CN101418154A - Method for preparing corrosion inhibition anion intercalated layered double hydroxides/oxide composite material and application - Google Patents
Method for preparing corrosion inhibition anion intercalated layered double hydroxides/oxide composite material and application Download PDFInfo
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- CN101418154A CN101418154A CNA2008101375822A CN200810137582A CN101418154A CN 101418154 A CN101418154 A CN 101418154A CN A2008101375822 A CNA2008101375822 A CN A2008101375822A CN 200810137582 A CN200810137582 A CN 200810137582A CN 101418154 A CN101418154 A CN 101418154A
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Abstract
The invention provides a corrosion-inhibiting anionic intercalated hydrotalcite/nano oxide composite material, a preparation method thereof and application of the corrosion-inhibiting anionic intercalated hydrotalcite/nano oxide composite material. The preparation method is as follows: corrosion-inhibiting anions are directly inserted between hydrotalcite layers by the one-step coprecipitation method and the roasting restoring method; the nano oxide is generated by means of in situ synchronization during the process of generation of hydrotalcite crystals by controlling the mixture ratio of divalent metal ions to trivalent metal ions, the pH value of a reaction solution and the reaction temperature; and the corrosion-inhibiting anionic intercalated hydrotalcite/nano oxide composite material with the anti-corrosive function is prepared. The invention is mainly characterized in that the in situ preparation method for the hydrotalcite/oxide composite material provided with a nano lamellar structure improves the release amount of a corrosion inhibitor and reduces the water absorption of a coating by leading into the corrosion inhibitor with the anti-corrosive function and the nano oxide which is generated in situ during the reaction process. The composite material can be used to be pigment of an anti-corrosive metallic coating system, and particularly has potential application value in improving the anti-corrosive performance of a magnesium alloy anti-corrosive coating.
Description
(1) technical field
What the present invention relates to is the preparation method of a kind of inhibiter intercalation houghite/nano-oxide matrix material.The invention still further relates to the anticorrosion application method of this matrix material.
(2) background technology
The corrosion-resistance treatment technology of traditional metal and alloy material thereof contains chromium or heavy non-ferrous metal is dangerous to human body, and development Chrome-free, effective, eco-friendly corrosion protection coating are the problems that domestic and international investigator earnestly studies intensively always in the past few decades.In recent years,, reduce cost, realize anticorrosion, environmental friendliness, attractive in appearance and have a worth especially problem of studying of application system of camouflage function and weather resistance (10 years or longer) with traditional coating process and novel material for strengthening the antiseptic property of metal and alloy thereof.Therefore the exploitation of the packing material of novel anti-corrosion function coating has wide space, should utilize nanometer size effect and dimensional limit effect, takes into account its chemical stability and corrosion resistance again, need consider that simultaneously production technique is simple and easy to do.
The investigator has carried out some fruitful research work in this respect both at home and abroad, and its achievement in research is published in domestic and international important periodical.At home, to be used for steel surface anticorrosion with mixing silane coupling agent in the zinc rich paint for the Ming doctor of the shed of Zhejiang University, prolonged zinc-rich coating the galvanic protection phase (shed is bright, Feng Hai, Ma Xiaochun. corrosion science and guard technology .2005 (17): 237.).The Han Enhou researcher of metal institute of the Chinese Academy of Sciences waits and makes an addition to nano zine oxide in the polyurethane coating in varing proportions, improved the anti-medium osmosis ability of nano-composite coating greatly, and obviously be better than common coating (Yang Lihong, Liu Fuchun, Han Enhou. investigation of materials journal .2006 (20): 354.).Abroad, Dyes Pigments 2007 (75): 687.K.J.Sreeram has successfully synthesized the NaCe of alternative chromate pigments based on the Anticorrosive Character of molybdenum, cerium compound
0.5(MoO
2) crystal.Document Mater.Corros.2001 (52): people such as 896.H.N.McMurray have studied Ce
3+And Ca
2+Cationic polynite is as the anticorrosive protective value of corrosion inhibitor to galvinized steel.From above domestic and international present Research we as can be seen, on the anticorrosion technology of organic coating, obtained a series of achievements that attract people's attention.
Because hydrotalcite has the good interlayer ion interchangeability and the retardancy of laminated structure, in recent years, hydrotalcite has caused people's extensive concern in the research of corrosion-resistant field.Document Scripta Mater.2007 (56): people such as 927.J.K.Lin are first with Mg-Al-CO
3 2-Hydrotalcite is used for the anticorrosive film of magnesium alloy.The present invention proposes the rust inhibition negatively charged ion is introduced hydrotalcite layers, simultaneously, original position generates nano-oxide in the building-up process of hydrotalcite, thereby a kind of rust inhibition anion intercalation hydrotalcite/nano-oxide matrix material with novel anti-corrosion function is provided, and this novel anti-corrosion function coating has good permeability resistance and non-corrosibility.
(3) summary of the invention
The object of the present invention is to provide a kind of by introducing have the inhibiter of anticorrosive effect and in reaction process generated in-situ nano-oxide improve the rust inhibition anion intercalation hydrotalcite/nano-oxide composite material and preparation method thereof of the burst size of inhibiter.The present invention also aims to provide a kind of water-absorbent that reduces coating, especially the antiseptic property that improves the magnesium alloy corrosion protection coating is had the application method of the rust inhibition anion intercalation hydrotalcite/nano-oxide matrix material of potential using value.
The object of the present invention is achieved like this:
The chemical constitution of rust inhibition anion intercalation hydrotalcite/nano-oxide matrix material is M
aO
b/ [M
2+ 1-xM
3+ x(OH)
2]
X+(A)
N- X/nMH
2O; M wherein
2+Representative+divalent metal ion is Mg
2+, Zn
2+, Ni
2+, Ce
2+Or Fe
2+M
3+Representative+3 valence metal ions are Al
3+, Cr
3+, Ce
3+, Fe
3+Or Ti
3+A
N-For having the negatively charged ion of slow release effect, be vanadate, molybdate, tungstate, chromic salt or phosphomolybdate; M
aO
bThe oxide compound of representative+divalent and+3 valence metal ions is based on the oxide compound of+divalent metal ion.
Described M
aO
bThe metal ion of the oxide compound of representative+divalent and+3 valence metal ions is Mg
2+, Zn
2+, Ni
2+Or Fe
3+
Rust inhibition anion intercalation hydrotalcite of the present invention/nano-oxide composite material and preparation method thereof is:
Under the room temperature, according to M
2+/ M
3+Mol ratio is that 2.2～3.5 ratio takes by weighing respectively+the solubility nitrate of divalent metal ion and+3 valence metal ions, is mixed with the 300mL nitrate aqueous solution, wherein M
2+Be Mg
2+, Zn
2+, Ni
2+, Ce
2+, Fe
2+In a kind of, M
3+Be Al
3+, Cr
3+, Ce
3+, Fe
3+, Ti
3+In a kind of, be the sodium salt of intercalant anion with a kind of in vanadate, molybdate, tungstate, chromic salt, the phosphomolybdate, the NaOH wiring solution-forming;
Earlier the sodium salt solution with intercalant anion places container, the pH value of regulator solution, again with nitrate aqueous solution and NaOH solution simultaneously dropwise constant speed join in the container, the pH value scope of controlling suspension is 10.5～11.5, after dropwising, at N
2Protection continues isothermal reaction 10h down, places 12h then under room temperature, filters, and removes CO
2Distilled water wash filter cake to neutrality obtains presoma, and presoma is dry in 80 ℃ of baking ovens, grinds.
Among the preparation method of the present invention with presoma in 80 ℃ of baking ovens before the drying step, earlier with presoma roasting 2～3h in retort furnace, 450～720 ℃ of maturing temperatures are dipped in except that CO after the roasting
2Distilled water, simultaneously dropwise constant speed drips the sodium salt solution and the alkaline solution of intercalant anion, at N
2Protection is reaction 4-10h down, satisfies A
N+/ M
3+Mol ratio is 0.8～1.5, and the pH scope is 8.5～9.5, filters, and removes CO
2The distilled water wash filter cake is to neutral.Described alkaline solution is an ammoniacal liquor.
Rust inhibition anion intercalation hydrotalcite/nano-oxide matrix material makes an addition to by the massfraction of 5%-35% and makes the corrosion protective coating coating that is used for iron and steel, aluminium alloy and magnesium alloy in the Resins, epoxy.
The invention provides a kind of rust inhibition anion intercalation hydrotalcite/nano-oxide matrix material, the preparation method of this matrix material and the application in protective system thereof.Adopt a step coprecipitation method and roasting restoring method directly to insert inhibitor anion in hydrotalcite layers.Proportioning by control divalent-metal ion and trivalent metal ion, the pH value of reaction soln, temperature of reaction is in hydrotalcite crystal generative process, in-situ synchronization generates nano-oxide, thereby preparation has the rust inhibition anion intercalation hydrotalcite/nano-oxide matrix material of anti-corrosion function.The present invention is characterized in: the in-situ preparation method of the hydrotalcite/oxide composite of nano-lamellar structure; The inhibiter that has anticorrosive effect by introducing reaches generated in-situ nano-oxide in reaction process, improves the burst size of inhibiter, reduces the water-absorbent of coating.This matrix material can be used for the pigment as the anticorrosive metal coating system, especially the antiseptic property that improves the magnesium alloy corrosion protection coating is had the potential using value.
(4) description of drawings
Fig. 1 is Zn-Al-MoO
4 2-The XRD figure of/ZnO matrix material.
Fig. 2 is Ni-Al-MoO
4 2-The XRD figure of/NiO matrix material.
Fig. 3 is Zn-Al-MoO
4 2-The transmission electron microscopy pattern picture of/ZnO matrix material and electron diffraction High-Resolution Map.
(5) embodiment
For example the present invention is done in more detail below and describes:
Implement 1: material synthesis method
Example one: the step coprecipitation method preparation of molybdate inhibiter intercalation zinc-aluminium hydrotalcite/nano zine oxide matrix material
Step: take by weighing a certain amount of Zn (NO
3)
26H
2O and Al (NO
3)
39H
2O guarantees Zn/Al=2.2～2.5 (mol ratio), is dissolved in 200mL and removes CO
2Distilled water is as salts solution; Make OH
-/ [Zn
2++ Al
3+The NaOH of]=2.2 (mol ratio) is made into 2M solution, as alkaline solution; Take by weighing a certain amount of Na
2MoO
4.2H
2O makes MoO
4 2-/ Al
3+Mol ratio is 2, is dissolved in 100mL and removes CO
2Move into three-necked bottle behind the distilled water, regulate pH=9～10, stand-by; At water-bath 75-80 ℃, stir down salts solution and alkaline solution dropwise be added drop-wise to Na is housed
2MoO
4In the three-necked bottle of solution, control NaOH pH value remains between 10.0～11.0.Nitrogen protection, heavyization 12h behind the back flow reaction 12h.Suction filtration, is dried in 80 ℃ of loft drier to pH=7.5 with the distilled water wash filter cake, grinds.
Example two: molybdate inhibiter intercalation nickel aluminum hydrotalcite/nano oxidized nickel composite material
Step: as example one preparation Ni-Al-CO
3 2-Hydrotalcite/nano-nickel oxide presoma, 620 ℃ of following roasting 3h.Sample is dipped in except that CO after the roasting
2Distilled water in, simultaneously dropwise constant speed drips Sodium orthomolybdate salts solution and alkaline solution (ammoniacal liquor of dilution), at N
2Protection is reaction 4h down, satisfies MoO
4 2-/ Al
3+Mol ratio is 0.8～1.2, and pH is 9.5.Filter, remove CO
2The distilled water wash filter cake is to neutral, and is dry in 80 ℃ of baking ovens, grinds.
Above examples of implementation are further described technical scheme of the present invention, and still, employed concrete grammar, prescription and explanation are not limitation of the present invention.
Implement 2: the preparation of the matrix material/epoxy coat of magnesium alloy
Step 1: use 800 orders, 1500 order sand paper manual grinding scale removals before the magnesium alloy test piece applying coating successively, acetone clean surface; Pickling 30 seconds.Wherein, the composition of pickle solution is: oxalic acid 10g/L, hydrofluoric acid 5g/L.
Step 2: join in the Resins, epoxy with the certain quality mark through the powder that fully grinds, make thinner with butanols and dimethylbenzene mixed solution and make mother liquor respectively, the certain rotating speed of ball mill disperses; Ultra-sonic dispersion is a solidifying agent with low molecular weight polycaprolactone acyl ammonia 651 again, behind the slaking 2h, is brushing through on the magnesium alloy plate of pre-treatment.Condition of cure is: behind the drying at room temperature 12h, at 60 ℃ of dry 8h, room temperature is placed 7d.
Claims (6)
1, a kind of rust inhibition anion intercalation hydrotalcite/nano-oxide matrix material, it is characterized in that: its chemical constitution is M
aO
b/ [M
2+ 1-xM
3+ x(OH)
2]
X+(A)
N- X/nMH
2O; M wherein
2+Representative+divalent metal ion is Mg
2+, Zn
2+, Ni
2+, Ce
2+Or Fe
2+M
3+Representative+3 valence metal ions are Al
3+, Cr
3+, Ce
3+, Fe
3+Or Ti
3+A
N-For having the negatively charged ion of slow release effect, be vanadate, molybdate, tungstate, chromic salt or phosphomolybdate; M
aO
bThe oxide compound of representative+divalent and+3 valence metal ions is based on the oxide compound of+divalent metal ion.
2, rust inhibition anion intercalation hydrotalcite according to claim 1/nano-oxide matrix material is characterized in that: described M
aO
bThe metal ion of the oxide compound of representative+divalent and+3 valence metal ions is Mg
2+, Zn
2+, Ni
2+Or Fe
3+
3, the preparation method of a kind of rust inhibition anion intercalation hydrotalcite/nano-oxide matrix material is characterized in that:
Under the room temperature, according to M
2+/ M
3+Mol ratio is that 2.2～3.5 ratio takes by weighing respectively+the solubility nitrate of divalent metal ion and+3 valence metal ions, is mixed with the 300mL nitrate aqueous solution, wherein M
2+Be Mg
2+, Zn
2+, Ni
2+, Ce
2+, Fe
2+In a kind of, M
3+Be Al
3+, Cr
3+, Ce
3+, Fe
3+, Ti
3+In a kind of, be the sodium salt of intercalant anion with a kind of in vanadate, molybdate, tungstate, chromic salt, the phosphomolybdate, the NaOH wiring solution-forming;
Earlier the sodium salt solution with intercalant anion places container, the pH value of regulator solution, again with nitrate aqueous solution and NaOH solution simultaneously dropwise constant speed join in the container, the pH value scope of controlling suspension is 10.5～11.5, after dropwising, at N
2Protection continues isothermal reaction 10h down, places 12h then under room temperature, filters, and removes CO
2Distilled water wash filter cake to neutrality obtains presoma, and presoma is dry in 80 ℃ of baking ovens, grinds.
4, the preparation method of rust inhibition anion intercalation hydrotalcite according to claim 3/nano-oxide matrix material, it is characterized in that: with presoma in 80 ℃ of baking ovens before the drying step, earlier with presoma roasting 2～3h in retort furnace, 450～720 ℃ of maturing temperatures are dipped in except that CO after the roasting
2Distilled water, simultaneously dropwise constant speed drips the sodium salt solution and the alkaline solution of intercalant anion, at N
2Protection is reaction 4-10h down, satisfies A
N+/ M
3+Mol ratio is 0.8～1.5, and the pH scope is 8.5～9.5, filters, and removes CO
2The distilled water wash filter cake is to neutral.
5, the preparation method of rust inhibition anion intercalation hydrotalcite according to claim 4/nano-oxide matrix material, it is characterized in that: described alkaline solution is an ammoniacal liquor.
6, the application of a kind of rust inhibition anion intercalation hydrotalcite/nano-oxide matrix material is characterized in that: rust inhibition anion intercalation hydrotalcite/nano-oxide matrix material makes an addition to by the massfraction of 5%-35% and makes the corrosion protective coating coating that is used for iron and steel, aluminium alloy and magnesium alloy in the Resins, epoxy.
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