CN102392240B - Zinc alloy blackening liquid - Google Patents
Zinc alloy blackening liquid Download PDFInfo
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- CN102392240B CN102392240B CN 201110367157 CN201110367157A CN102392240B CN 102392240 B CN102392240 B CN 102392240B CN 201110367157 CN201110367157 CN 201110367157 CN 201110367157 A CN201110367157 A CN 201110367157A CN 102392240 B CN102392240 B CN 102392240B
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- hair blackening
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Abstract
The invention relates to a zinc alloy blackening liquid. The zinc alloy blackening liquid comprises, by mass, 0.1-15% of an acid, 0.01-5% of an acid salt, 0.1-10% of hydrogen peroxide, 0.01-2% of a hydrogen peroxide stabilizing agent, 0.1-10% of copper sulfate, and the balance water. A preparation method of the zinc alloy blackening liquid comprises the following steps: 1, mixing 60-80% of above formula amount of water with 0.1-15% of the acid, 0.01-5% of the acid salt, 0.1-10% of hydrogen peroxide, 0.01-2% of the hydrogen peroxide stabilizing agent and 0.1-10% of copper sulfate in order; 2, adding a surplus formula amount of water; and 3, stirring for more than 5min to obtain the zinc alloy blackening liquid. The zinc alloy blackening liquid is used according to a usage method which comprises the following technological processes: removing oil from zinc alloy, washing with water, activating, washing with water, blackening, washing with water, enclosing, washing with water, and drying. According to the invention, the zinc alloy can reach a same film blacky effect of galvanized parts without galvanizing; and the blackening liquid of the invention has the advantages of nontixicity, no pollution, easy wastewater treatment, and simple usage operation.
Description
Technical field
The present invention relates to field of metal surface treatment, concrete, the present invention relates to a kind of zinc alloy hair blackening liquid, its preparation method and using method thereof.
Background technology
Zinc and zinc alloy are widely used in fields such as steamer, family property, light fixture, automobile, for the product appearance of beautifying the zinc alloy device and the requirement of satisfying some particular device surface light absorptive, zinc alloy surface need be processed into black.
In at present traditional industrial production, zinc and zinc alloy surface turn black in the employed prescription, the overwhelming majority all contains toxic ingredients such as trivalent chromium, sexavalent chrome, selenium salt, rare metal salts or prussiate, and serious threat operator's health causes severe contamination to environment.
CN 101283117A provides with acid, neutral, alkaline zinc-plated bath kind and has or not the nickel eutectoid to have nothing to do, be used to form the treatment soln of the uniform and stable black of black, glossy appearance and erosion resistance 3 valency chromaking conversion films and the method for formation black 3 valency chromaking conversion films.This invention is provided for forming the treatment soln that black does not contain the chemical conversion film of 6 valency chromium at zinc or zinc alloy, and it contains: 3 valency chromium ions; Can form the sequestrant of water soluble complex with 3 valency chromium; Be selected from the metal ion more than a kind in cobalt ion, nickel ion and the iron ion; And as formic acid or its salt of hydrogen ion concentration buffer reagent.
CN 102149848 A provide having the metal part surface of zinc or zinc alloy surface, the chemical transformation processing aqueous solution of giving the Chrome-free surface treatment method of good blackness and rustless property and can using in this treatment process.This aqueous solution does not contain 3 valencys and 6 valency chromium ions, in 1 liter of this aqueous solution, contains the phosphate anion of 5～20g, the divalent iron ion of 0.1～3g, and the divalent mn ion of 1～10g, the nitrate ion of 1～3g, pH are 1～3.Metal parts is immersed in this aqueous solution, forms Fe
3O
4Black coating film, the chemical transformation that then forms cerium oxide is filmed, and then forms siliceous filming.
For reaching state sewage emission standard, must the increase input processing of sewage effluent of surface treatment enterprise has increased production cost greatly; Most of prescription can produce dust or sediment in the blackout process, increased the intractability of cleaning and hair blackening liquid.
Summary of the invention
At the deficiencies in the prior art, one of purpose of the present invention is to provide a kind of zinc alloy hair blackening liquid.
Described zinc alloy hair blackening liquid is applicable to the protected decoration processing of zinc alloy, does not contain poisonous selenium salt and rare metal salts in the prescription, reaches the purpose of environmental protection, and the processing work outward appearance is consistent with traditional technology, and the working fluid cost is low, cuts down finished cost greatly.
Described zinc alloy hair blackening liquid, its composition comprises by mass percentage:
Described hydrogen peroxide can make the black rete combination more firmly of acquisition, difficult drop-off.
Preferably, described acid can be for organic acid or/and mineral acid, further preferred described acid is a kind or at least 2 kinds combination in hydrochloric acid, sulfuric acid, oxalic acid, acetic acid, carbonic acid, citric acid, phosphoric acid, the nitric acid, described combination typical case but the example of non-limit have: the combination of hydrochloric acid, oxalic acid, the combination of sulfuric acid, oxalic acid, acetic acid, the combination of acetic acid, carbonic acid, citric acid, phosphoric acid, the combination of carbonic acid, nitric acid etc. are preferably hydrochloric acid especially or/and citric acid.
As preferred version, described zinc alloy hair blackening liquid, its composition comprises by mass percentage:
Further preferred, described zinc alloy hair blackening liquid, its composition comprises by mass percentage:
Preferred especially, described zinc alloy hair blackening liquid, its composition comprises by mass percentage:
Preferably, described hydrochlorate is hydrosulfate or/and hydrosulphite, and more preferably hydrosulfate is preferably sodium pyrosulfate especially.
Preferably, described hydrogen peroxide stabilizer is water glass, ethylene dinitrilotetra-acetic acid sodium salt (EDTA), sodium stannate, trisodium phosphate, oxine, organophosphite, 1 kind or at least 2 kinds combination among the efficient hydrogen peroxide stabilizer Hansi OS that Hansi Chemical Article Co., Ltd., Changzhou produces, described combination typical case but the example of non-limit have: water glass, the combination of ethylene dinitrilotetra-acetic acid sodium salt (EDTA), sodium stannate, trisodium phosphate, the combination of oxine, organophosphite, the combination of the efficient hydrogen peroxide stabilizer Hansi OS that Hansi Chemical Article Co., Ltd., Changzhou produces etc., more preferably water glass is or/and the efficient hydrogen peroxide stabilizer Hansi OS that Hansi Chemical Article Co., Ltd., Changzhou produces is preferably the efficient hydrogen peroxide stabilizer Hansi OS that Hansi Chemical Article Co., Ltd., Changzhou produces especially.
Zinc alloy hair blackening liquid of the present invention both can use separately, also can be used with other component.
The person of ordinary skill in the field can add other compositions according to the specialized technical knowledge of its grasp in zinc alloy hair blackening liquid of the present invention, for example inhibiter etc.
One of purpose of the present invention also is to provide a kind of preparation method of described zinc alloy hair blackening liquid.
The preparation method of described zinc alloy hair blackening liquid is: with the water of formula ratio 50%～90%, and acid, hydrochlorate, hydrogen peroxide, hydrogen peroxide stabilizer, the copper sulfate of formula ratio mix successively, the water that adds the formula ratio surplus at last stirred more than 5 minutes, namely got the zinc alloy hair blackening liquid.
Preferably, the preparation method of described zinc alloy hair blackening liquid is: with the water of formula ratio 50%～90%, and hydrochloric acid, hydrochlorate, citric acid, hydrogen peroxide, hydrogen peroxide stabilizer, the copper sulfate of formula ratio mix successively, the water that adds the formula ratio surplus at last, stir more than 5 minutes, namely get the zinc alloy hair blackening liquid.
Preferably, twice adding of described moisture, the water yield that adds is 60%～80% of formula ratio for the first time, that is, if contain 70g water in the described zinc alloy hair blackening liquid that finally makes, when then preparing, add for the first time 70g * 60%～70g * 80%, namely 42～56g water is further preferred, the water yield that adds is 65%～75% of formula ratio for the first time, and the preferred especially water yield that adds for the first time is 70% of formula ratio.
Preferably, described churning time is more than 10 minutes, for example 11 minutes, 12 minutes, 15 minutes, 30 minutes, 2 hours, 12 hours etc., is preferably especially and stirs 10 minutes.
Preferably, liquid stirrers is adopted in described stirring.
One of purpose of the present invention also is to provide a kind of using method of described zinc alloy hair blackening liquid.
The using method of described zinc alloy hair blackening liquid comprises following technical process: zinc alloy → oil removing → washing → activation → washing → blackout → washing → sealing → washing → oven dry.
Preferably, conventional activation hydrochlorate is adopted in described activation, can be by commercially available or prepared according to the expertise/new technology of its grasp by one of ordinary skill in the art; Described activation hydrochlorate consumption is 10～200g/L, is preferably 30～150g/L, is preferably 50～100g/L especially.
The preferred water that adopts of described activation hydrochlorate dilution dilutes.
Preferably, described zinc alloy hair blackening liquid consumption is 10～100mL/L, being about to the hair blackening liquid dilution uses, described consumption is dilution back concentration, described zinc alloy hair blackening liquid working concentration is with the value after the dilution of zinc alloy hair blackening liquid, for example adds 990mL water in the 10mL zinc alloy hair blackening liquid, and then the concentration of zinc alloy hair blackening liquid is 10mL/L, more preferably 20～70mL/L is preferably 25-50ml/L especially.
Preferably, it is water or/and the liquid that dissolves each other with water that solvent is adopted in the dilution of described zinc alloy hair blackening liquid, and for example alcohols is preferably water especially.
Preferably, described zinc alloy hair blackening liquid use temperature is 15～60 ℃, more preferably 20～50 ℃, is preferably 20～40 ℃ especially.
Preferably, the described blackout treatment time is 0.1～8 minute, more preferably 0.3～5 minute, is preferably 0.5～3 minute especially.
Preferably, the conventional confining liquid of described sealing can be by commercially available or prepared according to the expertise/new technology of its grasp by one of ordinary skill in the art; Described confining liquid is that stoste is used, and does not namely need to concentrate or dilution; Be preferably 0.1～5 minute described off-period, more preferably 0.3～2 minute, is preferably 0.5～1 minute especially.
Preferably, described bake out temperature is no more than 100 ℃, further preferably is no more than 90 ℃, especially preferably is no more than 80 ℃.
Preferably, it is black that described hair blackening liquid is applicable to that zinc alloy directly dyes, and need not electro-galvanizing processing.
Beneficial effect of the present invention is as follows:
(1) zinc alloy need not the zinc-plated pitch-black effect of the same rete of galvanized workpiece that reaches;
(2) described hair blackening liquid is nontoxic, pollution-free, and waste water is easily handled;
(3) use is simple to operate.
Embodiment
For ease of understanding the present invention, it is as follows that the present invention enumerates embodiment.Those skilled in the art should understand that described embodiment helps to understand the present invention, should not be considered as concrete restriction of the present invention.
Embodiment 1
47.9g water, 0.05g sulfuric acid, 0.01g sodium pyrosulfate, 10g oxalic acid, 0.1g hydrogen peroxide, 0.01g water glass, 10g copper sulfate are joined liquid stirrers successively mix, add 31.9g water then and stirred 5 minutes, make the zinc alloy hair blackening liquid.
With pending zinc alloy oil removing, washing, the DC-A type that adopts the Guangzhou Dazhi Chemical Technology Co., Ltd to produce activates the activated in water solution of hydrochlorate 10g/L, and washing is the solution of 10mL/L with the hair blackening liquid dilute with water, 15 ℃ of processing 8 minutes of turning black down, washing then, the confining liquid sealing treatment that employing Jia, Shenzhen City virtue sufacing company limited produces 0.1 minute, washing, 80 ℃ of oven dry, make the black zinc alloy of good looking appearance.
Embodiment 2
Efficient hydrogen peroxide stabilizer Hansi OS, 0.1g copper sulfate that 41.42g water, 5g hydrochloric acid, 0.01g sodium bisulfite, 0.05g citric acid, 10g hydrogen peroxide, 2g Hansi Chemical Article Co., Ltd., Changzhou are produced join the liquid stirrers mixing successively, add 41.42g water then and stirred 10 minutes, make the zinc alloy hair blackening liquid.
With pending zinc alloy oil removing, washing, the KQ-13 type that adopts Guangzhou Kechuang sufacing company limited to produce activates the activated in water solution of hydrochlorate 200g/L, and washing is the solution of 100mL/L with the hair blackening liquid dilute with water, 60 ℃ of processing 0.1 minute of turning black down, washing then, the CX800 confining liquid sealing treatment that employing Changxian Sci. ﹠ Tech. Industrial Co., Ltd., Shenzhen City produces 5 minutes, washing, 100 ℃ of oven dry, make the black zinc alloy of good looking appearance.
Embodiment 3
Efficient hydrogen peroxide stabilizer Hansi OS, 0.5g copper sulfate that 76.2g water, 1g hydrochloric acid, 0.05g Potassium hydrogen sulfite, 5g citric acid, 8g hydrogen peroxide, 0.8g Hansi Chemical Article Co., Ltd., Changzhou are produced join the liquid stirrers mixing successively, add 8.45g water then and stirred 11 minutes, make the zinc alloy hair blackening liquid.
With pending zinc alloy oil removing, washing, the KQ-13 type that adopts Guangzhou Kechuang sufacing company limited to produce activates the activated in water solution of hydrochlorate 50g/L, and washing is the solution of 50mL/L with the hair blackening liquid alcohol dilution, 30 ℃ of processing 5 minutes of turning black down, washing then, the CX800 confining liquid sealing treatment that employing Changxian Sci. ﹠ Tech. Industrial Co., Ltd., Shenzhen City produces 1 minute, washing, 90 ℃ of oven dry, make the black zinc alloy of good looking appearance.
Applicant's statement, the present invention illustrates detailed process equipment of the present invention and technical process by above-described embodiment, but the present invention is not limited to above-mentioned detailed process equipment and technical process, does not mean that namely the present invention must rely on above-mentioned detailed process equipment and technical process could be implemented.The person of ordinary skill in the field should understand, any improvement in the present invention to the interpolation of the equivalence replacement of each raw material of product of the present invention and ancillary component, the selection of concrete mode etc., all drops within protection scope of the present invention and the open scope.
Claims (41)
1. zinc alloy hair blackening liquid, its composition comprises by mass percentage:
Described acid is a kind or at least 2 kinds combination in hydrochloric acid, sulfuric acid, oxalic acid, acetic acid, carbonic acid, citric acid, phosphoric acid, the nitric acid;
Described hydrochlorate is that hydrosulfate is or/and hydrosulphite;
Described hydrogen peroxide stabilizer is a kind or at least 2 kinds combination among the efficient hydrogen peroxide stabilizer Hansi OS that produces of water glass, ethylene dinitrilotetra-acetic acid sodium salt, sodium stannate, trisodium phosphate, oxine, organophosphite, Hansi Chemical Article Co., Ltd., Changzhou.
2. zinc alloy hair blackening liquid as claimed in claim 1 is characterized in that, described acid is that hydrochloric acid is or/and citric acid.
3. zinc alloy hair blackening liquid as claimed in claim 1 is characterized in that, described zinc alloy hair blackening liquid, and its composition comprises by mass percentage:
Described hydrochlorate is that hydrosulfate is or/and hydrosulphite;
Described hydrogen peroxide stabilizer is a kind or at least 2 kinds combination among the efficient hydrogen peroxide stabilizer Hansi OS that produces of water glass, ethylene dinitrilotetra-acetic acid sodium salt, sodium stannate, trisodium phosphate, oxine, organophosphite, Hansi Chemical Article Co., Ltd., Changzhou.
4. zinc alloy hair blackening liquid as claimed in claim 1 is characterized in that, described zinc alloy hair blackening liquid, and its composition comprises by mass percentage:
Described hydrochlorate is that hydrosulfate is or/and hydrosulphite;
Described hydrogen peroxide stabilizer is a kind or at least 2 kinds combination among the efficient hydrogen peroxide stabilizer Hansi OS that produces of water glass, ethylene dinitrilotetra-acetic acid sodium salt, sodium stannate, trisodium phosphate, oxine, organophosphite, Hansi Chemical Article Co., Ltd., Changzhou.
5. zinc alloy hair blackening liquid as claimed in claim 1 is characterized in that, described zinc alloy hair blackening liquid, and its composition comprises by mass percentage:
Described hydrochlorate is that hydrosulfate is or/and hydrosulphite;
Described hydrogen peroxide stabilizer is a kind or at least 2 kinds combination among the efficient hydrogen peroxide stabilizer Hansi OS that produces of water glass, ethylene dinitrilotetra-acetic acid sodium salt, sodium stannate, trisodium phosphate, oxine, organophosphite, Hansi Chemical Article Co., Ltd., Changzhou.
6. as the described zinc alloy hair blackening liquid of one of claim 1-5, it is characterized in that described hydrogen peroxide stabilizer is that water glass is or/and the efficient hydrogen peroxide stabilizer Hansi OS that Hansi Chemical Article Co., Ltd., Changzhou produces.
7. zinc alloy hair blackening liquid as claimed in claim 6 is characterized in that, described hydrogen peroxide stabilizer is the efficient hydrogen peroxide stabilizer Hansi OS that Hansi Chemical Article Co., Ltd., Changzhou produces.
8. as the described zinc alloy hair blackening liquid of one of claim 1-5, it is characterized in that described hydrochlorate is hydrosulfate.
9. zinc alloy hair blackening liquid as claimed in claim 8 is characterized in that, described hydrochlorate is sodium pyrosulfate.
10. preparation method as each described zinc alloy hair blackening liquid of claim 1-9, it is characterized in that, described method is: with the water of formula ratio 50%～90%, and acid, hydrochlorate, hydrogen peroxide, hydrogen peroxide stabilizer, the copper sulfate of formula ratio mix successively, the water that adds the formula ratio surplus at last, stir more than 5 minutes, namely get the zinc alloy hair blackening liquid.
11. method as claimed in claim 10, it is characterized in that, the preparation method of described zinc alloy hair blackening liquid is: with the water of formula ratio 50%～90%, and hydrochloric acid, hydrochlorate, citric acid, hydrogen peroxide, hydrogen peroxide stabilizer, the copper sulfate of formula ratio mix successively, the water that adds the formula ratio surplus at last, stir more than 5 minutes, namely get the zinc alloy hair blackening liquid.
12. as claim 10 or 11 described preparation methods, it is characterized in that, twice adding of described moisture, the water yield that adds is 60%～80% of formula ratio for the first time.
13. preparation method as claimed in claim 12 is characterized in that, the water yield that adds is 65%～75% of formula ratio for the first time.
14. preparation method as claimed in claim 13 is characterized in that, the water yield that adds is 70% of formula ratio for the first time.
15., it is characterized in that described churning time is more than 10 minutes as claim 10 or 11 described preparation methods.
16. preparation method as claimed in claim 15 is characterized in that, stirs 10 minutes.
17., it is characterized in that liquid stirrers is adopted in described stirring as claim 10 or 11 described preparation methods.
18. using method as each described zinc alloy hair blackening liquid of claim 1-9, it is characterized in that the using method of described zinc alloy hair blackening liquid comprises following technical process: zinc alloy → oil removing → washing → activation → washing → blackout → washing → sealing → washing → oven dry.
19. method as claimed in claim 18 is characterized in that, conventional activation hydrochlorate is adopted in described activation, and described activation hydrochlorate consumption is 10～200g/L.
20. method as claimed in claim 19 is characterized in that, described activation hydrochlorate consumption is 30～150g/L.
21. method as claimed in claim 20 is characterized in that, described activation hydrochlorate consumption is 50～100g/L.
22. method as claimed in claim 19 is characterized in that, the water dilution is adopted in described activation hydrochlorate dilution.
23. method as claimed in claim 18 is characterized in that, described hair blackening liquid consumption is 10～100mL/L, is about to the hair blackening liquid dilution and uses, and described consumption is dilution back concentration.
24. method as claimed in claim 23 is characterized in that, described hair blackening liquid consumption is 20～70mL/L.
25. method as claimed in claim 24 is characterized in that, described hair blackening liquid consumption is 25-50ml/L.
26. method as claimed in claim 23 is characterized in that, it is water or/and the liquid that dissolves each other with water that solvent is adopted in the dilution of described hair blackening liquid.
27. method as claimed in claim 26 is characterized in that, described solvent is alcohols.
28. method as claimed in claim 26 is characterized in that, described solvent is water.
29. method as claimed in claim 18 is characterized in that, described hair blackening liquid use temperature is 15～60 ℃.
30. method as claimed in claim 29 is characterized in that, described hair blackening liquid use temperature is 20～50 ℃.
31. method as claimed in claim 30 is characterized in that, described hair blackening liquid use temperature is 20～40 ℃.
32. method as claimed in claim 18 is characterized in that, the described blackout treatment time is 0.1～8 minute.
33. method as claimed in claim 32 is characterized in that, the described blackout treatment time is 0.3～5 minute.
34. method as claimed in claim 33 is characterized in that, the described blackout treatment time is 0.5～3 minute.
35. method as claimed in claim 18 is characterized in that, the conventional confining liquid of described sealing, described confining liquid are that stoste is used, and be 0.1～5 minute described off-period.
36. method as claimed in claim 35 is characterized in that, be 0.3～2 minute described off-period.
37. method as claimed in claim 36 is characterized in that, be 0.5～1 minute described off-period.
38. method as claimed in claim 18 is characterized in that, described bake out temperature is no more than 100 ℃.
39. method as claimed in claim 38 is characterized in that, described bake out temperature is no more than 90 ℃.
40. method as claimed in claim 39 is characterized in that, described bake out temperature is no more than 80 ℃.
41. method as claimed in claim 18 is characterized in that, it is black that described hair blackening liquid is applicable to that zinc alloy directly dyes, and need not electro-galvanizing processing.
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| CN 201110367157 CN102392240B (en) | 2011-11-18 | 2011-11-18 | Zinc alloy blackening liquid |
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| CN103849868A (en) * | 2014-02-14 | 2014-06-11 | 浙江工业大学 | Blackening liquid for chromium-free titanium-zinc panel surface and using method of blackening liquid |
| CN104789956A (en) * | 2015-04-15 | 2015-07-22 | 吉林莱德化学科技有限公司 | Black trivalent chromium passivation agent with high corrosion resistance |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| EP1712659A1 (en) * | 2005-04-11 | 2006-10-18 | Elisha Holding LLC | Corrosion resistant article and method of production thereof |
| CN101580935A (en) * | 2009-06-24 | 2009-11-18 | 昆明理工大学 | Clean galvanized part silicate colorful passivating process |
| CN101876071A (en) * | 2009-11-24 | 2010-11-03 | 昆明理工大学 | Environmentally-friendly black chrome-silver-free zinc-plating passivation solution and preparation method thereof |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| EP1712659A1 (en) * | 2005-04-11 | 2006-10-18 | Elisha Holding LLC | Corrosion resistant article and method of production thereof |
| CN101580935A (en) * | 2009-06-24 | 2009-11-18 | 昆明理工大学 | Clean galvanized part silicate colorful passivating process |
| CN101876071A (en) * | 2009-11-24 | 2010-11-03 | 昆明理工大学 | Environmentally-friendly black chrome-silver-free zinc-plating passivation solution and preparation method thereof |
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