CN106118146A - The preparation method of the fire-retardant corrosion resistant coating that a kind of nano composite material is modified - Google Patents

The preparation method of the fire-retardant corrosion resistant coating that a kind of nano composite material is modified Download PDF

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CN106118146A
CN106118146A CN201610481188.5A CN201610481188A CN106118146A CN 106118146 A CN106118146 A CN 106118146A CN 201610481188 A CN201610481188 A CN 201610481188A CN 106118146 A CN106118146 A CN 106118146A
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preparation
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coating
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room temperature
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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
    • 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

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  • Chemical & Material Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Wood Science & Technology (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Paints Or Removers (AREA)

Abstract

The present invention relates to the preparation method of the modified fire-retardant corrosion resistant coating of a kind of nano composite material, nano-perovskite oxide and metallic organic framework ZIF material are jointly added in phyllosilicate, significantly improve the thermostability of coating, corrosion resistance, reduce the ageing time of coating, can keep the most non-degradable under high temperature action, and preferable flame retardant effect can also be kept.

Description

The preparation method of the fire-retardant corrosion resistant coating that a kind of nano composite material is modified
Technical field
The present invention relates to the preparation method of the modified fire-retardant corrosion resistant coating of a kind of 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 the fire-retardant corrosion resistant that a kind of nano composite material is modified 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) MTiO is prepared3With ZIF-90, wherein nano-perovskite oxide M TiO3Middle M=Ba, Sr or Ca；
(3) suspension step (1) prepared adds the MTiO that CNT, intercalator and step (2) obtain3With ZIF- 90, 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 temperature After, 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, stirring 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 oxide M TiO3Preparation method be:
0.05-0.5mol/l tetrabutyl titanate is dissolved in 10ml glycol monoethyl ether, ultrasonic disperse, stirs, add 25wt% ammonia, obtains the hydroxide precipitation of titanium, and deionization washs, is subsequently adding KOH aqueous solution, stirs 10-20 minute, mixed Close uniformly, move into hydrothermal crystallizing still, at 140-200 DEG C, react 1-4h, after reaction terminates, washing, it is dried, obtains Nano titanate Template；
In Nano titanate template, drip 15-20mlM (NO3)2Solution and 10-15ml tetramethylammonium hydroxide aqueous solution, stir Mix 2h, after being sufficiently mixed uniformly, then carry out 180-220 DEG C of hydro-thermal reaction 1-4h, cool down precipitation afterwards, the final product obtained Respectively with deionized water, methanol washing.
Wherein, the concretely comprising the following steps of described ZIF-90: by 2.1mmol Zn (NO3)2· 6H2O and 3.0mmol imidazoles-2- Formaldehyde ICA is dissolved in the DMF of 30mL and stirs that the reactant liquor obtained is transferred to volume is 40mL teflon lined Reactor at 100 DEG C, react 18h naturally cool to room temperature.
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.
The application sounds out ZIF-90 material as the material of composite flame-retardant agent, can improve the resistance to elevated temperatures of coating, Thus improve service life.Owing to metal-organic framework materials is the coordination polymer with metal ion as junction point, with phenol When urea formaldehyde material combines, both can utilize compatible on high molecular chemical characters of imidazole skeleton and phenolic resin material in polymer Property, is formed with efficient construction, utilizes the tetrahedral structure can effective dispersion space electric charge, it is to avoid the gathering of space charge, improves resistance to High temperature, ageing-resistant performance；On the other hand, containing metal ion in ZIFS, inorganic compound can be formed, and inorganic compound is such as Nano inorganic magnesium oxide, ferrum oxide etc. are one of fire retardants of this area, can utilize nothing with phenolic resin material after being combined The complementary action of machine material, the charge transport efficiency of further enhanced coating, improves fire resistance, improves the resistance to height of coating Temperature, ageing-resistant performance.
The present invention uses nano-perovskite oxide M TiO first3As inorganic nano flame retardant constituent, join coating In, due to the addition of nano-perovskite, thus it is possible to vary carrier transfer ways in medium, reduce trap level, make current-carrying Son is prone to transport along being perpendicular to thickness direction, effectively inhibits the injection of carrier through-thickness and space charge in medium Accumulation. semi-conductive layer weakens extra electric field on thickness of sample direction to a certain extent, reduces semi-conductive layer and insulation Field intensity at bed boundary, decreases the space charge amount that negative electrode injects, a small amount of space charge of final residual in sample after short circuit, fall The low aggregation of electric charge, improves the electricity saving performance of material, improves the aging resistance of coating, resistance to elevated temperatures, plays efficient Fire-retardant purpose.
The coating of the present invention uses nano-perovskite oxide material, utilizes its advantage space structure, and multiple with ZIF material Closing, a part can produce more inorganic nano flame-retardant composition, and another part can utilize the vacant skeleton knot with UIO in space Structure, comprehensive covering of the carbon-forming performance of aggregation thing material, beneficially fire proofing, fire resistance is greatly improved.Can be big Big reduction is aging, improves 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) BaTiO is prepared3With ZIF-90:
A () prepares Nano titanate template: 0.1mol/l tetrabutyl titanate is dissolved in 10ml glycol monoethyl ether, ultrasonic point Dissipating, stir, add 25% ammonia, obtain the hydroxide precipitation of titanium, deionization washs.It is subsequently adding 1mol/lKOH water-soluble Liquid, stirs 10-20 minute, mix homogeneously, moves into hydrothermal crystallizing still, reacts 1-4h at 140-200 DEG C.After reaction terminates, washing, It is dried, obtains Nano titanate template；
In 2g Nano titanate nano-form, dropping 15ml concentration is the barium nitrate solution of 0.2mol/l and 10ml concentration is The tetramethylammonium hydroxide aqueous solution of 0.1mol/l, stirs 2h, after being sufficiently mixed uniformly, then carries out 180-220 DEG C of hydro-thermal anti- Answer 1-4h, cool down precipitation afterwards.The final product obtained is respectively with deionized water, methanol washing.The BaTiO obtained3Oxide Mean diameter is 45-55nm.
B prepared by () ZIF-90: by Zn (NO3)2 6H2O (2.1mmol) and imidazoles-2-formaldehyde ICA (3.0mmol) are dissolved in The DMF of 30mL stirs and the reactant liquor obtained is transferred to the reactor that volume is 40mL teflon lined exists Reacting 18h at 100 DEG C, to naturally cool to room temperature standby.
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 BaTiO3With ZIF-90 3g altogether, after reacting 12h under the conditions of 160 DEG C, take out water heating kettle, from The heart filters, washing, dries, obtains nano level modified silicate.Described CNT is SWCN, diameter 1 ~ 100nm, Pipe range 5 ~ 500 μm, purity 99.5wt%, 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) by the BaTiO in embodiment 13It is adjusted to SrTiO3, remaining is 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) by the BaTiO in embodiment 13It is adjusted to CaTiO3, remaining is 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 MTiO3, other experiment parameters are with embodiment 1.
Comparative example 2
Being added without ZIF-90 material, other experiment parameters are with embodiment 1.
Comparative example 3
Attapulgite is used to replace the MTiO of the present invention3, 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. 24 27. 25 28. 26 29. 24 30. 23 31. 24 32. GB/T1732-1993
33. impact resistances (kg x cm) 34. 59 35. 58 36. 60 37. 41 38. 41 39. 40 40. GB/T9264-2012
41. salt fog resistances (h) 42. 279 43. 288 44. 292 45. 208 46. 202 47. 201 48. GB/T1771-1991
There is the above results it can be seen that CNT, MTiO3Coating is advantageously reduced with metallic organic framework ZIF-90 modification Density, 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 of a nano composite material modification, 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) nano-perovskite oxide M TiO is prepared3With ZIF-90, wherein nano-perovskite oxide M TiO3Middle M=Ba, Sr or Ca；
(3) in the 8 mass parts suspensions that step (1) prepares, CNT 3 mass parts, intercalator 1 mass parts, step are added (2) MTiO obtained3With ZIF-90 totally 3 mass parts, and it is placed in high pressure water heating kettle under the conditions of 150 DEG C～190 DEG C permanent Temperature 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, stirring 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 oxide M TiO3Preparation method be:
0.05-0.5mol/l tetrabutyl titanate is dissolved in 10ml glycol monoethyl ether, ultrasonic disperse, stirs, add 25wt% ammonia, obtains the hydroxide precipitation of titanium, and deionization washs, is subsequently adding KOH aqueous solution, stirs 10-20 minute, mixed Close uniformly, move into hydrothermal crystallizing still, at 140-200 DEG C, react 1-4h, after reaction terminates, washing, it is dried, obtains Nano titanate Template；
In Nano titanate template, drip 15-20mlM (NO3)2Solution and 10-15ml tetramethylammonium hydroxide aqueous solution, stir Mix 2h, after being sufficiently mixed uniformly, then carry out 180-220 DEG C of hydro-thermal reaction 1-4h, cool down precipitation afterwards, the final product obtained Respectively with deionized water, methanol washing.
3. preparation method as claimed in claim 1 or 2, it is characterised in that described ZIF-90 concretely comprises the following steps: will 2.1mmol Zn(NO3)2· 6H2O and 3.0mmol imidazoles-2-formaldehyde ICA is dissolved in the DMF of 30mL and stirs and will obtain Reactant liquor be transferred to the reactor that volume is 40mL teflon lined and at 100 DEG C, react 18h naturally cool to room Temperature.
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.
CN201610481188.5A 2016-06-28 2016-06-28 The preparation method of the fire-retardant corrosion resistant coating that a kind of nano composite material is modified Pending CN106118146A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113861433A (en) * 2021-09-06 2021-12-31 浙大宁波理工学院 Synergistic flame retardant and preparation method and application thereof
CN114181550A (en) * 2021-12-31 2022-03-15 苏州软石智能装备有限公司 Preparation and application method of ultrahigh temperature and humidity sensor

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102139914A (en) * 2011-04-20 2011-08-03 浙江大学 Method for preparing calcium titanate nanoparticles
CN103044463A (en) * 2012-12-12 2013-04-17 中国科学院宁波材料技术与工程研究所 Method for high-efficiency preparing zeolite imidazole metal organic frame ZIF-90
CN104212270A (en) * 2014-09-19 2014-12-17 江苏海晟涂料有限公司 Inorganic electrostatic electricity-conductive rust removal antiseptic paint and preparation method thereof
CN105017965A (en) * 2015-08-21 2015-11-04 朱蕾 Preparation method of carbon nanotube-montmorillonite-silicone modified zinc-rich paint with corrosion resistance

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102139914A (en) * 2011-04-20 2011-08-03 浙江大学 Method for preparing calcium titanate nanoparticles
CN103044463A (en) * 2012-12-12 2013-04-17 中国科学院宁波材料技术与工程研究所 Method for high-efficiency preparing zeolite imidazole metal organic frame ZIF-90
CN104212270A (en) * 2014-09-19 2014-12-17 江苏海晟涂料有限公司 Inorganic electrostatic electricity-conductive rust removal antiseptic paint and preparation method thereof
CN105017965A (en) * 2015-08-21 2015-11-04 朱蕾 Preparation method of carbon nanotube-montmorillonite-silicone modified zinc-rich paint with corrosion resistance

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113861433A (en) * 2021-09-06 2021-12-31 浙大宁波理工学院 Synergistic flame retardant and preparation method and application thereof
CN114181550A (en) * 2021-12-31 2022-03-15 苏州软石智能装备有限公司 Preparation and application method of ultrahigh temperature and humidity sensor

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Application publication date: 20161116