CN104357817B - Compound chrome-free tanning agent of magnesium alloy and preparation method thereof - Google Patents
Compound chrome-free tanning agent of magnesium alloy and preparation method thereof Download PDFInfo
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- CN104357817B CN104357817B CN201410639541.9A CN201410639541A CN104357817B CN 104357817 B CN104357817 B CN 104357817B CN 201410639541 A CN201410639541 A CN 201410639541A CN 104357817 B CN104357817 B CN 104357817B
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- magnesium alloy
- tanning agent
- molybdate
- free tanning
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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
- C23C22/02—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 non-aqueous solutions
-
- 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
- C23C22/02—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 non-aqueous solutions
- C23C22/03—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 non-aqueous solutions containing phosphorus compounds
-
- 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
- C23C2222/00—Aspects relating to chemical surface treatment of metallic material by reaction of the surface with a reactive medium
- C23C2222/20—Use of solutions containing silanes
Abstract
The invention discloses a kind of compound chrome-free tanning agent of magnesium alloy and preparation method thereof, component and each constituent mass number are as follows: molybdate 4 ~ 10 parts, tungstates 2 ~ 6 parts, 1 ~ 3 part of potassium permanganate, ammonium titanium fluoride 2 ~ 5 parts, six phosphate ester of cyclohexanhexanol 6 ~ 15 parts, oleic acid 5 ~ 15 parts, MTES 1 ~ 5 part, tetraethyl orthosilicate 1 ~ 5 part.Also include phosphate 3 ~ 8 parts, 1 ~ 5 part of nitrate.Also include that siloxanes methylates 1 ~ 2 part of potassium.Described molybdate is sodium molybdate or ammonium molybdate.Described tungstates is sodium tungstate, artificial schellite or Zinc Tungstate.Described phosphate is sodium phosphate, and described nitrate is calcium nitrate.Passivator uses organic deactivation matter and mineral-type deactivation matter to proportion and forms compound chrome-free tanning agent, without chromium, safety non-toxic, environmentally safe, can form passivating film at alloy surface, improve the corrosion resistance of magnesium alloy.
Description
Technical field
The invention belongs to metal surface treatment chemical product technical field, be specifically related to a kind of compound chromium-free deactivation of magnesium alloy
Agent and preparation method thereof.
Background technology
Magnesium elements distribution on earth is extremely extensive, and reserves are huge, and magnesium alloy has a lot of characteristic, mainly has:
1, it is structural metallic materials the lightest in current all series alloys;2, electromagnetic wave shielding is good, is high-quality conductor;3, specific strength and
Specific stiffness is superior to iron and steel and aluminium alloy, is slightly poorer than best fibre reinforced plastics;4, processing characteristics is splendid, and with low cost;
5, absorb vibrations excellent performance, be conducive to the impact that reduction vibrations and noise are brought;6, high-termal conductivity, is better than aluminium alloy;7、
Performance nontoxic, recyclable is high, meets the requirement of sustainable development and environmental protection.Therefore during magnesium alloy is widely used in all trades and professions.
In highway vehicles field, the application of magnesium alloy mainly includes bicycle industry, auto industry and motorcycle
Industry etc..Magnesium alloy has great technological merit in combination property, from last century the nineties, Korea S, Japan and
American-European each high maneuver car produces commercial city and gradually Magnesium Alloys Components is incorporated on production line, is used for manufacturing control wheel, instrument
The parts such as dial plate, seat frame.
In war industry and aerospace field, magnesium alloy has obtained substantial amounts of application, its light weight, damping and noise reduction etc.
Feature, can very well meet the requirement to manufacturing material of this field.Currently it is mainly used in rocket, guided missile, aircraft, satellite
Parts produce and manufacture.There is the carbon of high specific strength, high ratio modulus and good thermal stability or the magnesium gold of graphite fibre enhancing
Metal-matrix composite material, is the preferable structural material of space industry, for artificial satellite wireless skeleton, bracing frame, reflecting mirror and sky
Between stand framework etc., structure efficiency is the highest.
In medical field, rustless steel is widely used in plastic surgery because of machinery and the corrosion resisting property of its excellence
Skeletal fixation, artificial joint and skeleton and the expandable stent etc. at esophageal stricture position, but need after physical recovery health
Carry out second operation to be extractd, bring another wound to health.Magnesium alloy itself has good mechanical performance, and magnesium unit
Element is one of necessary macroelement of human body, internal metabolic has been smoothed out irreplaceable positive role to raw.
Along with deepening continuously and New Processing fast development of magnesium alloy research, research and clinical practice for medical material bring
New opportunity, the emphasis that degradable magnesium alloy material has become present material science and field of biomedical materials receives much concern
And focus, have broad application prospects and business potential.
Manufacturing field at electric appliance and electronic, magnesium alloy not only has low, the excellent mechanics mechanical performance of lightweight, valency, well dissipates
Hot and recoverable, has outstanding electromagnetic wave shielding simultaneously, is eliminating mobile phone electromagnetic wave on Health Impact
There is positive effect, also comply with the 3C product exploitation demand to novel product.
Magnesium alloy has a lot of excellent performance, but decay resistance becomes a short slab in its many performance, limit
Make it extensively to apply.The corrosion of magnesium alloy occurs mainly on its surface contacted with media environment, corrosion rate mainly by
Surface and the medium of alloy are determined, therefore, the corrosion protection technology of magnesium alloy is typically all round media environment and alloy
Interface is carried out.The surfacecti proteon process of magnesium alloy can obtain extensive industrial applications for it and have weight with increasing the service life
The meaning wanted.Meanwhile, surface process is to improve with low cost, simple to operate in all multi-methods of corrosion stability of magnesium alloy but also capable having not only
The means of effect.Applying the most simple and effective in Corrosion Behaviors of Magnesium Alloys protective treatment at present is passivation of metal surfaces treatment technology, chromic acid
Salt is passivated as outstanding corrosion
Preparation is widely used in Treatment of Metal Surface.Chromating technique is the most ripe, but owing to Cr VI has
There is carcinogenecity, biological and human body can be produced fatal threat.Cr VI is the material that a kind of toxicity is the biggest simultaneously, and it is the most dirty
Dye environment, the symptom such as Long Term Contact can cause people to have a headache, goes into a coma, rhinitis, nasal perforation, skin ulcer and the various cancerations of initiation is right
Environmental and human health impacts is very harmful.Therefore, exploitation safety non-toxic free of contamination novel magnesium alloy passivator it is badly in need of.
Summary of the invention
It is an object of the invention to provide a kind of compound chrome-free tanning agent of magnesium alloy and preparation method thereof, passivator uses to be had
Machine class deactivation matter and mineral-type deactivation matter proportion and form compound chrome-free tanning agent, and without chromium, safety non-toxic, to ring
Border is pollution-free, can form passivating film at alloy surface, improve the corrosion resistance of magnesium alloy.
To achieve these goals, the technological means that the present invention uses is:
A kind of compound chrome-free tanning agent of magnesium alloy, component and each constituent mass number are as follows: molybdate 4 ~ 10 parts, tungsten
Hydrochlorate 2 ~ 6 parts, 1 ~ 3 part of potassium permanganate, ammonium titanium fluoride 2 ~ 5 parts, six phosphate ester of cyclohexanhexanol 6 ~ 15 parts, oleic acid 5 ~ 15 parts,
MTES 1 ~ 5 part, tetraethyl orthosilicate 1 ~ 5 part.
Also include phosphate 3 ~ 8 parts, 1 ~ 5 part of nitrate.
Also include that siloxanes methylates 1 ~ 2 part of potassium.
Described molybdate is sodium molybdate or ammonium molybdate.
Described tungstates is sodium tungstate, artificial schellite or Zinc Tungstate.
Described phosphate is sodium phosphate, and described nitrate is calcium nitrate.
The compound chrome-free tanning agent of magnesium alloy, component and each constituent mass number are as follows: molybdate 6 ~ 8 parts, tungstates 3
~ 5 parts, 2 parts of potassium permanganate, ammonium titanium fluoride 2.5 ~ 4.2 parts, phosphate 4 ~ 6 parts, 2 ~ 4 parts of nitrate, cyclohexanhexanol six phosphoric acid
Ester 8 ~ 12 parts, oleic acid 8 ~ 12 parts, MTES 2 ~ 4 parts, tetraethyl orthosilicate 2 ~ 4 parts, siloxanes methylates potassium
1.8 part.
The compound chrome-free tanning agent of magnesium alloy, component and each constituent mass number are as follows: molybdate 7 parts, tungstates 4
Part, 2 parts of potassium permanganate, ammonium titanium fluoride 3.6 parts, phosphate 5 parts, 3 parts of nitrate, six phosphate ester of cyclohexanhexanol 10 parts, oil
Acid 10 parts, MTES 3 parts, tetraethyl orthosilicate 3 parts, siloxanes methylates 1.8 parts of potassium.
The preparation method of the compound chrome-free tanning agent of magnesium alloy, mixes molybdate, tungstates, potassium permanganate, ammonium titanium fluoride
Close uniformly, obtain inorganic passivation;By six phosphate ester of cyclohexanhexanol, oleic acid, MTES, tetraethyl orthosilicate mixing
Uniformly, organic passivation thing is obtained;The most inorganic passivation is joined in organic passivation thing, be heated to 30 ~ 80 DEG C, stir
Mix uniformly, obtain compound chrome-free tanning agent.
Heating-up temperature is preferably 45 DEG C.
Beneficial effect: compound chrome-free tanning agent of magnesium alloy that the present invention provides and preparation method thereof, passivator uses to be had
Machine class deactivation matter and mineral-type deactivation matter proportion and form compound chrome-free tanning agent, and without chromium, safety non-toxic, to ring
Border is pollution-free, can form passivating film at alloy surface, improve the corrosion resistance of magnesium alloy.
Detailed description of the invention
Embodiment 1
A kind of compound chrome-free tanning agent of magnesium alloy, component and each constituent mass number are as follows: sodium molybdate 4 parts, Zinc Tungstate
2 parts, 1 part of potassium permanganate, ammonium titanium fluoride 2 parts, six phosphate ester of cyclohexanhexanol 6 parts, oleic acid 5 parts, MTES
1 part, tetraethyl orthosilicate 1 part.
By sodium molybdate, Zinc Tungstate, potassium permanganate, ammonium titanium fluoride mix homogeneously, obtain inorganic passivation;By cyclohexanhexanol six phosphorus
Acid esters, oleic acid, MTES, tetraethyl orthosilicate mix homogeneously, obtain organic passivation thing;The most before use by nothing
Machine passivation joins in organic passivation thing, is heated to 40 DEG C, stirs, and obtains compound chrome-free tanning agent.
Embodiment 2
A kind of compound chrome-free tanning agent of magnesium alloy, component and each constituent mass number are as follows: sodium molybdate 10 parts, Zinc Tungstate
6 parts, 3 parts of potassium permanganate, ammonium titanium fluoride 5 parts, six phosphate ester of cyclohexanhexanol 15 parts, oleic acid 15 parts, MTES 5
Part, tetraethyl orthosilicate 5 parts.
By sodium molybdate, Zinc Tungstate, potassium permanganate, ammonium titanium fluoride mix homogeneously, obtain inorganic passivation;By cyclohexanhexanol six phosphorus
Acid esters, oleic acid, MTES, tetraethyl orthosilicate mix homogeneously, obtain organic passivation thing;The most before use by nothing
Machine passivation joins in organic passivation thing, is heated to 40 DEG C, stirs, and obtains compound chrome-free tanning agent.
Embodiment 3
The compound chrome-free tanning agent of magnesium alloy, component and each constituent mass number are as follows: ammonium molybdate 6 parts, sodium tungstate 3
Part, 2 parts of potassium permanganate, ammonium titanium fluoride 2.5 parts, sodium phosphate 4 parts, calcium nitrate 2 parts, six phosphate ester of cyclohexanhexanol 8 parts, oil
Acid 8 parts, MTES 2 parts, tetraethyl orthosilicate 2 ~ 4 parts, siloxanes methylates 1.8 parts of potassium.
By ammonium molybdate, sodium tungstate, potassium permanganate, ammonium titanium fluoride, sodium phosphate, calcium nitrate mix homogeneously, obtain inorganic passivation;
Methylate potassium mix homogeneously by six phosphate ester of cyclohexanhexanol, oleic acid, MTES, tetraethyl orthosilicate, siloxanes,
Obtain organic passivation thing;The most inorganic passivation is joined in organic passivation thing, is heated to 50 DEG C, stirs,
Obtain compound chrome-free tanning agent.
Embodiment 4
The compound chrome-free tanning agent of magnesium alloy, component and each constituent mass number are as follows: ammonium molybdate 8 parts, sodium tungstate 5 parts,
2 parts of potassium permanganate, ammonium titanium fluoride 4.2 parts, sodium phosphate 6 parts, calcium nitrate 4 parts, six phosphate ester of cyclohexanhexanol 12 parts, oleic acid 12 parts,
MTES 2 ~ 4 parts, tetraethyl orthosilicate 4 parts, siloxanes methylates 1.8 parts of potassium.
By ammonium molybdate, sodium tungstate, potassium permanganate, ammonium titanium fluoride, sodium phosphate, calcium nitrate mix homogeneously, obtain inorganic passivation;
Methylate potassium mix homogeneously by six phosphate ester of cyclohexanhexanol, oleic acid, MTES, tetraethyl orthosilicate, siloxanes,
Obtain organic passivation thing;The most inorganic passivation is joined in organic passivation thing, is heated to 50 DEG C, stirs,
Obtain compound chrome-free tanning agent.
Embodiment 5
The compound chrome-free tanning agent of magnesium alloy, component and each constituent mass number are as follows: sodium molybdate 7 parts, artificial schellite 4
Part, 2 parts of potassium permanganate, ammonium titanium fluoride 3.6 parts, sodium phosphate 5 parts, calcium nitrate 3 parts, six phosphate ester of cyclohexanhexanol 10 parts, oil
Acid 10 parts, MTES 3 parts, tetraethyl orthosilicate 3 parts, siloxanes methylates 1.8 parts of potassium.
By sodium molybdate, artificial schellite, potassium permanganate, ammonium titanium fluoride, sodium phosphate and calcium nitrate mix homogeneously, obtain inorganic passivation
Thing;The potassium that six phosphate ester of cyclohexanhexanol, oleic acid, MTES, tetraethyl orthosilicate and siloxanes methylated mixing is all
Even, obtain organic passivation thing;The most inorganic passivation is joined in organic passivation thing, be heated to 30 ~ 80 DEG C, stirring
Uniformly, compound chrome-free tanning agent is obtained.
DK7732 type electric spark CNC wire-cut machine used for magnesium alloy is processed into specification is 13mm × 13mm × 5mm
Small pieces, polishing, until surface exposes metallic luster, smooth and no marking, as test sample, magnesium alloy is used reality
The compound chrome-free tanning agent executing example 1 ~ 5 is coated passivation, and coated weight is 5mL/g, and then 80 DEG C of dry 20min, then enter
Row performance test, the results are shown in Table 1.
With reference to machinery industry standard JB/T 6073-1992, use the compound chrome-free tanning agent of immersion corrosion test determination
The corrosion resisting property of coating is formed: taking sample and immerse immersion in 5% NaCl solution, sample plastic ties is hanged at Mg alloy surface
Hanging, upper end is away from liquid level more than 2cm, and solution pH value is 6.5, changes primary brine, uncovered placement, temperature 25 every six days
± 2 DEG C, recording each sample and the time of first red rust occur, the anti-corrosion time is as Evaluation of Corrosion Resistance result.
Neutral salt spray test:
Temperature in proof box is maintained at 35 DEG C, and compressed air to be preheating between 45 DEG C and be adjusted to enough pressure.
The mass concentration of sodium chloride solution is 5% ± 1%, and after condensation, the pH value of solution is between 6.5-7.2.During salt spray test,
Fall mist amount should control in following scope: every 80cm2In horizontal plane, between the fall mist amount average out to 1.0 ~ 2.0ml collected per hour,
Sample is placed in proof box and sprays continuously 72 hours, measure planar portions extent of corrosion.
Film adhesive is tested:
The film of test film is spaced 1mm and portrays the most vertical line, judge according to the size of gap slight crack extension
The fragility of film and the best to the adhesion property of this material.
Table 1:
Claims (6)
1. the compound chrome-free tanning agent of magnesium alloy, it is characterised in that component and each constituent mass number are as follows: molybdate 7
Part, tungstates 4 parts, 2 parts of potassium permanganate, ammonium titanium fluoride 3.6 parts, phosphate 5 parts, 3 parts of nitrate, cyclohexanhexanol six phosphorus
Acid esters 10 parts, oleic acid 10 parts, MTES 3 parts, tetraethyl orthosilicate 3 parts, siloxanes methylates 1.8 parts of potassium.
The compound chrome-free tanning agent of magnesium alloy the most according to claim 1, it is characterised in that: described molybdate be sodium molybdate or
Person's ammonium molybdate.
The compound chrome-free tanning agent of magnesium alloy the most according to claim 1, it is characterised in that: described tungstates be sodium tungstate,
Artificial schellite or Zinc Tungstate.
The compound chrome-free tanning agent of magnesium alloy the most according to claim 2, it is characterised in that: described phosphate is sodium phosphate,
Described nitrate is calcium nitrate.
5. the preparation method of the compound chrome-free tanning agent of magnesium alloy described in any one in claim 1 ~ 4, it is characterised in that: will
Molybdate, tungstates, potassium permanganate, ammonium titanium fluoride mix homogeneously, obtain inorganic passivation;By six phosphate ester of cyclohexanhexanol, oleic acid
, MTES, tetraethyl orthosilicate mix homogeneously, obtain organic passivation thing;The most inorganic passivation is added
Enter in organic passivation thing, be heated to 30 ~ 80 DEG C, stir, obtain compound chrome-free tanning agent.
The preparation method of the compound chrome-free tanning agent of magnesium alloy the most according to claim 5, it is characterised in that: heating-up temperature
It it is 45 DEG C.
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CN107488845B (en) * | 2016-06-11 | 2019-11-19 | 上海梅山钢铁股份有限公司 | A kind of chromium-free passivation liquid and its application method for tin plate |
CN107326355A (en) * | 2017-06-19 | 2017-11-07 | 苏州莱特复合材料有限公司 | A kind of preparation method of electrical component powdered-metal passivator |
CN109023334A (en) * | 2018-08-23 | 2018-12-18 | 云南科威液态金属谷研发有限公司 | A kind of aluminum alloy surface slows down protective film of liquid metal corrosion and preparation method thereof |
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CN1327487A (en) * | 1999-03-24 | 2001-12-19 | 电化学工程股份有限公司 | Chemically passivated object made of magnesium or alloys thereof |
CN101250699A (en) * | 2008-03-27 | 2008-08-27 | 武汉科技大学 | Chromium-free passivation liquid for galvanized sheet and manufacture method thereof |
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CN1327487A (en) * | 1999-03-24 | 2001-12-19 | 电化学工程股份有限公司 | Chemically passivated object made of magnesium or alloys thereof |
CN101250699A (en) * | 2008-03-27 | 2008-08-27 | 武汉科技大学 | Chromium-free passivation liquid for galvanized sheet and manufacture method thereof |
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镀锌板无铬钝化技术进展;姜琴等;《腐蚀与防护》;20130228;第34卷(第2期);第101-106页 * |
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