CN112126918B - Passivating agent for processing aluminum foil and preparation method thereof - Google Patents
Passivating agent for processing aluminum foil and preparation method thereof Download PDFInfo
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- CN112126918B CN112126918B CN202010888769.7A CN202010888769A CN112126918B CN 112126918 B CN112126918 B CN 112126918B CN 202010888769 A CN202010888769 A CN 202010888769A CN 112126918 B CN112126918 B CN 112126918B
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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
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Abstract
The invention discloses a passivating agent for processing an aluminum foil, and relates to the technical field of surface processing of metal materials. Comprises 0.3-1 part of chromium solution, 0.5-2 parts of modified phenolic resin, 2-5 parts of potassium zirconium carbonate, 2-5 parts of diisobutyl naphthalene sulfonate, 0.5-2 parts of barium tellurate, 40-55 parts of ethanol and 35-40 parts of water. Mixing and uniformly stirring a chromium solution, modified phenolic resin, ethanol and water, and then standing to obtain a mixed solution; and sequentially adding potassium zirconium carbonate, sodium diisobutylnaphthalenesulfonate and barium tellurate into the mixed solution, heating and standing to prepare the passivating agent. According to the invention, the passivating agent is prepared by taking the chromium solution and the phenolic resin as basic raw materials, an oxide film layer can be formed on the surface of the aluminum foil, and the corrosion resistance and the liquid resistance of the aluminum foil are effectively improved; the oxide film layer formed by the passivating agent is a colorless transparent film layer, and the surface color of the aluminum foil is not changed completely.
Description
Technical Field
The invention relates to the technical field of metal material surface treatment, in particular to a passivating agent for treating aluminum foil and a preparation method thereof.
Background
The metal surface treatment can effectively improve the corrosion resistance of the metal. However, the treated layer is susceptible to corrosion in a humid environment, causing corrosion products to form on the surface or becoming dull-colored, affecting the appearance, and must be passivated. The phenomenon that a dense oxide protective layer is generated on the surface of metal such as steel, aluminum and the like so as to prevent further reaction with the metal is called passivation phenomenon. Currently, chromate passivation is recognized as the most effective passivation method. The main reasons are simple chromate passivating treatment process and low cost. The chromium/base metal mixed oxide film is formed after chromate treatment, and the chromium in the film mainly exists in a hexavalent form and a trivalent form. However, hexavalent chromium is a carcinogen and has serious potential harm to human bodies and the environment; however, the corresponding performance of chromate passivation cannot be achieved by passivation with trivalent chromium alone.
Therefore, it is an urgent technical problem to be solved by those skilled in the art to provide a trivalent chromium-based passivator for treating aluminum foil, which has high corrosion resistance and high liquid resistance, and a preparation method thereof.
Disclosure of Invention
In view of the above, the present invention provides a passivation agent for treating an aluminum foil, which has high corrosion resistance and strong liquid resistance.
In order to achieve the purpose, the invention adopts the following technical scheme:
a passivating agent for processing aluminum foil comprises the following raw materials in parts by weight: 0.3-1 part of chromium solution, 0.5-2 parts of modified phenolic resin, 2-5 parts of potassium zirconium carbonate, 2-5 parts of sodium diisobutylnaphthalenesulfonate, 0.5-2 parts of barium tellurate, 40-55 parts of ethanol and 35-40 parts of water.
The invention has the beneficial effects that: the passivating agent is prepared by taking the chromium solution and the phenolic resin as basic raw materials, an oxide film layer can be formed on the surface of the aluminum foil, and the corrosion resistance and the liquid resistance of the aluminum foil are effectively improved; the formed oxide film layer is a colorless transparent film layer, and the surface color of the aluminum foil can not be changed completely.
Further, the concentration of the chromium solution is 8-10%.
Furthermore, the chromium solution is prepared by adopting a trivalent chromium compound; the trivalent chromium compound is chromium hydroxide, chromium sulfate or chromium chloride.
The beneficial effect of adopting the further scheme is that: the trivalent chromium solution adopted by the invention has no potential hazard to human bodies and environment, and the corrosion resistance of the trivalent chromium passivator can be effectively improved by matching with the raw materials such as ethanol and the like adopted by the invention.
Further, the ethanol is 60-90% ethanol.
Adopt above-mentioned further beneficial effect to lie in: the invention adopts 60-90% ethanol which can be matched with the chromium solution, and the formed chromium/matrix metal mixed oxide film has no harm and can improve various basic performances of the film.
The invention also provides a preparation method of the passivating agent for treating the aluminum foil, which comprises the following steps:
(1) Weighing the raw materials in parts by weight;
(2) Mixing and uniformly stirring the chromium solution, the phenolic resin, the ethanol and the water, and then standing to obtain a mixed solution;
(3) And (3) sequentially adding potassium zirconium carbonate, diisobutyl naphthalene sulfonate and barium tellurate into the mixed solution obtained in the step (2), and heating and standing to obtain the passivator for treating the aluminum foil.
Further, the preparation method of the modified phenolic resin comprises the following steps: mixing phenolic resin and carboxylic acid according to the mass ratio of 1 (1-1.5) to carry out esterification reaction to obtain phenolic resin derivatives containing carboxyl; then, carrying out ring-opening reaction on the carboxyl of the phenolic resin derivative containing the carboxyl and ethylene oxide according to the mass ratio of 1-1.5 to obtain a phenolic resin derivative containing the hydroxyl; and carrying out secondary reaction on hydroxyl of the phenolic resin derivative containing hydroxyl and epoxy ethyl according to the mass ratio of 1-1.5 to obtain the epoxy modified phenolic resin.
Further, the carboxylic acid is formic acid, acetic acid or propionic acid.
Adopt above-mentioned further beneficial effect to lie in: the phenolic resin is modified by the passivating agent, so that the corrosion resistance and toughness of the phenolic resin can be improved, and the corrosion resistance of an oxide film formed by the passivating agent can be further improved by applying the passivating agent.
Further, in the step (2), the stirring speed is 50-100r/min, the stirring time is 2-3h, and the standing time is 4-6h.
Further, the heating temperature in the step (3) is 80-120 ℃, and the standing heating time is 8-12h.
Adopt above-mentioned further beneficial effect to lie in: according to the invention, the raw materials are stirred and mixed to promote uniform mixing with the raw materials, so that an oxide film layer formed by the passivator in the use process is more uniform and compact.
The invention has the beneficial effects that: the passivating agent disclosed by the invention can form an oxide film layer on the surface of the aluminum foil, so that the corrosion resistance and the liquid resistance of the aluminum foil are effectively improved.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
A preparation method of a passivator for treating aluminum foil comprises the following steps:
(1) Mixing phenolic resin and formic acid according to the mass ratio of 1; then, carrying out ring-opening reaction on the carboxyl of the phenolic resin derivative containing the carboxyl and ethylene oxide according to the mass ratio of 1; carrying out secondary reaction on hydroxyl of the phenolic resin derivative containing hydroxyl and epoxy ethyl according to the mass ratio of 1;
(2) Weighing 0.3kg of chromium hydroxide solution with the chromium ion concentration of 8%, 2kg of modified phenolic resin, 2kg of potassium zirconium carbonate, 5kg of diisobutyl naphthalene sulfonate, 2kg of barium tellurate, 40kg of 90% ethanol and 40kg of water;
(3) Mixing the chromium solution, the phenolic resin, ethanol and water, stirring for 3 hours at the speed of 50r/min, and then standing for 4 hours to obtain a mixed solution;
(4) And (4) sequentially adding potassium zirconium carbonate, diisobutyl naphthalene sulfonate and barium tellurate into the mixed solution obtained in the step (3), and heating and standing at 120 ℃ for 8 hours to obtain the passivator for treating the aluminum foil.
Example 2
A preparation method of a passivator for treating aluminum foil comprises the following steps:
(1) Mixing phenolic resin and propionic acid according to the mass ratio of 1.5 for esterification reaction to obtain a phenolic resin derivative containing carboxyl; then, carrying out ring-opening reaction on the carboxyl of the phenolic resin derivative containing the carboxyl and ethylene oxide according to the mass ratio of 1.5 to obtain a phenolic resin derivative containing the hydroxyl; carrying out secondary reaction on hydroxyl of the phenolic resin derivative containing hydroxyl and epoxy ethyl according to the mass ratio of 1.5;
(2) Weighing 1kg of chromium chloride solution with the chromium ion concentration of 10%, 0.5kg of modified phenolic resin, 5kg of potassium zirconium carbonate, 2kg of sodium diisobutylnaphthalenesulfonate, 0.5kg of barium tellurate, 55kg of 60% ethanol and 35kg of water;
(3) Mixing the chromium solution, the phenolic resin, ethanol and water, stirring for 2 hours at the speed of 100r/min, and then standing for 6 hours to obtain a mixed solution;
(4) And (4) sequentially adding potassium zirconium carbonate, diisobutyl naphthalene sulfonate and barium tellurate into the mixed solution obtained in the step (3), and heating and standing at 80 ℃ for 12 hours to obtain the passivator for treating the aluminum foil.
Example 3
A preparation method of a passivator for treating aluminum foil comprises the following steps:
(1) Mixing phenolic resin and acetic acid according to the mass ratio of 1.25 for esterification reaction to obtain phenolic resin derivatives containing carboxyl; then, carrying out ring-opening reaction on the carboxyl of the phenolic resin derivative containing the carboxyl and ethylene oxide according to the mass ratio of 1.25 to obtain a phenolic resin derivative containing the hydroxyl; carrying out secondary reaction on hydroxyl of the phenolic resin derivative containing hydroxyl and epoxy ethyl according to a mass ratio of 1.25 to obtain modified phenolic resin;
(2) Weighing 0.5kg of chromium chloride solution with the chromium ion concentration of 9%, 1.5kg of modified phenolic resin, 4kg of potassium zirconium carbonate, 3kg of sodium diisobutylnaphthalenesulfonate, 1.5kg of barium tellurate, 45kg of 75% ethanol and 35kg of water;
(3) Mixing the chromium solution, the phenolic resin, ethanol and water, stirring for 2.5 hours at the speed of 80r/min, and then standing for 4 hours to obtain a mixed solution;
(4) And (3) sequentially adding potassium zirconium carbonate, sodium diisobutylnaphthalenesulfonate and barium tellurate into the mixed solution obtained in the step (3), and heating and standing for 10 hours at 100 ℃ to obtain the passivator for treating the aluminum foil.
Example 4
A preparation method of a passivator for treating aluminum foil comprises the following steps:
(1) Mixing phenolic resin and formic acid according to the mass ratio of 1.1 for esterification reaction to obtain phenolic resin derivatives containing carboxyl; then, performing ring opening reaction on the carboxyl of the phenolic resin derivative containing the carboxyl and ethylene oxide according to the mass ratio of 1.1; carrying out secondary reaction on hydroxyl of the phenolic resin derivative containing hydroxyl and epoxy ethyl according to the mass ratio of 1.1;
(2) Weighing 0.8kg of chromium sulfate solution with the chromium ion concentration of 8%, 2kg of modified phenolic resin, 4kg of potassium zirconium carbonate, 2kg of sodium diisobutylnaphthalenesulfonate, 1kg of barium tellurate, 50kg of 80% ethanol and 38kg of water;
(3) Mixing the chromium solution, phenolic resin, ethanol and water, stirring for 2 hours at 75r/min, and then standing for 5 hours to obtain a mixed solution;
(4) And (3) sequentially adding potassium zirconium carbonate, sodium diisobutylnaphthalenesulfonate and barium tellurate into the mixed solution obtained in the step (3), and heating and standing for 8 hours at 110 ℃ to obtain the passivator for treating the aluminum foil.
Example 5
A preparation method of a passivator for treating aluminum foil comprises the following steps:
(1) Mixing phenolic resin and acetic acid according to the mass ratio of 1.25 for esterification reaction to obtain phenolic resin derivatives containing carboxyl; then, performing ring opening reaction on the carboxyl of the phenolic resin derivative containing the carboxyl and ethylene oxide according to the mass ratio of 1.3; carrying out secondary reaction on hydroxyl of the phenolic resin derivative containing hydroxyl and epoxy ethyl according to the mass ratio of 1.2 to obtain modified phenolic resin;
(2) Weighing 0.4kg of chromium hydroxide solution with the chromium ion concentration of 10%, 1kg of modified phenolic resin, 5kg of potassium zirconium carbonate, 3kg of sodium diisobutylnaphthalenesulfonate, 1.2kg of barium tellurate, 50kg of 85% ethanol and 40kg of water;
(3) Mixing the chromium solution, the phenolic resin, ethanol and water, stirring for 3 hours at the speed of 60r/min, and then standing for 4 hours to obtain a mixed solution;
(4) And (3) sequentially adding potassium zirconium carbonate, sodium diisobutylnaphthalenesulfonate and barium tellurate into the mixed solution obtained in the step (3), and heating and standing at 80 ℃ for 9 hours to obtain the passivator for treating the aluminum foil.
Test examples
The passivators prepared in the embodiments 1 to 5 of the invention and the traditional chromate passivator are used as comparative examples to be coated on an aluminum foil to form an oxide film layer, and then the performances of the corrosion resistance, the liquid resistance and the film adhesion are tested;
wherein the corrosion resistance test adopts an acidic solution to soak for 20min, the adopted acidic solution is obtained by mixing hydrochloric acid and a saturated copper chloride solution, and the pH value is 1; the liquid resistance test is that the aluminum foil is put into an oven with 80 ℃ and filled with electrolyte for two weeks; the film adhesion performance test comprises an indoor hanging piece test, a film grid test (GB/9286-98) and a film impact resistance test (50 kG cm, GB/T1732-93); the test results are shown in table 1.
TABLE 1
In the present specification, the embodiments are described in a progressive manner, each embodiment focuses on differences from other embodiments, and the same and similar parts among the embodiments are referred to each other.
The previous description of the disclosed embodiments is provided to enable any person skilled in the art to make or use the present invention. Various modifications to these embodiments will be readily apparent to those skilled in the art, and the generic principles defined herein may be applied to other embodiments without departing from the spirit or scope of the invention. Thus, the present invention is not intended to be limited to the embodiments shown herein but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.
Claims (4)
1. The preparation method of the passivator for treating the aluminum foil is characterized by comprising the following steps of:
(1) Weighing 0.3-1 part of chromium solution, 0.5-2 parts of modified phenolic resin, 2-5 parts of potassium zirconium carbonate, 2-5 parts of sodium diisobutylnaphthalenesulfonate, 0.5-2 parts of barium tellurate, 40-55 parts of ethanol and 35-40 parts of water in parts by weight;
the concentration of the chromium solution is 8-10%; the chromium solution is prepared from a trivalent chromium compound; the trivalent chromium compound is chromium hydroxide, chromium sulfate or chromium chloride;
the preparation method of the modified phenolic resin comprises the following steps: mixing phenolic resin and carboxylic acid according to a mass ratio of 1: (1-1.5) mixing and carrying out esterification reaction to obtain an ester group-containing phenolic resin derivative, wherein the carboxylic acid is formic acid, acetic acid or propionic acid; then, carrying out a ring opening reaction on the phenolic resin derivative containing the ester group and ethylene oxide according to a mass ratio of 1; carrying out secondary reaction on hydroxyl of a phenolic resin derivative containing hydroxyl and epoxy ethyl according to the mass ratio of 1-1.5 to obtain the modified phenolic resin;
(2) Mixing and uniformly stirring the chromium solution, the modified phenolic resin, ethanol and water, and then standing to obtain a mixed solution;
(3) And (3) sequentially adding potassium zirconium carbonate, diisobutyl naphthalene sulfonate and barium tellurate into the mixed solution obtained in the step (2), and heating and standing to obtain the passivator for treating the aluminum foil.
2. The method for preparing the passivating agent for processing the aluminum foil according to claim 1, wherein the ethanol is ethanol with a concentration of 60-90%.
3. The method for preparing a passivating agent for processing aluminum foil according to claim 1, wherein in the step (2), the stirring speed is 50-100r/min, the stirring time is 2-3h, and the standing time is 4-6h.
4. The method for preparing a passivating agent for processing aluminum foil according to claim 1, wherein the heating temperature in step (3) is 80-120 ℃, and the standing heating time is 8-12h.
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| JPS6245607A (en) * | 1985-08-23 | 1987-02-27 | Asahi Denka Kogyo Kk | Production of improved phenolic resin |
| JP3570110B2 (en) * | 1996-10-07 | 2004-09-29 | Ｊｆｅスチール株式会社 | Resin chromate treated Al-Zn alloy plated steel sheet with excellent blackening resistance |
| CN107384153B (en) * | 2017-06-08 | 2020-05-19 | 中瀚新材料科技有限公司 | Tin can internal coating and preparation method thereof |
| CN107557774A (en) * | 2017-09-01 | 2018-01-09 | 宁国市润丰金属制品有限公司 | A kind of automobile component aluminum alloy surface passivating method |
| CN108179407A (en) * | 2017-12-19 | 2018-06-19 | 乐凯胶片股份有限公司 | A kind of soft package lithium battery passivating solution and its packaging material |
| CN109112525A (en) * | 2018-10-10 | 2019-01-01 | 安徽工业大学 | A kind of composite passivant for Al-alloy metal plate |
| CN109609944B (en) * | 2018-12-30 | 2021-01-12 | 临沂金湖彩涂铝业有限公司 | Aluminum alloy natural color chromium-free passivation treating agent and preparation method thereof |
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