CN105860616A - Preparation method of flame-retardant corrosion-resistant paint containing nano composite material - Google Patents

Preparation method of flame-retardant corrosion-resistant paint containing nano composite material Download PDF

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Publication number
CN105860616A
CN105860616A CN201610481012.XA CN201610481012A CN105860616A CN 105860616 A CN105860616 A CN 105860616A CN 201610481012 A CN201610481012 A CN 201610481012A CN 105860616 A CN105860616 A CN 105860616A
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preparation
solution
citric acid
nitrate
uio
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项敬来
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    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D1/00—Coating compositions, e.g. paints, varnishes or lacquers, based on inorganic substances
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
    • C09D5/08—Anti-corrosive paints
    • C09D5/10—Anti-corrosive paints containing metal dust
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
    • C09D5/08—Anti-corrosive paints
    • C09D5/10—Anti-corrosive paints containing metal dust
    • C09D5/106—Anti-corrosive paints containing metal dust containing Zn
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
    • C09D5/18—Fireproof paints including high temperature resistant paints
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
    • C09D7/40—Additives
    • C09D7/60—Additives non-macromolecular
    • C09D7/61—Additives non-macromolecular inorganic
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
    • C09D7/40—Additives
    • C09D7/70—Additives characterised by shape, e.g. fibres, flakes or microspheres

Abstract

The invention relates to a preparation method of flame-retardant corrosion-resistant paint containing a nano composite material. Carbon nanotube, nano perovskite oxide and a metal organic framework UIO material are jointly added into layered silicage, so that heat resistance and corrosion resistance of the paint are improved remarkably, aging time of the paint is reduced, long-time non-degradability at high temperature can be maintained, and good flame-retardant effect can be maintained.

Description

A kind of preparation method of the fire-retardant corrosion resistant coating comprising nano composite material
Technical field
The present invention relates to the preparation method of a kind of fire-retardant corrosion resistant coating comprising nano composite material, belong to construction material Field.
Background technology
Anticorrosive paint is a kind of priming paint being provided that cathodic protection, is commonly used to industrial equipment.Steel substrate can be protected, Reducing the risk of corrosion, this coating is with the weatherability of its excellence, solvent resistance, outstanding anticorrosive property and selfreparing merit Can, in the heavy antisepsis fields such as railroad bridge, port and pier, shipping container, obtained large-scale application.
Study general uses inorganic non-metallic corrosion inhibiter or is mixed into additive to replace part zinc particles to improve at present The corrosion resistance of coating, or change zinc particles pattern study it to coating corrupting influence.Additionally, the thickness pair of coating Antiseptic property also has large effect, if in general coating is relatively thin, and the formation crack of zinc oxide, near zinc oxide, add The infiltration of speed electrolyte, is therefore unfavorable for anticorrosion.The most current coating yet suffers from the shortcoming that flame-proof heat-resistant performance is the strongest.
Determine it owing to CNT has preferable one-dimentional structure there is special character, the most excellent mechanics, electricity The character such as, calorifics so that it is hand over justice ambit to show wide application prospect material science, chemistry, physics etc., Add CNT to be modified having broad application prospects to coating.
Summary of the invention
The many deficiencies existed for existing coating, the invention provides a kind of fire-retardant corrosion resistant comprising nano composite material The preparation method of erosion coating, concrete preparation process includes:
(1) phyllosilicate is placed in water, is configured to the mixing suspension that mass fraction is 5%～25%, stir 2h～4h, Then stand 12min～40min, then ultrasonic disperse 0.5h～2h, form uniform suspension；
(2) La is preparedxSr1-xCoO3With UIO-66；
(3) suspension step (1) prepared adds the La that CNT, intercalator and step (2) obtainxSr1-xCoO3With UIO-66, and it is placed in high pressure water heating kettle isothermal reaction 7h～14h under the conditions of 150 DEG C～190 DEG C, naturally cool to room Wen Hou, centrifugal filtration, washing, dry, obtain nano level modified silicate；
(4) the nano level modified silicate that step (3) prepares is joined in deionized water and alcohol mixeding liquid, adjust pH value and arrive 8.5 ~ 9.5, at room temperature, stir 2 ~ 4h, then 20 ~ 50g aluminum zinc powder or zinc-aluminium solution are at room temperature joined above-mentioned solution In, stir 0.5 ~ 2h, products therefrom centrifuge separates, and uses washing with alcohol, in an oven 40 ~ 60 DEG C of drying, obtains described Corrosion resistant coating.
Wherein, nano-perovskite La in step (2)xSr1-xCoO3Preparation method be:
A () weighs Lanthanum (III) nitrate, cobalt nitrate, strontium nitrate and nitric acid in proportion, be dissolved in deionized water, be configured to mixed nitrate molten Liquid, wherein nitric acid: metal ion: the mol ratio of water is (1-4): (2 ~ 4): 70；Separately weigh citric acid to be dissolved in deionized water, join Making citric acid solution, wherein the mol ratio of citric acid and water is (4 ~ 8): 40；
B nitrate solution is heated to 70 ~ 80 DEG C by (), drip citric acid solution under stirring, the citric acid amount of addition and metal from The mol ratio of son is 1:1 ~ 1:2；Nitrate solution and citric acid solution adjust pH value of solution to 7 with strong aqua ammonia after being sufficiently mixed uniformly； Gel is obtained after keeping 2 ~ 3 hours at 75 ~ 80 DEG C；
C () is dried into xerogel gained gel at 90 ~ 100 DEG C, then process 0.5 ~ 1 hour at 350 ~ 400 DEG C, received Rice perovskite oxide La1-XSrXCoO3。
Wherein, in step (2), the preparation method of UIO-66 is: weigh 0.932g ZrC1 respectively4With 1.32 g terephthaldehydes Acid, in polytetrafluoroethylliner liner, adds 24 mL DMF solvent and is dissolved, and is subsequently adding 0.665 mL concentrated hydrochloric acid, and mixing is all Even, supersound process 5 min, inner bag is sealed, puts in baking oven in 120 DEG C of reacting by heating 16h, then reduce the temperature to room temperature, By mixture after reaction is centrifuged, bottom centrifuge tube, obtains white precipitate, be UiO-66.
Wherein, described CNT is SWCN or multi-walled carbon nano-tubes, diameter 1 ~ 100nm, pipe range 5 ~ 500 μ M, purity 99.5wt%.
Wherein, described intercalator is cetyl trimethylammonium bromide, hexadecyltrimethylammonium chloride, diallyl two Any one of ammonio methacrylate.
Wherein, during layered silicate is Kaolin, Vermiculitum, Muscovitum one or more.
Wherein, described zinc-aluminium solution is zinc phosphate or aluminum phosphate solution.
Beneficial effects of the present invention:
Coating is studied by the present invention at the antiseptic property of cold rolling steel matrix, have employed phyllosilicate and CNT Coordinate being modified of intercalator, be prepared for the coating of a kind of high corrosion-resistant, add CNT and can promote inorganic coating pair The adhesive force of metal, improves its interface property, has preferably antiseptic property not only for thicker coating, for relatively thin Coating still can keep the anti-corrosive properties of its excellence.
UiO-66, chemical formula is Zr6O4(OH)4(CO2)12, its structure collapse temperature is higher than 500 DEG C.Stablizing of it Property carrys out the inorganic metal unit Zr of high degree of symmetry6O4(OH)4, and this Zr6Octahedra core and carboxyl oxygen O in part Strong interaction.One Zr6Octahedra core and 12 p-phthalic acid ligands, form tetrahedron and octahedron two kinds The hole cage of type, on eight faces of each octahedra cage, is all connected with a tetrahedron cage, and this connected mode is at three dimensions not Disconnected extension, thus form the MOFs with 6 apertures.Therefore, the present invention using UIO-66 material as composite nano materials, can To improve the resistance to elevated temperatures of coating, thus improve service life.
The present invention uses nano-perovskite oxide LaxSr1-xCoO3(0.6 < x < 1) as inorganic nano flame retardant constituent, Join in coating, due to the addition of nano-perovskite, thus it is possible to vary carrier transfer ways in medium, reduce trap energy Level, makes carrier be prone to along being perpendicular to thickness direction and transports, and effectively inhibits injection and the space electricity of carrier through-thickness Lotus accumulation in medium. semi-conductive layer weakens extra electric field on thickness of sample direction to a certain extent, reduces and partly leads Field intensity at electric layer and interfacial dielectric layer, decreases the space charge amount that negative electrode injects, and after short circuit, in sample, final residual is a small amount of Space charge, reduces the aggregation of electric charge, improves the electricity saving performance of material, improves the aging resistance of coating, resistance to elevated temperatures, Play efficient fire-retardant purpose.
The coating of the present invention, owing to using nano-perovskite oxide material first, utilizes its advantage space structure, and with UIO Material cladding, a part can produce more inorganic nano flame-retardant composition, another part can utilize space vacant with The framing structure of UIO, comprehensive covering of the carbon-forming performance of aggregation thing material, beneficially fire proofing, it is greatly improved fire-retardant Performance.Can be substantially reduced aging, improve high temperature resistant, the use intensity of coating and resistance to fire resistance.
Detailed description of the invention
Below in conjunction with detailed description of the invention, the present invention is further detailed explanation.
Embodiment 1
1) 10g Kaolin is dissolved in 80mL deionized water, high speed machine stirring 1h, ultrasound wave dispersion 1h, is allowed to be formed all Even mixing suspension, makes the abundant imbibition of Kaolin.
2) complex La is prepared0.7Sr0.3CoO3With UIO-66:
A () weighs Lanthanum (III) nitrate, cobalt nitrate, strontium nitrate and nitric acid in proportion, be dissolved in deionized water, be configured to nitrate solution, Wherein nitric acid: metal ion: the mol ratio of water is 1:4:70；Separately weigh citric acid to be dissolved in deionized water, be configured to citric acid Solution, wherein the mol ratio of citric acid and water is 6:40；
B mixed nitrate solution is heated to 70 DEG C by (), drip citric acid solution under stirring, the citric acid amount of addition and metal from The mol ratio of son is 1:1；Nitrate solution and citric acid solution adjust pH value of solution to 7 with strong aqua ammonia after being sufficiently mixed uniformly；80 Gel is obtained after keeping 2 hours at DEG C；
C () is dried into xerogel gained gel at 100 DEG C, then process 1 hour at 400 DEG C, obtain nano-perovskite and urge Agent La0.7Sr0.3CoO3。
D prepared by () UIO-66: weigh 0.932gZrC1 respectively4With 1.32 g p-phthalic acids, in polytetrafluoroethylliner liner In, add 24 mL DMF solvent and dissolved, be subsequently adding 0.665 mL concentrated hydrochloric acid, mix homogeneously, supersound process 5 min, incite somebody to action Inner bag seal, put in baking oven in 120 DEG C of reacting by heating 16h, then reduce the temperature to room temperature, by reaction after mixture from The heart, obtains white precipitate bottom centrifuge tube, is UiO-66.
3) above-mentioned suspension is poured in 100mL tetrafluoro inner bag steel high-pressure water heating kettle, tighten kettle cover, put into constant temperature and dry Case, is slowly added to the mixing suspension of 8g step 1), 3g CNT, continues dispersed with stirring 30min, adds 1.0g cetyl Trimethylammonium bromide, then adds La0.7Sr0.3CoO3With UIO-66 3g altogether, after reacting 12h under the conditions of 160 DEG C, take out water Hot still, centrifugal filtration, washing, dry, obtain nano level modified silicate.
Described CNT is SWCN, diameter 1 ~ 100nm, pipe range 5 ~ 500 μm, and purity 99.5wt% is amorphous Carba < 5%, ash impurity < 3wt%, specific surface area 300 ~ 1000m2/g.
4) in step 3) prepare nano level modified silicate join in deionized water and alcohol mixeding liquid, adjust pH value to 9, At room temperature, stir 2h, then 30g zinc powder is at room temperature joined in above-mentioned solution, stir 2h, products therefrom centrifuge Separate, use washing with alcohol, in an oven 50 DEG C of drying, obtain described fire-retardant corrosion resistant coating.
Embodiment 2
1) silicate in embodiment 1 being adjusted to Vermiculitum, remaining is with embodiment 1.
2) with embodiment 1.
3) with embodiment 1.
4) zinc powder in embodiment 1 is adjusted to aluminum phosphate solution.
Embodiment 3
1) silicate in embodiment 1 being adjusted to Muscovitum, remaining is with embodiment 1.
2) with embodiment 1.
3) cetyl trimethylammonium bromide in embodiment 1 being adjusted to diallyldimethylammonium chloride, remaining is with real Execute example 1.
4) zinc powder in embodiment 1 is adjusted to aluminum phosphate solution.
Comparative example 1
It is added without nano-perovskite LaxSr1-xCoO3, other experiment parameters are with embodiment 1.
Comparative example 2
Being added without UIO material, other experiment parameters are with embodiment 1.
Comparative example 3
Attapulgite is used to replace the La of the present inventionxSr1-xCoO3, other experiment parameters are with embodiment 1.
Concrete detection
Concrete outcome is shown in Table 1.
Each Testing index of coating
1. 2. embodiment 1 3. embodiment 2 4. embodiment 3 5. comparative example 1 6. comparative example 2 7. comparative example 3 8. examination criteria
9. adhesive force 10. 1 grade 11. 1 grades 12. 1 grades 13. 2 grades 14. 2 grades 15. 2 grades 16. GB/T9286-1998
17. hardness 18. H 19. H 20. H 21. HB 22. HB 23. HB 24. GB/T1723-1993
25. viscosity (cps) 26. 23 27. 24 28. 23 29. 24 30. 24 31. 24 32. GB/T1732-1993
33. impact resistances (kg x cm) 34. 55 35. 58 36. 60 37. 42 38. 41 39. 40 40. GB/T9264-2012
41. salt fog resistances (h) 42. 269 43. 281 44. 292 45. 208 46. 207 47. 205 48. GB/T1771-1991
There is the above results it can be seen that CNT, LaxSr1-xCoO3Advantageously reduce with metallic organic framework UIO-66 modification The density of coating, significantly improves the anti-flammability of coating, decay resistance.
The above, the only detailed description of the invention of the present invention, but protection scope of the present invention is not limited thereto, and any Those of ordinary skill in the art in the technical scope that disclosed herein, the change that can expect without creative work or Replace, all should contain within protection scope of the present invention.Therefore, protection scope of the present invention should be limited with claims Fixed protection domain is as the criterion.

Claims (7)

1. the preparation method of the fire-retardant corrosion resistant coating comprising nano composite material, it is characterised in that concrete preparation process Including:
(1) phyllosilicate is placed in water, is configured to the mixing suspension that mass fraction is 5%～25%, stir 2h～4h, Then stand 12min～40min, then ultrasonic disperse 0.5h～2h, form uniform suspension；
(2) La is preparedxSr1-xCoO3With UIO-66；
(3) 8 mass parts suspensions step (1) prepared add CNT 3 mass parts, intercalator 1 mass parts and step (2) La obtainedxSr1-xCoO3With UIO-66 totally 3 mass parts, and it is placed in high pressure water heating kettle in 150 DEG C～190 DEG C of conditions Lower isothermal reaction 7h～14h, after naturally cooling to room temperature, centrifugal filtration, washing, dry, obtain nano level modified silicate；
(4) the nano level modified silicate that step (3) prepares is joined in deionized water and alcohol mixeding liquid, adjust pH value and arrive 8.5 ~ 9.5, at room temperature, stir 2 ~ 4h, then 20 ~ 50g aluminum zinc powder or zinc-aluminium solution are at room temperature joined above-mentioned solution In, stir 0.5 ~ 2h, products therefrom centrifuge separates, and uses washing with alcohol, in an oven 40 ~ 60 DEG C of drying, obtains described Corrosion resistant coating.
2. preparation method as claimed in claim 1, it is characterised in that nano-perovskite La in step (2)xSr1-xCoO3System Preparation Method is:
A () weighs Lanthanum (III) nitrate, cobalt nitrate, strontium nitrate and nitric acid in proportion, be dissolved in deionized water, be configured to mixed nitrate molten Liquid, wherein nitric acid: metal ion: the mol ratio of water is (1-4): (2 ~ 4): 70；Separately weigh citric acid to be dissolved in deionized water, join Making citric acid solution, wherein the mol ratio of citric acid and water is (4 ~ 8): 40；
B nitrate solution is heated to 70 ~ 80 DEG C by (), drip citric acid solution under stirring, the citric acid amount of addition and metal from The mol ratio of son is 1:1 ~ 1:2；Nitrate solution and citric acid solution adjust pH value of solution to 7 with strong aqua ammonia after being sufficiently mixed uniformly； Gel is obtained after keeping 2 ~ 3 hours at 75 ~ 80 DEG C；
C () is dried into xerogel gained gel at 90 ~ 100 DEG C, then process 0.5 ~ 1 hour at 350 ~ 400 DEG C, received Rice perovskite oxide La1-XSrXCoO3。
3. preparation method as claimed in claim 1 or 2, it is characterised in that in step (2), the preparation method of UIO-66 is: point Another name takes 0.932g ZrC14With 1.32 g p-phthalic acids, in polytetrafluoroethylliner liner, add 24 mL DMF solvent by it Dissolve, be subsequently adding 0.665 mL concentrated hydrochloric acid, mix homogeneously, supersound process 5 min, inner bag sealed, puts in baking oven in 120 DEG C reacting by heating 16h, then reduces the temperature to room temperature, by being centrifuged mixture after reaction, obtains white bottom centrifuge tube Precipitation, is UiO-66.
4. preparation method as claimed in claim 1, it is characterised in that described CNT is SWCN or many walls carbon Nanotube, diameter about 1 ~ 100nm, pipe range about 5 ~ 500 μm, purity 99.5wt%.
5. preparation method as claimed in claim 1, it is characterised in that described intercalator be cetyl trimethylammonium bromide, Hexadecyltrimethylammonium chloride, diallyldimethylammonium chloride any one.
6. preparation method as claimed in claim 1, it is characterised in that layered silicate is Kaolin, Vermiculitum, Muscovitum etc. In one or more.
7. preparation method as claimed in claim 1, it is characterised in that described zinc-aluminium solution is zinc phosphate or aluminum phosphate solution.
CN201610481012.XA 2016-06-28 2016-06-28 Preparation method of flame-retardant corrosion-resistant paint containing nano composite material Pending CN105860616A (en)

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CN107578927A (en) * 2017-09-07 2018-01-12 陕西科技大学 A kind of preparation method of polyaniline MOF nano composite material flexible super capacitors
CN110484093A (en) * 2019-08-27 2019-11-22 江苏冠军科技集团股份有限公司 A kind of graphene-perovskite doping corrosion-resistant epoxy paint and preparation method thereof
CN116855162A (en) * 2023-07-11 2023-10-10 江苏天时新材料科技有限公司 Scratch-resistant automobile paint and preparation method thereof

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107578927A (en) * 2017-09-07 2018-01-12 陕西科技大学 A kind of preparation method of polyaniline MOF nano composite material flexible super capacitors
CN107578927B (en) * 2017-09-07 2019-07-09 陕西科技大学 A kind of preparation method of polyaniline MOF nanocomposite flexible super capacitor
CN110484093A (en) * 2019-08-27 2019-11-22 江苏冠军科技集团股份有限公司 A kind of graphene-perovskite doping corrosion-resistant epoxy paint and preparation method thereof
CN116855162A (en) * 2023-07-11 2023-10-10 江苏天时新材料科技有限公司 Scratch-resistant automobile paint and preparation method thereof

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Application publication date: 20160817