CN106544665A - Nigrescence minute surface adds lustre to anticorrodent and preparation method thereof - Google Patents
Nigrescence minute surface adds lustre to anticorrodent and preparation method thereof Download PDFInfo
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- CN106544665A CN106544665A CN201611058527.5A CN201611058527A CN106544665A CN 106544665 A CN106544665 A CN 106544665A CN 201611058527 A CN201611058527 A CN 201611058527A CN 106544665 A CN106544665 A CN 106544665A
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- Prior art keywords
- parts
- nigrescence
- anticorrodent
- minute surface
- adds lustre
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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
Abstract
A kind of nigrescence minute surface adds lustre to anticorrodent, in terms of parts by weight, is made up of following raw material:15 25 parts of copper sulfate, 30 50 parts of metastannic acid, 5 15 parts of sodium thiosulfate, 15 25 parts of stannic disulfide, 15 25 parts of sodium stannate, 5 15 parts of nickel sulfate, 5 15 parts of potassium citrate, 300 400 parts of water.The nigrescence minute surface adds lustre to anticorrodent, after blackening process, it is not necessary to soak dewatering rust preventive oil, can preserve not corrosion in 6 months in natural environment.
Description
Technical field
The invention belongs to field of metal surface treatment technology, and in particular to a kind of nigrescence minute surface adds lustre to anticorrodent and its preparation
Method.
Background technology
Turn blue and process the iron and steel zero for being widely used in the industrial departments such as machine components, standard component, handicraft product, spring
On part.This process of surface treatment, can form appearance decoration very attractive in appearance on steel and iron parts surface, while iron and steel can also be made
Part has very strong corrosion resistance, therefore application firmly gets liking for client than wide.
The alkaline nigrescence minute surface anticorrodent that adds lustre to has high temperature blacking that pollution is big, power consumption is high, selects, it is necessary to
Exploitation one kind need not consume the energy, use, without poisonous and harmful substances such as Ya Xiao Suan Na ﹑ sodium nitrite under room temperature, it is adaptable to
Various types of steel.
Chinese patent CN 201010615813.3 discloses a kind of metal zinc coating blackening agent and preparation method thereof.This
Bright metal zinc coating blackening agent is made up of the raw material of following composition by weight:20-25 part ammonium molybdates, 0.5-0.7 part copper sulfate, 2-
3 parts of nickel sulfate, 1-3 part sodium sulfite, 2.5-3.5 part sodium thiosulfate, 3.5-4.5 part aluminum chloride, 3-4 part zinc chloride, 7-8 parts
Potassium chloride, 0.3-0.5 part chelating agent, appropriate pH value regulator, water 40-60 parts;Its pH value is between 1.0-1.5.The present invention sends out
Black dose can form compactness height, the nigrescence film layer that adhesive force is good, corrosion resistance is strong in Several Thiourea Derivatives on Zinc Plate Surface, and blackening is simple, nontoxic
Environmental protection.But the patent has the disadvantage that:1st, the patent of invention is just for zine plated layer on metal body, that is to say, that can only be in zinc layers
Form nigrescence film layer.2nd, containing heavy metal ion such as molybdenum, zinc in the patent, the pollution to environment should not be underestimated.3rd, the invention shape
Into nigrescence film layer without mirror effect, affect attractive in appearance.4th, after blackening process, need using dewatering rust preventive oil to strengthen anticorrosion energy
Power.
Chinese patent 201410051491.2 discloses a kind of titanium zine plate surface chromium-free blackening process liquid and using method, should
The raw material of blackening process liquid includes main salt, auxiliary element, chelating agent, pH adjusting agent and water, main salt be mass-volume concentration be 5~
In the silver nitrate of the sodium tungstate of molybdate or 0.5~10g/L or the copper sulfate of 0.5~20g/L or 5~40g/L of 40g/L one
Plant or several;Wherein auxiliary element includes that concentration is 1.0~4g/L nickel sulfate, 0.5~4g/L sodium sulfite, 1.0~5g/L sulfur
Sodium thiosulfate, 2.0~5g/L aluminum chloride, zinc chloride(2.0~5g/L)And 0~40g/L fluorate;By by titanium zine plate workpiece
Carry out a series of process and obtain the titanium zine plate black protective layer described in the present invention.The titanium zine plate black protective layer dense uniform,
It is pitch-black glossy, there is with low cost, chromium-free environment-friendly, and properties can reach the level of external product, with compared with
Strong application prospect and the market competitiveness.But the patent has the disadvantage that:1st, the patent of invention is just for titanium zine plate workpiece,
That is nigrescence film layer can only be formed on titanium zine plate, steel and iron parts may be suitable for.2nd, in the patent containing molybdenum, tungsten, copper,
The heavy metal ion such as silver, the pollution to environment should not be underestimated.3rd, the nigrescence film layer corrosion resisting property that the invention is formed is poor.4th, at nigrescence
After reason, need using dewatering rust preventive oil to strengthen anti-corrosion capability.
Chinese patent 201310199938.6 discloses a kind of self-healing Environmental Blackening Agent At Room Temperature For Steel, with molybdate/
Film component based on sulfur-mantoquita system, consisting of:Copper nitrate 12-22g/L, Ammonium Molybdate Tetrahydrate 14-24g/L, sodium thiosulfate
8-12g/L;Sodium dihydrogen phosphate 18-28g/L, oxalic acid 3-5g/L, nickel sulfate 6-13g/L;Dimethylformamide 3-5g/L, lanthana
0.5-1g/L;Aluminium potassium sulfate 30-40g/L, Sodium Chloride 4-10g/L, citric acid 2-6g/L;Surfactant.The blackening agent for surface blacks
Ability is strong, without selenium environmental protection, low production cost, process is simple, the Chemical Colouring of Steel at Room Temperature film layer of the gained that blacks has good anti-corrosion
Property and self-healing, black film flawless, film layer is homogeneous, color and luster is shiny black, and adhesive force is strong and the characteristics of excellent corrosion resistance, which blacks
Film layer technical specification is:3% cupric sulphate dropping test is 65s(It is not impregnated with antirust oil), 3% Sodium Chloride soak test is 8h, with reference to
Power is more than 187 times.But the patent has the disadvantage that:1st, the patent of invention is because containing Ammonium Molybdate Tetrahydrate, so prepare
Tank liquor gradually can increasingly be presented blueness when in use, be unfavorable for user or customer's discharge.2nd, contain chlorination in the patent
Sodium, can be corrosive to nigrescence film layer.3rd, after blackening process, need using dewatering rust preventive oil to strengthen anti-corrosion capability.
Chinese patent 201210518112.7 discloses a kind of non-toxic, environmental friendly Chemical Colouring of Steel at Room Temperature inorganic agent, by following quality
The component of percentage ratio is constituted:Copper sulphate pentahydrate 1-5%, zinc dihydrogen phosphate 1-4%, zinc nitrate 1-6%, citric acid 0.1-0.3%,
EDTA- disodium 1-2%, sodium thiosulfate 1-6%, ammonium molybdate 1-4%, nickel sulfate hexahydrate 0.5-1.5%, hydroquinone 0.1-0.6%,
Potassium dichromate 0.5-1.5% and water surplus.Preparation method is carried out successively as follows:First the water for calculating weighing is added to instead
In answering kettle, agitator is started, rotating speed is controlled for 60 revs/min, then will calculate the copper sulphate pentahydrate, the six water sulphuric acid that weigh successively
Nickel, citric acid, zinc dihydrogen phosphate, zinc nitrate, EDTA- disodiums, sodium thiosulfate, ammonium molybdate, hydroquinone, potassium dichromate blow slowly
It is added in reactor, often plus a kind of raw material must be all stirred to fully dissolving, finally stirs opaque in yellow green to solution
Uniform liquid.But the patent has the disadvantage that:1st, the patent of invention is because containing Ammonium Molybdate Tetrahydrate, so the tank liquor prepared
Blueness gradually can be increasingly presented when in use, be unfavorable for user or customer's discharge.2nd, after blackening process, need to be using dehydration
Antirust oil is strengthening anti-corrosion capability.3rd, the chemical strong oxidizing property thing prohibited containing this country of potassium dichromate in the patent
Matter.4th, the corrosion resisting property of the invention is poor, need to strengthen corrosion resistance using dewatering rust preventive oil.
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 nigrescence minute surface adds lustre to anticorrodent, should
Nigrescence minute surface adds lustre to after anticorrodent blackening process, it is not necessary to soak dewatering rust preventive oil, also can natural environment preserve 6 months it is stainless
Erosion;After blackening process, ironware surface atrouss uniformity, the smooth exquisiteness of film layer, just as minute surface.
The second object of the present invention is to provide the preparation method that above-mentioned nigrescence minute surface adds lustre to anticorrodent.
The technical solution adopted for the present invention to solve the technical problems is:
A kind of nigrescence minute surface adds lustre to anticorrodent, in terms of parts by weight, is made up of following raw material:
Copper sulfate 15-25 parts, metastannic acid 30-50 parts, sodium thiosulfate 5-15 parts, stannic disulfide 15-25 parts, sodium stannate 15-25
Part, nickel sulfate 5-15 parts, potassium citrate 5-15 parts, water 300-400 parts.
Wherein preferred 20-25 parts of copper sulfate;
Wherein preferred 35-45 parts of metastannic acid;
Wherein preferred 10-15 parts of sodium thiosulfate;
Wherein preferred 20-25 parts of stannic disulfide;
Wherein preferred 20-25 parts of sodium stannate;
Wherein preferred 10-15 parts of nickel sulfate;
Wherein preferred 10-15 parts of potassium citrate.
Nigrescence minute surface of the present invention add lustre to anticorrodent pH value between 3.8-5.5.PH value is conducive to the fast of film layer in scope
Speed is formed, and the smooth degree of film layer also depends on pH value.
Nigrescence minute surface of the present invention anticorrodent preparation method of adding lustre to is as follows:
Water is added in glass container, copper sulfate, metastannic acid, sodium thiosulfate, stannic disulfide, sodium stannate, sulphuric acid is separately added into
Nickel, potassium citrate stirring and dissolving are uniform, and the nigrescence minute surface for obtaining final product the present invention adds lustre to anticorrodent.
The add lustre to using method of anticorrodent of nigrescence minute surface of the present invention is:By above-mentioned nigrescence minute surface add lustre to anticorrodent and clear water by
Quality 1:9 match somebody with somebody groove, under room temperature insert wherein 5-7 minutes workpiece, and taking-up is cleaned with clear water.
The add lustre to advantage of anticorrodent of nigrescence minute surface of the present invention is:
1st, after blackening process, it is not necessary to soak dewatering rust preventive oil, also not corrosion in 6 months can be preserved in natural environment.It is general to black
The technological process of process:Defat-washing-pickling-washing-nigrescence-washing-leaching dewatering rust preventive oil, does not use dewatering rust preventive oil work
Part returns rust quickly, and the present invention does not require the use of antirust oil;
2nd, after blackening process, ironware surface atrouss uniformity, the smooth exquisiteness of film layer, just as minute surface;3rd, nigrescence film layer
, up to more than 10 microns, in the range of this thicknesses of layers, corrosion resisting property is good, and the porosity of film layer is low, and film layer is smooth bright for thickness;
4th, the neutral salt spray test time was up to more than 48 hours.
Specific embodiment
Below by embodiment, the invention will be further described, but not as a limitation of the invention.
The unit of each dispensing numerical value is g.
1 embodiment 1-8 nigrescence minute surface of table adds lustre to the composition of anticorrodent
Embodiment | 1 | 2 | 3 | 4 | 5 | 6 | 7 |
Copper sulfate | 20 | 21 | 22 | 23 | 24 | 25 | 19 |
Metastannic acid | 40 | 39 | 38 | 37 | 35 | 34 | 41 |
Sodium thiosulfate | 10 | 11 | 12 | 13 | 14 | 15 | 9 |
Stannic disulfide | 20 | 25 | 19 | 20 | 18 | 17 | 19 |
Sodium stannate | 20 | 18 | 17 | 19 | 25 | 19 | 20 |
Nickel sulfate | 10 | 12 | 13 | 14 | 15 | 9 | 11 |
Potassium citrate | 10 | 9 | 11 | 12 | 13 | 14 | 15 |
Water | 370 | 310 | 320 | 330 | 340 | 350 | 360 |
2 embodiment 8-12 of table and comparative example 1-3 nigrescence minute surface add lustre to the composition of anticorrodent
Embodiment | 8 | 9 | 10 | 11 | 12 | Comparative example 1 | Comparative example 2 | Comparative example 3 |
Copper sulfate | 18 | 20 | 21 | 22 | 20 | 20 | 20 | 20 |
Metastannic acid | 42 | 43 | 40 | 39 | 41 | - | 64 | - |
Citric acid | - | - | - | - | - | - | - | 41 |
Sodium thiosulfate | 8 | 7 | 10 | 11 | 11 | 11 | 11 | 11 |
Stannic disulfide | 24 | 23 | 21 | 19 | 21 | 21 | 21 | 21 |
Sodium stannate | 21 | 19 | 25 | 24 | 23 | 64 | - | 23 |
Nickel sulfate | 10 | 11 | 11 | 8 | 9 | 9 | 9 | 9 |
Potassium citrate | 11 | 8 | 9 | 10 | 11 | 11 | 11 | 11 |
Water | 310 | 320 | 330 | 340 | 350 | 350 | 350 | 350 |
Comparative example 1 eliminates metastannic acid on the basis of embodiment 12, and sodium stannate consumption is 12 metastannic acid of embodiment and sodium stannate
Consumption summation, comparative example 2 eliminates sodium stannate on the basis of embodiment 12, metastannic acid consumption be 12 metastannic acid of embodiment and
Metastannic acid is changed to citric acid on the basis of embodiment 12 by the consumption summation of sodium stannate, comparative example 3.
Each nigrescence minute surface described in above example 1-12, comparative example 1-3 add lustre to anticorrodent using method it is as follows:
The add lustre to using method of anticorrodent of nigrescence minute surface of the present invention is:Above-mentioned nigrescence minute surface is added lustre to into anticorrodent and clear water by quality
1:9 match somebody with somebody groove, under room temperature insert workpiece wherein 6 minutes, and taking-up is cleaned with clear water, it is not necessary to soak dewatering rust preventive oil, it is not necessary to seal
Close liquid process.
Effect is shown in Table 3, table 4 respectively.
3 embodiment 1-7 nigrescence minute surface of table adds lustre to the using effect of anticorrodent
Embodiment | 1 | 2 | 3 | 4 | 5 | 6 | 7 |
Naturally get rusty the time, day | ≥200 | ≥200 | ≥200 | ≥200 | ≥200 | ≥200 | ≥200 |
Neutral salt spray test time, hour | ≥ 48 | ≥ 48 | ≥ 48 | ≥ 48 | ≥ 48 | ≥ 48 | ≥ 48 |
Dewatering rust preventive oil whether is needed to use cooperatively | It is no | It is no | It is no | It is no | It is no | It is no | It is no |
During use, whether tank liquor changes colour | Keep primary colors | Keep primary colors | Keep primary colors | Keep primary colors | Keep primary colors | Keep primary colors | Keep primary colors |
Mirror effect and smooth degree | It is bright fine and smooth such as mirror | It is bright fine and smooth such as mirror | It is bright fine and smooth such as mirror | It is bright fine and smooth such as mirror | It is bright fine and smooth such as mirror | It is bright fine and smooth such as mirror | It is bright fine and smooth such as mirror |
3% cupric sulphate dropping test | 10min | 10min | 10min | 10min | 10min | 10min | 10min |
3% Sodium Chloride soak test | 24h | 24h | 24h | 24h | 24h | 24h | 24h |
4 embodiment 8-12 of table and comparative example 1-3 nigrescence minute surface add lustre to the using effect of anticorrodent
Embodiment | 8 | 9 | 10 | 11 | 12 | Comparative example 1 | Comparative example 2 | Comparative example 3 |
Naturally get rusty the time, day | ≥200 | ≥200 | ≥200 | ≥200 | ≥200 | ≤40 | ≤40 | ≤40 |
Neutral salt spray test time, hour | ≥ 48 | ≥ 48 | ≥ 48 | ≥ 48 | ≥ 48 | ≤4 | ≤4 | ≤4 |
Dewatering rust preventive oil whether is needed to use cooperatively | It is no | It is no | It is no | It is no | It is no | It is | It is | It is |
Tank liquor discoloration during use | Keep primary colors | Keep primary colors | Keep primary colors | Keep primary colors | Keep primary colors | Gradually change colour, be unfavorable for Discharge | Gradually change colour, it is unfavorable In discharge | Gradually change colour, it is unfavorable In discharge |
Mirror effect and smooth degree | It is bright fine and smooth such as mirror | It is bright fine and smooth such as mirror | It is bright fine and smooth such as mirror | It is bright fine and smooth such as mirror | It is bright fine and smooth such as mirror | Uniform and delicate is unglazed | Uniform and delicate is unglazed | Uniform and delicate is unglazed |
3% cupric sulphate dropping test | 10min | 10min | 10min | 10min | 10min | 30S | 90S | 60S |
3% Sodium Chloride soak test | 24h | 24h | 24h | 24h | 24h | 1h | 4h | 2h |
The method of testing of projects in table of the present invention:
3% cupric sulphate dropping test:GB/T 5936-1986《The method of testing dipping of light industrial goods ferrous metal chemical coating
Drop method》
3% Sodium Chloride soak test:GB/T 5936-1986《The method of testing dipping of light industrial goods ferrous metal chemical coating
Drop method》
Neutral salt spray test:GB/T 5936-1986 《The corrosion resistance test method of the light industrial goods coat of metal and chemical treatment layer
Neutral salt spray test(NSS)Method》.
Although the present invention and its advantage is described in detail with reference to specifically embodiment it should be appreciated that do not surpassing
Various changes can be carried out in the case of going out the spirit and scope of the present invention defined by the appended claims, is substituted and is become
Change.One of ordinary skilled in the art will readily appreciate that from the disclosure, can be used according to the present invention and be performed
The function essentially identical to corresponding embodiment described herein or acquisition result, the existing and future essentially identical with which will
The method and steps being developed.Therefore, appended claim is intended to include such method and steps in the range of them.
Claims (9)
1. a kind of nigrescence minute surface adds lustre to anticorrodent, it is characterised in that in terms of parts by weight, be made up of following raw material:Copper sulfate 15-
25 parts, metastannic acid 30-50 parts, sodium thiosulfate 5-15 parts, stannic disulfide 15-25 parts, sodium stannate 15-25 parts, nickel sulfate 5-15
Part, potassium citrate 5-15 parts, water 300-400 parts.
2. nigrescence minute surface according to claim 1 adds lustre to anticorrodent, it is characterised in that the copper sulfate is 20-25 parts.
3. nigrescence minute surface according to claim 1 adds lustre to anticorrodent, it is characterised in that the metastannic acid is 35-45 parts.
4. nigrescence minute surface according to claim 1 adds lustre to anticorrodent, it is characterised in that the sodium thiosulfate is 10-15
Part.
5. nigrescence minute surface according to claim 1 adds lustre to anticorrodent, it is characterised in that the stannic disulfide is 20-25 parts.
6. nigrescence minute surface according to claim 1 adds lustre to anticorrodent, it is characterised in that the sodium stannate is 20-25 parts.
7. nigrescence minute surface according to claim 1 adds lustre to anticorrodent, it is characterised in that the nickel sulfate is 10-15 parts.
8. nigrescence minute surface according to claim 1 adds lustre to anticorrodent, it is characterised in that the potassium citrate is 10-15 parts.
9. nigrescence minute surface adds lustre to the preparation method of anticorrodent according to claim 1, it is characterised in that comprise the steps:
Water is added in glass container, copper sulfate, metastannic acid, sodium thiosulfate, stannic disulfide, sodium stannate, nickel sulfate, lemon is separately added into
Lemon acid potassium stirring and dissolving is uniform.
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Application publication date: 20170329 |