CN105017965A - Preparation method of carbon nanotube-montmorillonite-silicone modified zinc-rich paint with corrosion resistance - Google Patents
Preparation method of carbon nanotube-montmorillonite-silicone modified zinc-rich paint with corrosion resistance Download PDFInfo
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- CN105017965A CN105017965A CN201510516882.1A CN201510516882A CN105017965A CN 105017965 A CN105017965 A CN 105017965A CN 201510516882 A CN201510516882 A CN 201510516882A CN 105017965 A CN105017965 A CN 105017965A
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Abstract
The invention relates to a preparation method of carbon nanotube-montmorillonite-silicone modified zinc-rich paint with corrosion resistance. The preparation method comprises the following steps: deionized water, Na-montmorillonite and carbon nanotubes are added, stirred and dispersed, a cation intercalation agent is added, the montmorillonite and the carbon nanotubes are intercalated in an aqueous phase, the mixture is subjected to ultrasonic processing, centrifugal filtration, washing and drying, and a cation modified montmorillonite A is obtained; organosilane is dissolved in a deionized water and ethanol mixed solution, the solution is stirred, zinc powder is added to the solution at the room temperature, and the solution is stirred for 0.5-2 h; the cation modified montmorillonite A is added, stirring is performed continuously, a product is separated by a centrifuge, is washed with ethanol and is dried in an oven at the temperature of 40-60 DEG C, and the carbon nanotube-montmorillonite-silicone modified zinc-rich paint with corrosion resistance is obtained. The carbon nanotube-montmorillonite-silicone modified zinc-rich paint is widely applied to the heavy corrosion-resistant fields such as a railroad bridge, a port wharf, a ship container and the like.
Description
Technical field
The present invention relates to a kind of preparation method of zinc-rich paint, particularly carbon nanotube-polynite-organic-silicon-modified corrosion-resistant zinc-rich paint preparation method.
Background technology
Zinc-rich paint is a kind of priming paint that can provide galvanic protection, is usually applied to industrial equipments.Steel substrate can be protected; reduce the risk of corrosion; inorganic zinc coating is with the weathering resistance of its excellence, thermotolerance, solvent resistance, and especially outstanding non-corrosibility and self-repair function, obtain large-scale application in the heavy antisepsis fields such as railroad bridge, port and pier, shipping container.
Can realize cathode protecting function normally in order to ensure coating, must contain the metallic zinc of sufficient amount in coating, if content is too low, its barrier propterty is not that galvanic protection determines, corrosion protection performance can be caused so greatly to reduce.For water-borne coatings normally dry film water-borne coatings weight more than 75%, solvent based coating is more than 82%, now the essential factor of its antiseptic power of electrical effect, and the size of zinc particles and pattern shadow are larger on the impact of its antiseptic property.
Current study general adopts inorganic non-metallic inhibiter or is mixed into additive to replace part zinc particles to improve the erosion resistance of coating, or the pattern changing zinc particles studies it to coating corrupting influence.But but study less for the surface modification of zinc particles merely.In addition, the thickness of coating also has larger impact to antiseptic property, if in general coating is thinner, the formation crack of zinc oxide, near zinc oxide, accelerates electrolytical infiltration, be therefore unfavorable for anticorrosion.
Summary of the invention
This patent is studied have studied the antiseptic property of zinc paint at cold rolling steel matrix, what have employed that polynite and carbon nanotube coordinate organosilicon to zinc powder carries out surface modification, prepare a kind of zinc-rich paint of high anti-corrosion, can promote that organic coating is to the sticking power of metal, stabilize the surface energy of zinc particles, improve its interface property, not only for thicker coating, there is preferably antiseptic property, still can keep the preservative property of its excellence for thinner coating.
Present invention employs following technical scheme.
Carbon nanotube-polynite-organic-silicon-modified corrosion-resistant zinc-rich paint preparation method, is characterized in that:
(1) in there-necked flask, 150 ~ 400g deionized water is added, stir, slowly add 2 ~ 10g sodium-based montmorillonite and carbon nanotube 3g, continue dispersed with stirring 30min, add 0.5 ~ 1.5g cation-intercalated dose of intercalated montmorillonite in aqueous phase, 4 ~ 6h is reacted at 60 ~ 95 DEG C of temperature, supersound process 0.5 ~ 2h, centrifuging, washing, dry, obtain cation-modified polynite A;
(2) in the deionized water 0.8 ~ 2.0g organosilane being dissolved in 150 ~ 400g weight ratio 1:9 and alcohol mixeding liquid, adjusted to ph, to 8.5 ~ 9.5, at room temperature, stirs 2 ~ 4h, then 20 ~ 50g zinc powder is at room temperature joined in above-mentioned solution, stir 0.5 ~ 2h.Then add the cation-modified polynite A of the 1 ~ 5g of above-mentioned (1), continue stirring 2 ~ 4h, products therefrom whizzer is separated, and adopts washing with alcohol, in an oven 40 ~ 60 DEG C of oven dry, obtains carbon nanotube-polynite-organic-silicon-modified corrosion-resistant zinc-rich paint;
Carbon nanotube is Single Walled Carbon Nanotube, diameter 1 ~ 100nm, pipe range 5 ~ 500 μm, purity 99.5wt%, and decolorizing carbon is mixed <5%, ash impurity <3wt%, specific surface area 300 ~ 1000m
2/ g; Cation-intercalated dose of polynite be cetyl trimethylammonium bromide, palmityl trimethyl ammonium chloride, diallyldimethylammonium chloride, two (1, the 3-dithiole-2-thioketones-4.5-sulfo-diene) aurate of octadecyl ester alkyl dimethyl ammonium chloride any one; Organosilane be n-propyl triethoxyl silane, APTES, two (3-trimethoxy-silylpropyl) amine any one; Zinc Particles Morphology is spherical, is of a size of 1 ~ 5 μm.
Embodiment
the present invention is further illustrated below in conjunction with example.
Example one
(1) in there-necked flask, 200g deionized water is added, stir, slowly add 8g sodium-based montmorillonite and carbon nanotube 3g, continue dispersed with stirring 30min, add 1.0g cetyl trimethylammonium bromide, at 90 DEG C of temperature, react 4h, supersound process 0.5h, centrifuging, washing, dries, obtain cation-modified polynite A, described carbon nanotube is Single Walled Carbon Nanotube, diameter 1 ~ 100nm, pipe range 5 ~ 500 μm, purity 99.5wt%, decolorizing carbon is mixed <5%, ash impurity <3wt%, specific surface area 300 ~ 1000m
2/ g;
(2) in deionized water 1.2g n-propyl triethoxyl silane being dissolved in 250g weight ratio 1:9 and alcohol mixeding liquid, adjusted to ph is to 9.0, at room temperature, stir 2h, then by 20g zinc powder, (Zinc Particles Morphology is spherical, be of a size of 1 ~ 5 μm) at room temperature join in above-mentioned solution, the cation-modified polynite A of 1g is added after stirring 1.5h, stir 2h again, gained zinc powder whizzer is separated, adopt ethanol 60ml repetitive scrubbing, 50 DEG C of oven dry in an oven, obtain carbon nanotube-polynite-organic-silicon-modified corrosion-resistant zinc-rich paint.
Example two
(1) in there-necked flask, 400g deionized water is added, stir, slowly add 10g sodium-based montmorillonite and carbon nanotube 3g, continue dispersed with stirring 30min, add 1.5g palmityl trimethyl ammonium chloride, at 95 DEG C of temperature, react 3h, supersound process 1h, centrifuging, washing, dries, obtain cation-modified polynite A, described carbon nanotube is Single Walled Carbon Nanotube, diameter 1 ~ 100nm, pipe range 5 ~ 500 μm, purity 99.5wt%, decolorizing carbon is mixed <5%, ash impurity <3wt%, specific surface area 300 ~ 1000m
2/ g;
(2) in the deionized water two (3-trimethoxy-silylpropyl) amine 2g being dissolved in 400g weight ratio 1:9 and alcohol mixeding liquid, adjusted to ph is to 9.5, at room temperature, stir 2h, then by 45g zinc powder, (Zinc Particles Morphology is spherical, be of a size of 1 ~ 5 μm) at room temperature join in above-mentioned solution, stir 2h, then the cation-modified polynite A of 5g is added, continue to stir 4h, modified zinc powder whizzer is separated, adopt ethanol 70ml washing, products therefrom is 60 DEG C of oven dry in an oven, obtain carbon nanotube-polynite-organic-silicon-modified corrosion-resistant zinc-rich paint.
Example three
(1) in there-necked flask, 150g deionized water is added, stir, slowly add 2.5g sodium-based montmorillonite and carbon nanotube 3g, continue dispersed with stirring 30min, add 1.2g diallyldimethylammonium chloride, at 85 DEG C of temperature, react 2.5h, supersound process 0.5h, centrifuging, washing, dries, obtain cation-modified polynite A, described carbon nanotube is Single Walled Carbon Nanotube, diameter 1 ~ 100nm, pipe range 5 ~ 500 μm, purity 99.5wt%, decolorizing carbon is mixed <5%, ash impurity <3wt%, specific surface area 300 ~ 1000m
2/ g;
(2) in deionized water 0.8g n-propyl triethoxyl silane being dissolved in 180g weight ratio 1:9 and alcohol mixeding liquid, adjusted to ph is to 9.5, at room temperature, stir 1h, then by 25g zinc powder, (Zinc Particles Morphology is spherical, be of a size of 1 ~ 5 μm) at room temperature join in above-mentioned solution, stir 2.5h, then the cation-modified polynite A of 1.5g is added, continue to stir 2.5h, products therefrom whizzer is separated, and adopts 80ml ethanol repetitive scrubbing, 60 DEG C of oven dry in an oven, obtain carbon nanotube-polynite-organic-silicon-modified corrosion-resistant zinc-rich paint.
Example four
(1) in there-necked flask, 300g deionized water is added, stir, slowly add 6g sodium-based montmorillonite and carbon nanotube 3g, continue dispersed with stirring 30min, add 0.8 g palmityl trimethyl ammonium chloride and EDTA-2K 0.4g, 1.5h is reacted at 80 DEG C of temperature, supersound process 0.5h, centrifuging, washing, dry, obtain cation-modified polynite A, described carbon nanotube is Single Walled Carbon Nanotube, diameter 1 ~ 100nm, pipe range 5 ~ 500 μm, purity 99.5wt%, decolorizing carbon is mixed <5%, ash impurity <3wt%, specific surface area 300 ~ 1000m
2/ g,
(2) in deionized water APTES 1.5g being dissolved in 350g weight ratio 1:9 and alcohol mixeding liquid, adjusted to ph is to 8.5, at room temperature, stir 3h, then by 45g zinc powder, (Zinc Particles Morphology is spherical, be of a size of 1 ~ 5 μm) at room temperature join in above-mentioned solution, stir 3.5h, then the cation-modified polynite A of 4.5g is added, continue to stir 3.5h, products therefrom whizzer is separated, adopt 80ml ethanol repetitive scrubbing, 55 DEG C of oven dry in an oven, obtain carbon nanotube-polynite-organic-silicon-modified corrosion-resistant zinc-rich paint.
Example five
(1) in there-necked flask, 250g deionized water is added, stir, slowly add 6g sodium-based montmorillonite and carbon nanotube 3g, continue dispersed with stirring 30min, add 1g octadecyl ester alkyl dimethyl ammonium chloride two (1, 3-dithiole-2-thioketones-4.5-sulfo-diene) aurate, 5h is reacted at 90 DEG C of temperature, supersound process 2h, centrifuging, washing, dry, obtain cation-modified polynite A, described carbon nanotube is Single Walled Carbon Nanotube, diameter 1 ~ 100nm, pipe range 5 ~ 500 μm, purity 99.5wt%, decolorizing carbon is mixed <5%, ash impurity <3wt%, specific surface area 300 ~ 1000m
2/ g,
(2) in deionized water APTES 1.2g being dissolved in 300g weight ratio 1:9 and alcohol mixeding liquid, adjusted to ph is to 9, at room temperature, stir 4h, then by 40g zinc powder, (Zinc Particles Morphology is spherical, be of a size of 1 ~ 5 μm) at room temperature join in above-mentioned solution, stir 4h, then the cation-modified polynite A of 4g is added, continue to stir 3h, products therefrom whizzer is separated, and adopts 90ml ethanol repetitive scrubbing, 50 DEG C of oven dry in an oven, obtain carbon nanotube-polynite-organic-silicon-modified corrosion-resistant zinc-rich paint.
Beneficial effect of the present invention is further illustrated below by relevant experimental data:
Carbon nanotube-polynite prepared by the present invention four-organic-silicon-modified corrosion-resistant zinc-rich paint is applied in conventional zinc-rich paint formula (see table 1), and coating is coated on cold-rolled steel sheet.Sample is immersed in 48h in 4% sodium chloride solution, and rear employing electrochemical impedance spectroscopy detects the erosion resistance of coating.Experimental result shows compared with the zinc particles of non-modified, and after zinc-rich paint coating prepared by montmorillonite/organic modified Zn particle, no matter thickness coating all has good erosion resistance.The current potential of zinc-rich paint layer is respectively about-900mV, can be used as anode coating and shields to steel substrate, and static Corrosion Protection comparatively cold-rolled steel sheet raising 59%, salt spray resistance 800h performance also increases considerably (the results are shown in Table 2).
Table 1 zinc-rich paint basic recipe
| Raw material | Quality (g) |
| Modified Zn particle | 51 |
| Polyester | 22 |
| Epoxy resin | 4.5 |
| Solidifying agent | 3.5 |
| Catalyzer | 0.3 |
| Solvent | 28.7 |
Table 2 cold-reduced sheet, spelter coating plate salt spray resistance 800h performance comparison
| Cold-reduced sheet (not adding zinc-rich paint) | Zinc-rich paint laminate | |
| One-sided expansion erosion width/mm | 2 | 5 |
| Expand the erosion degree of depth/mm | Corrosion failure | 52 |
Claims (5)
1. carbon nanotube-polynite-organic-silicon-modified corrosion-resistant zinc-rich paint preparation method, is characterized in that:
(1) in there-necked flask, 150 ~ 400g deionized water is added, stir, slowly add 2 ~ 10g sodium-based montmorillonite and carbon nanotube 3g, continue dispersed with stirring 30min, add 0.5 ~ 1.5g cation-intercalated dose of intercalated montmorillonite in aqueous phase, 4 ~ 6h is reacted at 60 ~ 95 DEG C, supersound process 0.5 ~ 2h, centrifuging, washing, dry, obtain cation-modified polynite A;
(2) in the deionized water 0.8 ~ 2.0g organosilane being dissolved in 150 ~ 400g weight ratio 1:9 and alcohol mixeding liquid, adjusted to ph is to 8.5 ~ 9.5, at room temperature, stir 2 ~ 4h, then 20 ~ 50g zinc powder is at room temperature joined in above-mentioned solution, stir 0.5 ~ 2h, then the cation-modified polynite A of the 1 ~ 5g of above-mentioned (1) is added, continue stirring 2 ~ 4h, products therefrom whizzer is separated, adopt washing with alcohol, in an oven 40 ~ 60 DEG C of oven dry, obtain carbon nanotube-polynite-organic-silicon-modified corrosion-resistant zinc-rich paint.
2. carbon nanotube-polynite-organic-silicon-modified corrosion-resistant zinc-rich paint preparation method as claimed in claim 1, it is characterized in that, described carbon nanotube is Single Walled Carbon Nanotube, diameter 1 ~ 100nm, pipe range 5 ~ 500 μm, purity 99.5wt%, decolorizing carbon is mixed <5%, ash impurity <3wt%, specific surface area 300 ~ 1000m
2/ g.
3. carbon nanotube-polynite-organic-silicon-modified corrosion-resistant zinc-rich paint preparation method as claimed in claim 1, it is characterized in that, cation-intercalated dose of polynite be cetyl trimethylammonium bromide, palmityl trimethyl ammonium chloride, diallyldimethylammonium chloride, two (1, the 3-dithiole-2-thioketones-4.5-sulfo-diene) aurate of octadecyl ester alkyl dimethyl ammonium chloride any one.
4. carbon nanotube-polynite-organic-silicon-modified corrosion-resistant zinc-rich paint preparation method as claimed in claim 1, it is characterized in that, organosilane be n-propyl triethoxyl silane, APTES, two (3-trimethoxy-silylpropyl) amine any one.
5. carbon nanotube-polynite-organic-silicon-modified corrosion-resistant zinc-rich paint preparation method as claimed in claim 1, it is characterized in that, Zinc Particles Morphology is spherical, is of a size of 1 ~ 5 μm.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105860616A (en) * | 2016-06-28 | 2016-08-17 | 项敬来 | Preparation method of flame-retardant corrosion-resistant paint containing nano composite material |
| CN105949832A (en) * | 2016-07-20 | 2016-09-21 | 张哲夫 | Modified graphene containing inflaming-retarding corrosion-resisting coating |
| CN106118146A (en) * | 2016-06-28 | 2016-11-16 | 项敬来 | The preparation method of the fire-retardant corrosion resistant coating that a kind of nano composite material is modified |
| CN106189455A (en) * | 2016-07-20 | 2016-12-07 | 张哲夫 | A kind of preparation method of the fire-retardant corrosion resistant coating comprising modified graphene |
| CN112974799A (en) * | 2021-02-05 | 2021-06-18 | 中国人民解放军陆军装甲兵学院 | Composite powder for preparing self-repairing coating, preparation method of composite powder, titanium-based wear-resistant self-repairing coating and preparation method of titanium-based wear-resistant self-repairing coating |
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2015
- 2015-08-21 CN CN201510516882.1A patent/CN105017965A/en active Pending
Non-Patent Citations (1)
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| 于海鹏等: "《木质建材微环境设计》", 30 June 2009 * |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105860616A (en) * | 2016-06-28 | 2016-08-17 | 项敬来 | Preparation method of flame-retardant corrosion-resistant paint containing nano composite material |
| CN106118146A (en) * | 2016-06-28 | 2016-11-16 | 项敬来 | The preparation method of the fire-retardant corrosion resistant coating that a kind of nano composite material is modified |
| CN105949832A (en) * | 2016-07-20 | 2016-09-21 | 张哲夫 | Modified graphene containing inflaming-retarding corrosion-resisting coating |
| CN106189455A (en) * | 2016-07-20 | 2016-12-07 | 张哲夫 | A kind of preparation method of the fire-retardant corrosion resistant coating comprising modified graphene |
| CN112974799A (en) * | 2021-02-05 | 2021-06-18 | 中国人民解放军陆军装甲兵学院 | Composite powder for preparing self-repairing coating, preparation method of composite powder, titanium-based wear-resistant self-repairing coating and preparation method of titanium-based wear-resistant self-repairing coating |
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