CN104451648A - Iron and steel normal temperature rapid blackening solution and preparation method thereof - Google Patents
Iron and steel normal temperature rapid blackening solution and preparation method thereof Download PDFInfo
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- CN104451648A CN104451648A CN201410829195.0A CN201410829195A CN104451648A CN 104451648 A CN104451648 A CN 104451648A CN 201410829195 A CN201410829195 A CN 201410829195A CN 104451648 A CN104451648 A CN 104451648A
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- iron
- normal temperature
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- black liquid
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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
- C23C22/50—Treatment of iron or alloys based thereon
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C2222/00—Aspects relating to chemical surface treatment of metallic material by reaction of the surface with a reactive medium
- C23C2222/10—Use of solutions containing trivalent chromium but free of hexavalent chromium
Abstract
The invention provides an iron and steel normal temperature rapid blackening solution. The blackening solution comprises the following components in the following contents: 3-12 g/L of copper sulfate pentahydrate, 1.5-3.5 g/L of chromium oxide, 5-15 g/L of ammonium chloride, 3-10 g/L of citric acid, 1-10 g/L of octaphenyl polyoxyethyiene, 0.2-0.5 g/L of ammonium citrate, 5-10 g/L of sodium thiosulfate, 0.73-0.76 g/L of sulfuric acid, 0.6-0.8 g/L of boric acid and the balance of water. The iron and steel normal temperature rapid blackening solution has the advantages of stable solution, short blackening time, proper color, convenient and simple used process, sufficient raw material, low cost and the like, and particularly, the adhesion and the corrosion resistance capacity of a blackening film layer are obviously improved. The blackening solution has the characteristics of no pollution, energy saving, no steel type selectivity and the like.
Description
Technical field
The present invention relates to field of metal surface treatment technology, in particular, relate to a kind of iron and steel normal temperature quick black liquid and preparation method thereof.
Background technology
Steel blackening liquid is widely used in iron and steel parts surface blackening decoration and the protective treatment of the industrial sectors such as mechanical component, standardized component, handicraft product, spring.Steel blackening liquid of the prior art mostly is alkalescence, and high temperature blackout is polluted greatly, it is high to consume energy, have the problems such as die selectivity.
Chinese patent CN1139706 discloses one and the invention discloses the nontoxic hair blackening liquid of a kind of iron and steel normal temperature, and it contains the CuSO of 3-8g/L
45H
2the CrO of O, 1.5-3.5g/L
3, the NH of 4-9g/L
4the Sunmorl N 60S of Cl, 3-8g/L, the polyoxyethylene glycol of 2-5ml/L, content is make hair blackening liquid pH value be the acid of 1.5-2.5.Have nontoxic, free from environmental pollution, the advantages such as labor condition is good, simple to operate, and work efficiency is high, and film forming properties is excellent.But the blackout rete uneven color that this patent is formed, poor, the ornamental difference of erosion resistance of blackout rete.
Summary of the invention
An object of the present invention is to overcome the deficiencies in the prior art, a kind of iron and steel normal temperature quick black liquid is provided, this iron and steel normal temperature quick black liquid have solution-stabilized, the blackout time is short, color and luster is suitable, operation is convenient and simple, starting material are sufficient, low cost and other advantages, sticking power, the resistance to corrosion of the rete that particularly turns black significantly improve.It has pollution-free, economize the energy, without features such as die selectivity.
Two of object of the present invention is the preparation method providing above-mentioned iron and steel normal temperature quick black liquid.
A kind of iron and steel normal temperature quick black liquid, in described solution, each feed composition and content thereof are:
Cupric sulfate pentahydrate dam 3-12 g/L, chromic oxide 1.5-3.5 g/L, ammonium chloride 5-15 g/L, citric acid 3-10 g/L, polyoxyethylene octylphenol ether 1-10 g/L, ammonium citrate 0.2-0.5g/L, Sulfothiorine 5-10 g/L, sulfuric acid 0.73-0.75 g/L, boric acid 0.6-0.8 g/L, surplus is water.
The wherein preferred 8.5-10 g/L of cupric sulfate pentahydrate;
The preferred 2-3 g/L of chromic oxide;
The preferred 9-15 g/L of ammonium chloride;
The preferred 5-8 g/L of citric acid;
The preferred 2-5 g/L of polyoxyethylene octylphenol ether;
The preferred 0.3-0.5g/L of ammonium citrate;
The preferred 5-8 g/L of Sulfothiorine;
The preparation method of iron and steel normal temperature quick black liquid of the present invention is as follows:
(1) get three/disome ponding and first add cupric sulfate pentahydrate, sulfuric acid, ammonium chloride, be stirred to whole dissolving;
(2) add chromic oxide, be stirred to whole dissolving, add boric acid, citric acid, ammonium citrate, Sulfothiorine, be stirred to whole dissolving;
(3) add polyoxyethylene octylphenol ether, be stirred to whole dissolving;
(4) add water to volume required, stir evenly, obtain iron and steel normal temperature quick black liquid of the present invention.
The cardinal principle of iron and steel normal temperature quick black liquid of the present invention is as follows:
Iron and steel parts after activation treatment immerses in hair blackening liquid, the iron of workpiece surface and cupric sulfate pentahydrate generation replacement(metathesis)reaction, copper is formed at workpiece surface, simultaneous oxidation chromium is strong oxidizer in acidic medium, with copper generation redox reaction, cupric oxide copper being oxidized to black is wrapped in the surface of workpiece, forms blackout rete.Sulfuric acid in hair blackening liquid, boric acid provide required hydrogen ion for redox reaction, and make hair blackening liquid pH value be stabilized between 1.5-2.5, make redox reaction velocity-stabilization, and good with replacement(metathesis)reaction synchronism, and the bonding force of blackout rete is strong.Polyoxyethylene octylphenol ether (OP-10) in hair blackening liquid is tensio-active agent, workpiece surface is soaked everywhere, abundant contact hair blackening liquid, and obtain even, fine and closely woven, bright blackout layer, citric acid, ammonium citrate are copper ion complexing agent, Sulfothiorine is the reductive agent of cupric ion, its effect is the speed regulating copper, iron replacement(metathesis)reaction, ammonium chloride is then the catalyzer of redox reaction, their acting in conjunction ensures that replacement(metathesis)reaction is synchronous with the oxidizing reaction of copper, to obtain the strong cupric oxide rete of bonding force.
The using method of iron and steel normal temperature quick black liquid of the present invention is as follows:
Through pre-treatment and the workpiece cleaned up can proceed to room temperature blackening process:
1, join tank liquor: be working fluid by above-mentioned formula, the pH value of working fluid remains 1.5-2.5.
2, turn black: workpiece to enter after room temperature blackening working fluid 1 minute, workpiece can be shaken up and down for several times, surface is made fully to contact hair blackening liquid, blackout time 2-5 minute, grasping the blackout time is the key obtaining high-quality black film, different materials, the different working fluid concentration blackout time is different, the foundation of judgement: have one deck homogeneous black film depending on workpiece surface.After blackout, stop 1-2 minute in atmosphere, then through washing, the raffinate on surface can be made full use of, reduce the consumption of hair blackening liquid, reduce costs.
3, tank liquor adjustment: hair blackening liquid in use, should be noted checking pH value, should be adjusted when pH value is more than 2.5, method for first solution being crossed elimination precipitation, then adds normal temperature blackening agent for iron and steel surface, makes pH value return to 1.5-2.5, can continue to use, after adjusting 2-3 time, will hair blackening liquid be changed.When tank liquor pH value is difficult to adjustment more than more than 3, can turn black the time until till can not using, generally the longest is 6-7 minute by proper extension, ability film forming, changes tank liquor after using for some time again.
4, " aftereffect " problem of hair blackening liquid, room temperature blackening part is after complete operation process, and the chemical reaction in top layer does not finally complete, under the effect of oxygen in atmosphere, this conversion process, can improve film strength and sticking power, and the homogeneity of blackness also increases, the blackening process time should be short, should not grow, as long as surface black uniformity can go out groove, make full use of after effect, the consumption of hair blackening liquid can be reduced like this and improve the quality of product, reducing costs.
Iron and steel normal temperature quick black liquid of the present invention have solution-stabilized, the blackout time is short, color and luster is suitable, operation is convenient and simple, starting material are sufficient, low cost and other advantages, sticking power, the resistance to corrosion of the rete that particularly turns black significantly improve.It has pollution-free, economize the energy, without features such as die selectivity.
Rear effect analysis is used to be listed as follows:
In the embodiment of the present invention, after blackening process, neutral salt spray corrosion test (NSS) method of workpiece is: with reference to ISO3768 standard, salt-mist corrosion tester put into by selected workpiece after blackening process, salt solution is containing 5%(wt) sodium-chlor, pH value 6.5 ~ 7.2, temperature (35 ± 2) DEG C, fall mist amount 1 ~ 2mL/ (hcm2), after 72 hours time, survey corrosion area, calculate corrosion area and account for the long-pending per-cent of workpiece surface.
After blackening process, the natural Rust Test condition of workpiece is: workpiece is arranged vertically on synthetic glass specimen holder, be placed in temperature (25 ± 2) DEG C, in the fixed temperature and humidity closed room of relative humidity (80 ± 5) %, every day observes once, the test number of days of first workpiece generation corrosion is deducted one day as the number of days that becomes rusty on not.
Black film sticking power grade: the cross cut test standard according to GB 9286-1998 paint and varnish paint film is tested.
Black film layer porosity: go bail for exist in brown bottle, massfraction is sodium-chlor 14%, the distilled water solution of the Tripotassium iron hexacyanide 3%, tensio-active agent perfluorooctanoic acid ammonium 0.1%, filter paper is cut into the scraps of paper that length and width is 10 centimetres, with plastic tweezer, the scraps of paper are immersed in above-mentioned solution, propose to drip clean unnecessary test solution, cover the black film surface (black film length and width is all greater than 10 centimetres) of workpiece, test paper is removed after 1 minute, observe workpiece film surface, have blue color spot point place to indicate aperture sections.Draw blue spot area percentage.
Embodiment
Below in conjunction with specific embodiment, further detailed description is done to the present invention.
Embodiment 1-12 sets forth the raw material composition of iron and steel normal temperature quick black liquid of the present invention, concrete listed by table 1, table 2, and wherein, the unit of each batching numerical value is g/L, and liquor capacity is 1L.
Table 1 embodiment 1-6 fills a prescription composition
Table 2 embodiment 7-12 fills a prescription composition
The preparation method of above embodiment is as follows:
(1) get three/disome ponding and first add cupric sulfate pentahydrate, sulfuric acid, ammonium chloride, be stirred to whole dissolving;
(2) add chromic oxide, be stirred to whole dissolving, add boric acid, citric acid, ammonium citrate, Sulfothiorine, be stirred to whole dissolving;
(3) add polyoxyethylene octylphenol ether, be stirred to whole dissolving;
(4) add water to volume required, stir evenly, obtain iron and steel normal temperature quick black liquid of the present invention.
Table 3 is comparative example formula, and the unit of each batching numerical value is g.
Table 3 comparative example formula
Note: the above polyoxyethylene glycol to be molecular weight be 400 polyethylene glycol reagents.
The preparation method of above comparative example is as follows:
Each component be dissolved in water respectively, remix, stirs, and is diluted with water to the solution of 1L, is namely worth the Chemical Colouring of Steel at Room Temperature liquid of comparative example.
The using method of above embodiment, comparative example is as follows:
1, join tank liquor: be working fluid by above-mentioned formula, the pH value of working fluid remains 2.
2, turn black: workpiece to enter after room temperature blackening working fluid 1 minute, workpiece can be shaken up and down for several times, make surface fully contact hair blackening liquid, the 4 minutes time of blackout.After blackout, stop 2 minutes in atmosphere, then through washing.
The result of use of above embodiment, comparative example is respectively in table 4, table 5, table 6.
The result of use of table 4 embodiment 1-6
The result of use of table 5 embodiment 7-12
The result of use of table 6 comparative example
Above content description ultimate principle of the present invention and principal character; the present invention is not restricted to the described embodiments; without departing from the spirit and scope of the present invention, the present invention also has various changes and modifications, and these changes and improvements all fall in the claimed scope of the invention.Application claims protection domain is defined by appending claims and equivalent thereof.
Claims (9)
1. an iron and steel normal temperature quick black liquid, is characterized in that each feed composition and content thereof are:
Cupric sulfate pentahydrate 3-12 g/L,
Chromic oxide 1.5-3.5 g/L,
Ammonium chloride 5-15 g/L,
Citric acid 3-10 g/L,
Polyoxyethylene octylphenol ether 1-10 g/L,
Ammonium citrate 0.2-0.5 g/L,
Sulfothiorine 5-10 g/L,
Sulfuric acid 0.73-0.75 g/L,
Boric acid 0.6-0.8 g/L,
Surplus is water.
2. iron and steel normal temperature quick black liquid as claimed in claim 1, is characterized in that described cupric sulfate pentahydrate content is 8.5-10 g/L.
3. iron and steel normal temperature quick black liquid as claimed in claim 1, is characterized in that described chromic oxide content is 2-3 g/L.
4. iron and steel normal temperature quick black liquid as claimed in claim 1, is characterized in that described ammonium chloride content is 9-15 g/L.
5. iron and steel normal temperature quick black liquid as claimed in claim 1, is characterized in that described citric acid content is 5-8 g/L.
6. iron and steel normal temperature quick black liquid as claimed in claim 1, is characterized in that described polyoxyethylene octylphenol ether content is 2-5 g/L.
7. iron and steel normal temperature quick black liquid as claimed in claim 1, is characterized in that described ammonium citrate content is 0.3-0.5g/L.
8. iron and steel normal temperature quick black liquid as claimed in claim 1, is characterized in that described sodium thiosulfate content is 5-8 g/L.
9. the preparation method of iron and steel normal temperature quick black liquid as claimed in claim 1 is as follows:
(1) get three/disome ponding and first add cupric sulfate pentahydrate, sulfuric acid, ammonium chloride, be stirred to whole dissolving;
(2) add chromic oxide, be stirred to whole dissolving, add boric acid, citric acid, ammonium citrate, Sulfothiorine, be stirred to whole dissolving;
(3) add polyoxyethylene octylphenol ether, be stirred to whole dissolving;
(4) add water to volume required, stir evenly.
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| CN201410829195.0A CN104451648B (en) | 2014-12-26 | 2014-12-26 | Steel normal temperature quick black liquid and preparation method thereof |
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| CN201410829195.0A CN104451648B (en) | 2014-12-26 | 2014-12-26 | Steel normal temperature quick black liquid and preparation method thereof |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105063718A (en) * | 2015-08-17 | 2015-11-18 | 深圳市依诺威电子有限公司 | Slowing agent applied to metal surface treatment |
| CN105420711A (en) * | 2015-11-25 | 2016-03-23 | 安徽红桥金属制造有限公司 | Anticorrosion treatment process of cast workpiece |
| CN105420727A (en) * | 2015-11-25 | 2016-03-23 | 安徽红桥金属制造有限公司 | Anticorrosion treatment process of zinc alloy die casting |
| CN110042380A (en) * | 2019-03-27 | 2019-07-23 | 祝亚琴 | Zinc blackening agent for surface |
| CN111826646A (en) * | 2020-07-27 | 2020-10-27 | 重庆盈锋不锈钢有限公司 | Stainless steel blackening agent and blackening treatment method |
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| CN1139706A (en) * | 1995-07-04 | 1997-01-08 | 吕进东 | Nontoxic blackening liquid for iron and steel surface at normal temp. |
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2014
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105063718A (en) * | 2015-08-17 | 2015-11-18 | 深圳市依诺威电子有限公司 | Slowing agent applied to metal surface treatment |
| CN105420711A (en) * | 2015-11-25 | 2016-03-23 | 安徽红桥金属制造有限公司 | Anticorrosion treatment process of cast workpiece |
| CN105420727A (en) * | 2015-11-25 | 2016-03-23 | 安徽红桥金属制造有限公司 | Anticorrosion treatment process of zinc alloy die casting |
| CN110042380A (en) * | 2019-03-27 | 2019-07-23 | 祝亚琴 | Zinc blackening agent for surface |
| CN111826646A (en) * | 2020-07-27 | 2020-10-27 | 重庆盈锋不锈钢有限公司 | Stainless steel blackening agent and blackening treatment method |
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| CN104451648B (en) | 2017-07-11 |
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