CN110079795B - Galvanized part surface treating agent and preparation method thereof - Google Patents
Galvanized part surface treating agent and preparation method thereof Download PDFInfo
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- CN110079795B CN110079795B CN201910537440.3A CN201910537440A CN110079795B CN 110079795 B CN110079795 B CN 110079795B CN 201910537440 A CN201910537440 A CN 201910537440A CN 110079795 B CN110079795 B CN 110079795B
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- galvanized
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- ethylenediamine
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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
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Abstract
The invention discloses a galvanized part surface treating agent, which is prepared from the following raw materials: 15-20 g/L of titanyl sulfate, 20-30 g/L of sodium silicate, 1-5 g/L of phytic acid, 30-35 g/L of sodium nitrate, 5-10 g/L of ammonium bifluoride, 3-5 mL/L of sulfuric acid, 5-10 g/L of lanthanum chloride, 10-15 mL/L, N of hydrogen peroxide, 1-3 g/L of N, N ', N' -tetra (hydroxymethyl) ethylenediamine and the balance of water. The invention improves the formula of the existing chromium-free color passivation solution, adds N, N, N ', N' -tetra (hydroxymethyl) ethylenediamine with specific dosage, and replaces the fluoride with ammonium bifluoride, so that the appearance of the passivated galvanized part keeps the natural color of the galvanized layer, the corrosion resistance of the galvanized part is improved, the market acceptance of the passivated galvanized part is greatly improved, and the chromium-free color passivation solution has considerable economic benefit and wide application prospect.
Description
Technical Field
The invention belongs to the field of metal surface treatment, and particularly relates to a galvanized part surface treating agent and a preparation method thereof.
Background
The passivation treatment is a surface treatment method for forming a firm, compact and high-stability film on the plating layer by performing chemical or electrochemical treatment in a certain solution, and the passivation further improves the corrosion resistance of the plating layer and increases the surface gloss and the pollution resistance. For example, the surface of a workpiece treated by chemical plating, electroplating, acid washing, water washing and the like is very active, so that passivation treatment is immediately carried out, and a layer of protective film is formed on the treated metal surface to slow down corrosion. The workpiece is passivated comprehensively, so that the corrosion resistance of the workpiece can be improved, and the service life of the workpiece can be prolonged.
The passivation formula and the passivation process mainly comprise chromium passivation and chromium-free passivation. The more mature and early used of these studies is chromate passivation, but as hexavalent chromium is highly toxic and carcinogenic, with the growing awareness of environmental protection, it is increasingly desirable to find new formulations and new processes that can replace chromic acid passivation. At present, some technical solutions of chromium-free passivation treating agents for galvanized parts have been disclosed in the prior art, for example, chinese patent application with publication number CN105779983A discloses a chromium-free color passivation solution, which comprises the following components in percentage by weight: 15-20 g/L of titanyl sulfate, 20-30 g/L of sodium silicate, 1-5 g/L of phytic acid, 30-35 g/L of sodium nitrate, 5-10 g/L of fluoride, 3-5 mL/L of sulfuric acid, 5-10 g/L of lanthanum chloride, 10-15 mL/L of hydrogen peroxide, and the balance of water H2O, wherein the pH value of the passivation solution is 1-3; the passivation solution does not contain harmful substances of heavy metals such as chromium and the like, is harmless to the environment and human body, has good stability, and is a brand-new environment-friendly passivation solution with high corrosion resistance of a passivation film formed on the surface of a zinc coating. However, the galvanized part treated by the chromium-free color passivation solution is colored in appearance, and the surface of the galvanized part is required to keep the natural color of a galvanized layer in many application occasions. Therefore, the appearance color reduces the market application prospect of the chromium-free color passivation solution product. Therefore, it is an urgent need to develop a chromium-free passivation treating agent which does not change the appearance of the zinc coating layer and can further improve the corrosion resistance.
Disclosure of Invention
In order to overcome the defects of the prior art, the invention aims to provide a chromium-free passivation surface treating agent which does not change the appearance of a zinc coating, mainly solves the technical problem that a zinc-plated piece subjected to passivation treatment in the prior art is colored in appearance, and further improves the corrosion resistance of the zinc-plated piece.
In order to realize the purpose, the invention adopts the following technical scheme:
a galvanized part surface treating agent is prepared from the following raw materials: 15-20 g/L of titanyl sulfate, 20-30 g/L of sodium silicate, 1-5 g/L of phytic acid, 30-35 g/L of sodium nitrate, 5-10 g/L of ammonium bifluoride, 3-5 mL/L of sulfuric acid, 5-10 g/L of lanthanum chloride, 10-15 mL/L, N of hydrogen peroxide, 1-3 g/L of N, N ', N' -tetra (hydroxymethyl) ethylenediamine and the balance of water.
The sulfuric acid is concentrated sulfuric acid with the mass fraction of 98%.
The preparation method of the galvanized part surface treating agent is simple and convenient, the raw materials are sequentially added into water according to the sequence of titanyl sulfate, sodium silicate, phytic acid, sodium nitrate, ammonium bifluoride, sulfuric acid, lanthanum chloride, hydrogen peroxide, N, N, N ', N' -tetra (hydroxymethyl) ethylenediamine, stirred and dissolved uniformly, and the following raw materials can be added after one raw material is completely dissolved each time.
Compared with the prior art, the invention has the beneficial effects that: the invention improves the formula of the existing chromium-free color passivation solution, adds N, N, N ', N' -tetra (hydroxymethyl) ethylenediamine with specific dosage, and replaces the fluoride with ammonium bifluoride, so that the appearance of the passivated galvanized part keeps the natural color of the galvanized layer, the corrosion resistance of the galvanized part is improved, the market acceptance of the passivated galvanized part is greatly improved, and the chromium-free color passivation solution has considerable economic benefit and wide application prospect.
Detailed Description
The invention is further described below by way of examples.
Example 1:
a galvanized part surface treating agent is prepared from the following raw materials: 15g/L of titanyl sulfate, 20g/L of sodium silicate, 3g/L of phytic acid, 30g/L of sodium nitrate, 5g/L of ammonium bifluoride, 3mL/L of concentrated sulfuric acid with the mass fraction of 98%, 5g/L of lanthanum chloride, 10mL/L, N of hydrogen peroxide, 2 g/L of N, N ', N' -tetra (hydroxymethyl) ethylenediamine and the balance of water.
The preparation method of the galvanized part surface treating agent comprises the following steps: the raw materials are sequentially added into water according to the sequence of titanyl sulfate, sodium silicate, phytic acid, sodium nitrate, ammonium bifluoride, sulfuric acid, lanthanum chloride, hydrogen peroxide and N, N, N ', N' -tetra (hydroxymethyl) ethylenediamine, stirred and dissolved uniformly, and the later raw materials can be added after one raw material is completely dissolved.
Example 2:
a galvanized part surface treating agent is prepared from the following raw materials: 20g/L of titanyl sulfate, 20g/L of sodium silicate, 5g/L of phytic acid, 30g/L of sodium nitrate, 10g/L of ammonium bifluoride, 3mL/L of concentrated sulfuric acid with the mass fraction of 98%, 10g/L of lanthanum chloride, 10mL/L, N of hydrogen peroxide, 3g/L of N, N ', N' -tetra (hydroxymethyl) ethylenediamine and the balance of water.
The preparation method of the galvanized part surface treating agent is the same as that of the example 1.
Example 3:
a galvanized part surface treating agent is prepared from the following raw materials: 15g/L of titanyl sulfate, 30g/L of sodium silicate, 1g/L of phytic acid, 35g/L of sodium nitrate, 5g/L of ammonium bifluoride, 5mL/L of concentrated sulfuric acid with the mass fraction of 98%, 5g/L of lanthanum chloride, 15mL/L, N of hydrogen peroxide, 1g/L of N, N ', N' -tetra (hydroxymethyl) ethylenediamine and the balance of water.
The preparation method of the galvanized part surface treating agent is the same as that of the example 1.
Comparative example 1:
a galvanized part surface treating agent is prepared from the following raw materials: 15g/L of titanyl sulfate, 20g/L of sodium silicate, 3g/L of phytic acid, 30g/L of sodium nitrate, 5g/L of ammonium bifluoride, 3mL/L of concentrated sulfuric acid with the mass fraction of 98%, 5g/L of lanthanum chloride, 10mL/L of hydrogen peroxide and the balance of water.
Comparative example 1 is different from example 1 in that N, N, N ', N' -tetrakis (hydroxymethyl) ethylenediamine was not added, and other raw material components and preparation method were the same as example 1.
Comparative example 2:
a galvanized part surface treating agent is prepared from the following raw materials: 15g/L of titanyl sulfate, 20g/L of sodium silicate, 3g/L of phytic acid, 30g/L of sodium nitrate, 5g/L of sodium fluoride, 3mL/L of concentrated sulfuric acid with the mass fraction of 98%, 5g/L of lanthanum chloride, 10mL/L, N of hydrogen peroxide, 2 g/L of N, N ', N' -tetra (hydroxymethyl) ethylenediamine and the balance of water.
Comparative example 2 differs from example 1 in that sodium fluoride is used instead of ammonium bifluoride, and the other raw material components and preparation method are the same as those of example 1.
Comparative example 3:
a galvanized part surface treating agent is prepared from the following raw materials: 15g/L of titanyl sulfate, 20g/L of sodium silicate, 3g/L of phytic acid, 30g/L of sodium nitrate, 5g/L of ammonium bifluoride, 3mL/L of concentrated sulfuric acid with the mass fraction of 98%, 5g/L of lanthanum chloride, 10mL/L, N of hydrogen peroxide, 0.2 g/L of N, N ', N' -tetra (hydroxymethyl) ethylenediamine and the balance of water.
Comparative example 3 is different from example 1 in that the amount of N, N, N ', N' -tetrakis (hydroxymethyl) ethylenediamine used was reduced to 0.2 g/L, and other raw material components and preparation method were the same as example 1.
Comparative example 4:
a galvanized part surface treating agent is prepared from the following raw materials: 15g/L of titanyl sulfate, 20g/L of sodium silicate, 3g/L of phytic acid, 30g/L of sodium nitrate, 5g/L of ammonium bifluoride, 3mL/L of concentrated sulfuric acid with the mass fraction of 98%, 5g/L of lanthanum chloride, 10mL/L, N of hydrogen peroxide, 5g/L of N, N ', N' -tetra (hydroxymethyl) ethylenediamine and the balance of water.
Comparative example 4 is different from example 1 in that the amount of N, N, N ', N' -tetrakis (hydroxymethyl) ethylenediamine used was increased to 5g/L, and other raw material components and preparation method were the same as example 1.
The galvanized part surface treatment agent prepared in the embodiments 1-3 and the comparative examples 1-4 is used for passivating the same batch of hot-dip galvanized steel plates, and specifically comprises the following steps: soaking at room temperature for 60s, washing with water, and drying.
After the salt spray corrosion test is carried out on the passivated hot-dip galvanized steel sheet for 120 hours according to GB/T10125-1997 salt spray test for artificial atmosphere corrosion test, the grade evaluation is carried out by referring to GB/T6461-2002 grade of samples and test pieces after corrosion tests of metals and other inorganic coatings on metal substrates, and the results are shown in Table 1:
TABLE 1 evaluation results of neutral salt spray corrosion protection level
| Appearance of the product | White rust area A/%) | Protection class | |
| Example 1 | Zinc coating natural color | Is free of | 10 |
| Example 2 | Zinc coating natural color | 0~0.1 | 9 |
| Example 3 | Zinc coating natural color | 0~0.1 | 9 |
| Comparative example 1 | Light blue purple | 5.0~10 | 3 |
| Comparative example 2 | Blue and white | 10~25 | 2 |
| Comparative example 3 | Light blue purple | 2.5~5.0 | 4 |
| Comparative example 4 | Zinc coating natural color | 10~25 | 2 |
As can be seen from table 1, the galvanized parts treated with the surface treatment agents of examples 1 to 3 of the present invention maintain the original color of the galvanized layer, and the treated galvanized parts have excellent salt spray corrosion resistance, wherein in example 1, after 120h of a salt spray test, the surface still does not start to rust, and example 1 is the best technical solution of the present invention. Comparative example 1 no N, N' -tetrakis (hydroxymethyl) ethylenediamine was added to the treatment agent, the surface of the treated galvanized article was bluish violet, and more than 5.0% of the surface area was rusted after 120 hours of salt spray test; comparative example 2 sodium fluoride is used in the treating agent to replace ammonium bifluoride, the surface of the galvanized part after treatment is blue-white, and more than 10% of the surface is rusted after 120 hours of salt spray test; comparative example 3 the amount of N, N' -tetrakis (hydroxymethyl) ethylenediamine in the treatment agent was reduced to 0.2 g/L, the treated galvanized surface was bluish-purple and over 2.5% area rust on the surface after 120h of salt spray test; comparative example 4 the amount of N, N' -tetrakis (hydroxymethyl) ethylenediamine used in the treatment agent was increased to 5g/L, and the surface of the galvanized article after the treatment maintained the natural color of the galvanized layer, but the surface was rusted over 10% of the area after 120 hours of the salt spray test. It can be seen that when the treating agent is not added with N, N, N ', N' -tetra (hydroxymethyl) ethylenediamine or the addition amount is too low, the effect of keeping the natural color of the galvanized part cannot be achieved, and when the addition amount of the N, N, N ', N' -tetra (hydroxymethyl) ethylenediamine is too high, the passivation effect is seriously affected.
The above description is only for the preferred embodiment of the present invention, and is not intended to limit the scope of the present invention. That is, all equivalent changes and modifications made according to the content of the claims of the present invention should be within the technical scope of the present invention.
Claims (6)
1. A galvanized part surface treating agent is characterized by being prepared from the following raw materials: 15-20 g/L of titanyl sulfate, 20-30 g/L of sodium silicate, 1-5 g/L of phytic acid, 30-35 g/L of sodium nitrate, 5-10 g/L of ammonium bifluoride, 3-5 mL/L of sulfuric acid, 5-10 g/L of lanthanum chloride, 10-15 mL/L, N of hydrogen peroxide, 1-3 g/L of N, N ', N' -tetra (hydroxymethyl) ethylenediamine and the balance of water.
2. The galvanized member surface treatment agent according to claim 1, which is prepared from the following raw materials: 15g/L of titanyl sulfate, 20g/L of sodium silicate, 3g/L of phytic acid, 30g/L of sodium nitrate, 5g/L of ammonium bifluoride, 3mL/L of sulfuric acid, 5g/L of lanthanum chloride, 10mL/L, N of hydrogen peroxide, 2 g/L of N, N ', N' -tetra (hydroxymethyl) ethylenediamine and the balance of water.
3. A galvanized part surface treating agent is characterized by being prepared from the following raw materials: 20g/L of titanyl sulfate, 20g/L of sodium silicate, 5g/L of phytic acid, 30g/L of sodium nitrate, 10g/L of ammonium bifluoride, 3mL/L of sulfuric acid, 10g/L of lanthanum chloride, 10mL/L, N of hydrogen peroxide, 3g/L of N, N ', N' -tetra (hydroxymethyl) ethylenediamine and the balance of water.
4. A galvanized part surface treating agent is characterized by being prepared from the following raw materials: 15g/L of titanyl sulfate, 30g/L of sodium silicate, 1g/L of phytic acid, 35g/L of sodium nitrate, 5g/L of ammonium bifluoride, 5mL/L of sulfuric acid, 5g/L of lanthanum chloride, 15mL/L, N of hydrogen peroxide, 1g/L of N, N ', N' -tetra (hydroxymethyl) ethylenediamine and the balance of water.
5. The surface treatment agent for galvanized parts according to any one of claims 1 to 4, wherein the sulfuric acid is concentrated sulfuric acid with a mass fraction of 98%.
6. The method for preparing the galvanized member surface treatment agent according to any one of claims 1 to 4, wherein the raw materials are sequentially added to water in the order of titanyl sulfate, sodium silicate, phytic acid, sodium nitrate, ammonium bifluoride, sulfuric acid, lanthanum chloride, hydrogen peroxide, and N, N, N ', N' -tetrakis (hydroxymethyl) ethylenediamine, and are uniformly stirred and dissolved.
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Citations (4)
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|---|---|---|---|---|
| CN1858302A (en) * | 2006-06-09 | 2006-11-08 | 广东多正化工科技有限公司 | High anti-corrosion zinc coating trivalent chromium lue-white passivating agent and its preparing method |
| CN104087884A (en) * | 2014-07-15 | 2014-10-08 | 无锡伊佩克科技有限公司 | Metal galvanization and passivation method and use of chelating agent |
| CN105779983A (en) * | 2016-04-19 | 2016-07-20 | 昆明理工大学 | Chromium-free iridescent passivation liquid |
| CN109609944A (en) * | 2018-12-30 | 2019-04-12 | 王冬生 | A kind of aluminium alloy true qualities chromium-free passivating treatment agent and preparation method thereof |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1858302A (en) * | 2006-06-09 | 2006-11-08 | 广东多正化工科技有限公司 | High anti-corrosion zinc coating trivalent chromium lue-white passivating agent and its preparing method |
| CN104087884A (en) * | 2014-07-15 | 2014-10-08 | 无锡伊佩克科技有限公司 | Metal galvanization and passivation method and use of chelating agent |
| CN105779983A (en) * | 2016-04-19 | 2016-07-20 | 昆明理工大学 | Chromium-free iridescent passivation liquid |
| CN109609944A (en) * | 2018-12-30 | 2019-04-12 | 王冬生 | A kind of aluminium alloy true qualities chromium-free passivating treatment agent and preparation method thereof |
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