CN106637173B - A kind of hot galvanizing environmental protection passivating solution and preparation method thereof - Google Patents
A kind of hot galvanizing environmental protection passivating solution and preparation method thereof Download PDFInfo
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- CN106637173B CN106637173B CN201710025057.0A CN201710025057A CN106637173B CN 106637173 B CN106637173 B CN 106637173B CN 201710025057 A CN201710025057 A CN 201710025057A CN 106637173 B CN106637173 B CN 106637173B
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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
- C23C22/40—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 containing molybdates, tungstates or vanadates
- C23C22/44—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 containing molybdates, tungstates or vanadates containing also fluorides or complex fluorides
Abstract
The present invention discloses a kind of hot galvanizing environmental protection passivating solution and preparation method thereof, belong to field of metal material surface treatment, the solution includes following ingredient acrylic resin soln 80-150mL/L, sodium tungstate 10-30g/L, sodium nitrate 15-25g/L, thiocarbamide 5-20g/L, sodium fluoride 8-22g/L, sodium citrate 5-20g/L, H2O22-5mL/L, remaining is deionized water water；Wherein acrylic resin soln includes following components：The ammonium hydroxide mass percent that acrylic resin mass percent is 30-55%, isopropanol 25-50%, mass fraction are 26% is 8-20%；The invention also discloses the preparation methods of the hot galvanizing environmental protection passivating solution；Passivating solution of the invention does not use the higher chromate of toxicity, environment and human body will not be damaged, it will form one layer of smooth, smooth, uniform passivating film using Several Thiourea Derivatives on Zinc Plate Surface prepared by passivating solution of the invention, and there is very strong corrosion resisting property, the corrosion rate of coating can effectively be slowed down, the time that white rust occurs in neutral salt spray test is more than 80 hours.
Description
Technical field
The present invention relates to a kind of hot galvanizing environmental protection passivating solutions and preparation method thereof, belong to field of metal surface treatment technology.
Background technique
Hot dipping coating technology is to popularize extensive and simple to operate steel material anticorrosion technique.Hot dipping is also named in hot galvanizing
Zinc and galvanizing by dipping are that the steel part after derusting immerses in the zinc liquid of 500 DEG C or so fusings, steel member surface are made to adhere to zinc layers,
To play corrosion-resistant purpose, it is a kind of effective anti-corrosion of metal mode, is mainly used on the metal structure facility of every profession and trade.Heat
Zinc-plated developed by more ancient hot-dipping method, and hot dip Zn Cr coating is the hair at full speed with cold-strip steel in recent decades
Exhibition just obtains extensive development.Hot dipping zinc-plating workpiece after being cooled by water, is needing long period storage and transportation, in storage and transport process easily
Corrosion phenomenon occurs, Surface Creation " white embroidery ", white rust, need to be passivated processing on its surface, to protect workpiece to exist in order to prevent
It will not be corroded in transportational process.
Industrial most common passivation of metal surfaces treatment process is chromating technique now.Main cause is chromic acid
Salt passivation technology is simple, and cost is relatively low, and etch resistant properties are excellent, and chromate passivation film has stronger self-healing ability, chromate
Chromium in passivating solution mainly exists in the form of Cr VI and trivalent chromium, but Cr VI is more toxic, and is carcinogen,
Serious pollution environment, injures human body；Though trivalent chromium toxicity is small, in use, oxidizable trivalent chromium is Cr VI, still
Not the problem of not can solve pollution.So studying, a kind of that the environmentally friendly passivation mode of chromate can be replaced to have far-reaching significance is wide
Application prospect.
Mainly there are two major classes to the research of chromium-free deactivation both at home and abroad at present：First is that inorganic matter is passivated mode, such as silicate, molybdenum
Hydrochlorate, titanium salt, tungstates, rare earth metal salt etc., second is that organic passivation mode, such as organic silanes, phytic acid are passivated, tannic acid is blunt
Change etc..But the passivation effect of both modes is all undesirable, and some film layers are loose, and compactness is inadequate, and corrosion resisting property is poor, has
Film formation time it is longer, cumbersome, the mode higher cost in addition having, no matter inorganic passivation or organic passivation, all cannot
Reach the level of industrial application.
Summary of the invention
Acrylic resin is added in the present invention in passivating solution, improves the compactness of passivating film, improves passivation film outward appearance,
The corrosion resisting property of galvanized part can be improved.
The object of the present invention is to provide a kind of hot galvanizing environmental protection passivating solutions, including following components：Acrylic resin soln 80-
150mL/L, sodium tungstate 10-30g/L, sodium nitrate 15-25g/L, thiocarbamide 5-20g/L, sodium fluoride 8-22g/L, sodium citrate 5-
20g/L, H2O22-5mL/L, remaining is water.
The mixture that the acrylic resin soln is acrylic resin, the ammonium hydroxide of isopropanol, mass fraction 26% forms,
Wherein the mass percent of acrylic resin is 30-55%, the mass percent of isopropanol is 25-50%, the ammonia of mass fraction 26%
The mass percent of water is 8-20%.
The sodium tungstate, sodium nitrate, thiocarbamide, sodium fluoride, sodium citrate, H2O2It is commercially available analysis pure chemistry reagent, water
For deionized water.
It is another object of the present invention to provide the preparation methods of the hot galvanizing environmental protection passivating solution, and specific steps are such as
Under：Sodium tungstate, sodium nitrate, thiocarbamide, sodium fluoride, sodium citrate are dissolved in water in proportion, when dissolution be heated to 50 DEG C-
It 60 DEG C and stirs, several solns is mixed after being completely dissolved, add H2O2It stirs evenly, stands 15min；Proportionally prepare
Acrylic resin soln is proportionally added into mixed solution by acrylic resin soln, is slowly added to using pipette, side edged
Stirring, until being completely dissolved, then plus water is settled to required volume to get hot galvanizing environmental protection passivating solution is arrived.
In use, being put into after heat zinc coating plate is cleaned in passivating solution and constantly shaking, room temperature is passivated 40-60s, completes passivation
Take out kept dry.
Beneficial effects of the present invention：Hot galvanizing environmental protection passivating solution of the present invention, passivation technology is simple, at low cost, and is preparing
Harmful substance is not added in the process, does not generate toxic gas in preparation process, environment will not be polluted, human body will not be made
At injury, and Several Thiourea Derivatives on Zinc Plate Surface generate passivating film densification it is smooth, smooth, passivating film corrosion resistance is good, to matrix have compared with
Good protective effect.
Specific embodiment
With reference to embodiment, the present invention will be further described, but protection scope of the present invention and is limited to institute
State content.
Embodiment 1
The component and content of hot galvanizing environmental protection passivating solution described in the present embodiment be：Acrylic resin soln 80mL/L, wolframic acid
Sodium 10g/L, sodium nitrate 15g/L, thiocarbamide 5g/L, sodium fluoride 8g/L, sodium citrate 5g/L, H2O22mL/L, remaining is to remove deionization
Water, wherein the mixture for the ammonium hydroxide composition that acrylic resin soln is acrylic resin, isopropanol, mass fraction are 26%,
The matter for the ammonium hydroxide that the mass percent of middle acrylic resin is 55%, the mass percent of isopropanol is 25%, mass fraction is 26%
Measuring percentage is 20%.
Hot galvanizing environmental protection passivating solution described in 1L the present embodiment is prepared, specific step is as follows：
（1）A clean beaker is taken, 50mL deionized water is added, takes 10g sodium tungstate to be added into beaker, beaker is placed
It is heated to 60 DEG C of water-baths, stirs to being completely dissolved, be cooled to room temperature；
（2）A clean beaker is taken, 50mL deionized water is added, takes 15g sodium nitrate to be added into beaker, beaker is placed
It is heated to 60 DEG C of water-baths, stirs to being completely dissolved, be cooled to room temperature；
（3）A clean beaker is taken, 30mL deionized water is added, takes 5g thiocarbamide to be added in beaker, beaker is placed into 60
The heating of DEG C water-bath, stirs to being completely dissolved, is cooled to room temperature；
（4）A clean beaker is taken, 50mL deionized water is added, takes 8g sodium fluoride to be added in beaker, beaker is placed into
60 DEG C of water-bath heating, stir to being completely dissolved, are cooled to room temperature；
（5）A clean beaker is taken, 30mL deionized water is added, takes 5g sodium citrate to be added in beaker, beaker is placed
It is heated to 60 DEG C of water-baths, stirs to being completely dissolved, be cooled to room temperature；
（6）A clean beaker is taken, 500ml deionized water is added, by step（1）,（2）,（3）,（4）,（5）What is obtained is molten
Liquid is added in beaker and mixes, and 2mL hydrogen peroxide is added, stirs evenly；
（7）80mL acrylic resin soln is prepared, wherein the mass percent of acrylic resin is the matter of 55%, isopropanol
Amount percentage is 25%, the mass percent of the ammonium hydroxide of mass fraction 26% is 20%, a clean pipette is taken, by 80mL propylene
Acid resin solution is slowly added into step using pipette（6）In mixed liquor beaker in, it is stirring while adding, make its completely it is molten
Solution, later plus water is settled to 1L to get 1L hot galvanizing environmental protection passivating solution is arrived.
Hot galvanizing environmental protection passivating solution manufactured in the present embodiment is used for the Passivation Treatment of hot-dip galvanizing sheet steel：Using chemical immersion
Method, galvanized part are 40mm × 60mm × 2mm galvanized sheet, and the present embodiment preparation is put into after galvanized part is cleaned in deionized water
In obtained passivating solution, galvanized part is constantly shaken, is passivated 40s, passivation temperature is room temperature, completes naturally dry after being passivated and is doing
It is saved under the conditions of dry.
Hot galvanizing environmental protection passivating solution manufactured in the present embodiment, passivation technology is simple, at low cost, has not generated in preparation process
Poisonous gas will not pollute environment, will not damage to human body；And it is fine and close in the passivating film that Several Thiourea Derivatives on Zinc Plate Surface generates
Smooth, uniform, smooth, passivating film corrosion resistance is good, has preferable protective effect to matrix, white rust occurs in neutral salt spray test
Time is 82 hours.
Embodiment 2
The component and content of hot galvanizing environmental protection passivating solution described in the present embodiment be：Acrylic resin soln 100mL/L, wolframic acid
Sodium 15g/L, sodium nitrate 18g/L, thiocarbamide 10g/L, sodium fluoride 12g/L, sodium citrate 10g/L, H2O23mL/L, remaining is to go
Ionized water, wherein the mixing for the ammonium hydroxide composition that acrylic resin soln is acrylic resin, isopropanol, mass fraction are 26%
Object, the ammonia that wherein mass percent of acrylic resin is 30%, the mass percent of isopropanol is 50%, mass fraction is 26%
The mass percent of water is 20%.
Hot galvanizing environmental protection passivating solution described in 1L the present embodiment is prepared, specific step is as follows：
（1）A clean beaker is taken, 50mL deionized water is added, takes 15g sodium tungstate to be added into beaker, beaker is placed
It is heated to 50 DEG C of water-baths, stirs to being completely dissolved, be cooled to room temperature；
（2）A clean beaker is taken, 50mL deionized water is added, takes 18g sodium nitrate to be added into beaker, beaker is placed
It is heated to 50 DEG C of water-baths, stirs to being completely dissolved, be cooled to room temperature；
（3）A clean beaker is taken, 30mL deionized water is added, takes 10g thiocarbamide to be added in beaker, beaker is placed into 50
The heating of DEG C water-bath, stirs to being completely dissolved, is cooled to room temperature；
（4）A clean beaker is taken, 50mL deionized water is added, takes 12g sodium fluoride to be added in beaker, beaker is placed into
60 DEG C of water-bath heating, stir to being completely dissolved, are cooled to room temperature；
（5）A clean beaker is taken, 30mL deionized water is added, takes 10g sodium citrate to be added in beaker, beaker is placed
It is heated to 60 DEG C of water-baths, stirs to being completely dissolved, be cooled to room temperature；
（6）A clean beaker is taken, 500ml deionized water is added, by step（1）,（2）,（3）,（4）,（5）What is obtained is molten
Liquid is added in beaker and mixes, and 3mL hydrogen peroxide is added, stirs evenly；
（7）100mL acrylic resin soln is prepared, wherein the mass percent of acrylic resin is the matter of 30%, isopropanol
Amount percentage is 50%, the mass percent for the ammonium hydroxide that mass fraction is 26% is 20%.A clean pipette is taken, by 100mL third
Olefin(e) acid resin solution is slowly added into step using pipette（6）In mixed liquor beaker in, it is stirring while adding, make its completely it is molten
Solution, later plus water is settled to 1L to get 1L hot galvanizing environmental protection passivating solution is arrived.
Hot galvanizing environmental protection passivating solution manufactured in the present embodiment is used for the Passivation Treatment of hot-dip galvanizing sheet steel：Using chemical immersion
Method, galvanized part are 40mm × 60mm × 2mm galvanized sheet, are put into the present embodiment after galvanized part is cleaned in going deionized water and match
In the passivating solution being made, constantly shaking galvanized part, be passivated 40s, passivation temperature is room temperature, complete passivation after naturally dry and
It is saved under drying condition.
Hot galvanizing environmental protection passivating solution manufactured in the present embodiment, passivation technology is simple, at low cost, has not generated in preparation process
Poisonous gas will not pollute environment, will not damage to human body；And it is fine and close in the passivating film that Several Thiourea Derivatives on Zinc Plate Surface generates
Smooth, uniform, smooth, passivating film corrosion resistance is good, has preferable protective effect to matrix, white rust occurs in neutral salt spray test
Time is 84 hours.
Embodiment 3
The component and content of hot galvanizing environmental protection passivating solution described in the present embodiment be：Acrylic resin soln 120mL/L, wolframic acid
Sodium 25g/L, sodium nitrate 20g/L, thiocarbamide 15g/L, sodium citrate 15g/L, sodium fluoride 18g/L, H2O2 4mL/L, remaining is to go
Ionized water, wherein the mixing for the ammonium hydroxide composition that acrylic resin soln is acrylic resin, isopropanol, mass fraction are 26%
Object, the ammonia that wherein mass percent of acrylic resin is 48%, the mass percent of isopropanol is 44%, mass fraction is 26%
The mass percent of water is 8%.
Hot galvanizing environmental protection passivating solution described in 1L the present embodiment is prepared, specific step is as follows：
（1）A clean beaker is taken, 50mL deionized water is added, takes 25g sodium tungstate to be added into beaker, beaker is placed
It is heated to 55 DEG C of water-baths, stirs to being completely dissolved, be cooled to room temperature；
（2）A clean beaker is taken, 50mL deionized water is added, takes 20g sodium nitrate to be added into beaker, beaker is placed
It is heated to 55 DEG C of water-baths, stirs to being completely dissolved, be cooled to room temperature；
（3）A clean beaker is taken, 30mL deionized water is added, takes 15g thiocarbamide to be added in beaker, beaker is placed into 55
The heating of DEG C water-bath, stirs to being completely dissolved, is cooled to room temperature；
（4）A clean beaker is taken, 50mL deionized water is added, takes 18g sodium fluoride to be added in beaker, beaker is placed into
50 DEG C of water-bath heating, stir to being completely dissolved, are cooled to room temperature；
（5）A clean beaker is taken, 30mL deionized water is added, takes 15g sodium citrate to be added in beaker, beaker is placed
It is heated to 50 DEG C of water-baths, stirs to being completely dissolved, be cooled to room temperature；
（6）A clean beaker is taken, 500ml deionized water is added, by step（1）,（2）,（3）,（4）,（5）What is obtained is molten
Liquid is added in beaker and mixes, and 4mL hydrogen peroxide is added, stirs evenly；
（7）120mL acrylic resin soln is prepared, wherein acrylic resin mass percent is 48g/L, isopropanol quality
The ammonium hydroxide mass percent that percentage is 44%, mass fraction is 26% is 8%.A clean pipette is taken, by 120mL acrylic acid
Resin solution is slowly added into step using pipette（6）In mixed liquor beaker in, it is stirring while adding, make it completely dissolved,
Later plus water is settled to 1L to get 1L hot galvanizing environmental protection passivating solution is arrived.
Hot galvanizing environmental protection passivating solution manufactured in the present embodiment is used for the Passivation Treatment of hot-dip galvanizing sheet steel：Using chemical immersion
Method, galvanized part are 40mm × 60mm × 2mm galvanized sheet, are put into the present embodiment after galvanized part is cleaned in going deionized water and match
In the passivating solution being made, constantly shaking galvanized part, be passivated 50s, passivation temperature is room temperature, complete passivation after naturally dry and
It is saved under drying condition.
Hot galvanizing environmental protection passivating solution manufactured in the present embodiment, passivation technology is simple, at low cost, has not generated in preparation process
Poisonous gas will not pollute environment, will not damage to human body；And it is fine and close in the passivating film that Several Thiourea Derivatives on Zinc Plate Surface generates
Smooth, uniform, smooth, passivating film corrosion resistance is good, has preferable protective effect to matrix, white rust occurs in neutral salt spray test
Time is 85 hours.
Embodiment 4
The component and content of hot galvanizing environmental protection passivating solution described in the present embodiment be：Acrylic resin soln 150mL/L, wolframic acid
Sodium 30g/L, sodium nitrate 25g/L, thiocarbamide 20g/L, sodium citrate 20g/L, sodium fluoride 22g/L, H2O25mL/L, remaining is to go
Ionized water, wherein the mixing for the ammonium hydroxide composition that acrylic resin soln is acrylic resin, isopropanol, mass fraction are 26%
Object, the ammonia that wherein mass percent of acrylic resin is 52%, the mass percent of isopropanol is 30%, mass fraction is 26%
The mass percent of water is 18%.
Hot galvanizing environmental protection passivating solution described in 1L the present embodiment is prepared, specific step is as follows：
（1）A clean beaker is taken, 50mL deionized water is added, takes 30g sodium tungstate to be added into beaker, beaker is placed
It is heated to 50 DEG C of water-baths, stirs to being completely dissolved, be cooled to room temperature；
（2）A clean beaker is taken, 50mL deionized water is added, takes 25g sodium nitrate to be added into beaker, beaker is placed
It is heated to 50 DEG C of water-baths, stirs to being completely dissolved, be cooled to room temperature；
（3）A clean beaker is taken, 30mL deionized water is added, takes 20g thiocarbamide to be added in beaker, beaker is placed into 55
The heating of DEG C water-bath, stirs to being completely dissolved, is cooled to room temperature；
（4）A clean beaker is taken, 50mL deionized water is added, takes 22g sodium fluoride to be added in beaker, beaker is placed into
55 DEG C of water-bath heating, stir to being completely dissolved, are cooled to room temperature；
（5）A clean beaker is taken, 30mL deionized water is added, takes 20g sodium citrate to be added in beaker, beaker is placed
It is heated to 55 DEG C of water-baths, stirs to being completely dissolved, be cooled to room temperature；
（6）A clean beaker is taken, 500ml deionized water is added, by step（1）,（2）,（3）,（4）,（5）What is obtained is molten
Liquid is added in beaker and mixes, and 5mL hydrogen peroxide is added, stirs evenly；
（7）150mL acrylic resin soln is prepared, wherein acrylic resin mass percent is 52%, isopropanol quality hundred
The mass percent than the ammonium hydroxide for being 26% for 30%, mass fraction is divided to be 18%.A clean pipette is taken, by 150mL acrylic acid
Resin solution is slowly added into step using pipette（6）In mixed liquor beaker in, it is stirring while adding, make it completely dissolved,
Later plus water is settled to 1L to get 1L hot galvanizing environmental protection passivating solution is arrived.
Hot galvanizing environmental protection passivating solution manufactured in the present embodiment is used for the Passivation Treatment of hot-dip galvanizing sheet steel：Using chemical immersion
Method, galvanized part are 40mm × 60mm × 2mm galvanized sheet, are put into the present embodiment after galvanized part is cleaned in going deionized water and match
In the passivating solution being made, constantly shaking galvanized part, be passivated 60s, passivation temperature is room temperature, complete passivation after naturally dry and
It is saved under drying condition.
Hot galvanizing environmental protection passivating solution manufactured in the present embodiment, passivation technology is simple, at low cost, has not generated in preparation process
Poisonous gas will not pollute environment, will not damage to human body；And it is fine and close in the passivating film that Several Thiourea Derivatives on Zinc Plate Surface generates
Smooth, uniform, smooth, passivating film corrosion resistance is good, has preferable protective effect to matrix, white rust occurs in neutral salt spray test
Time is 88 hours.
Claims (1)
1. a kind of hot galvanizing environmental protection passivating solution, which is characterized in that including following components：Acrylic resin soln 80-150mL/L,
Sodium tungstate 10-30g/L, sodium nitrate 15-25g/L, thiocarbamide 5-20g/L, sodium fluoride 8-22g/L, sodium citrate 5-20g/L, H2O2
2-5mL/L, remaining is water, and the acrylic resin soln is the ammonium hydroxide composition of acrylic resin, isopropanol, mass fraction 26%
Mixture, wherein the mass percent of acrylic resin is 30-55%, the mass percent of isopropanol is 25-50%, quality
The mass percent for the ammonium hydroxide that score is 26% is 8-20%.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101307451B (en) * | 2008-06-26 | 2010-08-18 | 北京科技大学 | Surface passivation treating liquid for organic-inorganic composite metals |
| CN100594263C (en) * | 2008-11-21 | 2010-03-17 | 常熟华冶薄板有限公司 | chromium-less passivation liquid used for continuous hot dip of galvanized sheet steel |
| CN101886260A (en) * | 2010-07-08 | 2010-11-17 | 南通飞拓生物科技有限公司 | Composite film chromium-free passivant |
| CN103334098A (en) * | 2013-06-14 | 2013-10-02 | 山东全通精密薄板有限公司 | Zinc-coated steel plate |
| CN103695891A (en) * | 2013-12-12 | 2014-04-02 | 江苏克罗德科技有限公司 | Environment-friendly hot-dipped galvanized steel plate and production method for same |
| CN104060257A (en) * | 2014-05-26 | 2014-09-24 | 安徽红桥金属制造有限公司 | Chromium-free passivator for zinc coating and preparation method of chromium-free passivator |
| CN104404492B (en) * | 2014-12-24 | 2017-07-11 | 湖南金裕化工有限公司 | Chromium-free passivation liquid, preparation method and its application method |
| CN105779983B (en) * | 2016-04-19 | 2018-05-25 | 昆明理工大学 | A kind of Chrome-free color passivation solution |
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