CN104451648B - Steel normal temperature quick black liquid and preparation method thereof - Google Patents
Steel normal temperature quick black liquid and preparation method thereof Download PDFInfo
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- CN104451648B CN104451648B CN201410829195.0A CN201410829195A CN104451648B CN 104451648 B CN104451648 B CN 104451648B CN 201410829195 A CN201410829195 A CN 201410829195A CN 104451648 B CN104451648 B CN 104451648B
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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 a kind of steel normal temperature quick black liquid, wherein each component and its content is：The g/L of cupric sulfate pentahydrate 3 12, the g/L of chromium oxide 1.5 3.5, the g/L of ammonium chloride 5 15, the g/L of citric acid 3 10, the g/L of OPEO 1 10, the g/L of ammonium citrate 0.2 0.5, the g/L of sodium thiosulfate 5 10, the g/L of sulfuric acid 0.73 0.75, the g/L of boric acid 0.6 0.8, surplus is water.The steel normal temperature quick black liquid has that solution-stabilized, the nigrescence time is short, color and luster suitable, using technique is convenient and simple, raw material are sufficient, low cost and other advantages, and particularly the adhesive force of nigrescence film layer, resistance to corrosion are significantly improved.It has it is pollution-free, save the energy, without die it is selective the features such as.
Description
Technical field
The present invention relates to field of metal surface treatment technology, in particular, it is related to a kind of steel normal temperature quick black liquid
And preparation method thereof.
Background technology
Steel blackening liquid is widely used in the iron and steel parts of the industrial departments such as machine components, standard component, handicraft product, spring
Surface blackening is decorated and protective treatment.Steel blackening liquid of the prior art is generally alkalescence, high temperature nigrescence pollution is big, power consumption is high,
There is the problems such as die is selective.
Chinese patent CN1139706 discloses one kind the invention discloses a kind of nontoxic hair blackening liquid of steel normal temperature, and it contains
3-8g/L CuSO4·5H2O, 1.5-3.5g/L CrO3, 4-9g/L NH4Cl, 3-8g/L sodium gluconate, 2-5ml/L
Polyethylene glycol, content is the acid for making hair blackening liquid pH value be 1.5-2.5.Free from environmental pollution with nontoxic, working condition is good, behaviour
Make simple, work efficiency is high, the advantages of filming performance is excellent.But the nigrescence film layer irregular colour of patent formation is even, nigrescence film layer
Corrosion resistance is poor, dicoration is poor.
The content of the invention
An object of the present invention is to overcome the deficiencies in the prior art there is provided a kind of steel normal temperature quick black liquid, should
Steel normal temperature quick black liquid has that solution-stabilized, the nigrescence time is short, color and luster suitable, using technique is convenient and simple, raw material fill
Foot, particularly low cost and other advantages, the adhesive force of nigrescence film layer, resistance to corrosion are significantly improved.It has pollution-free, province's energy
Source, without die it is selective the features such as.
The second object of the present invention is the preparation method for providing above-mentioned steel normal temperature quick black liquid.
Each raw material components and its content are in a kind of steel normal temperature quick black liquid, the solution：
Cupric sulfate pentahydrate dam 3-12 g/L, chromium oxide 1.5-3.5 g/L, ammonium chloride 5-15 g/L, citric acid 3-10
G/L, OPEO 1-10 g/L, ammonium citrate 0.2-0.5g/L, sodium thiosulfate 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 chromium 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 OPEO；
The preferred 0.3-0.5g/L of ammonium citrate；
The preferred 5-8 g/L of sodium thiosulfate；
The preparation method of steel normal temperature quick black liquid of the present invention is as follows：
(1) 2/3rds volume of water are taken first to add cupric sulfate pentahydrate, sulfuric acid, ammonium chloride, stirring to whole dissolvings；
(2) chromium oxide is added, stirring to whole dissolvings adds boric acid, citric acid, ammonium citrate, sodium thiosulfate, stirring
To whole dissolvings；
(3) OPEO, stirring to whole dissolvings are added；
(4) required volume is added water to, is stirred evenly, steel normal temperature quick black liquid of the invention is obtained.
The cardinal principle of steel normal temperature quick black liquid of the present invention is as follows:
In iron and steel parts immersion hair blackening liquid after activation process, displacement occurs for iron and the cupric sulfate pentahydrate of workpiece surface instead
Should, in workpiece surface formation copper, simultaneous oxidation chromium is strong oxidizer in acid medium, occurs redox reaction with copper, will
The cupric oxide that copper is oxidized to black is wrapped in the surface of workpiece, forms nigrescence film layer.Sulfuric acid, boric acid in hair blackening liquid are gone back for oxidation
Hydrogen ion needed for original reaction offer, and make hair blackening liquid pH value stable between 1.5-2.5, make redox reaction speed steady
Fixed and good with displacement reaction synchronism, the adhesion of nigrescence film layer is strong.OPEO in hair blackening liquid（OP-10）
For surfactant, workpiece surface is soaked everywhere, fully contact hair blackening liquid, and obtain uniform, fine and closely woven, bright nigrescence layer,
Citric acid, ammonium citrate are copper ion complexing agent, and sodium thiosulfate is the reducing agent of copper ion, and it is to adjust copper, iron to put that it, which is acted on,
The speed of reaction is changed, ammonium chloride is then the catalyst of redox reaction, and their collective effect is to ensure displacement reaction and copper
Oxidation reaction it is synchronous, to obtain the oxidation copper film layer of adhesion by force.
The application method of steel normal temperature quick black liquid of the present invention is as follows：
Room temperature blackening processing can be transferred to through pre-treatment and the workpiece that cleans up：
1st, with tank liquor：It is working solution by above-mentioned formula, the pH value of working solution remains 1.5-2.5.
2nd, black：Workpiece enters after room temperature blackening working solution 1 minute, can will be shaken above and below workpiece for several times, make surface abundant
Hair blackening liquid is contacted, is blacked time 2-5 minute, it is the key for obtaining high-quality black film to grasp the nigrescence time, different materials, no
The same working solution concentration nigrescence time is different, the foundation of judgement：There is one layer of homogeneous black film depending on workpiece surface.Black
Bi Hou, is stopped 1-2 minutes in atmosphere, then through washing, can make full use of the raffinate on surface, reduces the consumption of hair blackening liquid, reduction
Cost.
3rd, tank liquor is adjusted：Hair blackening liquid is in use, it should be noted that checks pH value, should be adjusted when pH value is more than 2.5,
Method precipitates for solution first is crossed into elimination, then adds normal temperature blackening agent for iron and steel surface, pH value is returned to 1.5-2.5, you can be continuing with,
Hair blackening liquid is changed after adjusting 2-3 times.When tank liquor pH value more than more than 3 be difficult adjustment, can proper extension black the time until
Untill can not using, typically up to 6-7 minutes, could film forming, using changing tank liquor again after a period of time.
4th, " aftereffect " problem of hair blackening liquid, room temperature blackening part is after operating process is completed, and the chemical reaction in top layer is not
Finally complete, in atmosphere in the presence of oxygen, this conversion process can improve film strength and adhesive force, the uniformity of blackness
Also increase, the blackening process time is preferably short, should not grow, as long as surface black uniformity can go out groove, make full use of aftereffect
Effect, can so reduce the consumption of hair blackening liquid and improve the quality of product, reduce cost.
Steel normal temperature quick black liquid of the present invention has that solution-stabilized, the nigrescence time is short, color and luster suitable, convenient using technique
Simply, raw material abundance, particularly low cost and other advantages, the adhesive force of nigrescence film layer, resistance to corrosion are significantly improved.It has
It is pollution-free, save the energy, without die it is selective the features such as.
Effect analysis after use is listed as follows：
In the embodiment of the present invention, the neutral salt spray corrosion test of workpiece after blackening process（NSS）Method is：Reference
Selected workpiece after ISO3768 standards, blackening process is put into salt-mist corrosion tester, and salt solution contains 5%（wt）Sodium chloride, pH value
6.5~7.2, temperature (35 ± 2) DEG C, 1~2mL/ of amount of fog (hcm2) surveys corrosion area after 72 hours time, calculate corrosion
Area accounts for the percentage of workpiece surface product.
The natural Rust Test condition of workpiece is after blackening process：Workpiece is arranged vertically on lucite specimen holder, is put
In in temperature (25 ± 2) DEG C, relative humidity (80 ± 5) % constant temperature and humidity closed room, observe once daily, by first work
The experiment number of days of part generation corrosion, which is subtracted, is not used as rust number of days for one day.
Black film adhesive force grade:Surveyed according to the cross cut test standard of GB 9286-1998 paint and varnish paint films
Examination.
Black film layer porosity：Go bail for exist in brown bottle, mass fraction be sodium chloride 14%, the potassium ferricyanide 3%, surface
The distilled water solution of activating agent perfluorooctanoic acid ammonium 0.1%, is cut into the scraps of paper that length and width is 10 centimetres by filter paper, uses plastic tweezer
The scraps of paper are immersed in above-mentioned solution, the net unnecessary test solution of drop is proposed, is covered in the black film surface of workpiece（Black film length and width is big
In 10 centimetres）, test paper is removed after 1 minute, workpiece film surface is observed, having indicate aperture sections at blue spot.Draw indigo plant
Color spot point area percentage.
Embodiment
Further detailed description is done to the present invention below in conjunction with specific embodiment.
Embodiment 1-12 sets forth the raw material composition of steel normal temperature quick black liquid of the present invention, specific such as table 1, table 2
It is listed, wherein, the unit of each dispensing numerical value is g/L, and liquor capacity is 1L.
The embodiment 1-6 of table 1 formula compositions
The embodiment 7-12 of table 2 formula compositions
The preparation method of above example is as follows：
(1) 2/3rds volume of water are taken first to add cupric sulfate pentahydrate, sulfuric acid, ammonium chloride, stirring to whole dissolvings；
(2) chromium oxide is added, stirring to whole dissolvings adds boric acid, citric acid, ammonium citrate, sodium thiosulfate, stirring
To whole dissolvings；
(3) OPEO, stirring to whole dissolvings are added；
(4) required volume is added water to, is stirred evenly, steel normal temperature quick black liquid of the invention is obtained.
Table 3 is comparative example formula, and the unit of each dispensing numerical value is g.
The comparative example formula of table 3
Note：The above polyethylene glycol is the polyethylene glycol reagents that molecular weight is 400.
The preparation method of above comparative example is as follows：
Each component is dissolved in water respectively, remixed, is stirred, 1L solution is diluted with water to, that is, is worth comparative example
Chemical Colouring of Steel at Room Temperature liquid.
Above example, the application method of comparative example are as follows：
1st, with tank liquor：It is working solution by above-mentioned formula, the pH value of working solution remains 2.
2nd, black：Workpiece enters after room temperature blackening working solution 1 minute, can will be shaken above and below workpiece for several times, make surface abundant
Hair blackening liquid is contacted, is blacked 4 minutes time.After nigrescence is finished, stop 2 minutes in atmosphere, then through washing.
Above example, the using effect of comparative example are shown in Table 4, table 5, table 6 respectively.
The embodiment 1-6 of table 4 using effect
The embodiment 7-12 of table 5 using effect
The using effect of the comparative example of table 6
Above content describes the general principle and principal character of the present invention, and the present invention is not limited to the above embodiments,
Without departing from the spirit and scope of the present invention, various changes and modifications of the present invention are possible, and these changes and improvements are all
Fall into scope of the claimed invention.The claimed scope of the invention is by appending claims and its equivalent circle
It is fixed.
Claims (2)
1. a kind of steel normal temperature quick black liquid, it is characterised in that each raw material components and its content are：
Cupric sulfate pentahydrate 8g/L,
Chromium oxide 1.5g/L,
Ammonium chloride 10g/L,
Citric acid 8g/L,
OPEO 5g/L,
Ammonium citrate 0.5g/L,
Sodium thiosulfate 10g/L,
Sulfuric acid 0.73g/L,
Boric acid 0.6g/L,
Surplus is water.
2. the preparation method of steel normal temperature quick black liquid as claimed in claim 1 is as follows：
(1) 2/3rds volume of water are taken first to add cupric sulfate pentahydrate, sulfuric acid, ammonium chloride, stirring to whole dissolvings；
(2) chromium oxide is added, stirring to whole dissolvings adds boric acid, citric acid, ammonium citrate, sodium thiosulfate, stirred to complete
Dissolve in portion；
(3) OPEO, stirring to whole dissolvings are added；
(4) required volume is added water to, is stirred evenly.
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| Application Number | Priority Date | Filing Date | Title |
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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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| CN104451648B true CN104451648B (en) | 2017-07-11 |
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Families Citing this family (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 |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1139706A (en) * | 1995-07-04 | 1997-01-08 | 吕进东 | Nontoxic blackening liquid for iron and steel surface at normal temp. |
| CN1453394A (en) * | 2002-04-26 | 2003-11-05 | 柳州市建筑机械总厂 | Iron and steel surface sensitizing and blackening agent and relevant blackening process |
| WO2003091480A1 (en) * | 2002-04-26 | 2003-11-06 | Liuzhou Construction Machinery Factory General | Corrosion resistant prestressed steel bar and its preparing process |
| CN102011117A (en) * | 2010-12-02 | 2011-04-13 | 合肥华清金属表面处理有限责任公司 | Environmental-friendly room-temperature steel blackening agent and preparation method thereof |
| CN103668149A (en) * | 2013-12-19 | 2014-03-26 | 湖南金裕化工有限公司 | Normal-temperature rapid phosphating solution and preparing method thereof |
-
2014
- 2014-12-26 CN CN201410829195.0A patent/CN104451648B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1139706A (en) * | 1995-07-04 | 1997-01-08 | 吕进东 | Nontoxic blackening liquid for iron and steel surface at normal temp. |
| CN1453394A (en) * | 2002-04-26 | 2003-11-05 | 柳州市建筑机械总厂 | Iron and steel surface sensitizing and blackening agent and relevant blackening process |
| WO2003091480A1 (en) * | 2002-04-26 | 2003-11-06 | Liuzhou Construction Machinery Factory General | Corrosion resistant prestressed steel bar and its preparing process |
| CN102011117A (en) * | 2010-12-02 | 2011-04-13 | 合肥华清金属表面处理有限责任公司 | Environmental-friendly room-temperature steel blackening agent and preparation method thereof |
| CN103668149A (en) * | 2013-12-19 | 2014-03-26 | 湖南金裕化工有限公司 | Normal-temperature rapid phosphating solution and preparing method thereof |
Non-Patent Citations (1)
| Title |
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| Cu-S钢铁常温无毒化学发黑液;周书天等;《电镀与涂饰》;19970331;第16卷(第1期);实验过程及结果部分的3.2节 * |
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