CN108531899A - High corrosion-resistant admiro surface trivalent chromium deactivating liquid and preparation method thereof - Google Patents
High corrosion-resistant admiro surface trivalent chromium deactivating liquid and preparation method thereof Download PDFInfo
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- CN108531899A CN108531899A CN201810434872.7A CN201810434872A CN108531899A CN 108531899 A CN108531899 A CN 108531899A CN 201810434872 A CN201810434872 A CN 201810434872A CN 108531899 A CN108531899 A CN 108531899A
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- Prior art keywords
- trivalent chromium
- preparation
- admiro
- resistant
- high corrosion
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Classifications
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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
-
- 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
Abstract
The present invention provides a kind of high corrosion-resistant admiro surface trivalent chromium deactivating liquid and preparation method thereof, wherein the preparation method includes the following steps：S1, chromic salt is provided, be dissolved in water, and carry out agitating and heating；S2, sodium fluoride is added into trivalent chromium salt solution, reacts under agitation；S3, after the reaction was complete after chromium ion and fluorine ion, cobalt nitrate and sodium nitrate stirring and dissolving is added, continuously adds sodium sulphate, is stirred well to and is completely dissolved, obtain the trivalent chromium deactivating liquid of the present invention.The passivating solution of the present invention does not contain Cr VI in entire production process, and passivating solution ingredient is simple, is discharged convenient for wastewater treatment.
Description
Technical field
The present invention relates to a kind of passivating solution more particularly to a kind of high corrosion-resistant admiro surface trivalent chromium deactivating liquid and its
Preparation method.
Background technology
For the chromate passivation film of early stage mainly using Cr VI as main salt, the film performance of formation is excellent, passivating solution stability
It is good.But due to the harmfulness of Cr VI, the research to chromium-free deactivation has been expanded at present.However, non-chromium inactivating technique type
Complicated, technique is also still immature, cannot be satisfied industrial requirement.And trivalent chromium can also form passivating film in acid condition, because
This trivalent chromium passivation has obtained more and more extensive attention, and the research based on trivalent chromium passivation is also more both at home and abroad at present, but this
Kind trivalent chromium passivation system generally existing trivalent chromic ion concentration is high, and gained film layer effect especially corrosion resistance is much worse than sexavalence
Chromium.Therefore, in view of the above-mentioned problems, it is necessary to propose further solution.
Invention content
The purpose of the present invention is to provide a kind of preparation method of high corrosion-resistant admiro surface trivalent chromium deactivating liquid and
Preparation method, to overcome problems of the prior art.
For achieving the above object, the present invention provides a kind of system of high corrosion-resistant admiro surface trivalent chromium deactivating liquid
Preparation Method comprising following steps：
S1, chromic salt is provided, be dissolved in water, and carry out agitating and heating；
S2, sodium fluoride is added into trivalent chromium salt solution, reacts under agitation；
S3, after the reaction was complete after chromium ion and fluorine ion, cobalt nitrate and sodium nitrate stirring and dissolving is added, continuously adds sodium sulphate,
It is stirred well to and is completely dissolved, obtain the trivalent chromium deactivating liquid of the present invention.
The improvement of the preparation method of trivalent chromium deactivating liquid as the present invention in the S1, weighs 60 ~ 150 grams of trivalent
Chromic salts is soluble in water, is heated with stirring to 60 ~ 100 DEG C.
The improvement of the preparation method of trivalent chromium deactivating liquid as the present invention, in the step S2, to trivalent chromium salt solution
Middle addition 20 ~ 80g sodium fluorides, react 2h under agitation.
The improvement of the preparation method of trivalent chromium deactivating liquid as the present invention, reacts 2h, Cr under agitation3+Concentration is about
Account for the 1% ~ 10% of reaction solution.
The improvement of the preparation method of trivalent chromium deactivating liquid as the present invention, in the step S3, wait for chromium ion and fluorine from
Son is added 20 ~ 120 grams of cobalt nitrates and 20 ~ 100 grams of sodium nitrate stirring and dissolvings, continuously adds 20 ~ 80 grams of sulfuric acid after the reaction was complete
Sodium is stirred well to and is completely dissolved, and obtains the trivalent chromium deactivating liquid of the present invention.
For achieving the above object, the present invention provides a kind of high corrosion-resistant admiro surface trivalent chromium deactivating liquid,
It is obtained by preparation method as described above.
Compared with prior art, the beneficial effects of the invention are as follows：
（1）The passivating solution of the present invention does not contain Cr VI in entire production process, and passivating solution ingredient is simple, convenient at waste water
Reason discharge.
（2）Trivalent chromic ion concentration is very low in the passivating solution of the present invention, and gained passivating film is colourless uniformly, salt spray resistance pole
It is good.Admiro is 240 hours small without white rust, 1000 through GB/T 6461-2002 neutral salt spray tests after true qualities passivation closing
When without red rust, substantially increase product quality.Trivalent chromium substitution Cr VI is realized to be passivated.
Specific implementation mode
With reference to specifically embodiment, the present invention is described in detail, but it should explanation, these embodiment party
Formula is not limitation of the present invention, and those of ordinary skill in the art are according to function, method or knot made by these embodiments
Equivalent transformation on structure or replacement, all belong to the scope of protection of the present invention within.
The preparation method of the high corrosion-resistant admiro surface trivalent chromium deactivating liquid of the present invention includes the following steps：
S1, chromic salt is provided, be dissolved in water, and carry out agitating and heating.
Preferably, it is soluble in water to weigh 60 ~ 150 grams of chromic salt, is heated with stirring to 60 ~ 100 DEG C.
S2, sodium fluoride is added into trivalent chromium salt solution, reacts under agitation.
Preferably, 20 ~ 80g sodium fluorides are added into trivalent chromium salt solution, react 2h under agitation.Wherein, it is stirring
2h, Cr are reacted under the conditions of mixing3+Concentration accounts for about the 1% ~ 10% of reaction solution.
S3, after the reaction was complete after chromium ion and fluorine ion, cobalt nitrate and sodium nitrate stirring and dissolving is added, continuously adds sulfuric acid
Sodium is stirred well to and is completely dissolved, and obtains the trivalent chromium deactivating liquid of the present invention.
Preferably, after the reaction was complete after chromium ion and fluorine ion, 20 ~ 120 grams of cobalt nitrates and 20 ~ 100 grams of sodium nitrate are added
Stirring and dissolving continuously adds 20 ~ 80 grams of sodium sulphate, is stirred well to and is completely dissolved, and obtains the trivalent chromium deactivating liquid of the present invention.
Chromic salt provides Cr3+ in the passivating solution of the present invention, and chromium is the main component of passivating film, common trivalent chromium
Salt has chromium chloride, chromic nitrate and chromium sulfate etc..The preferred chromium trichloride of the present invention is main salt, because chlorion can both be used as auxiliary
Complexing agent is good film forming accelerating again, and the addition of chlorion enhances the bond strength of passivating film.
Further, passivation film of good performance is obtained, complexing agent is crucial, and according to the difference of film forming, selection is closed
Suitable complexing agent.The too strong complexing agent concentration of complexing agent complexing power is excessively high so that film forming is difficult, is difficult to be formed, and complexing agent energy
Power is excessively weak and can make the too fast quality for influencing film of film forming and influence the stability of solution.
For the present invention water white transparency passivating film characteristic, select fluoride as main complexing agent, stablized and at
The moderate true qualities passivating solution of film speed.In addition, in view of the strong complexing power of fluoride, select nitrate as oxidation in the present invention
Agent, sulfate obtain passivating film of good performance as accelerating agent, auxiliary film forming.
The preparation method of the present invention is illustrated with reference to specifically embodiment.
Embodiment 1
It weighs 60g chromium trichlorides to be dissolved in 860g water, is heated to 60 ~ 100 DEG C.20g sodium fluorides are slowly added to, 2h is stirred to react,
Ensure that chromium ion reacts completely with fluorine ion.20g cobalt nitrates and 20g sodium nitrate are sequentially added, 20g sulphur is added after stirring and dissolving
Sour sodium, stirring is to being completely dissolved to get to trivalent chromium true qualities passivating solution.
For the passivating solution that the present embodiment obtains, its performance is detected as follows：
It takes the passivating solution 40ml prepared that water is added to be made into 1L working solutions, pH is adjusted extremely with 20% dilute sodium hydroxide and 20% dust technology
4.0, it is heated to 40 DEG C.Zinc-nickel alloy layer is passivated 50s in the passivating solution, and surface water white transparency does salt fog after closing, is less than
120h goes out white rust.
It takes the passivating solution 100ml prepared that water is added to be made into 1L working solutions, is adjusted with 20% dilute sodium hydroxide and 20% dust technology
PH to 4.0 is heated to 40 DEG C.Zinc-nickel alloy layer is passivated 90s in the passivating solution, and surface water white transparency does salt fog after closing,
Go out white rust less than 180h.
Embodiment 2
It weighs 150g chromium trichlorides to be dissolved in 470g water, is heated to 60 ~ 100 DEG C.80g sodium fluorides are slowly added to, 2h is stirred to react,
Ensure that chromium ion reacts completely with fluorine ion.120g cobalt nitrates and 100g sodium nitrate are sequentially added, 80g is added after stirring and dissolving
Sodium sulphate, stirring is to being completely dissolved to get to trivalent chromium true qualities passivating solution.
For the passivating solution that the present embodiment obtains, its performance is detected as follows：
It takes the passivating solution 40ml prepared that water is added to be made into 1L working solutions, pH is adjusted extremely with 20% dilute sodium hydroxide and 20% dust technology
4.0, it is heated to 40 DEG C.Zinc-nickel alloy layer is passivated 50s in the passivating solution, and surface water white transparency does salt fog after closing, is less than
180h goes out white rust.
It takes the passivating solution 100ml prepared that water is added to be made into 1L working solutions, is adjusted with 20% dilute sodium hydroxide and 20% dust technology
PH to 4.0 is heated to 40 DEG C.Zinc-nickel alloy layer is passivated 90s in the passivating solution, and surface is slightly turned to be yellow, and salt fog is done after closing,
Go out white rust less than 240h.
Embodiment 3
It weighs 100g chromium trichlorides to be dissolved in 670g water, is heated to 60 ~ 100 DEG C.50g sodium fluorides are slowly added to, 2h is stirred to react,
Ensure that chromium ion reacts completely with fluorine ion.70g cobalt nitrates and 60g sodium nitrate are sequentially added, 50g sulphur is added after stirring and dissolving
Sour sodium, stirring is to being completely dissolved to get to trivalent chromium true qualities passivating solution.
For the passivating solution that the present embodiment obtains, its performance is detected as follows：
It takes the passivating solution 40ml prepared that water is added to be made into 1L working solutions, pH is adjusted extremely with 20% dilute sodium hydroxide and 20% dust technology
4.0, it is heated to 40 DEG C.Zinc-nickel alloy layer is passivated 50s in the passivating solution, and surface water white transparency is salt fog, 240h after closing
Without white rust.
It takes the passivating solution 100ml prepared that water is added to be made into 1L working solutions, is adjusted with 20% dilute sodium hydroxide and 20% dust technology
PH to 4.0 is heated to 40 DEG C.Zinc-nickel alloy layer is passivated 90s in the passivating solution, and surface water white transparency does salt fog after closing,
Super 240h is without white rust.
In conclusion the beneficial effects of the invention are as follows：（1）The passivating solution of the present invention does not contain six in entire production process
Valence chromium, and passivating solution ingredient is simple, is discharged convenient for wastewater treatment.（2）Trivalent chromic ion concentration is very low in the passivating solution of the present invention,
Gained passivating film is colourless uniformly, and salt spray resistance is splendid.Admiro is after true qualities passivation closing, through in GB/T 6461-2002
Property salt spray test without red rust, substantially increases product quality in 1000 hours in 240 hours without white rust.Realize trivalent chromium substitution six
Valence chromium is passivated.
It is obvious to a person skilled in the art that invention is not limited to the details of the above exemplary embodiments, Er Qie
In the case of without departing substantially from spirit or essential attributes of the invention, the present invention can be realized in other specific forms.Therefore, no matter
From the point of view of which point, the present embodiments are to be considered as illustrative and not restrictive, and the scope of the present invention is by appended power
Profit requires rather than above description limits, it is intended that all by what is fallen within the meaning and scope of the equivalent requirements of the claims
Variation is included within the present invention.
In addition, it should be understood that although this specification is described in terms of embodiments, but not each embodiment is only wrapped
Containing an independent technical solution, this description of the specification is merely for the sake of clarity, and those skilled in the art should
It considers the specification as a whole, the technical solutions in the various embodiments may also be suitably combined, forms those skilled in the art
The other embodiment being appreciated that.
Claims (6)
1. a kind of preparation method of high corrosion-resistant admiro surface trivalent chromium deactivating liquid, which is characterized in that the preparation method
Include the following steps：
S1, chromic salt is provided, be dissolved in water, and carry out agitating and heating；
S2, sodium fluoride is added into trivalent chromium salt solution, reacts under agitation；
S3, after the reaction was complete after chromium ion and fluorine ion, cobalt nitrate and sodium nitrate stirring and dissolving is added, continuously adds sodium sulphate,
It is stirred well to and is completely dissolved, obtain the trivalent chromium deactivating liquid of the present invention.
2. the preparation method of high corrosion-resistant admiro according to claim 1 surface trivalent chromium deactivating liquid, feature exist
In in the S1, it is soluble in water to weigh 60 ~ 150 grams of chromic salt, is heated with stirring to 60 ~ 100 DEG C.
3. the preparation method of high corrosion-resistant admiro according to claim 1 surface trivalent chromium deactivating liquid, feature exist
In in the step S2, into trivalent chromium salt solution, addition 20 ~ 80g sodium fluorides, react 2h under agitation.
4. the preparation method of high corrosion-resistant admiro according to claim 3 surface trivalent chromium deactivating liquid, feature exist
In reacting 2h, Cr under agitation3+Concentration accounts for about the 1% ~ 10% of reaction solution.
5. the preparation method of high corrosion-resistant admiro according to claim 1 surface trivalent chromium deactivating liquid, feature exist
In in the step S3, after the reaction was complete after chromium ion and fluorine ion, 20 ~ 120 grams of cobalt nitrates and 20 ~ 100 grams of sodium nitrate are added
Stirring and dissolving continuously adds 20 ~ 80 grams of sodium sulphate, is stirred well to and is completely dissolved, and obtains the trivalent chromium deactivating liquid of the present invention.
6. a kind of high corrosion-resistant admiro surface trivalent chromium deactivating liquid, which is characterized in that the high corrosion-resistant admiro table
Face trivalent chromium deactivating liquid is obtained by any one of claim 1 to 5 preparation method.
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Cited By (3)
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| CN111074254A (en) * | 2018-10-19 | 2020-04-28 | 沧州华润化工有限公司 | Preparation method of trivalent chromium passivator for surface passivation of metal plate |
| CN111485265A (en) * | 2020-04-20 | 2020-08-04 | 常州新纪元材料科技有限公司 | Composition of high corrosion-resistant blue zinc-nickel alloy passivator |
| CN113445036A (en) * | 2021-07-20 | 2021-09-28 | 科文特亚环保电镀技术（江苏）有限公司 | Zinc-nickel alloy blue passivator and preparation process thereof |
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Application publication date: 20180914 |