CN111455364A - Environment-friendly chromium-free passivation solution based on silicate and passivation process thereof - Google Patents
Environment-friendly chromium-free passivation solution based on silicate and passivation process thereof Download PDFInfo
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- CN111455364A CN111455364A CN202010400796.5A CN202010400796A CN111455364A CN 111455364 A CN111455364 A CN 111455364A CN 202010400796 A CN202010400796 A CN 202010400796A CN 111455364 A CN111455364 A CN 111455364A
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C22/00—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
- C23C22/05—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions
- C23C22/06—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions using aqueous acidic solutions with pH less than 6
- C23C22/48—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions using aqueous acidic solutions with pH less than 6 not containing phosphates, hexavalent chromium compounds, fluorides or complex fluorides, molybdates, tungstates, vanadates or oxalates
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D5/00—Electroplating characterised by the process; Pretreatment or after-treatment of workpieces
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D5/00—Electroplating characterised by the process; Pretreatment or after-treatment of workpieces
- C25D5/54—Electroplating of non-metallic surfaces
- C25D5/56—Electroplating of non-metallic surfaces of plastics
Abstract
The invention belongs to the technical field of electroplating processing, and particularly relates to an environment-friendly chromium-free passivation solution based on silicate and a passivation process thereof. The environment-friendly chromium-free passivation solution based on silicate provided by the invention comprises water, low molecular alcohol, sodium silicate, potassium silicate, sodium metasilicate, silane hydrolysate, diphenol propane, diethylene glycol monobutyl ether, sorbitol, phytic acid, glacial acetic acid, tannic acid, boric acid, sodium metabisulfite, sodium nitrate, sodium bisulfite and other components, has excellent stability, can be stably stored for more than three months, and has excellent corrosion resistance, blackening resistance and high-temperature baking resistance on the aspect of passivation performance. The passivation process of the silicate-based environment-friendly chromium-free passivation solution provided by the invention comprises the steps of dipping, airing, aging and the like, is simple and convenient to operate, has economic cost and stable and reliable quality, and has very high popularization and application values.
Description
Technical Field
The invention belongs to the technical field of electroplating processing, and particularly relates to an environment-friendly chromium-free passivation solution based on silicate and a passivation process thereof.
Background
Compared with a metal product, the plastic electroplating product not only can realize good metal texture, but also can reduce the weight of the product, effectively improves the appearance and the decoration of the plastic, and simultaneously improves the performances of the plastic in the aspects of electricity, heat, corrosion resistance and the like; in addition, plastic parts have excellent comprehensive performance, are easy to machine and form, and the surface of the material is easy to corrode so as to obtain higher coating binding force, so that plastic electroplating is widely applied. However, the conventional plastic electroplating process is not only expensive, but also inevitably causes environmental pollution, such as the need of noble metal palladium in the activation process and the need of highly polluted chromium in the passivation process. Palladium-free activation processes, chromium-free passivation processes, have been developed to address many of the drawbacks, but these processes still face many challenges in replacing conventional processes. Taking a chromium-free passivation process as an example, the existing chromium-free passivation process has the problems that a passivation solution is unstable and is not easy to store for a long time, the passivation effect is not durable enough, and the like.
Disclosure of Invention
In order to overcome the defects of the prior art, the invention provides an environment-friendly chromium-free passivation solution based on silicate and a passivation process thereof. The silicate-based environment-friendly chromium-free passivation solution comprises the following components in parts by weight:
100 portions of water
30-50 parts of low molecular alcohol
6-9 parts of sodium silicate
5-8 parts of potassium silicate
8-12 parts of sodium metasilicate
4-6 parts of silane hydrolysate
2-6 parts of diphenol propane
2-3 parts of diethylene glycol monobutyl ether
2-3 parts of sorbitol
5-6 parts of phytic acid
Glacial acetic acid 5-12 parts
1-2 parts of tannic acid
Boric acid 1-2 parts
2-3 parts of sodium metabisulfite
1-3 parts of sodium nitrate
1-2 parts of sodium bisulfite.
The invention provides an environment-friendly chromium-free passivation solution based on silicate, which takes silicate as a main film forming agent, is bonded on the surface of a coating layer under the action of silane hydrolysate, forms a stable and firm Me-O-Si covalent bond on the surface of the coating layer, and forms a compact three-dimensional reticular inorganic film protective layer taking Si-O-Si as a main body through crosslinking on the basis, thereby achieving the effect of chromium-free long-acting passivation.
Preferably, the low molecular alcohol is one or more of methanol, ethanol, n-propanol, isopropanol and ethylene glycol.
Preferably, the silicate-based environment-friendly chromium-free passivation solution is one or more of gamma-aminopropyltriethoxysilane, gamma- (methacryloyloxy) propyltrimethoxysilane, 3-mercaptopropyltrimethoxysilane and ethyl orthosilicate.
Furthermore, the environment-friendly chromium-free passivation solution based on silicate also comprises 3-5 parts of nano silicon dioxide.
Furthermore, the environment-friendly chromium-free passivation solution based on silicate also comprises 2-3 parts of pentasodium ethylene diamine tetra methylene phosphonate, 2-3 parts of amino trimethylene phosphonic acid and hydroxy ethylidene diphosphonic acid and 1-2 parts of tert-butyloxycarbonyl-L-octahydroindole-2-carboxylic acid.
Further, the environment-friendly chromium-free passivation solution based on silicate is prepared by the following steps:
a1: uniformly mixing water, low molecular alcohol, silane hydrolysate, phytic acid, glacial acetic acid, tannic acid, sorbitol, diphenol propane and diethylene glycol monobutyl ether according to the formula dosage;
a2: adding the rest components into the mixed solution obtained from A1 according to the formula amount, stirring for 30-50min at the temperature of 43-48 ℃, naturally cooling, and then continuing stirring for 20-30min to obtain the silicate-based environment-friendly chromium-free passivation solution.
Further, the passivation process of the environment-friendly chromium-free passivation solution based on the silicate comprises the following steps:
b1: immersing a workpiece in the environment-friendly chromium-free passivation solution based on silicate for 20-75s, and then taking out and standing for 15-30 s; repeating the steps for 2-3 times;
b2: immersing the workpiece in deionized water for 80-120s, taking out and drying at normal temperature;
b3: and heating and aging the workpiece.
Preferably, in the passivation process of the environment-friendly silicate-based chromium-free passivation solution, the temperature in the step B3 is set as follows: heating from normal temperature to 85 deg.C at a heating rate of 2 deg.C/min or less, maintaining at 85 deg.C for 30min, and naturally cooling.
Has the advantages that: the environment-friendly chromium-free passivation solution based on silicate provided by the invention has excellent stability and can be stably stored for more than three months; in the aspect of passivation performance, the passivated plating layer shows excellent corrosion resistance, blackening resistance and high-temperature baking resistance. The passivation process of the silicate-based environment-friendly chromium-free passivation solution provided by the invention is simple and convenient to operate, has economic cost and stable and reliable quality, and has very high popularization and application values.
Detailed Description
Example 1
An environment-friendly chromium-free passivation solution based on silicate comprises the following components in parts by weight:
100 portions of water
50 parts of low molecular alcohol
Sodium silicate 9 parts
8 portions of potassium silicate
12 portions of sodium metasilicate
6 parts of silane hydrolysate
6 parts of diphenol propane
Diethylene glycol monobutyl ether 3 parts
3 portions of sorbitol
Phytic acid 6 parts
Glacial acetic acid 12 parts
2 portions of tannic acid
Boric acid 2 parts
Sodium metabisulfite 3 parts
3 parts of sodium nitrate
And 2 parts of sodium bisulfite.
In this example, the low molecular weight alcohols were methanol and ethylene glycol 1: 2, or a mixture thereof.
In this embodiment, the silane hydrolysate is gamma-aminopropyltriethoxysilane and ethyl orthosilicate in a weight ratio of 3: 1.
In the embodiment, the silicate-based environment-friendly chromium-free passivation solution is prepared by the following steps:
a1: uniformly mixing water, low molecular alcohol, silane hydrolysate, phytic acid, glacial acetic acid, tannic acid, sorbitol, diphenol propane and diethylene glycol monobutyl ether according to the formula dosage;
a2: adding the rest components into the mixed solution obtained from A1 according to the formula amount, stirring for 50min at the temperature of 43 ℃, naturally cooling, and then continuing stirring for 30min to obtain the silicate-based environment-friendly chromium-free passivation solution.
In this embodiment, the passivation process of the silicate-based environment-friendly chromium-free passivation solution includes the following steps:
b1: immersing a workpiece in the environment-friendly chromium-free passivation solution based on silicate for 75s, and then taking out and standing for 30 s; repeating the steps for 3 times;
b2: immersing the workpiece in deionized water for 120s, taking out and drying at normal temperature;
b3: and heating and aging the workpiece for 30min at 60 ℃.
Example 2
An environment-friendly chromium-free passivation solution based on silicate comprises the following components in parts by weight:
100 portions of water
30 portions of low molecular alcohol
6 portions of sodium silicate
5 portions of potassium silicate
8 portions of sodium metasilicate
4 portions of silane hydrolysate
Diphenol propane 2 parts
Diethylene glycol monobutyl ether 2 parts
Sorbitol 2 parts
Phytic acid 5 parts
Glacial acetic acid 5 parts
1 part of tannic acid
Boric acid 1 part
Sodium metabisulfite 2 parts
1 part of sodium nitrate
And 1 part of sodium bisulfite.
In this embodiment, the low molecular alcohol is isopropyl alcohol.
In this embodiment, the silane hydrolysate is γ - (methacryloyloxy) propyl trimethoxysilane.
In the embodiment, the coating also comprises 3 parts of nano silicon dioxide.
In this example, the composition further includes 2 parts of pentasodium ethylenediamine tetramethylene phosphonate, 2 parts of aminotrimethylene phosphonic acid and hydroxyethylidene diphosphonic acid, and 1 part of t-butoxycarbonyl-L-octahydroindole-2-carboxylic acid.
In the embodiment, the silicate-based environment-friendly chromium-free passivation solution is prepared by the following steps:
a1: uniformly mixing water, low molecular alcohol, silane hydrolysate, phytic acid, glacial acetic acid, tannic acid, sorbitol, diphenol propane and diethylene glycol monobutyl ether according to the formula dosage;
a2: adding the rest components into the mixed solution obtained from A1 according to the formula amount, stirring for 30min at 48 ℃, naturally cooling, and then continuing stirring for 20min to obtain the silicate-based environment-friendly chromium-free passivation solution.
In this embodiment, the passivation process of the silicate-based environment-friendly chromium-free passivation solution includes the following steps:
b1: immersing a workpiece in the environment-friendly chromium-free passivation solution based on silicate for 20s, and then taking out and standing for 15 s; repeating the above steps for 2 times;
b2: immersing the workpiece in deionized water for 80s, taking out and drying at normal temperature;
b3: heating and aging the workpiece, wherein the temperature is set as follows: heating from normal temperature to 85 deg.C, heating at a rate of 2 deg.C/min, maintaining at 85 deg.C for 30min, and naturally cooling.
Example 3
An environment-friendly chromium-free passivation solution based on silicate comprises the following components in parts by weight:
100 portions of water
42 parts of low-molecular alcohol
8 portions of sodium silicate
7 portions of potassium silicate
8 portions of sodium metasilicate
Silane hydrolysate 5 parts
4 parts of diphenol propane
Diethylene glycol monobutyl ether 2 parts
Sorbitol 2 parts
Phytic acid 5 parts
Glacial acetic acid 8 parts
1 part of tannic acid
Boric acid 2 parts
Sodium metabisulfite 3 parts
2 parts of sodium nitrate
And 1 part of sodium bisulfite.
In this embodiment, the low molecular alcohol is a mixture of methanol, ethanol, and n-propanol in a ratio of 1:1:1 by weight.
In this example, the silane hydrolysate is a mixture of gamma-aminopropyltriethoxysilane, gamma- (methacryloyloxy) propyltrimethoxysilane and 3-mercaptopropyltrimethoxysilane in a ratio of 1:1:1 by weight.
In this example, 3 parts of pentasodium ethylenediaminetertramethylenephosphonate, 3 parts of aminotrimethylenephosphonic acid and hydroxyethylidenediphosphonic acid, and 2 parts of t-butoxycarbonyl-L-octahydroindole-2-carboxylic acid were also included.
In the embodiment, the silicate-based environment-friendly chromium-free passivation solution is prepared by the following steps:
a1: uniformly mixing water, low molecular alcohol, silane hydrolysate, phytic acid, glacial acetic acid, tannic acid, sorbitol, diphenol propane and diethylene glycol monobutyl ether according to the formula dosage;
a2: adding the rest components into the mixed solution obtained from A1 according to the formula amount, stirring for 50min at 45 ℃, naturally cooling, and then continuing stirring for 25min to obtain the silicate-based environment-friendly chromium-free passivation solution.
In this embodiment, the passivation process of the silicate-based environment-friendly chromium-free passivation solution includes the following steps:
b1: immersing a workpiece in the environment-friendly chromium-free passivation solution based on silicate for 60s, and then taking out and standing for 25 s; repeating the steps for 3 times;
b2: immersing the workpiece in deionized water for 90s, taking out and then airing at normal temperature;
b3: heating and aging the workpiece, wherein the temperature is set as follows: heating from normal temperature to 85 deg.C, heating at a rate of 1 deg.C/min, maintaining at 85 deg.C for 30min, and naturally cooling.
Example 4
An environment-friendly chromium-free passivation solution based on silicate comprises the following components in parts by weight:
100 portions of water
35 parts of low molecular alcohol
Sodium silicate 7 parts
8 portions of potassium silicate
10 portions of sodium metasilicate
Silane hydrolysate 5 parts
4 parts of diphenol propane
Diethylene glycol monobutyl ether 3 parts
3 portions of sorbitol
Phytic acid 6 parts
Glacial acetic acid 9 parts
2 portions of tannic acid
Boric acid 1 part
Sodium metabisulfite 2 parts
3 parts of sodium nitrate
And 2 parts of sodium bisulfite.
In this embodiment, the low molecular alcohol is ethylene glycol.
In this example, the silane hydrolysate is a 1:1 mixture of gamma- (methacryloyloxy) propyl trimethoxysilane and 3-mercaptopropyl trimethoxysilane by weight.
In the embodiment, the paint also comprises 5 parts of nano silicon dioxide.
In this example, 3 parts of pentasodium ethylenediaminetertramethylenephosphonate, 3 parts of aminotrimethylenephosphonic acid and hydroxyethylidenediphosphonic acid, and 1 part of t-butoxycarbonyl-L-octahydroindole-2-carboxylic acid were also included.
In the embodiment, the silicate-based environment-friendly chromium-free passivation solution is prepared by the following steps:
a1: uniformly mixing water, low molecular alcohol, silane hydrolysate, phytic acid, glacial acetic acid, tannic acid, sorbitol, diphenol propane and diethylene glycol monobutyl ether according to the formula dosage;
a2: adding the rest components into the mixed solution obtained from A1 according to the formula amount, stirring for 50min at the temperature of 43 ℃, naturally cooling, and then continuing stirring for 30min to obtain the silicate-based environment-friendly chromium-free passivation solution.
In this embodiment, the passivation process of the silicate-based environment-friendly chromium-free passivation solution includes the following steps:
b1: immersing a workpiece in the environment-friendly chromium-free passivation solution based on silicate for 75s, and then taking out and standing for 30 s; repeating the steps for 3 times;
b2: immersing the workpiece in deionized water for 100s, taking out and drying at normal temperature;
b3: heating and aging the workpiece, wherein the temperature is set as follows: heating from normal temperature to 85 deg.C at a heating rate of 2 deg.C/min or less, maintaining at 85 deg.C for 30min, and naturally cooling.
Comparative example 1
The other components, synthesis steps and passivation process were the same as in example 4 without adding silane hydrolysate.
Comparative example 2
The other components, synthesis steps and passivation process were the same as in example 4 without the addition of sodium metasilicate.
Comparative example 3
No phytic acid and tannic acid were added, and the other components, synthesis steps and passivation process were the same as in example 4.
Performance testing
In examples 1 to 5 and comparative examples 1 to 3, the treatment objects of the obtained passivation solutions were the same kind of galvanized plastic plate, and the passivation performances including corrosion resistance, blackening resistance and high-temperature baking resistance of the fresh passivation solution and the passivation solution after being stored for 90 days were respectively tested. Wherein the letters "A" are added before the serial numbers when the examples and comparative examples are recorded after 90 days of storage, for example, example 1 after 90 days of storage is described as example A1.
The corrosion resistance evaluation is carried out according to the standard GB/T10125-1997, a neutral salt spray test is carried out on the passivated galvanized plastic plate, the temperature in a salt spray box is 35 ℃, the salt solution is 50 g/L sodium chloride solution, the preparation method is that analytically pure sodium chloride solid is dissolved in distilled water with the conductivity not more than 20 mu S/cm, the pH value is 6.5-7.2, the time that no white spot appears on the surface of a passivated film after continuous spraying is recorded, the blackening resistance test is carried out, the passivated galvanized plastic plate is vertically inserted into boiling water to be soaked for 1h, the upper part of the water surface is exposed to half height, the color difference value △ E before and after the upper part of the water surface is dried is taken, the color difference value is not more than qualified, the color difference value is not more than 6, the high-temperature resistance baking performance is carried out, the passivated galvanized plastic plate is placed into an oven at 350 ℃ to be baked for 30min, the color difference value △ E value before and after the surface baking of the sample is determined, the color.
TABLE 1 test results
| Corrosion resistance (h) | Resistance to blackening | High temperature resistant baking | |
| Example 1 | 216 | Qualified | Qualified |
| Example 2 | 288 | Qualified | Qualified |
| Example 3 | >320 | Qualified | Qualified |
| Example 4 | >320 | Qualified | Qualified |
| Comparative example 1 | 36 | Fail to be qualified | Fail to be qualified |
| Comparative example 2 | 42 | Fail to be qualified | Fail to be qualified |
| Comparative example 3 | 84 | Fail to be qualified | Qualified |
| Example A1 | 198 | Qualified | Fail to be qualified |
| Example A2 | 276 | Qualified | Qualified |
| Example A3 | >320 | Qualified | Qualified |
| Example A4 | >320 | Qualified | Qualified |
| Comparative example A1 | <24 | Fail to be qualified | Fail to be qualified |
| Comparative example A2 | 36 | Fail to be qualified | Fail to be qualified |
| Comparative example A3 | 60 | Fail to be qualified | Fail to be qualified |
The foregoing is only a preferred embodiment of the present invention, and it should be noted that modifications can be made by those skilled in the art without departing from the principle of the present invention, and these modifications should also be construed as the protection scope of the present invention.
Claims (8)
1. An environment-friendly chromium-free passivation solution based on silicate is characterized in that: comprises the following components by weight:
100 portions of water
30-50 parts of low molecular alcohol
6-9 parts of sodium silicate
5-8 parts of potassium silicate
8-12 parts of sodium metasilicate
4-6 parts of silane hydrolysate
2-6 parts of diphenol propane
2-3 parts of diethylene glycol monobutyl ether
2-3 parts of sorbitol
5-6 parts of phytic acid
Glacial acetic acid 5-12 parts
1-2 parts of tannic acid
Boric acid 1-2 parts
2-3 parts of sodium metabisulfite
1-3 parts of sodium nitrate
1-2 parts of sodium bisulfite.
2. The silicate-based environment-friendly chromium-free passivation solution according to claim 1, characterized in that: the low molecular alcohol is one or more of methanol, ethanol, n-propanol, isopropanol and ethylene glycol.
3. The silicate-based environment-friendly chromium-free passivation solution according to claim 1, characterized in that: the silane hydrolysate is one or more of gamma-aminopropyltriethoxysilane, gamma- (methacryloyloxy) propyltrimethoxysilane, 3-mercaptopropyltrimethoxysilane and tetraethoxysilane.
4. The silicate-based environment-friendly chromium-free passivation solution according to claim 1, characterized in that: also comprises 3-5 parts of nano silicon dioxide.
5. The silicate-based environment-friendly chromium-free passivation solution as claimed in claim 1, further comprising 2-3 parts of pentasodium ethylene diamine tetra methylene phosphonate, 2-3 parts of amino trimethylene phosphonate and hydroxy ethylidene diphosphonic acid, and 1-2 parts of tert-butoxycarbonyl-L-octahydroindole-2-carboxylic acid.
6. The silicate-based environment-friendly chromium-free passivation solution according to any one of claims 1 to 5, characterized in that: the preparation method comprises the following steps:
a1: uniformly mixing water, low molecular alcohol, silane hydrolysate, phytic acid, glacial acetic acid, tannic acid, sorbitol, diphenol propane and diethylene glycol monobutyl ether according to the formula dosage;
a2: adding the rest components into the mixed solution obtained from A1 according to the formula amount, stirring for 30-50min at the temperature of 43-48 ℃, naturally cooling, and then continuing stirring for 20-30min to obtain the silicate-based environment-friendly chromium-free passivation solution.
7. The passivation process of the silicate-based environment-friendly chromium-free passivation solution according to claim 6, characterized in that: the method comprises the following steps:
b1: immersing a workpiece in the environment-friendly chromium-free passivation solution based on silicate for 20-75s, and then taking out and standing for 15-30 s; repeating the steps for 2-3 times;
b2: immersing the workpiece in deionized water for 80-120s, taking out and drying at normal temperature;
b3: and heating and aging the workpiece.
8. The passivation process of the silicate-based environment-friendly chromium-free passivation solution according to claim 7, characterized in that: the temperature in step B3 was set to: heating from normal temperature to 85 deg.C at a heating rate of 2 deg.C/min or less, maintaining at 85 deg.C for 30min, and naturally cooling.
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| CN114921775A (en) * | 2022-05-16 | 2022-08-19 | 浙江遂昌奥美化工科技有限公司 | Environment-friendly coating agent and preparation method thereof |
| CN114952081A (en) * | 2022-05-16 | 2022-08-30 | 湖南永盛新材料股份有限公司 | Excellent weldability protective agent and preparation method of nickel-plated steel strip based on excellent weldability protective agent |
| CN114952081B (en) * | 2022-05-16 | 2024-04-26 | 湖南永盛新材料股份有限公司 | Excellent welding property protective agent and preparation method of nickel-plated steel strip based on excellent welding property protective agent |
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Application publication date: 20200728 |