CN106756929A - A kind of passivating solution and preparation method thereof - Google Patents
A kind of passivating solution and preparation method thereof Download PDFInfo
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- CN106756929A CN106756929A CN201610233890.XA CN201610233890A CN106756929A CN 106756929 A CN106756929 A CN 106756929A CN 201610233890 A CN201610233890 A CN 201610233890A CN 106756929 A CN106756929 A CN 106756929A
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- passivating solution
- passivating
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- 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
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C22/00—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
- C23C22/05—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions
- C23C22/06—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions using aqueous acidic solutions with pH less than 6
- C23C22/34—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions using aqueous acidic solutions with pH less than 6 containing fluorides or complex fluorides
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- 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
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C2222/00—Aspects relating to chemical surface treatment of metallic material by reaction of the surface with a reactive medium
- C23C2222/10—Use of solutions containing trivalent chromium but free of hexavalent chromium
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- Chemical Kinetics & Catalysis (AREA)
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- Chemical Treatment Of Metals (AREA)
Abstract
The invention provides a kind of passivating solution, the passivating solution is to be dissolved in deionized water forming by plurality of raw materials, wherein each material component proportioning is：The g/L of six water chromium sulfate 69, the g/L of cobalt sulfate 24；The g/L of sodium chlorate 48, the g/L of ammonium fluoride 23, the g/L of sulfuric acid 12, the g/L of citric acid 23, balance of water.Gained passivating film corrosion resisting property is good, and salt spray test can reach more than 120 hours, and, without any white rust or hickie, porosity is low, it is not necessary to processed using sealer for workpiece surface.
Description
Technical field
The present invention relates to metal conditioner field, in particular, it is related to a kind of passivating solution, preparation method and its makes
Use method..
Background technology
Zinc coat is one of most important protective coating of steel-iron components, and zinc coat is very stable in dry environment, but
In hot and humid environment, the corrosion resistance of zinc coat is poor, is also easy to produce white rust or hickie.It is general to use high concentration or medium dense
The chromatedsolution of degree is passivated to improve the corrosion resistance of zinc coat.In recent years, to reduce Cr VI to the pollution of environment and
Harm to human body, the direction that the chromating of zinc coat is passivated towards chromic salt and chromate-free is developed.
Chinese patent application 201210465245.2 discloses a kind of high corrosion resistant trivalent chromium bright blue passivation liquid, based on every liter
Calculate, by the chromium sulfate of 5-25g, the sodium fluoride of 2-8g, the sodium hypophosphite of 1-6g, the citric acid of 0.3-1.5g, the sodium sulphate of 1-5g,
The cobalt sulfate of 5-15g and the deionized water composition of surplus.But the passivating solution is not sufficiently stable in use, service life
It is shorter, have that voidage is larger, corrosion resistance is poor, the low shortcoming of adhesive force using later stage gained passivating film.
The content of the invention
An object of the present invention is to overcome the deficiencies in the prior art, there is provided a kind of passivating solution, the passivating solution makes
Relatively stable during, service life is more long, using initial stage, later stage, gained passivating film it is colored basically identical, voidage is all
It is all higher than relatively low, adhesive force, all with fabulous Corrosion Protection, resistance to neutral salt spray ability be all up to 120 hours with
On.
The second object of the present invention is the preparation method for providing above-mentioned passivating solution.
The third object of the present invention is the application method for providing above-mentioned passivating solution.
To achieve the above object, the technical solution adopted by the present invention is as follows：
A kind of passivating solution, the passivating solution is to be dissolved in deionized water forming by plurality of raw materials, wherein each material component proportioning is：
Six water chromium sulfate 6-9 g/L
Cobalt sulfate 2-4 g/L
Sodium chlorate 4-8 g/L
Ammonium fluoride 2-3 g/L
Sulfuric acid 1-2 g/L
Citric acid 2-3 g/L
Water surplus.
The wherein described preferred 6-8 g/L of six water chromium sulfates；
The preferred 3-4 g/L of wherein described cobalt sulfate；
The preferred 6-8 g/L of wherein described sodium chlorate；
The preferred 2.5-3g/L of wherein described ammonium fluoride；
The preferred 1.5-2 g/L of wherein described sulfuric acid；
Wherein described citric acid preferably 3 g/L；
The preparation method of passivating solution of the present invention, in turn includes the following steps：
(1) 3/5 volume of aequum deionized water is added in a reservoir, adds sulfuric acid, citric acid to stir to dissolving, mix；
(2) six water chromium sulfates, cobalt sulfate, sodium chlorate are added, stirring is to being completely dissolved；
(3) ammonium fluoride is added, stirring is to being completely dissolved；Deionized water to overall solution volume is added, is stirred evenly, you can obtain the present invention
Passivating solution.
The application method of passivating solution of the present invention, in turn includes the following steps：
（1）The steel galvanization workpiece for treating passivation carries out purified treatment；
（2）The passivating solution is controlled into 20-60 DEG C of temperature, treatment 30-60 seconds is passivated to the steel galvanization workpiece after purification；
（3）The steel galvanization workpiece after passivation is dried with 50-60 DEG C of hot blast.
Wherein, step（2）In, the method that the metalwork after described pair of purification is passivated treatment is preferably soaked or is sprayed,
The Passivation Treatment time can adjust according to workpiece passivating film color regime；If workpiece treatment quantity is more, and according to workpiece surface
Passivation layer quality condition suitably supplements passivating solution of the present invention to passivation working solution, maintains passivation working solution pH value 1.5-2.5, excellent
Choosing maintains passivation working solution pH value 1.8-2.0.
The choosing principles of passivating solution each component of the present invention and effect are as follows：
（1）Chromium sulfate：The Main Ingredients and Appearance of color passivation solution, there is provided trivalent chromium；
（2）Cobaltous sulfate：Adjustment passivation film color；
（3）Sodium chlorate：Oxidant, has solution and maintains appropriate oxidability, can also accelerate reaction speed；
（4）Ammonium fluoride：Film forming accelerating, accelerates passivating film and forms speed, and refines passivation film structure, makes passivating film color more
It is bright-coloured；
（5）Citric acid：The stability of complexing agent, control film forming speed and passivating solution；
（6）Sulfuric acid：Stabilizer, trivalent chromium valence state and pH value in stabilization passivation working solution, there is provided H+Ion so that workpiece surface
Zinc dissolving, serve activation workpiece surface metal zinc layers effect, dissolve generation zinc ion also participate in film forming, be to be formed
The main component of passivating film.
Passivating solution of the present invention forms the general principle of passivating film in steel galvanization workpiece surface：The metallic zinc of workpiece surface connects
Acid passivation working solution is touched, dissolving forms zinc ion, while the formation of zinc ion consumes acid, causes metal surface solution
PH rises, and trivalent chromium and zinc ion, cobalt ions etc. react in pH metallic zinc surface solution layers higher, and formation is not
Soluble compound, adsorbs, is deposited on zinc surface, so as to form the preferable passivating film of corrosion resistance of colour.
Passivating solution of the present invention has the beneficial effect that：
1. passivation operation is carried out under 20-60 DEG C of normal temperature, and passivation working solution stabilization, Chromating Film On Zn Deposits are preferable and easily controllable；
2. the passivation pH value range that is allowed of working solution is wide, easy to control, the color of epithelium, bright when between pH value 1.5~2.5
Degree, corrosion resistance are relatively stablized, and effect more preferably, maintains pH value to ensure that passivation effect, i.e. Film color are fresh during pH value 1.8~2.0
Gorgeous, in normal iris, and corrosion resisting property reaches requirement, can determine passivating solution by control ph or passivating film color
Magnitude of recruitment；
3. passivation working solution concentration is relatively low or pH value close to the upper limit when, it is blunt needed for can still being reached by proper extension passivation time
Change effect；
4. film forming speed speed is moderate, and passivation time length is moderate, is passivated by hand outside transfer matic or line all easy to implement；
5. consumption is few, and workpiece throughput is big, low production cost；
6. gained passivating film corrosion resisting property is good, and salt spray test can reach more than 120 hours（Workpiece surface is without any white rust or white
Spot）, porosity is low, it is not necessary to processed using sealer；
7. under certain conditions, the blue white passivating solutions of the alternative Cr3+ of trivalent chromium colour passivator, can reach preferable effect；
8., using the mode of operation of single dose, operator easily grasps aborning, not error-prone.
In the embodiment of the present invention, the neutral salt spray corrosion test of workpiece after Passivation Treatment（NSS）Method is：Reference
ISO3768 standards, the selected workpiece after Passivation Treatment is put into salt-mist corrosion tester, and salt solution contains 5%（wt）Sodium chloride, pH value
6.5~7.2, temperature (35 ± 2) DEG C, 1~2mL/ of amount of fog (hcm2), after 120 hours time, observation has non-corroding, there is rust
Corrosion area is then surveyed in erosion, calculates the percentage that corrosion area accounts for workpiece surface product.
Specific embodiment
Further detailed description is done to the present invention below in conjunction with specific embodiment.
Embodiment 1-10
Embodiment 1-10 sets forth the composition of passivating solution of the present invention, specifically as listed in table 1, wherein, the unit of dispensing numerical value
It is g/L.
The embodiment 1-10 of table 1 formula compositions
| Embodiment | 1 | 2 | 3 | 4 | 5 | 6 | 7 | 8 | 9 | 10 |
| Six water chromium sulfates | 5 | 5 | 6 | 6 | 7 | 7 | 8 | 8 | 9 | 9 |
| Cobalt sulfate | 2 | 4 | 3 | 4 | 2 | 3 | 4 | 2 | 4 | 3 |
| Sodium chlorate | 4 | 7 | 6 | 5 | 8 | 6 | 7 | 4 | 5 | 8 |
| Ammonium fluoride | 2 | 3 | 2.5 | 2 | 3 | 2.5 | 2 | 3 | 2 | 3 |
| Sulfuric acid | 1 | 2 | 1.5 | 2 | 1 | 1.5 | 2 | 1 | 1.5 | 2 |
| Citric acid | 2 | 3 | 2 | 3 | 2 | 3 | 3 | 2 | 3 | 2 |
| Deionized water | Surplus | Surplus | Surplus | Surplus | Surplus | Surplus | Surplus | Surplus | Surplus | Surplus |
The preparation method of above example 1-10 passivating solutions is as follows：As a example by preparing 1000ml passivating solutions, successively including following step
Suddenly：600ml deionized waters are added in 2000ml beakers, adds sulfuric acid, citric acid to stir to dissolving, mix；Add six water sulphur
Sour chromium, cobalt sulfate, sodium chlorate, stirring is to being completely dissolved；Ammonium fluoride is added, stirring is to being completely dissolved；Add deionized water
To overall solution volume 1000ml, stir evenly, you can obtain passivating solution of the present invention.
Comparative example 11-13
Table 2 is the formula as the comparative example 1-3 trivalent blue-white chromating liquid of prior art, and the unit of each dispensing numerical value is g/L.
The comparative example 1-3 trivalent blue-white chromating formula of liquid of table 2
| Comparative example | 11 | 12 | 13 |
| Chromium sulfate | 10 | 10 | 25 |
| Sodium hypophosphite | 5 | 3 | 5 |
| Citric acid | 0.3 | 1 | 1.5 |
| Sodium sulphate | 2 | 3 | 5 |
| Cobalt sulfate | 5 | 10 | 10 |
| Sodium fluoride | 5 | 4 | 8 |
| Deionized water | Surplus | Surplus | Surplus |
The preparation method of above comparative example 11-13 passivating solutions is as follows, respectively with liquid 1000ml：600ml is added in 2000ml beakers
Deionized water, adds chromium sulfate to stir to being completely dissolved；Citric acid is added, stirring is to being completely dissolved；Add sodium hypophosphite, sulfuric acid
Sodium, stirring is to being completely dissolved；Cobalt sulfate is added, stirring is to being completely dissolved；Sodium fluoride is added, deionized water to solution is added
Cumulative volume 1000ml, persistently stirs 2 hours.
It is below test piece just to complete No. 45 steel thin slice galvanized parts that are zinc-plated and washing, is described separately above example 1-10
Passivating solution, the application method of comparative example 1-3 trivalent blue-white chromating liquid and passivation effect, specimen size are all 120x120x2mm,
100 above-mentioned test pieces, at 25 DEG C, are passivated treatment, passivation time 60 seconds, test piece warp after passivation by passivating solution 100ml successively
After 60 DEG C of deionized water rinsings, then with 60 DEG C of hot-air seasoning.The passivation situation situation consistent with color and luster of every test piece is observed, point
Not taking the 10th, 30,50,70,100 carries out neutral salt spray corrosion test.For the examination of comparative example 1-3 trivalent blue-white chromating liquid
Piece also have passed through 0.5% sulfuric acid activated and deionized water washing process in advance.
Above example, the using effect of comparative example are shown in Table 3, table 4 respectively.
The using effect of the embodiment 1-10 passivating solutions of table 3
| Embodiment | 1 | 2 | 3 | 4 | 5 | 6 | 7 | 8 | 9 | 10 |
| Passivating film color | Uniform color | Uniform color | Uniform color | Uniform color | Uniform color | Uniform color | Uniform color | Uniform color | Uniform color | Uniform color |
| Neutral salt spray is rotten Corrosion test | Workpiece surface without White rust or hickie | Workpiece surface without White rust or hickie | Workpiece surface without White rust or hickie | Workpiece surface without White rust or hickie | Workpiece surface without White rust or hickie | Workpiece surface without White rust or hickie | Workpiece surface without White rust or hickie | Workpiece surface without White rust or hickie | Workpiece surface without White rust or hickie | Workpiece surface is without white rust Or hickie |
The using effect of the comparative example 1-3 passivating solutions of table 4
| Comparative example | 1 | 2 | 3 |
| Passivating film color | Blue and white | Blue and white | Blue and white |
| Neutral salt spray corrosion test（Workpiece surface whether there is white rust or hickie, or corrosion area） | 0.1% | 0.2% | Nothing |
Embodiment 14
With the passivating solution 100ml of embodiment 6, at 25 DEG C, treatment, passivation time 60 are passivated successively to 100 above-mentioned test pieces
Second, after test piece is through 60 DEG C of deionized water rinsings after passivation, then with 60 DEG C of hot-air seasoning.The every passivation situation of test piece of observation is all
Preferably, color and luster is consistent, and the 10th, 30,50,70,100 are taken respectively carries out neutral salt spray corrosion test, is attained by listed by table 3
Passivation effect situation.
Above content describes general principle of the invention and principal character, and the present invention is not limited to the above embodiments,
Without departing from the spirit and scope of the present invention, various changes and modifications of the present invention are possible, and these changes and improvements are all
Fall into scope of the claimed invention.The claimed scope of the invention is by appending claims and its equivalent circle.
It is fixed.
Claims (8)
1. a kind of passivating solution, is dissolved in deionized water by plurality of raw materials and formed, wherein each material component proportioning is：Six water chromium sulfates
6-9 g/L, cobalt sulfate 2-4 g/L, sodium chlorate 4-8 g/L, ammonium fluoride 2-3 g/L, sulfuric acid 1-2 g/L, citric acid 2-3
G/L, balance of water.
2. passivating solution as claimed in claim 1, it is characterised in that six described water chromium sulfates are 6-8g/L.
3. passivating solution as claimed in claim 1, it is characterised in that described cobalt sulfate is 3-4 g/L.
4. passivating solution as claimed in claim 1, it is characterised in that described sodium chlorate is 6-8 g/L.
5. passivating solution as claimed in claim 1, it is characterised in that described ammonium fluoride is 2.5-3g/L.
6. passivating solution as claimed in claim 1, it is characterised in that described sulfuric acid is 1.5-2g/L.
7. passivating solution as claimed in claim 1, it is characterised in that described citric acid is 3g/L.
8. the preparation method of passivating solution as claimed in claim 1, in turn includes the following steps：
(1) 3/5 volume of aequum deionized water is added in a reservoir, adds sulfuric acid, citric acid to stir to dissolving, mix；
(2) six water chromium sulfates, cobalt sulfate, sodium chlorate are added, stirring is to being completely dissolved；
(3) ammonium fluoride is added, stirring is to being completely dissolved；Deionized water to overall solution volume is added, is stirred evenly.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109853013A (en) * | 2019-03-06 | 2019-06-07 | 成都飞机工业（集团）有限责任公司 | A kind of trivalent chromium passivator and preparation method thereof for cyanide zinc plating wastewater |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104498923A (en) * | 2014-12-26 | 2015-04-08 | 湖南金裕化工有限公司 | Colorful trivalent chromium passivation liquid, preparation method and use method thereof |
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- 2016-04-16 CN CN201610233890.XA patent/CN106756929A/en active Pending
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104498923A (en) * | 2014-12-26 | 2015-04-08 | 湖南金裕化工有限公司 | Colorful trivalent chromium passivation liquid, preparation method and use method thereof |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109853013A (en) * | 2019-03-06 | 2019-06-07 | 成都飞机工业（集团）有限责任公司 | A kind of trivalent chromium passivator and preparation method thereof for cyanide zinc plating wastewater |
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