CN109267052B - Chromium-free passivation solution based on dendritic macromolecules - Google Patents
Chromium-free passivation solution based on dendritic macromolecules Download PDFInfo
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- 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
- C23C22/36—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 containing also phosphates
- C23C22/361—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 containing also phosphates containing titanium, zirconium or hafnium compounds
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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
- C23C22/07—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 phosphates
- C23C22/08—Orthophosphates
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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
- C23C22/07—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 phosphates
- C23C22/08—Orthophosphates
- C23C22/18—Orthophosphates containing manganese cations
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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
- C23C22/36—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 containing also phosphates
- C23C22/364—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 containing also phosphates containing also manganese cations
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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
- C23C2222/20—Use of solutions containing silanes
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Abstract
The invention discloses a chromium-free passivation solution based on dendritic macromolecules, which comprises the following components in percentage by weight, 0.2-15% of at least one silane which only contains epoxy functional groups; 0.1-5% of transition metal compound; 0.1-5% of at least one dendritic macromolecule; 0.1-20% of phosphoric acid and/or phosphate; the balance being water. The chromium-free passivation solution based on dendritic macromolecules disclosed by the invention is an energy-saving environment-friendly passivation solution which does not contain chromium, has extremely high storage stability, high solid content and low-temperature film-forming property, and solves the problems of related defects and application limitations of the traditional passivation solution, especially the stability problem in the transportation processes of high temperature, high humidity, high salinity, long distance and the like.
Description
Technical Field
The invention relates to a chromium-free passivation solution based on dendritic macromolecules.
Background
The current metal surface passivation technologies, including both chromate passivation technologies and chromium-free passivation technologies, are in the trend and are gradually replacing chromate passivation technologies. The mainstream chromium-free passivation technology in the market at present is a silane-based technology, which usually contains a certain amount of metal salt, high molecular resin, film-forming additive and the like, and the defects of the product mainly comprise two aspects:
the first aspect is that the storage time is short, usually not more than 3-6 months, even not more than one month at high temperature in summer. The reason is that: 1. the silane has self-condensation and cross-condensation properties, can gradually form precipitates or gels with the increase of time, and is more serious especially in the case of compounding of various silanes; 2. the metal salt catalyzes the condensation reaction of silane, so that the stability is further reduced; 3. when the formula contains resin, the silane, the metal salt and the resin respectively react with each other, and the stability is further influenced.
The second aspect is that the solids content is usually not more than 30%, and at high concentrations, the self-condensation and cross-condensation reactions of the silanes are greatly accelerated, leading to rapid gelling of the product. The product contains more than 70 percent of water, so that the transportation cost is greatly increased, the requirement on the drying temperature of the passivation solution is high, and the passivation solution can be effectively dried by high-temperature baking at 80-100 ℃.
Disclosure of Invention
The invention aims to overcome the defects of the prior art, provides a chromium-free passivation solution based on dendritic macromolecules, is an energy-saving and environment-friendly passivation solution which does not contain chromium, has extremely high storage stability, high solid content and low-temperature film-forming property, and solves the problems of related defects and application limitations of the traditional passivation solution, especially the stability problem in the transportation process of high temperature, high humidity, high salinity, long distance and the like.
The technical scheme for realizing the purpose is as follows: a chromium-free passivation solution based on dendritic macromolecules comprises the following components in percentage by weight:
the balance being water.
The chromium-free passivation solution based on dendritic macromolecules does not comprise silane containing ammonia functional groups and substances containing chromium elements.
The chromium-free passivation solution based on dendritic macromolecules comprises silane with epoxy functional groups, silane without epoxy functional groups, and silane with epoxy functional groups; nor silanes having both epoxy and other functional groups.
The chromium-free passivation solution based on dendritic macromolecules comprises Zr, Ti, Mn, V, Co, Ni, Ce, Mo, W and H2ZrF6、H2TiF6、Zr(Ar)4、Zr-Ac、TiO2、ZrO2、V2O5And Ce (NO)3)3One or more of them.
The chromium-free passivation solution based on the dendritic macromolecule is characterized in that the dendritic macromolecule is a polyamide-amine dendritic macromolecule, and the structural general formula of the chromium-free passivation solution is as follows:
the chromium-free passivation solution based on dendritic macromolecules is prepared by mixing phosphoric acid and/or phosphate, and stirring the mixture to obtain the final product3PO4、NH4H2PO4、(NH4)2HPO4、(NH4)3PO4、NaH2PO4、(Na)2HPO4、(Na)3PO4、NaNH4HPO4、(Na)2NH4HPO4、Na(NH4)2HPO4And one or more of organic phosphoric acid.
Compared with the prior art, the chromium-free passivation solution based on dendritic macromolecules has the main advantages that:
(1) the traditional chromium-free passivation solution has short storage time, usually not more than 3-6 months, and even not more than one month at high temperature in summer; according to the invention, through introducing the dendritic macromolecules, hydrogen bond interaction can be formed with silane molecules, and the self-condensation and cross-condensation reaction of silane can be effectively inhibited; can also form a complex with metal ions, and effectively inhibit the mutual reaction of the metal ions and silane, resin, phosphate ions and the like. Thereby greatly improving the stability of the passivation solution and storing for more than 3 years;
(2) the solid content of the traditional chromium-free passivation solution is not more than 30 percent, and under the condition of high concentration, the self-condensation and cross-condensation reaction of silane can be greatly accelerated, so that the product can be quickly gelled. The product contains more than 70 percent of water, so that the transportation cost is greatly increased, the requirement on the drying temperature of the passivation solution is high, and the passivation solution can be effectively dried by high-temperature baking at 80-100 ℃; according to the invention, through the inhibition of the dendritic macromolecules on the silane condensation reaction, the condensation reaction of silane under high concentration is effectively prevented, so that the product can be made into concentrated solution with solid content of 60%, the transportation efficiency is improved, the transportation cost is reduced, meanwhile, the baking temperature is only 30-40 ℃, and the energy-saving and environment-friendly effects are achieved.
In general, the chromium-free passivation solution based on the dendritic macromolecule is an energy-saving environment-friendly passivation solution which does not contain chromium, has extremely high storage stability, high solid content and low-temperature film-forming property, solves the related defects and application limitations of the traditional passivation solution, particularly solves the stability problem in the transportation process of high temperature, high humidity, high salinity, long distance and the like, further meets the production requirements of the modern metal corrosion prevention industry, and simultaneously conforms to the development concept of cost saving, economy and environmental protection.
Detailed Description
In order that those skilled in the art will better understand the technical solution of the present invention, the following detailed description will be given of specific embodiments thereof:
example 1
A chromium-free passivation solution based on dendritic macromolecules comprises the following components according to the formula in Table 1:
| components | Content (wt%) |
| Epoxy silane | 5.1 |
| Zr compound | 2.2 |
| Polyamide-amine type dendrimer | 0.15 |
| H3PO4 | 3.3 |
| Water (W) | 89.25 |
TABLE 1
Example 2
A chromium-free passivation solution based on dendritic macromolecules comprises the following components according to the formula shown in Table 2:
| components | Content (wt%) |
| Epoxy silane | 4.1 |
| Ce compound | 3.1 |
| Polyamide-amine type dendrimer | 0.20 |
| (NH4)2HPO4 | 5.5 |
| Water (W) | 87.10 |
TABLE 2
Example 3
A chromium-free passivation solution based on dendritic macromolecules comprises the following components according to the formula shown in Table 3:
| components | Content (wt%) |
| Epoxy silane | 6.1 |
| V2O3Compound (I) | 1.8 |
| Polyamide-amine type dendrimer | 0.15 |
| (NH4)2HPO4 | 6.1 |
| Water (W) | 85.85 |
TABLE 3
Example 4
A chromium-free passivation solution based on dendritic macromolecules comprises the following components according to the formula shown in Table 4:
| components | Content (wt%) |
| Epoxy silane | 5.5 |
| H2TiF6Compound (I) | 1.5 |
| Polyamide-amine type dendrimer | 0.25 |
| (NH4)2HPO4 | 5.4 |
| Water (W) | 87.35 |
TABLE 4
Example 5
A chromium-free passivation solution based on dendritic macromolecules comprises the following components according to the formula shown in Table 5:
| components | Content (wt%) |
| Epoxy silane | 4.5 |
| H2TiF6 compound | 2.1 |
| Polyamide-amine type dendrimer | 0.30 |
| Hydroxyethylidene diphosphonic acid | 3.6 |
| Water (W) | 89.50 |
TABLE 5
The chromium-free passivation solution based on dendritic macromolecules does not contain silane containing ammonia functional groups and substances containing chromium elements.
Silanes that have and contain only epoxy functional groups do not include silanes that do not contain epoxy functional groups, such as ethyl silicate, aminosilanes, vinylsilanes, mercaptosilanes, and the like; nor silanes having both epoxy and other functional groups. The main objective of such design is that the non-epoxy functional group-containing silane has poor stability in the deactivator system described herein, and the use of a silane containing only epoxy functional groups maximizes the storage stability of the deactivator.
The dendritic macromolecule adopts polyamide-amine dendritic macromolecule, and the structural general formula is as follows:
the commercially available passivation solution is selected to be compared with the dendritic macromolecule-based chromium-free passivation solution (the product is consistent with the use object). The following tests show that the advantages or positive effects of the invention (including all the examples in the invention) compared with the prior art can be obtained.
Stability test
The prepared samples were stored at room temperature of 25 ℃ for a long-term stability test, and the state of the samples was recorded every day, and the results are shown in table 6:
TABLE 6
As can be seen from Table 6, the dendrimer-based chromium-free passivation solution of the present invention has an ultra-long stability compared to the commercially available samples. According to the invention, through introducing the dendritic macromolecules, hydrogen bond interaction can be formed with silane molecules, and the self-condensation and cross-condensation reaction of silane can be effectively inhibited; can also form a complex with metal ions, and effectively inhibit the mutual reaction of the metal ions and silane, resin, phosphate ions and the like. Thereby greatly improving the stability of the passivation solution and storing for more than 3 years.
Film formation temperature test
Firstly, attaching temperature measuring paper on the back surface of a substrate to be measured, coating passivation solution on the substrate by a coating method, then putting the substrate into an automatic oven for baking, and detecting the lowest film forming temperature, wherein the result is shown in table 7:
| sample name | Film Forming temperature (. degree. C.) |
| Commercial sample | 80-100 |
| The invention | 30-40 |
TABLE 7
As can be seen from table 7: compared with the commercially available sample, the chromium-free passivation solution based on the dendritic macromolecule has very low film forming temperature, can greatly reduce energy consumption and improve safety of practitioners, and is more energy-saving and environment-friendly. According to the invention, through the inhibition of the dendritic macromolecules on the silane condensation reaction, the condensation reaction of silane under high concentration is effectively prevented, so that the product can be made into concentrated solution with solid content of 60%, the transportation efficiency is improved, the transportation cost is reduced, meanwhile, the baking temperature is only 30-40 ℃, and the energy-saving and environment-friendly effects are achieved.
Corrosion resistance test
Salt spray amount 1-2m L/h, sodium chloride brine concentration 5%, pH 6.8-7.2. general industry standard requires less than 5% tarnish after 72 hours standing, the results are shown in table 8:
| sample name | Corrosion resistance (ASTM B117) ((hours)) |
| Commercial sample | 72-96 |
| The invention | 120-144 |
TABLE 8
As can be seen from table 8: compared with the commercially available samples, the chromium-free passivation solution based on the dendritic macromolecule has more excellent corrosion resistance.
The chromium-free passivation solution based on dendritic macromolecules can also meet other performance tests: moisture resistance, alkali resistance, solvent resistance and high temperature resistance.
The formulation (chromium-free passivation solution) was subjected to solvent, high temperature, alkali and humidity tests. The test was performed on galvanized steel panels having a thickness of about 0.5-2.0 mm. The colour change dE was measured before and after each test. The common requirement for these tests is dE < 3.0. The international commission on illumination technology (CIE) uses an interval brightness Δ E (also referred to as dE, dE or "Delta E") to represent color differences. The value is expressed based on the difference in brightness, hue and saturation. According to the CIE recommendation, the determination of Δ Eab is represented by an accurate graph of the corresponding device test
The L a b color space includes all perceptible colors, L, a, and b values are generally absolute, with a predefined range, luminance L represents the darkest black at L0, and brightest white at L100 color channels a and b represent true neutral gray values at a 0 and b 0.
Moisture resistance test:
(1) testing L a b values of the panel prior to testing;
(2) setting a humidity box: 100% RH at 50 ℃;
(3) placing the panel stacks in a humidity box together or separately for 120 h;
(4) the panel after the test was tested for L a b values and Δ E was obtained.
Alkali resistance test:
(1) testing L a b values of the panel prior to testing;
(2) preparing an alkaline solution (pH9-10) with an alkaline cleaner and heating to 50 deg.C;
(3) place the panel in the solution for 3 minutes;
(4) the panel after the test was tested for L a b values and Δ E was obtained.
Solvent resistance test:
(1) testing L a b values of the panel prior to testing;
(2) fixing the panel on a test board;
(3) setting wiping time, wiping load and wiping speed as required;
(4) impregnating the wiping gauze ball with a required solvent;
(5) starting ColorFlex EZ from Hunter L ab and starting the test;
(6) the panel after the test was tested for L a b values and Δ E was obtained.
High temperature resistance test:
(1) testing L a b values of the panel prior to testing;
(2) the panel was placed in an oven at 240 ℃ for 20 minutes;
(3) after 20 minutes, the panel was removed from the oven and cooled to room temperature;
(4) testing L a b values of the panels after cycle 1 testing and obtaining Δ E1;
(5) the panel was placed in an oven at 240 ℃ and heated for an additional 20 minutes, cooled to room temperature, tested and the Δ Ε 2 of cycle 2 test obtained;
(6) repeat step 5 to obtain Δ E × 3 and Δ E × 4.
The results of the humidity resistance, alkali resistance, solvent resistance and high temperature resistance tests are shown in Table 9:
TABLE 9
As can be seen from table 9: the chromium-free passivation solution disclosed by the invention is resistant to humidity, alkali, solvents and high temperature.
In conclusion, the chromium-free passivation solution based on the dendritic macromolecule is an energy-saving environment-friendly passivation solution which does not contain chromium, has extremely high storage stability, high solid content and low-temperature film-forming property, solves the related defects and application limitations of the traditional passivation solution, particularly solves the stability problem in the transportation process of high temperature, high humidity, high salinity, long distance and the like, further meets the production requirements of the modern metal corrosion prevention industry, and simultaneously conforms to the development concept of cost saving, economy and environmental protection.
It should be understood by those skilled in the art that the above embodiments are only for illustrating the present invention and are not to be used as a limitation of the present invention, and that changes and modifications to the above described embodiments are within the scope of the claims of the present invention as long as they are within the spirit and scope of the present invention.
Claims (2)
1. The chromium-free passivation solution based on dendritic macromolecules is characterized by comprising the following components in percentage by weight:
the balance of water;
the transition metal compound is H2ZrF6、H2TiF6、Zr(Ar)4、Zr-Ac、TiO2、ZrO2、V2O5And Ce (NO)3)3One or more of the above;
the dendritic macromolecule adopts polyamide-amine dendritic macromolecule, and the structural general formula is as follows:
the chromium-free passivation solution does not contain silane containing ammonia functional groups and substances containing chromium elements;
the silane having only epoxy functional groups does not include silanes having no epoxy functional groups; nor silanes having both epoxy and other functional groups.
2. The chromium-free dendrimer-based passivation solution according to claim 1, wherein the phosphoric acid and/or the phosphate is H3PO4、NH4H2PO4、(NH4)2HPO4、(NH4)3PO4、NaH2PO4、(Na)2HPO4、(Na)3PO4、NaNH4HPO4、(Na)2NH4HPO4、Na(NH4)2HPO4And one or more of organic phosphoric acid.
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