CN105177557B - A kind of blue-white passivator of high salt spray resistance zinc coat and preparation method thereof and deactivating process for the treatment of - Google Patents
A kind of blue-white passivator of high salt spray resistance zinc coat and preparation method thereof and deactivating process for the treatment of Download PDFInfo
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- CN105177557B CN105177557B CN201510481960.9A CN201510481960A CN105177557B CN 105177557 B CN105177557 B CN 105177557B CN 201510481960 A CN201510481960 A CN 201510481960A CN 105177557 B CN105177557 B CN 105177557B
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Abstract
The invention provides a kind of blue-white passivator of high salt spray resistance zinc coat and preparation method thereof and deactivating process for the treatment of, for the passivator using deionized water as solvent, solute is following component including concentration:10~20g/L of chromic nitrate, 2.5~4g/L of oxalic acid, 2~4g/L of malic acid, 1.5~3g/L of nitrilotriacetic acid, 3~5g/L of potassium hydroxide, 2~3g/L of cobalt nitrate, 0.5~0.8g/L of sodium tungstate, 0.4~4g/L of lanthanum nitrate 0.25~0.4g/L, γ aminopropyl triethoxysilane.The passivator of the present invention largely improves the salt spray resistance corrosion resisting property of galvanized part while Cr VI is free of in making plating solution, and plating piece is possessed blue and white film layer attractive in appearance simultaneously and improve dicoration, and compound method and passivation operation technique are simple, easily controllable.
Description
Technical field
The present invention relates to field of metal surface treatment technology, more particularly to a kind of blue-white passivator of high salt spray resistance zinc coat
And preparation method thereof and deactivating process for the treatment of.
Background technology
All kinds of galvanized steel ironwares because of its excellent corrosion resisting property, cheap price, and be widely used in building materials, automobile fitting,
The fields such as household electrical appliances.But simple galvanized steel ironware, easily corrode in a humid environment, make its product appearance and anti-corrosion
Property is severely impacted.In order to improve this shortcoming, traditional method is handled using chromating.Chromium in the passivating film
Mainly exist in the form of Cr VI, because passivating film has self-reparing capability, so its corrosion resisting property is higher.But Cr VI is height
Poison, carcinogen, seriously pollute environment, are detrimental to health.European Union has promulgated WEES and RoHS instructions, strict limit for 2002
The use of Cr VI processed, therefore, trivalent chromium passivation process arises at the historic moment.But compared to sexavalence chromium passivating, trivalent chromium passivation is resistance to
Corrosion, outward appearance etc. still have many deficiencies.As most trivalent chromium passivation process can not have high corrosion resistance and good concurrently
Dicoration, salt spray resistance is poor, and technological process is complicated, not easy operation control.
The content of the invention
The purpose of the present invention is aiming at above-mentioned the deficiencies in the prior art, there is provided a kind of indigo plant of high salt spray resistance zinc coat is white
Passivator and preparation method thereof and deactivating process for the treatment of, largely improved while Cr VI is free of in making plating solution zinc-plated
The salt spray resistance corrosion resisting property of part, and plating piece is possessed blue and white film layer attractive in appearance simultaneously and improve ornamental, compound method and passivation
Operating procedure is simple, easily controllable.
The present invention is achieved in the following ways:A kind of blue-white passivator of high salt spray resistance zinc coat of the present invention, with
Deionized water is solvent, and solute is following component including concentration:10~20g/L of chromic nitrate, 2.5~4g/L of oxalic acid, malic acid 2
~4g/L, 1.5~3g/L of nitrilotriacetic acid, 3~5g/L of potassium hydroxide, 2~3g/L of cobalt nitrate, 0.5~0.8g/L of sodium tungstate, nitric acid
0.25~0.4g/L of lanthanum, 0.4~4g/L of gamma-aminopropyl-triethoxy-silane.
A kind of preparation method of high salt spray resistance zinc coat blue-white passivator described above, comprises the following steps:
(1) chromic nitrate is added to the water stirring to being completely dissolved, sequentially adds oxalic acid, malic acid, nitrilotriacetic acid, fully
Stirring;
(2) potassium hydroxide is slowly added under constantly stirring, and heat temperature raising is fully reacted, then add successively
Enter cobalt nitrate, sodium tungstate, lanthanum nitrate, be sufficiently stirred;
(3) when temperature is down to below 40 DEG C, gamma-aminopropyl-triethoxy-silane is added.
In the step (1), water is previously heated to 55~60 DEG C.
In the step (2), 70~80 DEG C are heated to.
In the step (2), after heat temperature raising, it is stirred continuously under keeping warm mode more than 1 hour and is fully reacted.
A kind of zinc coating passivation processing method of blue-white passivator using high salt spray resistance zinc coat described above, its feature
It is, methods described includes contacting zinc coat with the bright blue passivation agent solution being passivated processing, is adjusted with watery hydrochloric acid blunt
The pH value of agent solution is to 2.0~3.0, and Passivation Treatment temperature is 20~35 DEG C, and passivation time is 20~40 seconds.
Beneficial effects of the present invention are mainly manifested in:Passivator of the present invention is aubergine supernatant liquid, without Cr VI,
The carcinogens such as mercury, lead, cadmium and phenylate class, it is harmless to human body and environment, belong to environment-friendly type passivator;The present invention is with industrial nitre
Sour chromium is raw material, makees mixing complexing agent by adding oxalic acid, malic acid and nitrilotriacetic acid, to control the film forming speed of passivating film,
Caused impurity in passivating process can be also complexed, malic acid can improve passivation film hardness, contribute to film layer wear-resistant, also because it has
There is inoxidizability and there is very strong complexing power, can be greatly improved blunt with fresh-keeping guarantor's color, aminotriacetic acid root
Change film film forming speed, and can effectively shelter the generation of iron tramp, greatly prolong the service life of passivator, reduction is produced into
This, while also there is certain chemical polishing to act on;Contain cobalt nitrate in passivator, cobalt nitrate is anti-salt spray resistance agent, can be improved
Salt-fog resistant time, the and can of radical compound containing nitric acid play good chemical polishing action on zinc coat;Added in passivator a small amount of
Sodium tungstate and lanthanum nitrate can improve the corrosion resistance of zinc coat;After gamma-aminopropyl-triethoxy-silane being added in passivator,
It can make the zinc coat after Passivation Treatment that there is moistureproof water-fast, the anti-aging performance such as anticorrosive;It is blunt using blue-white passivator of the present invention
Galvanized part after change processing carries out neutral salt spray test, its salt fog time with reference to GB/T 6461-2002, GB/T10125-1997
For more than 120 hours, high salt fog resistance is shown, and it is white in indigo plant uniformly, bright through the zinc coat outward appearance that the passivator is handled
Color, people are met to industrial products high corrosion-resistant and excellent ornamental demand, and prepare simple with operating procedure.
Embodiment
Below in conjunction with specific embodiment, the present invention is further illustrated:
Embodiment 1
A kind of blue-white passivator of high salt spray resistance zinc coat, using 1L deionized waters as solvent, solute is as follows including concentration
Component:Chromic nitrate 10g/L, oxalic acid 2.5g/L, malic acid 2g/L, nitrilotriacetic acid 1.5g/L, potassium hydroxide 3g/L, cobalt nitrate
3g/L, sodium tungstate 0.6g/L, lanthanum nitrate 0.3g/L, gamma-aminopropyl-triethoxy-silane 4g/L.
The preparation method of above-mentioned high salt spray resistance zinc coat blue-white passivator, comprises the following steps:(1) 300mL is first added to go
Ionized water adds 10g chromic nitrates in reaction vessel, after being heated to 55 DEG C and stirred to being completely dissolved, and sequentially adds 2.5g grass
Acid, 2g malic acid, 1.5g nitrilotriacetic acids, are sufficiently stirred;(2) 3g potassium hydroxide is slowly added under constantly stirring, so
Solution is warming up to 70 DEG C afterwards, and stirred 1 hour under keeping warm mode, sequentially adds 3g cobalt nitrates, 0.6g sodium tungstates, 0.3g
Lanthanum nitrate, it is sufficiently stirred;(3) when temperature is down to 30 DEG C, 4g gamma-aminopropyl-triethoxy-silanes is added, are sufficiently stirred, then added
Deionized water is settled to 1L, stirs, and produces passivating agent products.
The passivation operation technique of galvanized part:Pre-treatment → the washing such as galvanized part derusting oil removing → workpiece carries out electrogalvanizing → takes
Go out to wash → be passivated processing → washing → hot blast drying → and obtain light blue white chromating product.Passivator used is above-mentioned
Passivating agent products made from method, wherein the concrete technology for being passivated processing is adjusted to take 1L passivator solutions with watery hydrochloric acid
The pH value of solution contacts with solution to 3.0, by zinc coat and is passivated processing, and passivation temperature is 20 DEG C, and passivation time is 40 seconds,
Obtain the blue and white passivating film of appearance uniform, entire bright.By the galvanized part after passivation operation PROCESS FOR TREATMENT with reference to GB/T
6461-2002, GB/T10125-1997 progress neutral salt spray test, without there is obvious white embroidery, (area is small after 120 hours
In 1%), high salt fog resistance is shown.
Embodiment 2
A kind of blue-white passivator of high salt spray resistance zinc coat, using 1L deionized waters as solvent, solute is as follows including concentration
Component:Chromic nitrate 12g/L, oxalic acid 3.5g/L, malic acid 3g/L, nitrilotriacetic acid 2.5g/L, potassium hydroxide 4g/L, cobalt nitrate
2.5g/L, sodium tungstate 0.6g/L, lanthanum nitrate 0.35g/L, gamma-aminopropyl-triethoxy-silane 2g/L.
The preparation method of above-mentioned high salt spray resistance zinc coat blue-white passivator, comprises the following steps:(1) 400mL is first added to go
Ionized water adds 12g chromic nitrates in reaction vessel, after being heated to 55 DEG C and stirred to being completely dissolved, and sequentially adds 3.5g oxalic acid
3g malic acid, 2.5g nitrilotriacetic acids, are sufficiently stirred;(2) 4g potassium hydroxide is slowly added under constantly stirring, then will
Solution is warming up to 75 DEG C, and is stirred 1.5 hours under keeping warm mode, sequentially add 2.5g cobalt nitrates, 0.6g sodium tungstates,
0.35g lanthanum nitrates, are sufficiently stirred;(3) when temperature is down to 35 DEG C, 2g gamma-aminopropyl-triethoxy-silanes is added, are fully stirred
Mix, then add deionized water to be settled to 1L, stir, produce passivating agent products.
The passivation operation technique of galvanized part:Pre-treatment → the washing such as galvanized part derusting oil removing → workpiece carries out electrogalvanizing → takes
Go out to wash → be passivated processing → washing → hot blast drying → and obtain light blue white chromating product.Passivator used is above-mentioned
Passivating agent products made from method, wherein the concrete technology for being passivated processing is adjusted to take 1L passivator solutions with watery hydrochloric acid
The pH value of solution contacts with solution to 2.5, by zinc coat and is passivated processing, and passivation temperature is 20 DEG C, and passivation time is 35 seconds,
Obtain the blue and white passivating film of appearance uniform, entire bright.By the galvanized part after passivation operation PROCESS FOR TREATMENT with reference to GB/T
6461-2002, GB/T10125-1997 progress neutral salt spray test, without there is obvious white embroidery, (area is small after 120 hours
In 1%), high salt fog resistance is shown.
Embodiment 3
A kind of blue-white passivator of high salt spray resistance zinc coat, using 1L deionized waters as solvent, solute is as follows including concentration
Component:Chromic nitrate 15g/L, oxalic acid 3g/L, malic acid 3g/L, nitrilotriacetic acid 2g/L, potassium hydroxide 4g/L, cobalt nitrate 3g/L,
Sodium tungstate 0.5g/L, lanthanum nitrate 0.4g/L, gamma-aminopropyl-triethoxy-silane 2.2g/L.
The preparation method of above-mentioned high salt spray resistance zinc coat blue-white passivator, comprises the following steps:(1) 500mL is first added to go
Ionized water in reaction vessel, after being heated to 57 DEG C add 15g chromic nitrates stir to being completely dissolved, sequentially add 3g oxalic acid,
3g malic acid, 2g nitrilotriacetic acids, are sufficiently stirred;(2) 4g potassium hydroxide is slowly added under constantly stirring, then will be molten
Liquid is warming up to 75 DEG C, and is stirred 2 hours under keeping warm mode, sequentially adds 3g cobalt nitrates, 0.5g sodium tungstates, 0.4g nitric acid
Lanthanum, it is sufficiently stirred;(3) when temperature is down to 20 DEG C, 2.2g gamma-aminopropyl-triethoxy-silanes is added, are sufficiently stirred, then added and go
Ionized water is settled to 1L, stirs, and produces passivating agent products.
The passivation operation technique of galvanized part:Pre-treatment → the washing such as galvanized part derusting oil removing → workpiece carries out electrogalvanizing → takes
Go out to wash → be passivated processing → washing → hot blast drying → and obtain light blue white chromating product.Passivator used is above-mentioned
Passivating agent products made from method, wherein the concrete technology for being passivated processing is adjusted to take 1L passivator solutions with watery hydrochloric acid
The pH value of solution contacts with solution to 2.5, by zinc coat and is passivated processing, and passivation temperature is 25 DEG C, and passivation time is 30 seconds,
Obtain the blue and white passivating film of appearance uniform, entire bright.By the galvanized part after passivation operation PROCESS FOR TREATMENT with reference to GB/T
6461-2002, GB/T10125-1997 progress neutral salt spray test, without there is obvious white embroidery, (area is small after 120 hours
In 1%), high salt fog resistance is shown.
Embodiment 4
A kind of blue-white passivator of high salt spray resistance zinc coat, using 1L deionized waters as solvent, solute is as follows including concentration
Component:Chromic nitrate 20g/L, oxalic acid 4g/L, malic acid 4g/L, nitrilotriacetic acid 3g/L, potassium hydroxide 5g/L, cobalt nitrate 3g/L,
Sodium tungstate 0.8g/L, lanthanum nitrate 0.4g/L, gamma-aminopropyl-triethoxy-silane 0.4g/L.
The preparation method of above-mentioned high salt spray resistance zinc coat blue-white passivator, comprises the following steps:(1) 600mL is first added to go
Ionized water in reaction vessel, after being heated to 60 DEG C add 20g chromic nitrates stir to being completely dissolved, sequentially add 4g oxalic acid,
4g malic acid, 3g nitrilotriacetic acids, are sufficiently stirred;(2) 5g potassium hydroxide is slowly added under constantly stirring, then will be molten
Liquid is warming up to 80 DEG C, and is stirred 2 hours under keeping warm mode, sequentially adds 3g cobalt nitrates, 0.8g sodium tungstates, 0.4g nitric acid
Lanthanum, it is sufficiently stirred;(3) when temperature is down to 40 DEG C, 0.4g gamma-aminopropyl-triethoxy-silanes is added, are sufficiently stirred, then added and go
Ionized water is settled to 1L, stirs, and produces passivating agent products.
The passivation operation technique of galvanized part:Pre-treatment → the washing such as galvanized part derusting oil removing → workpiece carries out electrogalvanizing → takes
Go out to wash → be passivated processing → washing → hot blast drying → and obtain light blue white chromating product.Passivator used is above-mentioned
Passivating agent products made from method, wherein the concrete technology for being passivated processing is adjusted to take 1L passivator solutions with watery hydrochloric acid
The pH value of solution contacts with solution to 2.0, by zinc coat and is passivated processing, and passivation temperature is 35 DEG C, and passivation time is 20 seconds,
Obtain the blue and white passivating film of appearance uniform, entire bright.By the galvanized part after passivation operation PROCESS FOR TREATMENT with reference to GB/T
6461-2002, GB/T10125-1997 progress neutral salt spray test, without there is obvious white embroidery, (area is small after 120 hours
In 1%), superelevation salt fog resistance is shown.
Embodiment 5
A kind of blue-white passivator of high salt spray resistance zinc coat, using 1L deionized waters as solvent, solute is as follows including concentration
Component:Chromic nitrate 20g/L, oxalic acid 4g/L, malic acid 2g/L, nitrilotriacetic acid 1.5g/L, potassium hydroxide 5g/L, cobalt nitrate 2g/
L, sodium tungstate 0.5g/L, lanthanum nitrate 0.4g/L, gamma-aminopropyl-triethoxy-silane 4g/L.
The preparation method of above-mentioned high salt spray resistance zinc coat blue-white passivator, comprises the following steps:(1) 800mL is first added to go
Ionized water in reaction vessel, after being heated to 60 DEG C add 20g chromic nitrates stir to being completely dissolved, sequentially add 4g oxalic acid,
2g malic acid, 1.5g nitrilotriacetic acids, are sufficiently stirred;(2) 5g potassium hydroxide is slowly added under constantly stirring, then will
Solution is warming up to 80 DEG C, and is stirred 2.5 hours under keeping warm mode, sequentially adds 2g cobalt nitrates, 0.5g sodium tungstates, 0.4g nitre
Sour lanthanum, is sufficiently stirred;(3) when temperature is down to below 30 DEG C, 4g gamma-aminopropyl-triethoxy-silanes is added, are sufficiently stirred, then
Add deionized water to be settled to 1L, stir, produce passivating agent products.
The passivation operation technique of galvanized part:Pre-treatment → the washing such as galvanized part derusting oil removing → workpiece carries out electrogalvanizing → takes
Go out to wash → be passivated processing → washing → hot blast drying → and obtain light blue white chromating product.Passivator used is above-mentioned
Passivating agent products made from method, wherein the concrete technology for being passivated processing is adjusted to take 1L passivator solutions with watery hydrochloric acid
The pH value of solution contacts with solution to 2.0, by zinc coat and is passivated processing, and passivation temperature is 35 DEG C, and passivation time is 30 seconds,
Obtain the blue and white passivating film of appearance uniform, entire bright.By the galvanized part after passivation operation PROCESS FOR TREATMENT with reference to GB/T
6461-2002, GB/T10125-1997 progress neutral salt spray test, without there is obvious white embroidery, (area is small after 120 hours
In 1%), superelevation salt fog resistance is shown.
The above-described embodiments merely illustrate the principles and effects of the present invention, not for the limitation present invention.It is any ripe
Know the personnel of this technology all can carry out modifications and changes without prejudice under spirit and scope of the invention to above-described embodiment.Cause
This, the technical field those having ordinary skill in the art is completed under without departing from disclosed spirit and technological thought such as
All equivalent modifications or change, it should be covered by the claim of the present invention.
Claims (5)
1. a kind of preparation method of high salt spray resistance zinc coat blue-white passivator, it is characterised in that the high salt spray resistance zinc coat is blue
For white passivating agent using deionized water as solvent, solute is following component including concentration:10~20g/L of chromic nitrate, oxalic acid 2.5~
4g/L, 2~4g/L of malic acid, 1.5~3g/L of nitrilotriacetic acid, 3~5g/L of potassium hydroxide, 2~3g/L of cobalt nitrate, sodium tungstate 0.5
~0.8g/L, 0.25~0.4g/L of lanthanum nitrate, 0.4~4g/L of gamma-aminopropyl-triethoxy-silane;
Its preparation method comprises the following steps:
(1) chromic nitrate is added to the water stirring to being completely dissolved, sequentially adds oxalic acid, malic acid, nitrilotriacetic acid;
(2) potassium hydroxide is slowly added under constantly stirring, and heat temperature raising is fully reacted, and sequentially adds nitre
Sour cobalt, sodium tungstate, lanthanum nitrate;
(3) when temperature is down to below 40 DEG C, gamma-aminopropyl-triethoxy-silane is added.
2. the preparation method of high salt spray resistance zinc coat blue-white passivator according to claim 1, it is characterised in that:The step
Suddenly in (1), water is previously heated to 55~60 DEG C.
3. the preparation method of high salt spray resistance zinc coat blue-white passivator according to claim 2, it is characterised in that:The step
Suddenly in (2), 70~80 DEG C are heated to.
4. the preparation method of high salt spray resistance zinc coat blue-white passivator according to claim 3, it is characterised in that:The step
Suddenly in (2), after heat temperature raising, it is stirred continuously under keeping warm mode more than 1 hour and is fully reacted.
5. a kind of zinc coating passivation processing method of high salt spray resistance zinc coat blue-white passivator as claimed in claim 1, it is special
Sign is that methods described includes contacting zinc coat with the bright blue passivation agent solution being passivated processing, and adjustment passivator is molten
Liquid pH value is to 2.0~3.0, and Passivation Treatment temperature is 20~35 DEG C, and passivation time is 20~40 seconds.
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CN101158038A (en) * | 2007-10-11 | 2008-04-09 | 上海交通大学 | High corrosion resistant trivalent chromium blue-white deactivator and preparation method thereof |
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CN103668152A (en) * | 2012-09-06 | 2014-03-26 | 天津市大港镀锌厂 | Preparation method of high-efficiency blue-white passivation and closing passivator |
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US7029541B2 (en) * | 2002-01-24 | 2006-04-18 | Pavco, Inc. | Trivalent chromate conversion coating |
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CN101158038A (en) * | 2007-10-11 | 2008-04-09 | 上海交通大学 | High corrosion resistant trivalent chromium blue-white deactivator and preparation method thereof |
CN102400126A (en) * | 2011-11-17 | 2012-04-04 | 广州三孚新材料科技有限公司 | Two-in-one trivalent chromium blue white passivation solution for passivation and sealing and use process thereof |
CN103668152A (en) * | 2012-09-06 | 2014-03-26 | 天津市大港镀锌厂 | Preparation method of high-efficiency blue-white passivation and closing passivator |
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