CN108531900A - A kind of composite coloured passivating solution of environment-friendly type and preparation method thereof - Google Patents

A kind of composite coloured passivating solution of environment-friendly type and preparation method thereof Download PDF

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Publication number
CN108531900A
CN108531900A CN201810604760.1A CN201810604760A CN108531900A CN 108531900 A CN108531900 A CN 108531900A CN 201810604760 A CN201810604760 A CN 201810604760A CN 108531900 A CN108531900 A CN 108531900A
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China
Prior art keywords
acid
passivating solution
environment
passivating
friendly type
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Pending
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CN201810604760.1A
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Chinese (zh)
Inventor
范云鹰
雷玉娟
姜超
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Kunming University of Science and Technology
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Kunming University of Science and Technology
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Priority to CN201810604760.1A priority Critical patent/CN108531900A/en
Publication of CN108531900A publication Critical patent/CN108531900A/en
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    • CCHEMISTRY; METALLURGY
    • C23COATING 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
    • C23CCOATING 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
    • C23C22/00Chemical 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
    • C23C22/05Chemical 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
    • C23C22/06Chemical 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
    • C23C22/34Chemical 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
    • C23C22/36Chemical 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 containing also phosphates
    • C23C22/361Chemical 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 containing also phosphates containing titanium, zirconium or hafnium compounds
    • CCHEMISTRY; METALLURGY
    • C25ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25DPROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D5/00Electroplating characterised by the process; Pretreatment or after-treatment of workpieces
    • C25D5/48After-treatment of electroplated surfaces

Abstract

The invention discloses composite coloured passivating solutions of a kind of environment-friendly type and preparation method thereof, belong to technical field of metal material surface treatment.The component and content of the passivating solution be:5 ~ 8 g/L tannic acid, 4 ~ 8mL/L titanium trichlorides, 4 ~ 7mL/L nitric acid, 15 ~ 20mL/L hydrogen peroxide, 2 ~ 5mL/L concentrated sulfuric acids, 8 ~ 12mL/L phosphoric acid, 2 ~ 7g/L sodium metasilicate, 6 ~ 10g/L potassium fluorides, 2 ~ 5mL/L ascorbic acid, 4 ~ 7mL/L aminotrimethylenes pitch phosphonic acids, remaining is water, and pH value is 1.5 ~ 2.0.Using passivating solution of the present invention treated zinc coating passivating film, color is bright, and color and thicknesses of layers are uniform, corrosion resisting property is excellent, and trivalent chromium, Cr VI and other harmful substances are free of in passivating solution, environment friendly and pollution-free, passivation technology is simple, and passivation efficiency is high, and membranous layer corrosion resistance is good.

Description

A kind of composite coloured passivating solution of environment-friendly type and preparation method thereof
Technical field
The present invention relates to composite coloured passivating solutions of a kind of environment-friendly type and preparation method thereof, belong to metal material surface processing skill Art field.
Background technology
Electrogalvanizing is anticorrosive metal a kind of commonly method, widely apply to hardware electromechanics, steamer, electronic equipment, The various fields such as space flight, ocean platform.Since the corrosion potential of zinc is more negative than iron, and corrosion resistance is good in dry air, works as plating When part contact corrosion medium, can first it react with zinc, to protect matrix.But since the property of zinc is active, damp and hot Environmental condition under be easily corroded, if galvanized workpiece, without post-processing, coating just produce quickly by dimmed generations white corrosion Object weakens the antiseptic property of zinc coat significantly, and matrix continues that corrosion generation red rust occurs over time, loses corrosion-resistant effect Fruit.In order to improve steel corrosion resistance and decorative appearance performance, generally all processing can be passivated to workpiece again after zinc-plated, make plating One layer of passivating film of part Surface Creation.
Cr6+Toxicity is high, easily carcinogenic, harmful to the health of people.Cr3+Although toxicity only Cr6+One thousandth, but long-term Using with Cr can be also converted into transportational process6+, various regions government limited the use of chromate.2006, European Union issued RoHS greens instruct, the stringent use for limiting chromium in electronic electric equipment making, at present and continuous perfect.
Based on environmental requirement, exploitation environmental type chromium-free deactivation has become the research heat of the various fields such as electroplating anticorrosion Point.However silicate passivation has good application prospect, but the stability of passivating film and corrosion resistance are poor, need further perfect Silicate systems;And molybdate passivation film effect is preferable, but its is of high cost;Rare-earth salts passivation is tied to form that this is also high, and technological operation Complexity, efficiency are low;The film outward appearance of titanium salt passivation gained is sufficiently close to chromating, but corrosion resistance is poor can not show a candle to chromate. Organic passivation corrosion resistance is preferable in common non-chromium inactivating technique, but adhesive force and heat resistance are poor, and single inorganic passivation is resistance to Corrosion is slightly worse than organic passivation.
Invention content
The purpose of the present invention is to provide a kind of composite coloured passivating solution of environment-friendly type, the components and content of the passivating solution For:5 ~ 8 g/L tannic acid, 4 ~ 8 mL/L titanium trichlorides, 4 ~ 7 mL/L nitric acid, 15 ~ 20 mL/L hydrogen peroxide, 2 ~ 5 mL/L are dense Sulfuric acid, 8 ~ 12mL/L phosphoric acid, 2 ~ 7 g/L sodium metasilicate, 6 ~ 10 g/L potassium fluorides, 2 ~ 5 mL/L ascorbic acid, 4 ~ 7 mL/L ammonia Base trimethylene pitches phosphonic acids, remaining is water, and pH value is the .0 of 1 .5 ~ 2.
The preparation method of the composite coloured passivating solution of environment-friendly type of the present invention, is as follows:It successively will be a certain amount of Phosphoric acid, nitric acid, tannic acid, titanium trichloride, hydrogen peroxide, sodium metasilicate, potassium fluoride, phosphoric acid, ascorbic acid, aminotrimethylene pitch phosphine Acid is add to deionized water uniformly mixed, adds water constant volume to required volume to get environment-friendly type Organic-inorganic composite chromatic passivation Liquid.
It is tannic acid of the present invention, titanium trichloride, nitric acid, hydrogen peroxide, the concentrated sulfuric acid, phosphoric acid, sodium metasilicate, potassium fluoride, anti-bad Hematic acid, aminotrimethylene fork phosphonic acids are commercially available analysis pure chemistry reagent;Made in each technical process involved in the present invention Water is deionized water.
It is using the method that the composite coloured passivating solution of the present invention is passivated processing to plating Zinc material:Plating will be passed through The material of zinc is cleaned up with deionized water, after carrying out out light processing according to a conventional method, takes out material washing, then immerse the material into It is dry after taking out and washing with water after impregnating 30 ~ 40 seconds at room temperature in composite coloured passivating solution of the present invention.
It is described go out light processing be:Material after will be zinc-plated is put by HNO3And H2In the light-emitting solution of O compositions, soak at room temperature After 3 ~ 5 seconds, taking-up, wherein light-emitting solution are bubble:The HNO that mass concentration is 3%3Solution.
The cleaning method of the material after zinc-plated, light extraction and passivation is:Deionized water rinses, until by plating piece surface Cleaning up is advisable;It is described it is passivated after the drying means of zinc-plating material be:Naturally dry, or dried up with hair-dryer, or Person's 60 DEG C of constant temperature dryings of insulating box.
Beneficial effects of the present invention are:
(1)Composite coloured passivating solution of the present invention can be used for the zinc-plated aftertreatment technology of steel and iron parts, be carried out using this passivating solution Treated, and zinc coating passivating film color is bright, and color and thicknesses of layers are uniform, and corrosion resisting property is excellent, and passivation efficiency is high, color Predominantly red green;And trivalent chromium, Cr VI and other harmful substances, environment friendly and pollution-free, passivation technology are free of in passivating solution Simply, passivation efficiency is high, and membranous layer corrosion resistance is good.
(2)Passivating solution of the present invention combines the advantages of organic passivation and inorganic passivation, makes full use of organic and inorganic slow The synergistic effect between agent is lost, the corrosion resisting property of passivating film is improved using compounded technology, performance complement.Chromium is free of in passivating solution Equal noxious materials, overcome chromating technology toxicity it is big, not environmentally the shortcomings of, it can be achieved that galvanizing production clean manufacturing;
(3)The passivation process of passivating solution of the present invention is simple, and passivation time is short, and passivation efficiency is high, and film adhesion is strong, film layer Thickness is uniform;The passivating film handled through the passivating solution, excellent corrosion resistance, the white rust time occur through neutral salt spray test is more than 120 hours.The appearance of a sample dicoration handled through passivating solution of the present invention is fabulous, can reach chromic acid salt level.
Specific implementation mode
With reference to embodiment, the present invention will be further described, but the scope of the present invention be not limited only to it is described Content.All ranges for belonging to the present invention and being protected being modified on the basis of the present invention.
Embodiment 1
The group of the composite coloured passivating solution of the present embodiment environment-friendly type is divided into:5 g/L tannic acid, 4 mL/L titanium trichlorides, 4mL/L nitre Acid, 15mL/L hydrogen peroxide, the 2 mL/L concentrated sulfuric acids, 8mL/L phosphoric acid, 2g/L sodium metasilicate, 6g/L potassium fluorides, 2 mL/L ascorbic acid, 4mL/L aminotrimethylenes pitch phosphonic acids, pH value 2.0.
The preparation method of the composite coloured passivating solution of the present embodiment environment-friendly type is:According to said components by phosphoric acid, nitric acid, tannin Acid, titanium trichloride, hydrogen peroxide, sodium metasilicate, potassium fluoride, phosphoric acid, ascorbic acid, aminotrimethylene fork phosphonic acids are added sequentially to It is uniformly mixed in ionized water, adds water constant volume to required volume up to environment-friendly type Organic-inorganic composite color passivation solution.
The passivating solution that the present embodiment is prepared is for being passivated plated steel sheet:
(1)The plated steel sheet is obtained through following method:The low carbon steel plate of 40mm × 50mm × 0.5mm is being electroplated It routinely derusted before, oil removing, polishing, after the pre-treatments such as activation, be put into conventional electroplate liquid and carry out electroplating processes, it is zinc-plated The plating solution for the treatment of process forms and operating condition is:ZnCL270 175 g/L of g/L, KCL, 30 g/L of boric acid, brightener 0 .5mL/L, 7 mL/L of softening agent, plating solution pH value be 5 .4, current density be 1 .5 A/ dm2, temperature is room temperature, when plating Between be 20min, obtain plated steel sheet, it is spare.
(2)Prepare light-emitting solution:By the pure HNO of chemistry3A concentration of 3% light-emitting solution is configured to water, it is spare.
(3)By step(1)Clean rear immersion step is washed with deionized water in obtained plated steel sheet(2)In obtained light extraction It in liquid, stops 5 seconds, is washed with deionized water after taking-up totally, then immerse in passivating solution at room temperature, after impregnating 30 seconds at room temperature, taken Go out, is dried up with hair-dryer after deionized water wash clean.
Passivated liquid treated steel plate is green, bright in luster, color uniformly, film layer it is thicker, passivation efficiency is high, film layer Corrosion resistance is good, and it is more than 125 hours the white rust time occur through neutral salt spray test.
Embodiment 2
The group of the composite coloured passivating solution of the present embodiment environment-friendly type is divided into:7g/L tannic acid, 5mL/L titanium trichlorides, 5mL/L nitre Acid, 18mL/L hydrogen peroxide, the 3mL/L concentrated sulfuric acids, 10mL/L phosphoric acid, 5g/L sodium metasilicate, 9g/L potassium fluorides, 5 mL/L ascorbic acid, 5mL/L aminotrimethylenes pitch phosphonic acids, pH value 2.0.
The preparation method of the composite coloured passivating solution of the present embodiment environment-friendly type is:According to said components by phosphoric acid, nitric acid, tannin Acid, titanium trichloride, hydrogen peroxide, sodium metasilicate, potassium fluoride, phosphoric acid, ascorbic acid, aminotrimethylene fork phosphonic acids are added sequentially to It is uniformly mixed in ionized water, adds water constant volume to required volume up to environment-friendly type Organic-inorganic composite color passivation solution.
The passivating solution that the present embodiment is prepared is for being passivated plated steel sheet:
(1)The plated steel sheet is obtained through following method:The low carbon steel plate of 40mm × 50mm × 0.5mm is being electroplated It routinely derusted before, oil removing, polishing, after the pre-treatments such as activation, be put into conventional electroplate liquid and carry out electroplating processes, it is zinc-plated The plating solution for the treatment of process forms and operating condition is:ZnCL270 175 g/L of g/L, KCL, 30 g/L of boric acid, brightener 0 .5mL/L, 7 mL/L of softening agent, plating solution pH value be 5 .4, current density be 1 .7 A/ dm2, temperature is room temperature, when plating Between be 20min, obtain plated steel sheet, it is spare.
(2)Prepare light-emitting solution:By the pure HNO of chemistry3A concentration of 3% light-emitting solution is configured to water, it is spare.
(3)By step(1)Clean rear immersion step is washed with deionized water in obtained plated steel sheet(2)In obtained light extraction It in liquid, stops 5 seconds, is washed with deionized water after taking-up totally, then immerse in passivating solution at room temperature, after impregnating 35 seconds at room temperature, taken Go out, is dried up with hair-dryer after deionized water wash clean.
Passivated liquid treated steel plate, then Seal treatment is carried out with 1g/L potassium permanganate, obtained passivating film is red green Color, color is bright, and color is uniform, film layer thickens, and passivation efficiency is high, and membranous layer corrosion resistance is good, white rust occurs through neutral salt spray test Time is more than 140 hours.
Embodiment 3
The group of the composite coloured passivating solution of the present embodiment environment-friendly type is divided into:8g/L tannic acid, 8mL/L titanium trichlorides, 7mL/L nitre Acid, 20mL/L hydrogen peroxide, the 5mL/L concentrated sulfuric acids, 12mL/L phosphoric acid, 7g/L sodium metasilicate, 10 g/L potassium fluorides, 5mL/L Vitamin Cs Acid, 7mL/L aminotrimethylenes pitch phosphonic acids, pH value 1.5.
The preparation method of the composite coloured passivating solution of the present embodiment environment-friendly type is:According to said components by phosphoric acid, nitric acid, tannin Acid, titanium trichloride, hydrogen peroxide, sodium metasilicate, potassium fluoride, phosphoric acid, ascorbic acid, aminotrimethylene fork phosphonic acids are added sequentially to It is uniformly mixed in ionized water, adds water constant volume to required volume up to environment-friendly type Organic-inorganic composite color passivation solution.
The color passivation solution that the present embodiment is prepared is for being passivated certain model electrogalvanizing carbon steel bolt, nut:
(1)The processing of alkaline zinc-electroplating is carried out to certain model carbon steel bolt, nut:Certain model carbon steel bolt, nut are passed through Implement plating after the processing such as conventional derusting, oil removing, weak etch, preimpregnation, the plating solution composition and operating condition of zincincation are: ZnCL2The pH value of 70 175 g/L of g/L, KCL, 30 g/L of boric acid, 0 .5mL/L of brightener, 7 mL/L of softening agent, plating solution For 5 .4, current density is 1 .7 A/ dm2, temperature is room temperature, and the barrel plating time is 2h, obtains electrogalvanizing certain model electrogalvanizing Carbon steel bolt, nut, it is spare.
(2)Prepare light-emitting solution:By the pure HNO of chemistry3A concentration of 3% light-emitting solution is configured to water, it is spare.
(3)By step(1)Obtained electrogalvanizing carbon steel bolt, nut deionized water immerses step after cleaning up(2)In It in obtained light-emitting solution, stops 5 seconds at room temperature, is washed with deionized water after taking-up totally, then immerse in passivating solution, impregnates at room temperature After 40 seconds, takes out, dried up with hair-dryer after deionized water wash clean.
Passivated liquid treated bolt, nut are yellow, and color is bright, and color is uniform, and passivation efficiency is high, and film layer is anti-corrosion Property is good, and it is more than 120 hours the white rust time occur through neutral salt spray test.
The specific implementation mode of the present invention is explained in detail above, but the present invention is not limited to above-mentioned embodiment party Formula can also be done without departing from the purpose of the present invention within the knowledge of a person skilled in the art Go out various change.

Claims (2)

1. a kind of composite coloured passivating solution of environment-friendly type, it is characterised in that:The component and content of the passivating solution be:5 ~ 8 g/L are mono- Peaceful acid, 4 ~ 8mL/L titanium trichlorides, 4 ~ 7mL/L nitric acid, 15 ~ 20mL/L hydrogen peroxide, 2 ~ 5mL/L concentrated sulfuric acids, 8 ~ 12mL/L phosphorus Acid, 2 ~ 7g/L sodium metasilicate, 6 ~ 10g/L potassium fluorides, 2 ~ 5mL/L ascorbic acid, 4 ~ 7mL/L aminotrimethylenes pitch phosphonic acids, remaining For water, pH value is the .0 of 1 .5 ~ 2.
2. the preparation method of the composite coloured passivating solution of environment-friendly type described in claim 1, it is characterised in that:Successively by a certain amount of phosphorus Acid, nitric acid, tannic acid, titanium trichloride, hydrogen peroxide, sodium metasilicate, potassium fluoride, phosphoric acid, ascorbic acid, aminotrimethylene pitch phosphonic acids It is add to deionized water uniformly mixed, adds water constant volume to required volume to get environment-friendly type Organic-inorganic composite chromatic passivation Liquid.
CN201810604760.1A 2018-06-13 2018-06-13 A kind of composite coloured passivating solution of environment-friendly type and preparation method thereof Pending CN108531900A (en)

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Application publication date: 20180914