CN115247263A - Environment-friendly passivation composition for tin plate and preparation method and application thereof - Google Patents
Environment-friendly passivation composition for tin plate and preparation method and application thereof Download PDFInfo
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- CN115247263A CN115247263A CN202210696003.8A CN202210696003A CN115247263A CN 115247263 A CN115247263 A CN 115247263A CN 202210696003 A CN202210696003 A CN 202210696003A CN 115247263 A CN115247263 A CN 115247263A
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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
- C23C22/361—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
Abstract
The invention discloses an environment-friendly passivation composition for a tin plate, a preparation method and application thereof, wherein the environment-friendly passivation composition comprises the following components in percentage by weight: 0.05-2% of water-soluble composite fluoride containing transition metal element, 0.005-0.2% of Cr 3+ 0.005-0.2% hydrolyzed oligomer of trialkoxysilane containing organic functional group, 0.05-0.2% PO 4 3‑ The water soluble substance and pure water or deionized water are used, the traditional rapid film forming of the Zr-Ti nano passivation layer is maintained, the advantages of high-speed continuous tin plate production line, corrosion resistance, acid resistance and the like are achieved, and meanwhile, a trivalent chromium compound with good environmental protection property is introduced to form a chromium oxide (III) layer to strengthen the sulfuration resistance of the chromium-free Zr-Ti nano passivation layer, and the chromium-free Zr-Ti nano passivation layer is used for passivation treatment of the tin plate high-speed production line to ensure the long-term quality and food safety of canned food.
Description
Technical Field
The invention belongs to the field of surface treatment, and particularly relates to an environment-friendly passivation composition, a preparation method and application thereof, in particular to passivation treatment for a continuous production line of tin plates.
Background
The tin plate (also called tin plate) is mainly used for manufacturing tin cans, most of which are used for food packaging such as vegetable and fish cans, beverage and beer cans and the like, and a small amount of tin plate (accounting for about 2% -5% of the total production amount of the tin plate) is also used in non-food industries such as electronic (circuit boards), buildings (radiators), engineering (oil filters of automobiles) and the like. During transportation and storage, the tin plate without passivation treatment can naturally form a tin oxide layer on the surface, and the tin oxide layer not only destroys the binding force to subsequent varnish, but also makes the appearance of the tin plate dark and reduces the corrosion resistance of the tin plate, and has potential negative effects on the quality and safety of canned products. Therefore, in a continuous production line of tin plates, there is usually a passivation process, the purpose of passivation is to form a very thin passivation layer on the surface of the tin plate to inhibit the growth of tin oxide layer, and the cross-sectional structure of the tin plate coated and passivated is shown in fig. 1.
For many years, a hexavalent chromium electrolytic passivation-based process has been used in a tin plate production line, and a passivation film formed by the process can provide excellent overall properties to the tin plate, including: 1) Corrosion resistance (oxidation tin growth resistance): the growth of tin oxide in the transportation and storage process is prevented, and the surface of the tin plate is prevented from discoloring; 2) Coating property: the excellent binding force is provided in the subsequent painting, decoration and printing processes of the tin plate; 3) Weldability; 4) Resistance to vulcanization (or resistance to vulcanization mottling): has anti-staining effect on sulfide released from food containing natural protein. The electrolytic passivation process of the tin plate is to dip the tin plate into electrolyte and apply current to quickly form a layer of passivation film on the plate surface, and the hexavalent chromium electrolytic solution contains Na + 、Cr 2 O 7 、CrO 4 - 、H 2 Cr 2 O 7 And Na 2 Cr 2 O 7 The substances are various salt hydrate/ion mixed aqueous solutions, hexavalent chromium ions in the electrolyte are reduced into trivalent chromium and metal chromium in the passivation layer forming process, and the passivation layer mainly comprises the following components: 1) Containing trivalent chromium(Cr (III)) hydroxide, 2) oxide containing trivalent chromium (Cr (III)) and 3) metallic chromium, and although the finally obtained passivation layer does not contain hexavalent chromium substances harmful to human bodies and meets the safety requirements on canned foods, the solution containing hexavalent chromium ions used in the electrolytic process causes great harm to the health of field operation workers.
In recent decades, the tin plating industry has been actively developing various alternative passivation processes, and representative alternative passivation processes at present include zirconium-titanium oxide nano passivation (Zr-Ti), trivalent chromium electrolytic passivation, silane sol-gel passivation, manganese-based passivation, molybdate passivation, and the like, and patent documents related to these passivation processes include CN100564597C, CN101358340A, CN104099649A, WO2017092648A1, CN111304706A, CN105331966A, CN101638804A, CN104451636A, CN105543827A, CN101545107A, US10011915B2, US20130192995A1, US20180347051A1, and US20200325591A1. In recent years, the european union CTAC organizes and comprehensively evaluates the industrialization potential of the alternative passivation process, and the evaluation results are as follows: (1) passivating Zr-Ti nano oxide: the passivation film can be rapidly formed on the tin plate by a roller coating mode, and the main component is ZrO 2 /TiO 2 A mixture of phosphoric acid and a high molecular polymer, the combination property of which is equivalent to that of the traditional passivation layer, but the obvious defect is that the sulfuration resistance is inferior to that of the traditional passivation layer; (2) trivalent chromium electrolytic passivation: the method is similar to a hexavalent chromium electrolytic passivation process, the comprehensive performance of the passivation layer is similar to that of the traditional passivation layer, but the process is still in the initial development stage at present and is not applied in large-scale industrialization; (3) silane sol-gel passivation: the organic/inorganic silica crosslinked layer is formed by a roller coating mode, tests show that a silane film can not effectively prevent the growth of tin oxide, and the silane passivation process can not be applied to a high-speed production line due to the slow film forming speed, and if the linear speed is more than 500m/min, the requirements of industrialized production of tin-plated plates are not met; (4) manganese passivation: manganese (IV) oxide is formed by a roller coating or dipping mode, and the corrosion resistance of the manganese (IV) oxide does not meet the requirement of the food packaging industry, namely the growth of tin oxide cannot be effectively prevented; and (5) molybdate passivation: the molybdate conversion film is formed on the surface of the tinning plate in a dipping mode, the corrosion resistance of the molybdate conversion film is poor, and the molybdate can generate colored deposits and colorsThe color of the painted panel changes to brown along with the thickness of the passivation layer, and further changes in the canning and sterilization steps, and the color change does not meet the appearance requirement of the food packaging industry.
In summary, although no alternative passivation process can fully replace the traditional hexavalent chromium electrolytic passivation process at present, wherein the Zr-Ti oxide nano passivation process is generally considered to be the most possible alternative to the traditional passivation process in the industry, the obvious defects of the Zr-Ti nano passivation layer are that the resistance to vulcanization is inferior to that of the traditional passivation film, and the poor resistance to vulcanization leads to the failure to ensure the long-term quality and food safety of canned food. The anti-sulfuration of the tin plate is mainly protected by a varnish layer and a traditional passivation layer which takes chromium oxide (III) as the main component, and ZrO 2 -TiO 2 The passivation layer has no similar protective effect, resulting in poor sulfidation resistance of the Zi-Ti passivated tin plate.
Disclosure of Invention
In order to solve the problem of poor sulfuration resistance of the tin plate adopting a Zr-Ti oxide nano passivation process in the prior art, the invention mainly aims to provide an environment-friendly passivation composition, which is used for enhancing the sulfuration resistance of a chromium-free Zr-Ti nano passivation layer by introducing a trivalent chromium compound with good environmental protection to form a chromium oxide (III) layer while retaining the advantages of rapid film formation of a traditional Zr-Ti nano passivation layer, suitability for a high-speed continuous tin plate production line, corrosion resistance, acid resistance and the like, so that the long-term quality of canned food and the food safety are ensured.
Another objective of the present invention is to provide a method for preparing the above-mentioned passivation composition, which is simple in process and suitable for large-scale industrial production.
The invention also aims to provide the application of the environment-friendly passivation composition in the high-speed production line passivation treatment of the tin plate, and the environment-friendly passivation composition is particularly suitable for the high-speed production line passivation treatment of the tin plate for canned food.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows:
the invention provides an environment-friendly passivation composition, which consists of the following components in percentage by weight:
preferably, the transition metal element-containing water-soluble complex fluoride exists in the form of acid or salt, wherein the transition metal element is selected from one or more of Ti, zr and Si, and the acid of the transition metal element-containing water-soluble complex fluoride is selected from H 2 TiF 6 、H 2 ZrF 6 、H 2 SiF 6 Or a mixture thereof, the salt of the water-soluble complex fluoride containing a transition metal element being selected from K 2 TiF 6 、K 2 ZrF 6 、K 2 SiF 6 Or mixtures thereof.
More preferably, the transition metal element-containing water-soluble complex fluoride is H 2 TiF 6 And H 2 ZrF 6 According to the mass ratio of 2: 1.
Preferably, the Cr-containing component 3+ The water-soluble compound is one or more selected from chromium nitrate, chromium sulfate and chromium chloride, wherein Cr is 3+ The content of (B) is 50-2000ppm.
Preferably, the hydrolyzed oligomer of trialkoxysilane containing organic functional groups is formed by hydrolyzing a silane coupling agent, wherein the silane coupling agent is selected from one or more of gamma-aminopropyltriethoxysilane, gamma- (2,3-glycidoxy) propyltrimethoxysilane, gamma-methacryloxypropyltrimethoxysilane and gamma-mercaptopropyltrimethoxysilane, and the content of Si is 0.1-2%.
Preferably, the PO contains 4 3- The water soluble substance is selected from one or more of orthophosphoric acid and salts thereof, metaphosphoric acid and salts thereof, condensed phosphoric acid and salts thereof, wherein PO 4 3- In an amount of 50-2000ppm, as a corrosion inhibitor, can provide a certain self-lifeRepair "function, i.e. rapid passivation of damaged fresh metal surfaces.
Preferably, the PO contains 4 3- The water soluble substance is orthophosphoric acid and salts thereof, and is selected from one or more of phosphoric acid, dihydric phosphate and monohydrogen phosphate.
The invention also provides a preparation method of the environment-friendly passivation composition, which comprises the following steps:
(1) Weighing the hydrolyzed oligomer of trialkoxysilane containing organic functional groups according to the proportion, stirring and adding deionized water for hydrolysis until the solution is clear, and stabilizing the hydrolyzed solution by adjusting the pH value of the solution to 4-5;
(2) Under the condition of stirring, the Cr-containing material 3+ Adding the water-soluble compound of (1) to the above mixture, and stirring until dissolved;
(3) Under the condition of stirring, adding water-soluble composite fluoride containing transition metal elements into the mixture, and stirring until the mixture is uniform and clear;
(4) Under the condition of stirring, PO is contained 4 3- Adding the water-soluble raw materials into the mixture, and stirring until the water-soluble raw materials are dissolved;
the steps are all carried out at normal temperature and normal pressure.
The invention also provides application of the environment-friendly passivation composition in the passivation treatment of a tin plate high-speed production line, in particular to the passivation treatment of the tin plate for canned food on the high-speed production line.
Compared with the prior art, the invention has the following beneficial effects:
(1) The environment-friendly passivation composition does not contain hexavalent chromium compounds, and is an environment-friendly passivation composition.
(2) The passivation film obtained by carrying out tin plate passivation treatment on the environment-friendly passivation composition has excellent sulfuration resistance, and ensures the long-term quality and food safety of canned food.
(3) The environment-friendly passivation composition can quickly form a film, quickly form a passivation film on the surface of a tin plate, meet the operation requirement of a continuous tin plate high-speed production line, and obtain the passivation film with excellent performances of no color change, effective inhibition of growth of a tin oxide layer and the like.
Drawings
Fig. 1 is a schematic cross-sectional view of a prior art oiled and passivated tin plate.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions of the embodiments of the present invention will be clearly and completely described below with reference to the drawings of the embodiments of the present invention. It is to be understood that the embodiments described are only a few 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 described embodiments of the invention without any inventive step, are within the scope of protection of the invention.
The application method of the environment-friendly passivation composition in the following examples comprises spray extrusion and roll coating, and then a wringing roller is used for removing the redundant passivation solution, so that the environment-friendly passivation solution is uniformly distributed on the surface of the tin plate.
The performance test of the environment-friendly passivation composition comprises the following steps:
(1) And (3) antioxidant tin growth test:
the method comprises the following steps: the mixture was baked with hot air at 200 ℃ for 60 minutes.
The method 2 comprises the following steps: and storing at room temperature for three months, observing the color change condition of the tinned plate surface, and inspecting the oxidation-resistant tin growth condition of the passivation film.
(2) And (3) testing the coating performance: the varnish is common epoxy phenolic coating, is coated on a passivated tin plate, and the paint film of the dried coating is 6-8g/m 2 And after the surface of the paint film is subjected to ring marking and tape stripping, detecting the stripping condition of the paint film, and evaluating the coating performance according to the stripping area of the paint film by referring to a paint film adhesion evaluation method adopted by QB/T2763-2006.
(3) And (3) vulcanization resistance test: and (4) observing the generation condition of the vulcanization spots of the passivated board surface after the test by referring to the evaluation method of the anti-vulcanization spot performance of QB/T2763-2006.
(4) Acid resistance test: and (4) observing the generation condition of the acidification spots of the passivated board surface after the test by referring to the evaluation method of the acid resistance of QB/T2763-2006.
The compositions of the environmentally friendly passivation compositions of examples 1-12 are shown in Table 1, with the components present in mass percent (%) and the balance being water, wherein Zr is derived from an aqueous solution of fluorozirconic acid, ti is derived from an aqueous solution of fluorotitanic acid, and Cr is 3+ The ions being from chromium nitrate, PO 4 3- The ions were from a 75% phosphoric acid solution and the Si was from a hydrolyzed oligomer solution of gamma-aminopropyltriethoxysilane. After the solution is prepared, the content of each element is determined by ICP-MS (inductively coupled plasma mass spectrometer) measurement.
The environmental passivation compositions of examples 1-12 were applied to cleaned tin plates by roll coating, followed by squeezing off excess passivation solution with a squeeze roll to uniformly distribute the passivation solution film on the tin plate surface, and oven dried (PMT: 80-120 ℃, oven drying time 1-3 seconds) to obtain passivated tin plates, table 2 shows the performance test results, comparative example is commercial Zr — Ti product.
TABLE 1
| Examples | Zr(％) | Ti(％) | Cr 3+ (％) | PO 4 3- (％) | Si(％) |
| 1 | 0.5 | / | / | / | 0.3 |
| 2 | 0.5 | / | 0.05 | / | 0.3 |
| 3 | 0.5 | / | 0.1 | / | 0.3 |
| 4 | 0.5 | / | 0.1 | 0.1 | 0.3 |
| 5 | 0.25 | 0.5 | / | / | 0.2 |
| 6 | 0.25 | 0.5 | 0.05 | / | 0.2 |
| 7 | 0.25 | 0.5 | 0.1 | / | 0.2 |
| 8 | 0.25 | 0.5 | 0.1 | 0.1 | 0.2 |
| 9 | / | 1.0 | / | / | 0.4 |
| 10 | / | 1.0 | 0.05 | / | 0.4 |
| 11 | / | 1.0 | 0.1 | / | 0.4 |
| 12 | / | 1.0 | 0.1 | 0.1 | 0.4 |
TABLE 2
= performance equivalent to comparative example; + indicates better performance than the comparative example; -indicates inferior performance compared to the comparative examples.
As can be seen from Table 2, the environment-friendly passivation composition provided by the invention maintains the advantages of rapid film formation of the traditional Zr-Ti nano passivation layer, suitability for high-speed continuous tin plate production line, corrosion resistance, acid resistance and the like, and simultaneously, strengthens the sulfuration resistance of the chromium-free Zr-Ti nano passivation layer by introducing the environment-friendly trivalent chromium compound to form the chromium oxide (III) layer, so as to ensure the long-term quality and food safety of tin plating for canned food after passivation treatment, wherein H is 2 TiF 6 And H 2 ZrF 6 The mass ratio is 2: when the trivalent chromium ion-containing water-soluble compound is combined for synergistic action, the high-temperature corrosion resistance and the anti-vulcanization performance of the product are improved compared with those of a commercial Zr-Ti product, and the product is suitable for passivation treatment of a tin plate high-speed production line for canned food which is transported and stored for a long time.
The above description is only for the specific embodiments of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art can easily conceive of the changes or substitutions within the technical scope of the present invention, and all the changes or substitutions should be covered within the scope of the present invention. Therefore, the protection scope of the present invention shall be subject to the protection scope of the claims.
Claims (10)
1. An environment-friendly passivation composition is characterized by comprising the following components in percentage by weight:
2. the environmentally friendly passivation composition of claim 1, wherein the transition metal element-containing water-soluble complex fluoride is present in the form of acid or salt, wherein the transition metal element is selected from one or more of Ti, zr and Si, and the acid of the transition metal element-containing water-soluble complex fluoride is selected from H 2 TiF 6 、H 2 ZrF 6 、H 2 SiF 6 Or a mixture thereof, the salt of the water-soluble complex fluoride containing the transition metal element is selected from K 2 TiF 6 、K 2 ZrF 6 、K 2 SiF 6 Or mixtures thereof.
3. The environmentally friendly passivation composition of claim 2, wherein the transition metal element-containing water soluble complex fluoride is H 2 TiF 6 And H 2 ZrF 6 According to the mass ratio of 2: 1.
4. The environmentally friendly passivation composition of claim 1, wherein the Cr-containing is 3+ The water-soluble compound is one or more selected from chromium nitrate, chromium sulfate and chromium chloride.
5. The environmentally friendly passivation composition of claim 1, wherein the hydrolyzed oligomer of an organofunctional trialkoxysilane is formed by hydrolysis of a silane coupling agent, wherein the silane coupling agent is selected from one or more of gamma-aminopropyltriethoxysilane, gamma- (2,3-glycidoxy) propyltrimethoxysilane, gamma-methacryloxypropyltrimethoxysilane, and gamma-mercaptopropyltrimethoxysilane.
6. The environmentally friendly passivation composition of claim 1, wherein the PO is present 4 3- The water soluble substance is selected from orthophosphoric acid and salts thereof, metaphosphoric acid andone or more of salts thereof, condensed phosphoric acid and salts thereof.
7. The environmentally friendly passivation composition of claim 6, wherein the PO is present 4 3- The water soluble substance is orthophosphoric acid and salts thereof, and is selected from one or more of phosphoric acid, dihydric phosphate and monohydrogen phosphate.
8. A method for preparing the environmentally friendly passivating composition of any of claims 1 to 7, comprising the steps of:
(1) Weighing the hydrolyzed oligomer of trialkoxysilane containing organic functional groups according to the proportion, stirring and adding deionized water for hydrolysis until the solution is clear, and stabilizing the hydrolyzed solution by adjusting the pH value of the solution to 4-5;
(2) Under the condition of stirring, the Cr-containing material 3+ Adding the water-soluble compound of (1) to the above mixture, and stirring until dissolved;
(3) Under the condition of stirring, adding water-soluble composite fluoride containing transition metal elements into the mixture, and stirring until the mixture is uniform and clear;
(4) Under the condition of stirring, PO is contained 4 3- Adding the water-soluble raw materials into the mixture, and stirring until the water-soluble raw materials are dissolved; the steps are all carried out at normal temperature and normal pressure.
9. Use of the environmentally friendly passivation composition of any of claims 1 to 7 in the passivation treatment of tin plate high speed production lines.
10. The use according to claim 9, wherein the environmentally friendly passivation composition is used for high speed production line passivation of tin plate for canned food.
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