CN109778167A - A kind of trivalent chromium passivator and preparation method thereof that coating performance is splendid - Google Patents
A kind of trivalent chromium passivator and preparation method thereof that coating performance is splendid Download PDFInfo
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Abstract
The invention discloses a kind of trivalent chromium passivator and preparation method thereof that coating performance is splendid, the passivator is compounded by chromic salt, water soluble zirconium salt, nano level modified acidic silicasol, waterborne cation polyurethane and water.The trivalent chromium passivator the preparation method comprises the following steps: chromic salt, water soluble zirconium salt and water are added in reaction vessel, stirring and dissolving, sequentially add nano modification acidic silicasol and waterborne cation polyurethane, stir evenly.The passivator has splendid coating performance, but also has excellent corrosion resistance, alkali resistance, solvent resistance, water resistance and yellowing resistance.The preparation method is simple, easy to operate, and preparation cost is low.
Description
Technical field
The present invention relates to Treatment of Metal Surface and protection technology field, and in particular to a kind of trivalent chromium that coating performance is splendid
Passivator and preparation method thereof.
Background technique
White goods industry largely uses heat zinc coating plate, such as the outdoor unit of air-conditioning.Due to the outdoor unit permanent worker of air-conditioning
Make in outdoor, so having higher requirement to antiseptic property.Under normal circumstances, for the inner structural members of non-coating, use is blunt
Change plus the heat zinc coating plate of oiling generally uses the heat of non-passivation to the part (such as chassis, panel, outer cover) of coating to be carried out
Galvanized sheet makes coated article.When being produced in enormous quantities, there is following Railway Project to occur: first is that the heat zinc coating plate of non-passivation is transported
Oxidation during defeated；Second is that material is made a low multiple use；Third is that passivation plate and non-passivation plate are easy to mix up and confuse, cause to be passivated
Plate, which enters paint line or uses non-passivation plate, makes internal component.And general passivation plate surface due to have one layer it is smooth
The passivating film of low-surface-energy, so performance cannot be met the requirements sometimes in coating.If can invent a kind of with excellent painting
The passivator of performance is filled, can thus be used to avoid a production line two kinds of heat zinc coating plate (passivation and non-passivation),
Problem above is also just readily solved.
Traditional passivation of metal surfaces uses Cr VI passivation technology, although sexavalence chromium passivating has simple process, passivation
The good advantage of effect, but Cr VI is hypertoxic and easily carcinogenic substance and easily causes seriously to pollute to environment, American-European prosperity at present
Country has been strictly limited use, and China has also put into effect the use of relevant policies limitation Cr VI, and Cr VI passivator gradually moves back
The arena of history out.The toxicity of trivalent chromium only has 1 the percent of Cr VI, and trivalent chromium passivation at many aspects and is no less than
Sexavalence chromium passivating, so trivalent chromium passivator is widely used in field of metal surface treatment.
Currently, all reporting more trivalent chromium passivator both at home and abroad, but most of patent or other reported in the literature three
Valence chromium passivating agent is the passivation suitable for zinc-plated component, which is that component impregnates the regular hour in passivation tank liquor,
Such as CN100510178, WO2007/088030, JP2008/063963, such trivalent chromium passivator can not be applicable in
In the Passivation Treatment of the continuous hot dip galvanizing steel belt of steel mill.Other reports are suitable for steel plate quick roller coating Passivation Treatment incessantly
Trivalent chromium passivator patent or document, it is main it is emphasised that passivator corrosion resisting property, be seldom related to evaluating coating
Can, if patent CN103215580 reports a kind of trivalent chromium passivator for steel plate quick roller coating Passivation Treatment incessantly,
The passivator has preferable corrosion resistance, but does not evaluate the coating performance of the steel plate after passivation；Patent
A kind of trivalent chromium deactivating liquid for continuous zinc coating that CN101215701 is announced mainly highlights the passivating solution free from extraneous odour, formation
Passivating film has excellent corrosion resistance, does not also test the coating performance of the steel plate after passivation.
Summary of the invention
In order to solve the above-mentioned problems of the prior art, the present invention provides a kind of trivalent chromium that coating performance is splendid is blunt
Agent and preparation method thereof, the passivator have splendid coating performance, but also have excellent corrosion resistance, alkali resistance, resistance to
Solvent borne, water resistance and yellowing resistance.
The preparation method is simple, easy to operate, and preparation cost is low.
A kind of trivalent chromium passivator that coating performance is splendid, by chromic salt, water soluble zirconium salt, nano level modified acid silicon
Colloidal sol, waterborne cation polyurethane and water compound；
Trivalent chromium passivator described in every liter contains:
Further, the chromic salt is one of chromium sulfate, potassium chromium sulfate, chromic nitrate, chromic acetate, or any
Several combinations.
Further, the water soluble zirconium salt is one of zirconium sulfate, acetic acid zirconium and hexafluoro zirconate, or any several
Combination.
Further, the waterborne cation polyurethane the preparation method comprises the following steps:
Polypropylene glycol and isophorone diisocyanate are added in reaction vessel, two isocyanide of polypropylene glycol and isophorone
The mass ratio of acid esters is 0.6-0.75:1, is warming up to 70-80 DEG C, reacts 1-3h, is then cooled to 55-65 DEG C, and three hydroxyl first are added
The mass ratio of base propane, methyl diethanolamine and methyl ethyl ketone, trimethylolpropane and methyl diethanolamine is 1:4-6, is continued anti-
1-3h is answered, then cools down and is neutralized to neutrality with acetic acid, is added with stirring deionized water, distillation removes excessive methyl ethyl ketone, finally
Vinegar acid for adjusting pH value is added to 3.5-4.5.
A kind of preparation method for the trivalent chromium passivator that coating performance is splendid, includes the following steps:
Chromic salt, water soluble zirconium salt and water are added in reaction vessel, stirring and dissolving sequentially adds nano modification
Acidic silicasol and waterborne cation polyurethane, stir evenly, and obtain the splendid trivalent chromium passivator of the coating performance
The effect of each component is illustrated in the trivalent chromium passivator splendid to coating performance of the invention below:
Trivalent chromic ion is the main component of passivator, constitutes the skeleton of coating, assigns passivating film corrosion resisting property；
The addition of zirconium ion is particularly advantageous for improving coating performance, because zirconium ion can be by oxygen atom and painting
The firm connection of bed of material surface, facilitates the raising of coating performance；
The effect of nano modification acidic silicasol is to confer to passivating film alkali resistance and further increases the corrosion resistance of passivating film,
During galvanized sheet surface filming, silica solution is filled in the skeleton of trivalent chromic ion formation passivator, causes passivating film more
It is close, to improve the alkali resistance and corrosion resistance of passivating film；
Waterborne cation polyurethane is the film forming matter of passivator, by complicated with trivalent chromic ion, zirconium ion, silica solution
Ground weave in assigns passivating film water resistance, better flexible and compactness, this effect of polyurethane are that other resins are done
Less than, such as acrylic resin formed film is crisp, poor ductility, and active group in polyurethane and coating is organic
Functional group reacts or hydrogen bond action, facilitates the raising of binding force between passivating film and upper coating.
Compared with prior art, the advantages and beneficial effects of the present invention are:
1) in the present invention, trivalent chromic ion and nano modification acidic silicasol assign trivalent chromium passivator corrosion resistance, resistance to
The basic performances such as solvent, alkali resistance；Zirconium ion is firmly combined by oxygen atom and coating layer surface, facilitates trivalent chromium passivation film
The raising of coating performance；The addition of waterborne cation polyurethane assigns passivating film preferably flexible and compactness, while polyurethane
In active group and the organo-functional group of coating react or hydrogen bond action, further improve passivating film and upper coating
Between binding force.
2) there is splendid coating performance again with the galvanized steel plain sheet that the trivalent chromium passivator is handled, and corrosion resistance, alkaline-resisting
Other various aspects of performance such as property, solvent resistance, water resistance, color inhibition also all fully meet requirement.
Specific embodiment
The present invention is described in detail combined with specific embodiments below.
Nano level modified acidic silicasol used below the preparation method comprises the following steps: in a kettle be added 100L deionization
The acetic acid solution of water, 1L 2mol/L is warming up to 60 DEG C, is slowly added to 12kg tetraethyl orthosilicate, 2kg γ-(2,3- epoxies third
Oxygroup) propyl trimethoxy silicane, stirs lower 60 DEG C and hydrolyzes 2 hours, obtaining partial size is the colorless and transparent nano level modified of 25nm
Acidic silicasol.
Waterborne cation polyurethane used below the preparation method comprises the following steps: take 100 parts of molecular weight be 1000 polypropylene glycol,
68 parts of IPDI are added in reaction vessel, are warming up to 80 DEG C of reaction 2h, are then cooled to 60 DEG C, 3.2 parts of TMP, 16 parts of MDEA are added
With 95 parts of methyl ethyl ketone, the reaction was continued 2h, then 45 DEG C are cooled to, 8 parts of glacial acetic acid are added and neutralize, then 455 are added under high velocity agitation
Part deionized water after excessive solvent methylethylketone is distilled off, is eventually adding acetum and adjusts pH value to 4, obtains described
Waterborne cation polyurethane.
Embodiment 1
A kind of trivalent chromium passivator that coating performance is splendid, is compounded by following component:
The splendid trivalent chromium passivator of above-mentioned coating performance the preparation method comprises the following steps:
Chromium sulfate, zirconium sulfate and deionized water are added in reaction kettle, stirring and dissolving, sequentially add nano modification acid
Property silica solution and waterborne cation polyurethane, stir evenly, obtain the splendid trivalent chromium passivator of the coating performance.
Embodiment 2
A kind of trivalent chromium passivator that coating performance is splendid, is compounded by following component:
The splendid trivalent chromium passivator of above-mentioned coating performance the preparation method comprises the following steps:
Potassium chromium sulfate, zirconium sulfate and deionized water are added in reaction kettle, stirring and dissolving sequentially adds nano modification
Acidic silicasol and waterborne cation polyurethane, stir evenly, and obtain the splendid trivalent chromium passivator of the coating performance.
Embodiment 3
A kind of trivalent chromium passivator that coating performance is splendid, is compounded by following component:
The splendid trivalent chromium passivator of above-mentioned coating performance the preparation method comprises the following steps:
Chromic nitrate, hexafluoro zirconate and deionized water are added in reaction kettle, stirring and dissolving sequentially adds nano modification
Acidic silicasol and waterborne cation polyurethane, stir evenly, and obtain the splendid trivalent chromium passivator of the coating performance.
Embodiment 4
A kind of trivalent chromium passivator that coating performance is splendid, is compounded by following component:
The splendid trivalent chromium passivator of above-mentioned coating performance the preparation method comprises the following steps:
Chromic acetate, hexafluoro zirconate and deionized water are added in reaction kettle, stirring and dissolving sequentially adds nano modification
Acidic silicasol and waterborne cation polyurethane, stir evenly, and obtain the splendid trivalent chromium passivator of the coating performance.
Embodiment 5
A kind of trivalent chromium passivator that coating performance is splendid, is compounded by following component:
The splendid trivalent chromium passivator of above-mentioned coating performance the preparation method comprises the following steps:
Chromic acetate, zirconium acetate and deionized water are added in reaction kettle, stirring and dissolving, sequentially add nano modification acid
Property silica solution and waterborne cation polyurethane, stir evenly, obtain the splendid trivalent chromium passivator of the coating performance.
Embodiment 6
A kind of trivalent chromium passivator that coating performance is splendid, is compounded by following component:
The splendid trivalent chromium passivator of above-mentioned coating performance the preparation method comprises the following steps:
Chromic acetate, zirconium acetate and deionized water are added in reaction kettle, stirring and dissolving, sequentially add nano modification acid
Property silica solution and waterborne cation polyurethane, stir evenly, obtain the splendid trivalent chromium passivator of the coating performance.
Comparative example 1
A kind of trivalent chromium passivator, is compounded by following component:
Above-mentioned trivalent chromium passivator the preparation method comprises the following steps:
Chromic acetate and deionized water are added in reaction kettle, stirring and dissolving, it is molten to sequentially add nano modification acidity silicon
Glue and waterborne cation polyurethane, stir evenly, and obtain the trivalent chromium passivator.
Comparative example 2
A kind of trivalent chromium passivator, is compounded by following component:
Above-mentioned trivalent chromium passivator the preparation method comprises the following steps:
Chromic acetate, zirconium acetate and deionized water are added in reaction kettle, stirring and dissolving, add nano modification acidity silicon
Colloidal sol stirs evenly, and obtains the trivalent chromium passivator.
Comparative example 3
A kind of trivalent chromium passivator, is compounded by following component:
Chromic acetate 25g
Deionized water 1000g
Nano modification acidic silicasol 100g.
Above-mentioned trivalent chromium passivator the preparation method comprises the following steps:
Chromic acetate and deionized water are added in reaction kettle, stirring and dissolving, add nano modification acidic silicasol, stir
It mixes and uniformly obtains the trivalent chromium passivator.
The effect of the splendid trivalent chromium passivator of coating performance of the invention is evaluated and tested
1, the deactivating process for the treatment of of galvanized steel plain sheet
A) precleaning
To guarantee passivation effect, precleaning is carried out before galvanized steel plain sheet is coated with passivator.The purpose of precleaning is to remove to glue
The lubricant components such as attached antirust oil guarantee that trivalent chromium deactivating liquid is uniformly distributed in surface of steel plate.The reference method of precleaning is: will
Galvanized steel plain sheet is cleaned by spraying the degreasing agent of moderate alkaline, is then rinsed with tap water, is then rushed with deionized water
It washes, then galvanized steel plain sheet is removed to the water of adherency by the extruding between two rubber rollers, then dried up with the hot-air of compression；
B) it is coated with
Trivalent chromium passivator is coated on galvanized steel sheet surface by the way of roller coating, it can be according to adjusting galvanized steel plain sheet
The techniques such as the pressure of transmission speed and applicator roll adjust so that passivator wet film has 1~10 μm of thickness；
C) dry
Drying can carry out within the temperature range of the peak metal temperatures (PMT) preferably from 50 DEG C to 150 DEG C, preferably 70
It is carried out within the temperature range of~100 DEG C；
2, test method
1) coating is tested
The hot-dip galvanizing sheet steel for being coated with trivalent chromium passivator is cut into the size of 75mm*150mm, uses on test film
After electrostatic spraying polyester type powder paint, baking 10min forms the film that coating thickness is 20 μm under 180 DEG C of bakings.Then
Load will be applied and carry out hundred lattice tests, hundred lattice Erichsen tests, the test of hundred lattice of boiling, hundred lattice Erichsen test of boiling；
The test of hundred lattice: gained painting load is cut out in coating surface to hundred lattice of 1mm with blade, is then shelled with 3M adhesive tape
From measurement residual rate；
Hundred lattice Erichsen tests: gained painting load is cut out in coating surface to hundred lattice of 1mm with blade, is then used at hundred lattice
Cupping machine squeezes out the protrusion of 6mm, and 3M adhesive tape is removed, and measures residual rate；
The test of hundred lattice of boiling: gained painting load being put into the water for keeping boiling and impregnates 1h, then carries out hundred lattice tests again,
Measure residual rate；
Hundred lattice Erichsen test of boiling: gained painting load is put into the water for keeping boiling and impregnates 1h, then carries out hundred lattice again
Erichsen test measures residual rate；
2) salt spray resistance is tested
Salt spray test carries out according to national standards " GB/T 10125-2012 artificial atmosphere corrosion test salt spray test ", examination
35 ± 2 DEG C of temperature, 50 ± 5g/l of NaCl concentration are tested, the zinc-plated test piece that record is coated with trivalent chromium passivator of the invention occurs white
The time of rust area > 5%；
3) alkali resistance is tested
Template after passivation is placed in 60 DEG C of 2% degreasing agent and impregnates 2min.It is dried up after taking-up, observes specimen surface
Whether color changes, and the color difference of front and back is tested with Chinese spectrum HP-C210 precise colorimeter measurement；
4) solvent resistance test
By butanone with the specimen surface after the power of 500g back and forth 20 friction passivation.Visual condition is observed, and uses the Chinese
Compose the color difference of HP-C210 precise colorimeter measurement sample baking front and back；
5) water resistance test
With 100 DEG C of boiled water dripped on passivation film it is several drip, after water droplet is naturally solid in air, passivation film does not go out
Existing white powder substance, passivating film are not immersed in water destruction as qualification；
6) color inhibition is tested
Passivation galvanized sheet is placed in 200 DEG C of hot-blast stoves, is toasted 20 minutes, observes visual condition, and HP- is composed using the Chinese
C210 precise colorimeter measures the color difference of sample baking front and back；
3, evaluation criterion
The evaluation criterion of each correlated performance such as the following table 1:
Table 1: trivalent chromium passivation film evaluation criterion
| Serial number | Performance indicator | Evaluation criterion |
| 1 | Coating | Residual rate > 95% |
| 2 | Salt fog resistance | > 120h |
| 3 | Alkali resistance | Plate face is without whitening, △ E < 3 |
| 4 | Solvent resistance | Position is wiped without sharp trace, △ E < 3 |
| 5 | Water resistance | Position of dripping is unchanged |
| 6 | Color inhibition | Plate face is without jaundice, △ E < 3 |
4, sample test
The solid content of passivator made from passivator made from embodiment 1-6 and comparative example 1-3 is adjusted to 10% (to use
The method that water is diluted is adjusted), take 9 galvanized steel plain sheets with a thickness of 0.6mm to use embodiment 1-6 and comparative example respectively
Passivator made from 1-3 is tested.Each galvanized steel plain sheet is first subjected to precleaning, is then coated with passivation with 8 μm of painting cloth silk stick
Agent obtains 8 μm of wet film, then is dried in the case where drying temperature is 250 DEG C, peak metal temperatures (PMT) are 77 DEG C, obtains
0.8 μm of dry film.After the completion of each galvanized steel plain sheet Passivation Treatment, placement carries out each correlated performance detection afterwards for 24 hours；
5, test result:
The test result of each passivator of table 2
By upper 2 test data of table it is found that trivalent chromium passivator produced by the present invention is full in the test of various coating performances
Foot requires, and has splendid coating performance, and other each side such as corrosion resistance, alkali resistance, solvent resistance, water resistance, color inhibition
Face performance also all fully meets requirement.
When the coating performance test of passivator made from comparative example 1 and comparative example 2, the test of hundred lattice and hundred lattice Erichsen tests
In be able to satisfy requirement, but in further harsh hundred lattice Erichsen test of hundred lattice of boiling and boiling, be not able to satisfy residual
Stay the requirement of rate > 95%；Passivator made from comparative example 3 is when coating performance is tested, hundred lattice, hundred lattice cuppings, hundred lattice of boiling
And hundred lattice Erichsen test of boiling is unqualified.
Claims (5)
1. a kind of trivalent chromium passivator that coating performance is splendid, it is characterised in that: by chromic salt, water soluble zirconium salt, nanoscale
Modified acidic silicasol, waterborne cation polyurethane and water compound；
Trivalent chromium passivator described in every liter contains:
2. the splendid trivalent chromium passivator of coating performance according to claim 1, it is characterised in that: the chromic salt
For one of chromium sulfate, potassium chromium sulfate, chromic nitrate, chromic acetate, or any several combination.
3. the splendid trivalent chromium passivator of coating performance according to claim 1, it is characterised in that: the water-soluble zirconium
Salt is one of zirconium sulfate, acetic acid zirconium and hexafluoro zirconate, or any several combination.
4. the splendid trivalent chromium passivator of coating performance according to claim 1, it is characterised in that the described aqueous sun from
Sub- polyurethane the preparation method comprises the following steps:
Polypropylene glycol and isophorone diisocyanate are added in reaction vessel, polypropylene glycol and isophorone diisocyanate
Mass ratio be 0.6-0.75:1, be warming up to 70-80 DEG C, react 1-3h, be then cooled to 55-65 DEG C, trihydroxy methyl third is added
The mass ratio of alkane, methyl diethanolamine and methyl ethyl ketone, trimethylolpropane and methyl diethanolamine is 1:4-6, the reaction was continued 1-
3h, then cool down and be neutralized to neutrality with acetic acid, it is added with stirring deionized water, distillation removes excessive methyl ethyl ketone, is eventually adding
Vinegar acid for adjusting pH value is to 3.5-4.5.
5. a kind of a kind of preparation method for the trivalent chromium passivator that coating performance is splendid described in claim 1, it is characterised in that
Include the following steps:
Chromic salt, water soluble zirconium salt and water are added in reaction vessel, stirring and dissolving, sequentially add nano modification acidity
Silica solution and waterborne cation polyurethane, stir evenly, and obtain the splendid trivalent chromium passivator of the coating performance.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110760832A (en) * | 2019-12-05 | 2020-02-07 | 佛山市南海高益美环保实业有限公司 | Trivalent chromium cobalt-free color passivator with high corrosion resistance for electro-galvanized layer |
| CN111676472A (en) * | 2020-06-15 | 2020-09-18 | 武汉迪赛环保新材料股份有限公司 | Chromium-free passivator with high corrosion resistance for batch hot galvanizing |
| CN111690920A (en) * | 2020-07-22 | 2020-09-22 | 武汉迪赛环保新材料股份有限公司 | Modified silica sol chromium-free passivator for surface treatment of hot-dip galvanized steel sheet and preparation method and application thereof |
| CN113403615A (en) * | 2021-06-23 | 2021-09-17 | 上海兴赛尔表面材料有限公司 | Trivalent chromium passivation solution capable of providing deep processing performance and preparation method thereof |
| CN115247263A (en) * | 2022-06-20 | 2022-10-28 | 上海兴赛尔表面材料有限公司 | Environment-friendly passivation composition for tin plate and preparation method and application thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110760832A (en) * | 2019-12-05 | 2020-02-07 | 佛山市南海高益美环保实业有限公司 | Trivalent chromium cobalt-free color passivator with high corrosion resistance for electro-galvanized layer |
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| CN111690920A (en) * | 2020-07-22 | 2020-09-22 | 武汉迪赛环保新材料股份有限公司 | Modified silica sol chromium-free passivator for surface treatment of hot-dip galvanized steel sheet and preparation method and application thereof |
| CN111690920B (en) * | 2020-07-22 | 2022-02-08 | 武汉迪赛环保新材料股份有限公司 | Modified silica sol chromium-free passivator for surface treatment of hot-dip galvanized steel sheet and preparation method and application thereof |
| CN113403615A (en) * | 2021-06-23 | 2021-09-17 | 上海兴赛尔表面材料有限公司 | Trivalent chromium passivation solution capable of providing deep processing performance and preparation method thereof |
| CN115247263A (en) * | 2022-06-20 | 2022-10-28 | 上海兴赛尔表面材料有限公司 | Environment-friendly passivation composition for tin plate and preparation method and application thereof |
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