CN107201514A - Magnesium alloy chromium-free passivator and application method - Google Patents
Magnesium alloy chromium-free passivator and application method Download PDFInfo
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- CN107201514A CN107201514A CN201710339367.XA CN201710339367A CN107201514A CN 107201514 A CN107201514 A CN 107201514A CN 201710339367 A CN201710339367 A CN 201710339367A CN 107201514 A CN107201514 A CN 107201514A
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- passivator
- magnesium alloy
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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
- C23C22/57—Treatment of magnesium or alloys based thereon
-
- 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
- C23C22/68—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 solutions with pH between 6 and 8
Abstract
The invention discloses a kind of magnesium alloy chromium-free passivator and application method, following component is included：The compound and its derivative of titanium, the compound and its derivative of zirconium, nano-particle, thiocarbamide and silane coupler；The compound and its derivative of the titanium are diethanol amine metatitanic acid diisopropyl ester and one kind in triethanolamine metatitanic acid diisopropyl ester or its combination, and the compound and its derivative of the zirconium are one kind or its combination in fluorine zirconic acid, fluotitanic acid and triethanolamine zirconate；The silane coupler is titanate coupling agent, zirconic acid coupling agent, molybdates esters coupling agent and one kind in vanadic acid ester coupling agent or its combination.Magnesium alloy chromium-free passivator and application method that the present invention is provided; it is not only able to solve the problem of traditional chromaking washing causes a large amount of contaminated wastewaters, and solves the problem of Chrome-free product can not reach chromaking product effect to the anti-corrosion protection performance of metal and with the adhesion performance of coating simultaneously.
Description
Technical field
The present invention relates to a kind of passivator and application method, more particularly to a kind of magnesium alloy chromium-free passivator and user
Method.
Background technology
Magnesium alloy is most light structural metallic materials at present, and its intensity is close to aluminium alloy.Specific strength is higher than aluminium alloy and steel,
Slightly below specific strength highest fibre reinforced plastics.Its damping property is good, can bear larger impact shock load.Magnesium alloy is praised
It is that 21 century preferable electronic product casing and replacing for light vehicle use material.But magnesium is as lively as a cricket metal, corrosion resistance
Difference, constrains the use of magnesium alloy.Therefore appropriate surface treatment must be carried out when magnesium alloy is used as structural material, to carry
Its high corrosion resistance.
Chemical conversion treatment in the anti-corrosion measure used at present is existed in problem of environmental pollution, antiseptic treating agent mostly
Containing chromium or non-ferrous metal element, there is different degrees of harm to environment and human body.In view of the pressure of environmental protection, at present
The use of chromium-free environment-friendly treatment fluid is more and more, and various countries researcher is making great efforts exploitation more efficient, environmentally friendly magnesium and magnesium alloy
Process for treating surface.Existing patent achievement shows that the chromium-free deactivation film system of commercial Application is mostly molybdate series, zirconates
System, silane systems or rare-earth system direction, but the research of all directions there is no gratifying achievement in research at present, respectively
Direction product can not compare favourably to the anti-corrosion protection performance of metal and with the adhesion performance of coating with chromaking passivating film.
The content of the invention
The technical problems to be solved by the invention are to provide a kind of magnesium alloy chromium-free passivator and application method, are not only able to
The problem of traditional chromaking washing causes a large amount of contaminated wastewaters is solved, and solves anticorrosion guarantor of the Chrome-free product to metal simultaneously
Shield performance and the problem of can not reach chromaking product effect with the adhesion performance of coating.
The present invention for the technical scheme that uses of solution above-mentioned technical problem be to provide a kind of magnesium alloy chromium-free passivator and
Application method, includes following component：The compound and its derivative of titanium, the compound and its derivative of zirconium, nano-particle, thiocarbamide
And silane coupler.
Above-mentioned magnesium alloy chromium-free passivator, wherein, the compound and its derivative of the titanium are diethanol amine metatitanic acid two
Isopropyl ester and one kind in triethanolamine metatitanic acid diisopropyl ester or its combination, the compound and its derivative of the zirconium are fluorine zirconium
One kind or its combination in acid, fluotitanic acid and triethanolamine zirconate.
Above-mentioned magnesium alloy chromium-free passivator, wherein, the silane coupler be titanate coupling agent, zirconic acid coupling agent,
Molybdates esters coupling agent and one kind in vanadic acid ester coupling agent or its combination.
Above-mentioned magnesium alloy chromium-free passivator, wherein, the nano-particle be nano zirconium dioxide, nano titanium oxide,
One kind or its combination in nano silicon, Nano zinc dioxide impact-resistant, nano aluminium oxide and nano cupric oxide.
Above-mentioned magnesium alloy chromium-free passivator, wherein, also comprising following component：Carboxylic acid base class group organic matter, hydroxy kind
Group organic matter and fatty alcohol polyethenoxy ether class.
Above-mentioned magnesium alloy chromium-free passivator, wherein, the proportioning of each component is as follows：
The compound and its derivative of titanium：0.1~3mol/L；
The compound and its derivative of zirconium：0.1~3mol/L；
Nano-particle：0.1~1mol/L；
Thiocarbamide：0.1~1mol/L；
Silane coupler：10~1000ppm；
Carboxylic acid base class group organic matter：10~1000ppm；
Hydroxyl groups organic matter：10~1000ppm；
Fatty alcohol polyethenoxy ether class：10~1000ppm.
Above-mentioned magnesium alloy chromium-free passivator, wherein, the molecular formula of the carboxylic acid base class group organic matter is R-COOH, R-
(COOH) n or R- (COO) n-R ', the molecular formula of the hydroxyl groups organic matter is R-OH or R- (OH) n；The poly alkyl alcohol
Oxygen ethene ethers is C2 to C20 fatty alcohol polyethenoxy ether class organic matter and its polymer, R, R ' it is carbon containing organic functional
Group, n>=1.
The present invention also provides a kind of application method of above-mentioned magnesium alloy chromium-free passivator to solve above-mentioned technical problem, its
In, comprise the following steps：S1, by the compound and its derivative of titanium, the compound of zirconium and its derivative, nano-particle, thiocarbamide,
Silane coupler is proportionally added into water, is well mixed, and passivator pH value of adjusting is 4.5~6.5, obtains Non-water washing Trend of Chrome-free blunt
Agent；S2, pending material is soaked in above-mentioned passivator after oil removing cleaning, taken out, drying or natural after cleaning
Dry the material for obtaining and having Trend of Chrome-free passivating film to surface；S3 or above-mentioned passivator is sprayed in pending material surface, clearly
Dried after washing or dry the material for obtaining and having Trend of Chrome-free passivating film to surface naturally；S4 or be coated in above-mentioned passivator is treated
Material surface is handled, drying has the material of Non-water washing chromaking passivating film to surface after cleaning.
The application method of above-mentioned magnesium alloy chromium-free passivator, wherein, the water that passivator is configured in the step S1 is pure
Water or running water, dilution ratio 1：(10~60)；Nitric acid, acetic acid, sulfuric acid, hydrochloric acid, hydrofluoric acid, hydroxide are used in the step S1
Sodium, potassium hydroxide, ammoniacal liquor or ammonium hydrogen carbonate adjust the pH value of passivator.
The application method of above-mentioned magnesium alloy chromium-free passivator, wherein, soak time is 1~40 point in the step S2
Clock；0.5~1.5bar of spray pressure in the step S3, spray time is 20~180 seconds；Coating method is in the step S4
Roller coating, blade coating or dip-coating, coating time are 10~60 seconds.
Present invention contrast prior art has following beneficial effect：Magnesium alloy chromium-free passivator and use that the present invention is provided
Method, using titanate esters as the inorganic passivating film of the main salt of film forming, coordinates silicon-containing nano particle, zirconate etc. to form organic passivation film,
It can be in magnesium and its alloy surface formation passivating film；The passivating film has excellent naked film Corrosion Protection, at the same with powder or
Paint has fabulous adhesion property；So as to solve the problem of traditional chromaking washing causes a large amount of contaminated wastewaters, solve simultaneously
Chrome-free product to the anti-corrosion protection performance of metal and with the adhesion performance of coating can not reach chromaking product effect
Problem.
Embodiment
With reference to embodiment, the invention will be further described.
The present invention provides a kind of magnesium alloy chromium-free passivator, the passivator main component for the compound containing zirconium/titanium and its
At least one of derivative, corrosion inhibiter and deionized water, the wherein at least one of silane coupler, nano-particle, thiocarbamide.
The compound and its derivative of heretofore described zirconium are the classes such as fluorine zirconic acid/fluotitanic acid/triethanolamine zirconate
Learn thing one of which or compounding.
The compound and its derivative of heretofore described titanium are diethanol amine metatitanic acid diisopropyl ester or triethanolamine metatitanic acid
The titanate ester chemicals one of which such as diisopropyl ester or compounding.
Heretofore described corrosion inhibiter be triethanolamine, MEA, silane coupler and its derivative or thiocarbamide wherein
A kind of or compounding.
Heretofore described nano-particle may include nano zirconium dioxide, nano titanium oxide, nano silicon, nanometer
Zinc oxide, nano aluminium oxide, the wherein at least one or compounding of nano cupric oxide.
Heretofore described silane coupler can be zirconium ester coupling agent, titanate coupling agent, molybdates esters coupling agent, vanadic acid
The wherein at least one or compounding of ester coupling agent.
The passivator of the present invention also includes following component：Carboxylic acid base class group organic matter, hydroxyl groups organic matter and fat
Fat alcohol polyethenoxy ether class.Specific composition proportion is as follows：
The compound and its derivative of titanium：0.1~3mol/L
The compound and its derivative of zirconium：0.1~3mol/L
Nano-particle：0.1~1mol/L
Thiocarbamide：0.1~1mol/L
Silane coupler：10~1000ppm
Carboxylic acid base class group organic matter：10~1000ppm
Hydroxyl groups organic matter：10~1000ppm
Fatty alcohol polyethenoxy ether class：10~1000ppm
And with nitric acid, acetic acid, sulfuric acid, hydrochloric acid, hydrofluoric acid, sodium hydroxide, potassium hydroxide, ammoniacal liquor, ammonium hydrogen carbonate wherein
The acid-base value of at least one regulation passivator.
Carboxylic acid base class group organic matter can be for general formula R-COOH, R- (COOH) n or R- (COO) n-R ' (wherein in the present invention
R, R ' be carbon containing organo-functional group, n=or>1) organic matter and its polymer, modified molecular structure；The hydroxyl groups
Organic matter can be general formula R-OH or R- (OH) n (wherein R, R ' are carbon containing organo-functional group, n=or>1) organic matter and its poly-
Compound, modified molecular structure；The fatty alcohol polyethenoxy ether class can be organic for C2 to C20 fatty alcohol polyethenoxy ether class
Thing and its polymer, modified molecular structure.
Present invention also offers the application method of above-mentioned passivator, comprise the following steps：
1st, by the compound and its derivative of titanium, the compound of zirconium and its derivative, nano-particle, thiocarbamide, silane coupled
Agent is proportionally added into water, is well mixed, and passivator pH value of adjusting is 4.5~6.5, obtains Non-water washing Trend of Chrome-free passivator.
2nd, by pending material by oil removing cleaning after be soaked in above-mentioned passivator, take out, cleaning after drying or from
So dry the material for obtaining and having Trend of Chrome-free passivating film to surface.
3 or above-mentioned passivator is sprayed in pending material surface, dry or dry naturally after cleaning and obtain surface
There is the material of Trend of Chrome-free passivating film.
4 or above-mentioned passivator is coated in drying after pending material surface, cleaning there is Non-water washing chromium to surface
Change the material of passivating film.
5th, it is pure water, running water with the water of configuration passivator described in step 1
6th, passivator dilutable water described in step 1 is reused, dilution ratio 1：(10~60)
7th, described in step 1 adjust pH can adjust pH value according to being needed in actual production, can with nitric acid, acetic acid, sulfuric acid,
Hydrochloric acid, hydrofluoric acid, sodium hydroxide, potassium hydroxide, ammoniacal liquor, the wherein at least one of ammonium hydrogen carbonate adjust the acid-base value of passivator
8th, immersion treatment time described in step 2 can be according to needing regulation, preferably 1~40 point of soak time in actual production
Clock
9th, spray process pressure described in step 3 and time can be according to needing regulation, preferably spray pressure in actual production
0.5~1.5bar, spray time is 20~180 seconds.
10th, coating method described in step 4 is coating method commonly used in the art, such as roller coating, blade coating, dip-coating, is applied
The time of covering can be preferably coated with the time for 10~60 seconds according to regulation is needed in actual production.
11st, the material after the passivated dose of processing needs washing, and drying or drying naturally can directly carry out subsequently adding
Work, drying temperature is preferably smaller than 120 degree.
12nd, the material can be metal material, steel, zinc, aluminium, copper, magnesium and its alloy, preferably magnesium and its alloy.It is described
Material can possess following performance after subsequent treatment：
Therefore, magnesium alloy chromium-free passivator and application method that the present invention is provided, using titanate esters as the main salt of film forming
Inorganic passivating film, coordinates silicon-containing nano particle, zirconate etc. to form organic passivation film, it can form blunt in magnesium and its alloy surface
Change film；The passivating film has excellent naked film Corrosion Protection, while having fabulous adhesion property with powder or paint.Not only
Possess the excellent adhesion performance to the anti-corrosion protection performance of metal and with coating of traditional chromaking washing process, Er Qietong
When solve Chrome-free product and can not reach chromaking product to the anti-corrosion protection performance of metal and with the adhesion performance of coating
The problem of effect.
Claims (10)
1. a kind of magnesium alloy chromium-free passivator, it is characterised in that include following component：The compound and its derivative of titanium, zirconium
Compound and its derivative, nano-particle, thiocarbamide and silane coupler.
2. magnesium alloy chromium-free passivator as claimed in claim 1, it is characterised in that the compound and its derivative of the titanium be
Diethanol amine metatitanic acid diisopropyl ester and one kind in triethanolamine metatitanic acid diisopropyl ester or its combination, the compound of the zirconium and its
Derivative is one kind or its combination in fluorine zirconic acid, fluotitanic acid and triethanolamine zirconate.
3. magnesium alloy chromium-free passivator as claimed in claim 1, it is characterised in that the silane coupler is coupled for titanate esters
Agent, zirconic acid coupling agent, molybdates esters coupling agent and one kind in vanadic acid ester coupling agent or its combination.
4. magnesium alloy chromium-free passivator as claimed in claim 1, it is characterised in that the nano-particle is nanometer titanium dioxide
One kind in zirconium, nano titanium oxide, nano silicon, Nano zinc dioxide impact-resistant, nano aluminium oxide and nano cupric oxide or its
Combination.
5. magnesium alloy chromium-free passivator as claimed in claim 1, it is characterised in that also comprising following component：Carboxylic acid base class base
Group's organic matter, hydroxyl groups organic matter and fatty alcohol polyethenoxy ether class.
6. magnesium alloy chromium-free passivator as claimed in claim 5, it is characterised in that the proportioning of each component is as follows：
The compound and its derivative of titanium：0.1~3mol/L；
The compound and its derivative of zirconium：0.1~3mol/L；
Nano-particle：0.1~1mol/L；
Thiocarbamide：0.1~1mol/L；
Silane coupler：10~1000ppm；
Carboxylic acid base class group organic matter：10~1000ppm；
Hydroxyl groups organic matter：10~1000ppm；
Fatty alcohol polyethenoxy ether class：10~1000ppm.
7. magnesium alloy chromium-free passivator as claimed in claim 6, it is characterised in that point of the carboxylic acid base class group organic matter
Minor is R-COOH, R- (COOH) n or R- (COO) n-R ', and the molecular formula of the hydroxyl groups organic matter is R-OH or R-
(OH)n；The fatty alcohol polyethenoxy ether class be C2 to C20 fatty alcohol polyethenoxy ether class organic matter and its polymer, R,
R ' is carbon containing organo-functional group, n>=1.
8. a kind of application method of magnesium alloy chromium-free passivator as described in any one of claim 1~7, it is characterised in that bag
Include following steps：
S1, the compound and its derivative, the compound of zirconium and its derivative, nano-particle, thiocarbamide, silane coupler of titanium pressed
Ratio is added to the water, and is well mixed, and passivator pH value of adjusting is 4.5~6.5, obtains Non-water washing Trend of Chrome-free passivator；
S2, by pending material by oil removing cleaning after be soaked in above-mentioned passivator, take out, cleaning after drying or dry in the air naturally
Do the material for obtaining and having Trend of Chrome-free passivating film to surface；
S3 or above-mentioned passivator is sprayed in pending material surface, drying after cleaning or dry to obtain to surface naturally has
The material of Trend of Chrome-free passivating film；
S4 or above-mentioned passivator is coated in drying after pending material surface, cleaning there is Non-water washing chromaking to surface
The material of passivating film.
9. the application method of magnesium alloy chromium-free passivator as claimed in claim 8, it is characterised in that configured in the step S1
The water of passivator is pure water or running water, dilution ratio 1：(10~60)；Nitric acid, acetic acid, sulfuric acid, salt are used in the step S1
Acid, hydrofluoric acid, sodium hydroxide, potassium hydroxide, ammoniacal liquor or ammonium hydrogen carbonate adjust the pH value of passivator.
10. the application method of magnesium alloy chromium-free passivator as claimed in claim 8, it is characterised in that soaked in the step S2
The bubble time is 1~40 minute；0.5~1.5bar of spray pressure in the step S3, spray time is 20~180 seconds；The step
Coating method is roller coating, blade coating or dip-coating in rapid S4, and coating time is 10~60 seconds.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201710339367.XA CN107201514B (en) | 2017-05-15 | 2017-05-15 | Magnesium alloy chromium-free passivator and use method thereof |
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| CN201710339367.XA CN107201514B (en) | 2017-05-15 | 2017-05-15 | Magnesium alloy chromium-free passivator and use method thereof |
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| CN107201514B CN107201514B (en) | 2020-08-14 |
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| CN108642482A (en) * | 2018-07-03 | 2018-10-12 | 苏州大韩化工有限公司 | A kind of chromium-free passivation liquid and preparation method thereof |
| CN115613022A (en) * | 2022-09-28 | 2023-01-17 | 湖南金裕环保科技有限公司 | Chromium-free natural color passivating agent for aluminum and aluminum alloy and preparation method thereof |
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| CN1381532A (en) * | 2001-04-19 | 2002-11-27 | 日本油漆株式会社 | Nonchromate metal surface finishing agent, surface handling and method and processed steel products |
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| CN115613022A (en) * | 2022-09-28 | 2023-01-17 | 湖南金裕环保科技有限公司 | Chromium-free natural color passivating agent for aluminum and aluminum alloy and preparation method thereof |
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| CN107201514B (en) | 2020-08-14 |
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Effective date of registration: 20210316 Address after: 246000 No.1, Weisan Road, high tech Industrial Development Zone, Daguan District, Anqing City, Anhui Province Patentee after: Anhui Guanghua DIYe Chemical Co.,Ltd. Address before: No.28, Lane 156, Changji Road, Jiading District, Shanghai, 201800 Patentee before: EMPIRECHEM (SHANGHAI) Co.,Ltd. |
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