaces subsequent to a conversion coating, consisting essentially of an aqueous solution including pentavalent vanadium formed from at least one liquid concentrate which when combined in a working bath contains:
(a) from 10 to 100 parts per million a vanadium-containing compound selected from the group consisting of vanadium pentoxide, alkali metal vanadate, ammonium vanadate, vandium pentafluoride, vanadium oxytrichloride, vanadyl-containing species, vanadium tetroxide, vanadium tetrachloride, vanadium tetrafluoride, vanadium trichloride, vanadium dichloride, and vanadium metal;
(b) an alkali selected from the group consisting of alkali metal hydroxide, alkali metal oxide, and ammonium hydroxide; and
(c) an acid selected from the group consisting of nitric acid, phosphoric acid, sulfuric acid, hydrofluoric acid, hydrochloric acid, hydrobromic acid, hydroiodic acid, fluoroboric acid, fluosilicic acid, mono-fluorophosphoric acid, hexafluorophosphoric acid, fluorosulfuric acid, perchloric acid, perbromic acid, periodic acid, phytic acid, carboxylic acid and sulfonic acid, and wherein the aqueous solution has a pH of about 4 to 4.5.
2. An aqueous solution for sealing metal surfaces subsequent to a conversion coating as recited in claim 1 consisting essentially of, in weight percent:
______________________________________0.0018 to 0.18%    Vanadium Pentoxide0.0008 to 1.0%     Sodium Hydroxide0.0010 to 1.0%     Nitric Acid.______________________________________
3. An aqueous solution for sealing metal surfaces subsequent to a conversion coating as recited in claim 1 consisting essentially of, in weight percent:
______________________________________0.005 to 0.04%   Vanadium Pentoxide0.004 to 0.045%  Sodium Hydroxide0.005 to 0.05%   Nitric Acid0.001 to 0.005%  Hydrogen Peroxide (30%).______________________________________
4. An aqueous solution for sealing metal surfaces subsequent to a conversion coating as recited in claim1 consisting essentially of, in weight percent:
______________________________________0.018%            Vanadium Pentoxide0.001875%         Sodium Hydroxide0.0118%           Nitric Acid.______________________________________
5. An aqueous solution for sealing metal surfaces subsequent to a conversion coating as recited in claim 1 consisting essentially of, in weight percent:
______________________________________0.0018 to 0.18%  Vanadium Pentoxide0.0008 to 1.0%   Sodium Hydroxide0.0010 to 1.0%   Ammonium Bifluoride.______________________________________
6. An aqueous solution for sealing metal surfaces subsequent to a conversion coating as recited in claim 5 consisting essentially of, in weight percent:
______________________________________0.005 to 0.04%   Vanadium Pentoxide0.004 to 0.045%  Sodium Hydroxide0.005 to 0.05%   Ammonium Bifluoride0.001 to 0.005%  Hydrogen Peroxide (30%).______________________________________
7. An aqueous solution for sealing metal surfaces subsequent to a conversion coating as recited in claim 1 consisting essentially of, in weight percent:
______________________________________0.018%           Vanadium Pentoxide0.001875%        Sodium Hydroxide0.0117%          Ammonium Bifluoride.______________________________________
8. A concentrate for making an aqueous solution for the treatment of conversion coated metal surfaces, said aqueous solution having pentavalent vanadium ions, said concentrate comprising:
(a) a first aqueous solution consisting essentially of alkali metal hydroxide, and from 10 to 1000 parts per million vanadium pentoxide, said first solution being diluted with water to form a working bath; and
(b) a second aqueous solution consisting essentially of at least one member selected from the group consisting of nitric acid, ammonium bifluoride, and glycolic acid, said second solution being added to said working bath to lower the pH of the working bath to about 4 to 4.5.
9. The concentrate of claim 8 wherein said first solution is diluted on a volume to volume basis at a ratio of from 1 part per 80 to 1 part per 8000.
12. The concentrate of claim 8 wherein said first solution comprises consisting essentially of, in weight percent:
12.8% vanadium pentoxide,
6.2% sodium hydroxide,
0.8% hydrogen peroxide,
80.1% water; and
said second solution comprises:
31.2% nitric acid
13. The concentrate of claim 8 wherein said first solution consisting essentially of, in weight percent:
80. 1% water; and
31.3% ammonium bifluoride
68.7% water.
______________________________________V.sub.2 O.sub.5        vanadium pentoxideNH.sub.4 VO.sub.3        ammonium meta-vanadate, ammonium        vanadateNaVO.sub.3   sodium meta-vanadate (alkali metal        meta-vanadate)VOSO.sub.4   vanadyl sulfateVF.sub.5     vanadium pentafluorideNa.sub.3 VO.sub.4        sodium ortho-vanadate (alkali metal        ortho-vanadateV.sub.2 O.sub.4        vanadium tetroxideVCl.sub.4    vanadium tetrachlorideVFl.sub.4    vanadium tetrafluorideVCl.sub.3    vanadium trichlorideVOCl.sub.3   vanadium oxy trichloride(VO).sup.2+ X.sub.N        vanadyl containing speciesVCl.sub.2    vanadium dichlorideV            vanadium metal______________________________________
______________________________________HNO.sub.3      nitric acidH.sub.3 PO.sub.4          phosphoric acidH.sub.2 SO.sub.4          sulfuric acidHBF.sub.4      fluoroboric acidHF             hydroflouric acidHCl            hydroch1oric acidHBr            hydrobromic acidHI             hydroiodic acidH.sub.2 SiF.sub.6          fluosilicic acidHPF.sub.6      hexaflouro phosphoric acidHClO.sub.4     perchloric acidNH.sub.4 HF.sub.2          ammonium bifluorideH.sub.2 PO.sub.3 F          monofluoro phosphoric acidHPF.sub.6      hexafluoro phosphoric acidHBrO.sub.4     perbromic acidHIO.sub.4      periodic acidHSO.sub.3 NH.sub.2          sulfamic acid______________________________________
______________________________________NaOH            sodium hydroxideKOH             potassium hydroxideNH.sub.4 OH     ammonium hydroxideNa.sub.2 CO.sub.3           sodium carbonateNaVO.sub.3      sodium meta-vanadateNa.sub.3 VO.sub.4           sodium ortho-vanadateNH.sub.4 VO.sub.3           ammonium meta-vanadate(NH.sub.4).sub.2 CO.sub.3           diammonium carbonate______________________________________
__________________________________________________________________________Name of raw  Chemical             Best Preferred                           Broadmaterial     formula             %    range %  range %__________________________________________________________________________Vanadium Pentoxide        V.sub.2 O.sub.5             0.018%                  0.005%-0.04%                           0.0018%-0.18%Sodium Hydroxide        NaOH 0.00875%                  0.004-0.045%                           0.0008-1.0%Hydrogen Peroxide (30%)        H.sub.2 O.sub.2             0.0015%                  0.001-0.005%                           0.0005-1.0%(30%)Nitric Acid  HNO.sub.3             0.0118%                  0.005-0.050%                            0.001-1.0%Water        H.sub.2 O             Balance                  Balance  Balance__________________________________________________________________________
Steel test panels and galvanized test panels were cleaned first by wiping with a solvent based cleaner, commercially available available as Chemkleen 212, followed by spray application of an alkaline prephosphate cleaner, commercially available as Chemkleen 42, at 140° F. for sixty seconds. The panels were sprayed with a solution containing Jernstedt salts, commercially available as Rinse Conditioner from Chemfil Corporation, at 140° F. for sixty seconds. The panels were then phosphated with a zinc phosphate bath, commercially available as Chemfos 168, at 128° F. for sixty seconds and spray rinsed with ambient tap water for thirty seconds. The description of the panel processing contained in U.S. Pat. No. 4,330,345 is incorporated herein by reference.
The final rinse of the present invention was spray applied at room temperature for thirty seconds followed by a deionized water rinse at room temperature for fifteen seconds. The panels were then dried at 275° F. for five minutes. PPG Corporation's Uniprime ED 3150 was applied to the panels and baked. An enamel top coat, CIL-type, was applied and baked.
______________________________________Material             Wt______________________________________H.sub.2 O            Balance to                100    mlNaOH (pellets)       4.0    gV.sub.2 O.sub.5      0.9    gHNO.sub.3            8.5    g______________________________________ Dilution: 50:1 in water
______________________________________Material             Wt______________________________________H.sub.2 O            Balance to                100    mlNaOH (pellets)       4.0    gV.sub.2 O.sub.5      1.8    gH.sub.2 O.sub.2 (30%)                3.3    gHNO.sub.3            8.5    g______________________________________ Dilution: 100:1 in water
______________________________________Part 1              Part 2Material     Wt             Material                               Wt______________________________________H.sub.2 O    Balance to     H.sub.2 O                               Balance to        400    ml              100  mlNaOH (pellets)        28.0   g       HNO.sub.3                               34.0 gV.sub.2 O.sub.5        57.6   gH.sub.2 O.sub.2        4.8    g______________________________________ Dilution: Part 1 800:1 in water Part 2 2830:1 in water
______________________________________Material             Wt______________________________________H.sub.2 O            Balance to                100    mlNaOH                 4.0    gV.sub.2 O.sub.5      0.9    gGlycolic Acid        7.6    g______________________________________ Dilution: 50:1 in water
______________________________________Material             Wt______________________________________H.sub.2 O            Balance to                100    mlNaOH                 4.0    gV.sub.2 O.sub.5      3.6    gCitric Acid          15.4   g______________________________________ Dilution: 200:1 in water
______________________________________Part 1              Part 2Material    Wt              Material                              Wt______________________________________H.sub.2 O   Balance to      H.sub.2 O.sub.2                              100%       100    mlNaOH        4.00   gV.sub.2 O.sub.5       3.61   gCitric Acid 15.4   g______________________________________ Dilution: Part 1 200:1 in water Part 2 1333:1 in water
______________________________________Part 1             Part 2Material    Wt             Material Wt______________________________________H.sub.2 O   Balance to     H.sub.2 O.sub.2 (30%)                               100%       100    mlNaOH        4.0    gV.sub.2 O.sub.5       3.6    gCitric Acid 15.4   g______________________________________ Dilution: Part 1 200:1 in water Part 2 667:1 in water
______________________________________Part 1             Part 2Material    Wt             Material                              Wt______________________________________H.sub.2 O   Balance to     H.sub.2 O                              Balance to       100    ml              100  mlNaOH        4.00   g       NaNO.sub.3                              25.5 gV.sub.2 O.sub.5       3.6    gCitric Acid 15.4   g______________________________________ Dilution: Part 1 200:1 in water Part 2 500:1 in water
__________________________________________________________________________Part 1        Part 2      Part 3Material  Wt     Material                Wt   Material                           Wt__________________________________________________________________________H.sub.2 O  Balance to         H.sub.2 O.sub.2 (30%)                100% H.sub.2 O                           Balance to  100     ml                    100 mlNaOH   4.0     g               Ammonium                           17.5                               gV.sub.2 O.sub.5  3.6     g               MolybdateCitric Acid  15.4     g__________________________________________________________________________ Dilution: Part 1 200:1 in water Part 2 667:1 in water Part 3 500:1 in water
__________________________________________________________________________Part 1      Part 2     Part 3      Part 4Material Wt    Material              Wt  Material                        Wt    Material  Wt__________________________________________________________________________H.sub.2 O Balance to       H.sub.2 O.sub.2 (30%)              100%                  H.sub.2 O                        Balance to                              H.sub.2 O Balance to 100    ml                  100                           ml           100                                           mlNaOH  4.0    g             Ammonium                        17.5                           g  Titanium potassium                                        3.5                                           gV.sub.2 O.sub.5 3.6    g             Molybdate   oxalateCitric Acid 15.4    g__________________________________________________________________________ Dilution: Part 1 200:1 in water Part 2 667:1 in water Part 3 500:1 in water Part 4 50:1 in water
______________________________________Part 1              Part 2Material    Wt              Material Wt______________________________________H.sub.2 O   Balance to      H.sub.2 O.sub.2 (30%)                                 100%       100    mlNaOH        4.0    gV.sub.2 O.sub.5       0.9    gGlycolic Acid       7.6    g______________________________________ Dilution: Part 1 50:1 in water Part 2 1333:1 in water
______________________________________Part 1            Part 2Material   Wt             Material Wt______________________________________H.sub.2 O  Balance to     H.sub.2 O                              Balance to      100    ml               100  mlNaOH       4.0    g       Al(NO.sub.3).sub.3                              37.5 gV.sub.2 O.sub.5      1.8    g       9H.sub.2 OH.sub.2 O.sub.2 (30%)      3.3    gHNO.sub.3  8.5    g______________________________________ Dilution: Part 1 100:1 in water Part 2 250:1 in water
__________________________________________________________________________Part 1       Part 2      Part 3Material Wt     Material               Wt   Material                            Wt__________________________________________________________________________H.sub.2 O Balance to        H.sub.2 O.sub.2 (30%)               100% H.sub.2 O                            Balance to 100    ml                      100 mlNaOH  4.0    g               K.sub.2 TiO(C.sub.2 O.sub.4).sub.2                            3.5 gV.sub.2 O.sub.5 0.9    g               2H.sub.2 OHNO.sub.3 8.5    g__________________________________________________________________________ Dilution: Part 1 50:1 in water Part 2 1333:1 in water Part 3 50:1 in water
______________________________________Part 1            Part 2Material   Wt             Material Wt______________________________________H.sub.2 O  Balance to     H.sub.2 O                              Balance to      400    ml                 100  mlNaOH       28.0   g         NH.sub.4 HF.sub.2                                34.2 gV.sub.2 O.sub.5      57.6   gH.sub.2 O.sub.2      4.8    g______________________________________ Dilution: Part 1 800:1 in water Part 2 2930:1 in water
The GSC test is a four week test with each week of testing consisting of five twenty-four hour cycles comprising immersion in a 5% sodium chloride solution at room temperature followed by a 75 minute drying cycle at room temperature followed by 22.5 hours at 85% relative humidity at 140° F. The panels are maintained at 140° F. at 85% relative humidity over the two-day period to complete the week. Prior to testing, the test panels are scribed with a carbide tipped scribing tool. After the testing cycle is complete, the scribe is evaluated by simultaneously scraping the paint and blowing with an air gun. The test results were reported as rated from 0, indicating a total paint loss, to 5, indicating no paint loss.
The FSC test is the same as the GSC test except the test is for ten weeks and the temperature during the humidity exposure portion of the test is set at 120° F. and the scribe is evaluated by applying Scotch Brand 898 tape and removing it and rating as above.
The ASC test is comprised on 98 twelve hour cycles wherein each cycle consists of a four and three-quarter hour 95 to 100% humidity exposure followed by a 15 minute salt fog followed by seven hours of low humidity (less than 50 percent humidity) drying at 120° F. The ASC test is evaluated in the same way as the FSC test.
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U.S. Classification 106/14.13, 106/14.21, 106/14.14, 106/14.44
International Classification C23C22/83