CN101831648A - Organic precursor-based trivalent chromium black passivation solution and preparation method thereof - Google Patents
Organic precursor-based trivalent chromium black passivation solution and preparation method thereof Download PDFInfo
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- CN101831648A CN101831648A CN201010209695A CN201010209695A CN101831648A CN 101831648 A CN101831648 A CN 101831648A CN 201010209695 A CN201010209695 A CN 201010209695A CN 201010209695 A CN201010209695 A CN 201010209695A CN 101831648 A CN101831648 A CN 101831648A
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- acid
- trivalent chromium
- passivation solution
- solution
- passivation
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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
- C23C22/48—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 not containing phosphates, hexavalent chromium compounds, fluorides or complex fluorides, molybdates, tungstates, vanadates or oxalates
- C23C22/53—Treatment of zinc or alloys based thereon
-
- 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 invention relates to organic precursor-based trivalent chromium black passivation solution and a preparation method thereof, and belongs to the technical field of metal surface treatment. The passivation solution comprises 0.1 to 10g/L of Cr3+, 0.5 to 30g/L of organic carboxylic acid, 0.1 to 10g/L of acid mordant dye, 1 to 20g/L of NO3- and the balance of pure water. The preparation method for the passivation solution comprises the following steps of: dissolving the Cr3+ compound in the pure water; adding the organic carboxylic acid into the mixture; after the organic carboxylic acid is completely dissolved, heating the obtained product to the temperature of between 70 and 90 DEG C to perform a reaction for 1 to 2 hours; after the reaction is completed, cooling the solution to the temperature of between 20 and 30 DEG C; adding the NO3- into the solution; stirring and dissolving the mixture; adding the acid mordant dye into the obtained product to stir and dissolve the mixture; and supplementing the balance of water to a regulated volume to uniformly stir the mixture. The organic precursor-based trivalent chromium black passivation solution and the preparation method thereof have the advantages of simple passivation solution formula, simple and convenient preparation and passivation operation process of the passivation solution, low passivation cost and high added value of the product.
Description
Technical field
The present invention relates to metal surface treatment technology, specifically be meant a kind of trivalent chromium black passivation solution based on organic precursor and preparation method thereof.
Background technology
Zinc coating black passivation film outward appearance is pitch-black shinny, and color and luster is even, and is graceful serious.Black inactivation process is subjected to people's favor day by day in recent years, and use range is more and more wider.At present, zinc electroplating with black chromate conversion coating mainly uses the sexavalent chrome passivation technology.The sexavalent chrome black passivation solution contains hexavalent chromium compounds such as a large amount of chromic anhydrides, has high toxicity and strong carinogenicity, and there are serious hazardness in environment and HUMAN HEALTH.Along with the raising of people's environmental protection consciousness, its use day by day is restricted.Contradiction between the market requirement of black passivation film and the restriction sexavalent chrome technology is impelled people to develop the trivalent chromium black passivation technology to replace the sexavalent chrome black inactivation process.But still there are a lot of technological deficiencies in present existing trivalent chromium black passivation technology.As make the blackening agent for surface of zinc-plated trivalent chromium passivation in the patent of Japanese patent application publication No. JP2005187925A, JP2005206872A, JP2007154286A announcement with transition metal ion and organosulfur compound.Though the passive film blackness that this technology obtains still can, but the melanism composition granule that develops the color in the rete is thick, cause passivation film loose, no smooth finish, poor with basal body binding force, especially anti-neutral salt spray test (GB/T10125-1997) performance extreme difference is though through twice sealing, also fail to test by the neutral salt spray of 48h fully.Japanese patent application publication No. JP2007154286A for another example, U.S. Patent Publication No. US5415702A, US20040156999 make blackening agent for surface with transition metal ion and phosphate anion in the patent that Chinese patent publication number CN1729311A, CN101130865A announce.Though the fine and close light of the rete that these technologies obtain, solidity to corrosion are better, rete blackness deficiency, especially aging along with passivating solution, its blackness is adjusted more and more difficult.And, can cause the problem of eutrophication to environment owing to use phosphate anion in the passivating solution.
Summary of the invention
The objective of the invention is to,, provide a kind of trivalent chromium black passivation solution based on organic precursor and preparation method thereof at the deficiency that prior art exists, described preparation of passivation solution is simple, passivating solution preparation and passivation operation technology are easy, and the passivation cost is low, the added value of product height; Passivating solution does not contain sexavalent chrome and phosphate anion, and the production process non-hexavalent chromium pollutes, and also can not cause eutrophication to environment; Handle the product passivation film outward appearance densification that obtains, pitch-black shinny through passivating solution of the present invention, ornamental strong, solidity to corrosion is good.
One of technical solution of the present invention is, the composition of described trivalent chromium black passivation solution based on organic precursor is that every liter of this passivating solution kind contains:
Cr
3+ 0.1g—10g，
Organic carboxyl acid 0.5g-30g,
Acid mordant dye 0.1g-10g,
NO
3 - 1g—20g，
Water surplus;
Wherein:
Cr
3+Derive from Compound C rCl
36H
2O, Cr
2(SO
4)
36H
2O, Cr (NO
3)
39H
2O, KCr (SO
4)
212H
2O, NH
4Cr (SO4)
212H
2The arbitrary combination of one or more in O, chromium acetate or the chrome tanning agent; Contain Cr
3+The preferred CrCl of compound
36H
2O, Cr
2(SO
4)
36H
2O, Cr (NO
3)
39H
2O, most preferably Cr (NO
3)
39H
2O; Cr
3+The preferred 0.5g/L-5g/L of content, most preferably 1g/L-3g/L.
Described organic carboxyl acid is one or more the arbitrary combination in the following organic carboxyl acid:
Monocarboxylic acid, as formic acid, acetate, propionic acid etc.,
Di-carboxylic acid is as oxalic acid, propanedioic acid, hexanodioic acid etc.;
Hydroxycarboxylic acid is as oxyacetic acid, citric acid, tartrate, oxysuccinic acid, gluconic acid etc.;
Aminocarboxylic acid is as Padil, L-glutamic acid, EDTA, EDTA disodium etc.
The preferred hydroxycarboxylic acid of described organic carboxyl acid, aminocarboxylic acid, most preferably hydroxycarboxylic acid.Organic carboxyl acid content is 0.5g/L-30g/L, preferred 1g/L-20g/L, most preferably 5-10g/L.Wherein organic carboxyl acid and Cr
3+Mol ratio be 0.5-5, preferred 1-3, most preferably 1.5-2.5.
Acid mordant dye is one or both in acid mordant black PV (AcidMordantBlackPV) and the Mordant Black T (AcidChromeBlackT).Acid mordant dye content is 0.1g/L-10g/L, preferred 0.5g/L-8g/L, most preferably 1g/L-5g/L.
NO
3 -Derive from NaNO
3, KNO
3, NH
4NO
3, Ni (NO
3)
2, Cr (NO
3)
39H
2O, CoNO
3, MnNO
3, FeNO
3In one or more arbitrary combination; Preferred NaNO
3, KNO
3, NH
4NO
3, NaNO most preferably
3NO
3 -Content is 1-20g/L, preferred 3-15g/L, most preferably 5-10g/L.
Two of technical scheme of the present invention is, the preparation method of described trivalent chromium black passivation solution based on organic precursor is, by the composition and the content of aforementioned trivalent chromium black passivation solution, under continuously stirring, with Cr
3+Compound dissolution adds organic carboxyl acid again behind pure water; Treat Cr
3+After two kinds of raw materials of compound and organic carboxyl acid dissolve fully, be heated to 70
0C-90
0C reacts, reaction times 1-2h; Question response is finished, and solution is cooled to 20
0C-30
0Add NO during C
3 -, stirring and dissolving; Add the acid mordant dye stirring and dissolving again; Water to the prescribed volume of adding surplus stirs.
The using method of trivalent chromium black passivation solution of the present invention is: prepare above-mentioned Cr
3+Concentration is the black passivation solution of 1-3g/L, uses rare HNO
3Or rare NaOH to adjust passivating solution pH be 2.2-2.4, the passivation operation temperature is 20
0C-40
0C, passivation time are 5s-60s; Need carry out mechanical stirring or oil-free compressed air in the passivating process stirs.After passivation is finished, with 55
0C-65
0C hot water sealing 20s-40s is in 70
0C-80
0The oven dry of C temperature.
Know-why of the present invention is to bestow rational Cr in preparation of passivation solution
3+, organic carboxyl acid, chrome dye and oxygenant combination, thereby form pitch-black shinny, even compact of outward appearance and the high passivation film of solidity to corrosion.The mechanism that the present invention forms black passivation film is not fully aware of, but can reasonably infer according to existing scientific knowledge.Electroplate Zn layer H in passivating solution
+And NO
3 -Effect under lose electronics and generate Zn
2+, portions of electronics that loses and H
+Becoming hydrogen in conjunction with the generation hydrogen atom overflows.Along with H
+Obtain electronics and generate hydrogen atom and become hydrogen and overflow, electroplate that pH can local rising in the interfacial layer of Zn layer and passivating solution.At this moment, with the Cr of organic carboxyl acid complexing
3+Just part is dissociated into free ion with organic carboxyl acid, Cr
3+With OH
-Reaction generates gelatinous Cr (OH)
3Be deposited in the Zn surface and form passive film.Meanwhile, Cr
3+Out-shell electron has six unoccupied orbitals, can with acid mordant dye in-OH ,-N=N-,-the COOH complexing, in passivating process, form the complex compound black color lake of dyestuff-Cr-dyestuff, attached to gelatinous Cr (OH)
3In the precipitation, thereby obtain pitch-black shinny, even compact of outward appearance and the high passivation film of solidity to corrosion.
The present invention passes through Cr
3+In passivating process with acid mordant dye in-OH ,-N=N-,-the COOH complexing, the complex compound black color lake that forms dyestuff-Cr-dyestuff obtains black passivation film.Because the complex compound black color lake particle of dyestuff-Cr-dyestuff is tiny, color is pitch-black, be evenly distributed in passive film, so passivation film densification, pitch-black light, solidity to corrosion is good.
As known from the above, the present invention is that preparation of passivation solution is simple based on trivalent chromium black passivation solution of organic precursor and preparation method thereof, and passivating solution preparation and passivation operation technology are easy, and the passivation cost is low, the added value of product height; Passivating solution does not contain sexavalent chrome and phosphate anion, and the production process non-hexavalent chromium pollutes, and also can not cause eutrophication to environment; Handle the product passivation film outward appearance densification that obtains, pitch-black shinny through trivalent chromium black passivation solution of the present invention, ornamental strong, solidity to corrosion is good, measures through the 5%NaCl of GB/T10125-1997 neutral salt spray, and 72h does not go out the white rust point.
Embodiment
Below by specific embodiment technical scheme of the present invention is further described, but do not constitute limitation of the invention.
Embodiment 1:Under the continuously stirring, with 10gCr
2(SO
4)
36H
2After O is dissolved in the 500ml pure water, add 11g tartrate again; After treating that two kinds of raw materials dissolve fully, be heated to 80
0C reacts, reaction times 2h; Question response is finished solution and is cooled to 30
0Add 10gKNO during C
3, stirring and dissolving; Add 3g acid mordant black PV stirring and dissolving; The water of adding surplus stirs to 1000ml, promptly.
The using method of gained trivalent chromium black passivation solution is: prepare above-mentioned black passivation solution, use rare HNO
3Adjusting passivating solution pH is 2.2, and the passivation operation temperature is 40
0C, passivation time is 60S, passivating process stirs with oil-free compressed air.After passivation is finished, 60
0C hot water sealing 40s is in 75
0The oven dry of C temperature.Handle the product passivation film outward appearance densification that obtains, pitch-black shinny through trivalent chromium black passivation solution of the present invention, ornamental strong, solidity to corrosion is good.Measure through the 5%NaCl of GB/T10125-1997 neutral salt spray, 72h does not go out the white rust point.
Embodiment 2:Under the continuously stirring, with 23gCr (NO
3)
39H
2After O is dissolved in the 500ml pure water, add the 24g citric acid again; After treating that two kinds of raw materials dissolve fully, be heated to 90
0C reacts, reaction times 3h; Question response is finished solution and is cooled to 25
0Add 11gNaNO during C
3, stirring and dissolving; Add 4g Mordant Black T stirring and dissolving; The water of adding surplus stirs to 1000ml, promptly.
The using method of gained trivalent chromium black passivation solution is: prepare above-mentioned black passivation solution, use rare HNO
3Adjusting passivating solution pH is 2.3, and the passivation operation temperature is 35
0C, passivation time is 50S, passivating process stirs with oil-free compressed air.After passivation is finished, 55
0C hot water sealing 35s is in 80
0The oven dry of C temperature.Handle the product passivation film outward appearance densification that obtains, pitch-black shinny through trivalent chromium black passivation solution of the present invention, ornamental strong, solidity to corrosion is good.Measure through the 5%NaCl of GB/T10125-1997 neutral salt spray, 72h does not go out the white rust point.
Embodiment 3:Under the continuously stirring, with 5gCr
2(SO
4)
36H
2O and 10gCr (NO
3)
39H
2After O is dissolved in the 500ml pure water, add 12g citric acid and 5g tartrate again; After treating that two kinds of raw materials dissolve fully, be heated to 85
0C reacts, reaction times 2h; Question response is finished solution and is cooled to 30
0Add 11gNaNO during C
3, stirring and dissolving; Add 2g acid mordant black PV and 2g Mordant Black T stirring and dissolving; The water of adding surplus stirs to 1000ml, promptly.Gained
The using method of gained trivalent chromium black passivation solution is: prepare above-mentioned black passivation solution, use rare HNO
3Adjusting passivating solution pH is 2.2, and the passivation operation temperature is 30
0C, passivation time is 60S, passivating process stirs with oil-free compressed air.After passivation is finished, 60
0C hot water sealing 30s is in 70
0The oven dry of C temperature.Handle the product passivation film outward appearance densification that obtains, pitch-black shinny through trivalent chromium black passivation solution of the present invention, ornamental strong, solidity to corrosion is good.Measure through the 5%NaCl of GB/T10125-1997 neutral salt spray, 72h does not go out the white rust point.
Claims (7)
1. the trivalent chromium black passivation solution based on organic precursor is characterized in that, every liter of this passivating solution kind contains:
Cr
3+ 0.1g—10g，
Organic carboxyl acid 0.5g-30g,
Acid mordant dye 0.1g-10g,
NO
3 - 1g—20g，
Water surplus.
2. according to the described trivalent chromium black passivation solution of claim 1, it is characterized in that described Cr based on organic precursor
3+Derive from Compound C rCl
36H
2O, Cr
2(SO
4)
36H
2O, Cr (NO
3)
39H
2O, KCr (SO
4)
212H
2O, NH
4Cr (SO4)
212H
2The arbitrary combination of one or more in O, chromium acetate or the chrome tanning agent.
3. according to the described trivalent chromium black passivation solution of claim 1, it is characterized in that described organic carboxyl acid is one or more the arbitrary combination in the following organic carboxyl acid: monocarboxylic acid, di-carboxylic acid, hydroxycarboxylic acid, aminocarboxylic acid based on organic precursor.
4. according to the described trivalent chromium black passivation solution of claim 3, it is characterized in that described monocarboxylic acid is formic acid, acetate or propionic acid based on organic precursor; Described di-carboxylic acid is oxalic acid, propanedioic acid or hexanodioic acid; Described hydroxycarboxylic acid is oxyacetic acid, citric acid, tartrate, oxysuccinic acid or gluconic acid; Described aminocarboxylic acid is Padil, L-glutamic acid, EDTA or EDTA disodium.
5. according to the described trivalent chromium black passivation solution of claim 1, it is characterized in that described acid mordant dye is one or both in acid mordant black PV and the Mordant Black T based on organic precursor.
6. according to the described trivalent chromium black passivation solution of claim 1, it is characterized in that described NO based on organic precursor
3 -Derive from NaNO
3, KNO
3, NH
4NO
3, Ni (NO
3)
2, Cr (NO
3)
39H
2O, CoNO
3, MnNO
3, FeNO
3In one or more arbitrary combination.
7. the trivalent chromium black passivation solution preparation method based on organic precursor of one of claim 1 to 6 is characterized in that, by the composition and the content of described trivalent chromium black passivation solution, under continuously stirring, with Cr
3+Compound dissolution adds organic carboxyl acid again behind pure water; Treat Cr
3+After two kinds of raw materials of compound and organic carboxyl acid dissolve fully, be heated to 70
0C-90
0C reacts, reaction times 1-2h; Question response is finished, and solution is cooled to 20
0C-30
0Add NO during C
3 -, stirring and dissolving; Add the acid mordant dye stirring and dissolving again; Water to the prescribed volume of adding surplus stirs.
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|---|---|---|---|
| CN2010102096956A CN101831648B (en) | 2010-06-25 | 2010-06-25 | Organic precursor-based trivalent chromium black passivation solution and preparation method thereof |
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|---|---|---|---|
| CN2010102096956A CN101831648B (en) | 2010-06-25 | 2010-06-25 | Organic precursor-based trivalent chromium black passivation solution and preparation method thereof |
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| CN101831648B CN101831648B (en) | 2011-12-14 |
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ID=42715865
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|---|---|---|---|
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102011112A (en) * | 2010-12-15 | 2011-04-13 | 济南德锡科技有限公司 | Zinc and zinc alloy plating black passivation solution and preparation method thereof |
| CN102242359A (en) * | 2011-06-21 | 2011-11-16 | 湖南大学 | Trivalent chromium black passivation solution based on plant extract pigment, and preparation method and use method thereof |
| CN102644071A (en) * | 2012-05-25 | 2012-08-22 | 山东建筑大学 | Galvanized trivalent chromium black passivator |
| CN105937030A (en) * | 2016-06-29 | 2016-09-14 | 无锡伊佩克科技有限公司 | Method for preparing trivalent chromium black passivation solution |
| US20180216234A1 (en) * | 2017-02-01 | 2018-08-02 | Chemeon Surface Technology, Llc | Dyed trivalent chromium conversion coatings and methods of using same |
| CN108531902A (en) * | 2018-05-09 | 2018-09-14 | 昆山秀博表面处理材料有限公司 | Fluorine-free and environment-friendly trivalent blue-white chromating liquid and preparation method thereof |
| CN110158068A (en) * | 2019-06-17 | 2019-08-23 | 上海德修化工有限公司 | A kind of environment-friendly type admiro black passivation solution and its application method |
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| JP2009173978A (en) * | 2008-01-22 | 2009-08-06 | Dipsol Chem Co Ltd | Chemical conversion processing method for forming trivalent chromium chemically-processed coating film having excellent heat corrosion-resistance on zinc or zinc-alloy plating |
-
2010
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Patent Citations (2)
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| JPS5965839A (en) * | 1982-10-08 | 1984-04-14 | Fuji Photo Film Co Ltd | Heat developable color photosensitive material |
| JP2009173978A (en) * | 2008-01-22 | 2009-08-06 | Dipsol Chem Co Ltd | Chemical conversion processing method for forming trivalent chromium chemically-processed coating film having excellent heat corrosion-resistance on zinc or zinc-alloy plating |
Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102011112A (en) * | 2010-12-15 | 2011-04-13 | 济南德锡科技有限公司 | Zinc and zinc alloy plating black passivation solution and preparation method thereof |
| CN102011112B (en) * | 2010-12-15 | 2012-11-28 | 济南德锡科技有限公司 | Zinc and zinc alloy plating black passivation solution and preparation method thereof |
| CN102242359A (en) * | 2011-06-21 | 2011-11-16 | 湖南大学 | Trivalent chromium black passivation solution based on plant extract pigment, and preparation method and use method thereof |
| CN102644071A (en) * | 2012-05-25 | 2012-08-22 | 山东建筑大学 | Galvanized trivalent chromium black passivator |
| CN105937030A (en) * | 2016-06-29 | 2016-09-14 | 无锡伊佩克科技有限公司 | Method for preparing trivalent chromium black passivation solution |
| CN105937030B (en) * | 2016-06-29 | 2018-09-21 | 诸暨天雅科技有限公司 | A kind of preparation method of trivalent chromium black passivation solution |
| US20180216234A1 (en) * | 2017-02-01 | 2018-08-02 | Chemeon Surface Technology, Llc | Dyed trivalent chromium conversion coatings and methods of using same |
| US10533254B2 (en) * | 2017-02-01 | 2020-01-14 | Chemeon Surface Technology, Llc | Dyed trivalent chromium conversion coatings and methods of using same |
| CN108531902A (en) * | 2018-05-09 | 2018-09-14 | 昆山秀博表面处理材料有限公司 | Fluorine-free and environment-friendly trivalent blue-white chromating liquid and preparation method thereof |
| CN110158068A (en) * | 2019-06-17 | 2019-08-23 | 上海德修化工有限公司 | A kind of environment-friendly type admiro black passivation solution and its application method |
| CN110158068B (en) * | 2019-06-17 | 2021-03-05 | 上海德修化工有限公司 | Environment-friendly zinc-nickel alloy black passivation solution and use method thereof |
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|---|---|
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