CN103589281B - A kind of fire-resistant anticorrosion paint based on Graphene and preparation method thereof - Google Patents
A kind of fire-resistant anticorrosion paint based on Graphene and preparation method thereof Download PDFInfo
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Abstract
The present invention relates to a kind of fire-resistant anticorrosion paint based on Graphene and preparation method thereof, this fire-resistant anticorrosion paint is composed of the following components by mass percentage: epoxy resin 5-60%, polyphenylene sulfide 3-30%, aminoresin 3-30%, pigment 1-10%, Graphene 1-20%, propyl carbinol 3-50%, defoamer 0.1-0.3%, poly-hydroxy acid sodium salt 0.1-10%, dibutyl phthalate 0.1-5%, wilkinite 0.5-1.0%, flow agent 0.2-0.5%.Compared with prior art, the coating that the present invention obtains has the advantage such as splendid waterproof anti-corrosion, high temperature resistant, weathering resistance, alkali resistance, shock-resistant and artificial ageing resistance, and preparation method's controllability is good, and simple to operate, production cost is low, is easy to suitability for industrialized production.
Description
Technical field
The present invention relates to a kind of coating and preparation method thereof, especially relate to a kind of fire-resistant anticorrosion paint based on Graphene and preparation method thereof.
Background technology
High-temperature resistant coating is a kind of important coating, is applicable to chimney air flue, high temperature steam pipeline, heat exchanger, High Temperature Furnaces Heating Apparatus, high temperature desulfurizing equipment, petroleum and petrochemical industry cracker, engine parts and vapor pipe anticorrosion.The special fire-resistant anticorrosion paint of other is used widely in space flight and aviation, petroleum and petrochemical industry, metallurgy, electric power, national defence.Since the forties silicone industryization is produced, the high-temperature resistant coating prepared with its product, at high-temperature electric machine, electrical apparatus insulation aspect is widely applied.Such as organosilicon aluminium powder paint is used for the fire-resistant anticorrosion paint of aircraft engine, achieves great achievement, organosilicon glass-ceramic coating, meets the requirement of higher temperature rot-resistant.But due to the bad mechanical property of organosilicon own, sticking power, wear resistance, solvent resistance is low, and waste water and gas is more in producing, contaminate environment, inflammable, simultaneously harmful, therefore, the requirement of modern electrical machine, electrical equipment, aerospace and resistance to Special Medium more and more can not be met.
Graphene is a kind of novel material of the individual layer sheet structure be made up of carbon atom.Be a kind ofly form with sp2 hybridized orbital the flat film that hexangle type is honeycomb lattice by carbon atom, only have the two-dimensional material of a carbon atom thickness.Graphene is the thinnest in the world is at present the hardest nano material also, and it is almost completely transparent, only absorbs the light of 2.3%; Thermal conductivity is up to 5300W/mK, and higher than carbon nanotube and diamond, under normal temperature, its electronic mobility is more than 15000cm
2/ Vs, again than CNT (carbon nano-tube) or silicon wafer height, and resistivity only about 10
-6Ω cm, than copper or silver lower, be the material that at present in the world resistivity is minimum.At present, also report that no matter Graphene is directly prepare on copper or nickel, or transfer on other metals, all can provide anti-corrosion protection.Copper coating cultivates single-layer graphene, adopts chemical Vapor deposition process, and slower than naked copper seven times of corrosion meeting, nickel coating cultivates multi-layer graphene, corrodes slower than naked nickel more than 20 times.Single-layer graphene has identical anti-corrosion protection effect, and just as conventional organic coating, but the latter wants thick more than five times.Graphene coating can be used as desirable anticorrosive coating, because in some field, shallow layer is more favourable, such as micromodule, interconnection products, aircraft components and implanting device etc. are all like this.And Measures compare single-layer graphene being applied to metallic surface is complicated and condition is harsh, not easy to operate.
Chinese patent CN 102702959A discloses a kind of high-temperature-resistant metal anti-corrosive paint of improvement, content is composed of the following components by mass percentage: GHNK high temperature resistant binder 30-40 part, polyaniline/graphene composite material is 15-20 part, tinting pigment is 15-20 part, superfine talcum powder is 5-10 part, ultrafine mica powder is 5-10 part, kaolin is 5-10 part, SN-612 flow agent is 0.2-0.5 part, wetting agent X-405 is 0.3-0.5 part, dimethylethanolamine is 0.1-0.3 part, sanitas 981 is 0.1-0.3 part, GHP101 thickening material is 0.5-1 part, tributyl phosphate is 0.1-0.3 part, water is 4-13 part.The coating that this invention obtains has splendid waterproof anti-corrosion, high temperature resistant, the advantage such as alkali resistance, weathering resistance, scrub resistance and artificial ageing resistance, passivation and the inhibition of metal base can be realized, avoid the use of the heavy metals such as the chromium that can cause environmental pollution simultaneously.But its main component polyaniline/graphene composite material complicated process of preparation, and main what utilize is polyaniline high conductivity, raw material is cheap, be easy to the characteristics such as synthesis, but research shows that the preservative activity that polyaniline and Graphene are not mutually promoted, polyaniline and Graphene do not realize its real effect.
Chinese patent CN 103265881A discloses a kind of fire-resistant anticorrosion paint comprising poly-aryl silicone resin, be made up of according to weight ratio following composition: poly-aryl silicone resin 40 ~ 50 parts, P-hydroxybenzoic acid glycidyl ester 20 ~ 30 parts, acrylic resin 5 ~ 10 parts, mica powder 10 ~ 15 parts, Graphene 10 ~ 15 parts, vinyl acetic monomer 5 ~ 10 parts, thinner 10 ~ 20 parts.Thinner is butanols or dimethylbenzene.The fire-resistant anticorrosion paint made can reach 400 ~ 500 DEG C by tolerable temperature, has good preservative effect simultaneously.Add although this patent take Graphene as main stuffing, but just use the hybrid mode stirred that graphene uniform can not be made to disperse in its preparation method, thus do not have that its size is little, electron transmission speed is fast, good conductivity, hardness advantages of higher, and its not key effect of playing in this coating of explain oneself Graphene.
Summary of the invention
Object of the present invention be exactly in order to overcome above-mentioned prior art exist defect and a kind of fire-resistant anticorrosion paint based on Graphene and preparation method thereof is provided, by adding of Graphene, the high temperature resistant of this protective system and antiseptic property are significantly improved.
Object of the present invention can be achieved through the following technical solutions:
A kind of fire-resistant anticorrosion paint based on Graphene, composed of the following components by mass percentage: epoxy resin 5-60%, polyphenylene sulfide 3-30%, aminoresin 3-30%, pigment 1-10%, Graphene 1-20%, propyl carbinol 3-50%, defoamer 0.1-0.3%, poly-hydroxy acid sodium salt 0.1-10%, dibutyl phthalate 0.1-5%, wilkinite 0.5-1.0%, flow agent 0.2-0.5%.
Further, described epoxy resin is selected from 665 commercially available organosilicon epoxy resins or ES-06 organosilicon epoxy resin.
Further, described aminoresin is selected from the one in 520 commercially available urea-formaldehyde resins, 582 terpolycyantoamino-formaldehyde resins or 576-1 trimeric cyanamide benzene guanamine resin.
Further, described pigment is selected from the one in titanium dioxide, zinc oxide, red iron oxide or phthalocyanine green.
Further, described Graphene is obtained by oxidation reduction process or high temperature reduction method.
Further, described defoamer is selected from tributyl phosphate, polyethers defoamer, silica-type defoamer or methyl-silicone oil.
Further, described polyethers defoamer is selected from the one in commercially available GP type defoamer, GPE type defoamer or GPES type defoamer; Described silica-type defoamer is polysiloxane defoamers.
Further, described poly-hydroxy acid sodium salt is poly-2-hydroxy acid sodium-salt.
Further, described flow agent is selected from the one in silicone oil, polydimethylsiloxane, polyether polyester modified organic silicon oxygen alkane or alkyl-modified organo-siloxane.
Based on a preparation method for the fire-resistant anticorrosion paint of Graphene, the method comprises the following steps:
(1) Graphene, epoxy resin and polyphenylene sulfide are joined in propyl carbinol, ultrasonic agitation 30-180 minute;
(2) aminoresin, pigment, defoamer, poly-hydroxy acid sodium salt, dibutyl phthalate, flow agent are added in shredder by specified amount, be ground to fineness and be less than 30 microns;
(3) 10-120 minute is stirred after material mixing step (1) and step (2) obtained, continue to stir 10-60 minute after adding wilkinite, then at grinding machine for grinding 10-120 minute, filter, obtain the fire-resistant anticorrosion paint based on Graphene, then seal, pack.
Compared with prior art, Graphene, epoxy resin and polyphenylene sulfide join in propyl carbinol by the present invention, ultrasonic agitation 30-180 minute, and join in shredder together with other component and be fully ground to less than 30 microns, make full and uniform the mixing with other component of Graphene, the premium properties of Graphene is not fully exerted.Meanwhile, epoxy resin and polyphenylene sulfide are under the effect of Graphene, and high temperature resistant, erosion resistance strengthens greatly, can reach 700 DEG C by tolerable temperature.Meanwhile, the present invention also has the following advantages and beneficial effect:
(1) the two-dimentional laminated structure of Graphene is layering in coating, defines fine and close physical isolation layer, enhances the antiseptic property of coating;
(2) Graphene size is minimum, and thickness only has a carbon atom thick, can make in its cavity being filled into coating easily and defect, stops and delayed small molecules corrosive medium to invade metallic matrix, enhances the antiseptic property of coating;
(3) thermal conductivity of Graphene is up to 5300W/mK, has very strong thermal conductivity, and the interpolation of Graphene greatly strengthen the high thermal resistance of coating;
(4) under Graphene normal temperature electronic mobility more than 15000cm
2/ Vs, has conductive capability good fast, and the interpolation of Graphene improves the antiseptic power of material;
(5) Graphene has very strong water-repellancy, very poor to the wettability of water, and Graphene can stop water molecules to enter into metal base surface by layer, thus strengthens the antiseptic power of coating;
(6) coating that the present invention obtains has the advantage such as splendid waterproof anti-corrosion, high temperature resistant, weathering resistance, alkali resistance, shock-resistant and artificial ageing resistance;
(7) preparation method's controllability of the present invention is good, simple to operate, and production cost is low, is easy to suitability for industrialized production.
Embodiment
Below in conjunction with specific embodiment, the present invention is described in detail.
Embodiment 1
Each component is equipped with: epoxy resin (665 commercially available organosilicon epoxy resins) 20%, polyphenylene sulfide 20%, aminoresin (520 commercially available urea-formaldehyde resins) 20% by following mass percent, pigment (titanium dioxide) 5%, Graphene 10%, propyl carbinol 14%, defoamer (tributyl phosphate) 0.2%, poly-2-hydroxy acid sodium-salt 6%, dibutyl phthalate 4%, wilkinite 0.5%, flow agent (silicone oil) 0.3%.
The fire-resistant anticorrosion paint based on Graphene is obtained by following steps:
(1) Graphene, epoxy resin and polyphenylene sulfide are joined in propyl carbinol, ultrasonic agitation 150 minutes;
(2) aminoresin, pigment, defoamer, poly-hydroxy acid sodium salt, dibutyl phthalate, flow agent are added in shredder by specified amount, be ground to fineness and be less than 30 microns;
(3) stir 90 minutes after material mixing step (1) and step (2) obtained, continue stirring after adding wilkinite 40 minutes, then grinding machine for grinding 90 minutes, filter, obtain the fire-resistant anticorrosion paint based on Graphene, then seal, pack.
Embodiment 2
Each component is equipped with: epoxy resin (ES-06 organosilicon epoxy resin) 25%, polyphenylene sulfide 25%, aminoresin (582 terpolycyantoamino-formaldehyde resin) 15% by following mass percent, pigment (zinc oxide) 5%, Graphene 10%, propyl carbinol 10%, defoamer (GP type defoamer) 0.2%, poly-hydroxy acid sodium salt 5.5%, dibutyl phthalate 3%, wilkinite 0.8%, flow agent (polydimethylsiloxane) 0.5%.
The fire-resistant anticorrosion paint based on Graphene is obtained by following steps:
(1) Graphene, epoxy resin and polyphenylene sulfide are joined in propyl carbinol, ultrasonic agitation 150 minutes;
(2) aminoresin, pigment, defoamer, poly-hydroxy acid sodium salt, dibutyl phthalate, flow agent are added in shredder by specified amount, be ground to fineness and be less than 30 microns;
(3) stir 90 minutes after material mixing step (1) and step (2) obtained, continue stirring after adding wilkinite 40 minutes, then grinding machine for grinding 90 minutes, filter, obtain the fire-resistant anticorrosion paint based on Graphene, then seal, pack.
Embodiment 3
Each component is equipped with: epoxy resin (ES-06 organosilicon epoxy resin) 40%, polyphenylene sulfide 10%, aminoresin (576-1 trimeric cyanamide benzene guanamine resin) 10% by following mass percent, pigment (red iron oxide) 8%, Graphene 5%, propyl carbinol 20%, defoamer (GPE type defoamer) 0.3%, poly-hydroxy acid sodium salt 3.5%, dibutyl phthalate 2%, wilkinite 0.8%, flow agent (polyether polyester modified organic silicon oxygen alkane) 0.4%.
The fire-resistant anticorrosion paint based on Graphene is obtained by following steps:
(1) Graphene, epoxy resin and polyphenylene sulfide are joined in propyl carbinol, ultrasonic agitation 150 minutes;
(2) aminoresin, pigment, defoamer, poly-hydroxy acid sodium salt, dibutyl phthalate, flow agent are added in shredder by specified amount, be ground to fineness and be less than 30 microns;
(3) stir 90 minutes after material mixing step (1) and step (2) obtained, continue stirring after adding wilkinite 40 minutes, then grinding machine for grinding 90 minutes, filter, obtain the fire-resistant anticorrosion paint based on Graphene, then seal, pack.
Carry out according to GB the performance test of the fire-resistant anticorrosion paint based on Graphene of embodiment 1 ~ 3 gained, test result is in table 1.
The performance of table 1 fire-resistant anticorrosion paint
Embodiment 4
A kind of fire-resistant anticorrosion paint based on Graphene, composed of the following components by mass percentage: epoxy resin (665 commercially available organosilicon epoxy resins) 5%, polyphenylene sulfide 30%, aminoresin (520 commercially available urea-formaldehyde resins) 30%, pigment (phthalocyanine green) 10%, Graphene (being obtained by oxidation reduction process) 20%, propyl carbinol 3%, defoamer (GPES type defoamer) 0.3%, poly-2-hydroxy acid sodium-salt 0.1%, dibutyl phthalate 0.1%, wilkinite 1.0%, flow agent (alkyl-modified organo-siloxane) 0.5%.
Based on a preparation method for the fire-resistant anticorrosion paint of Graphene, the method comprises the following steps:
(1) Graphene, epoxy resin and polyphenylene sulfide are joined in propyl carbinol, ultrasonic agitation 30 minutes; (2) aminoresin, pigment, defoamer, poly-hydroxy acid sodium salt, dibutyl phthalate, flow agent are added in shredder by specified amount, be ground to fineness and be less than 30 microns; (3) stir 10 minutes after material mixing step (1) and step (2) obtained, continue stirring after adding wilkinite 10 minutes, then grinding machine for grinding 10 minutes, filter, obtain the fire-resistant anticorrosion paint based on Graphene, then seal, pack.
Embodiment 5
A kind of fire-resistant anticorrosion paint based on Graphene, composed of the following components by mass percentage: epoxy resin (commercially available ES-06 organosilicon epoxy resin) 60%, polyphenylene sulfide 3%, aminoresin (520 commercially available urea-formaldehyde resins) 3%, pigment (titanium dioxide) 1%, Graphene (being obtained by high temperature reduction method) 1%, propyl carbinol 16.2%, defoamer (polysiloxane defoamers) 0.1%, poly-2-hydroxy acid sodium-salt 10%, dibutyl phthalate 5%, wilkinite 0.5%, flow agent (polyether polyester modified organic silicon oxygen alkane) 0.2%.
Based on a preparation method for the fire-resistant anticorrosion paint of Graphene, the method comprises the following steps:
(1) Graphene, epoxy resin and polyphenylene sulfide are joined in E butanols, ultrasonic agitation 180 minutes; (2) aminoresin, pigment, defoamer, poly-hydroxy acid sodium salt, dibutyl phthalate, flow agent are added in shredder by specified amount, be ground to fineness and be less than 30 microns; (3) stir 120 minutes after material mixing step (1) and step (2) obtained, continue stirring after adding wilkinite 60 minutes, then grinding machine for grinding 120 minutes, filter, obtain the fire-resistant anticorrosion paint based on Graphene, then seal, pack.
Embodiment 6
A kind of fire-resistant anticorrosion paint based on Graphene, composed of the following components by mass percentage: epoxy resin (665 commercially available organosilicon epoxy resins) 10%, polyphenylene sulfide 10%, aminoresin (520 commercially available urea-formaldehyde resins) 10%, pigment (phthalocyanine green) 5%, Graphene (being obtained by oxidation reduction process) 6%, propyl carbinol 50%, defoamer (methyl-silicone oil) 0.2%, poly-2-hydroxy acid sodium-salt 5.8%, dibutyl phthalate 2%, wilkinite 0.7%, flow agent (alkyl-modified organo-siloxane) 0.3%.
Based on a preparation method for the fire-resistant anticorrosion paint of Graphene, the method comprises the following steps:
(1) Graphene, epoxy resin and polyphenylene sulfide are joined in propyl carbinol, ultrasonic agitation 120 minutes; (2) aminoresin, pigment, defoamer, poly-hydroxy acid sodium salt, dibutyl phthalate, flow agent are added in shredder by specified amount, be ground to fineness and be less than 30 microns; (3) stir 60 minutes after material mixing step (1) and step (2) obtained, continue stirring after adding wilkinite 30 minutes, then grinding machine for grinding 60 minutes, filter, obtain the fire-resistant anticorrosion paint based on Graphene, then seal, pack.
Claims (9)
1. the fire-resistant anticorrosion paint based on Graphene, it is characterized in that, composed of the following components by mass percentage: epoxy resin 5-60%, polyphenylene sulfide 3-30%, aminoresin 3-30%, pigment 1-10%, Graphene 1-20%, propyl carbinol 3-50%, defoamer 0.1-0.3%, poly-hydroxy acid sodium salt 0.1-10%, dibutyl phthalate 0.1-5%, wilkinite 0.5-1.0%, flow agent 0.2-0.5%;
Described Graphene is obtained by oxidation reduction process or high temperature reduction method.
2. a kind of fire-resistant anticorrosion paint based on Graphene according to claim 1, is characterized in that, described epoxy resin is selected from 665 commercially available organosilicon epoxy resins or ES-06 organosilicon epoxy resin.
3. a kind of fire-resistant anticorrosion paint based on Graphene according to claim 1, is characterized in that, described aminoresin is selected from the one in 520 commercially available urea-formaldehyde resins, 582 terpolycyantoamino-formaldehyde resins or 576-1 trimeric cyanamide benzene guanamine resin.
4. a kind of fire-resistant anticorrosion paint based on Graphene according to claim 1, it is characterized in that, described pigment is selected from the one in titanium dioxide, zinc oxide, red iron oxide or phthalocyanine green.
5. a kind of fire-resistant anticorrosion paint based on Graphene according to claim 1, is characterized in that, described defoamer is selected from tributyl phosphate, polyethers defoamer, silica-type defoamer or methyl-silicone oil.
6. a kind of fire-resistant anticorrosion paint based on Graphene according to claim 5, is characterized in that, described polyethers defoamer is selected from the one in commercially available GP type defoamer, GPE type defoamer or GPES type defoamer; Described silica-type defoamer is polysiloxane defoamers.
7. a kind of fire-resistant anticorrosion paint based on Graphene according to claim 1, is characterized in that, described poly-hydroxy acid sodium salt is poly-2-hydroxy acid sodium-salt.
8. a kind of fire-resistant anticorrosion paint based on Graphene according to claim 1, is characterized in that, described flow agent is selected from the one in silicone oil, polydimethylsiloxane, polyether polyester modified organic silicon oxygen alkane or alkyl-modified organo-siloxane.
9. a preparation method for the fire-resistant anticorrosion paint based on Graphene as described in as arbitrary in claim 1 ~ 8, it is characterized in that, the method comprises the following steps:
(1) Graphene, epoxy resin and polyphenylene sulfide are joined in propyl carbinol, ultrasonic agitation 30-180 minute;
(2) aminoresin, pigment, defoamer, poly-hydroxy acid sodium salt, dibutyl phthalate, flow agent are added in shredder by specified amount, be ground to fineness and be less than 30 microns;
(3) 10-120 minute is stirred after material mixing step (1) and step (2) obtained, continue to stir 10-60 minute after adding wilkinite, then at grinding machine for grinding 10-120 minute, filter, obtain the fire-resistant anticorrosion paint based on Graphene, then seal, pack.
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| CN100402617C (en) * | 2006-07-12 | 2008-07-16 | 山东省科学院新材料研究所 | Heat resistant anticorrosive composite polyphenylene sulfide epoxy paint and its prepn |
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| CN102702959A (en) * | 2012-06-08 | 2012-10-03 | 冯斌 | Improved high-temperature-resistant metal anti-corrosive paint |
| CN105086758B (en) * | 2013-03-06 | 2017-10-17 | 常州第六元素材料科技股份有限公司 | A kind of preparation method of graphene anticorrosive paint |
| CN103265881A (en) * | 2013-05-30 | 2013-08-28 | 苏州艾特斯环保材料有限公司 | High temperature resistant anticorrosive paint comprising polyaryl organic silicon resin |
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