CN105482645A - Anticorrosive polyaniline/silicon carbide/graphene composite coating and preparation method thereof - Google Patents
Anticorrosive polyaniline/silicon carbide/graphene composite coating and preparation method thereof Download PDFInfo
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Abstract
The invention discloses an anticorrosive polyaniline/silicon carbide/graphene composite coating and a preparation method thereof. Polyaniline and silicon carbide nanoparticles are composited through on-site polymerization firstly, then a polyaniline/silicon carbide material is coated with graphene oxide through electrostatic self-assembly, and a polyaniline/silicon carbide/graphene composite material is obtained through hydrazine hydrate reduction. Then the polyaniline/silicon carbide/graphene composite material is added to a solvent containing epoxy resin, a curing agent, a plasticizer and an antifoaming agent are added, and the anticorrosive polyaniline/silicon carbide/graphene composite coating is obtained finally. The adopted polyaniline and graphene have good electrical conductivity and can have an anticorrosive effect; silicon carbide is high in hardness and thermal stability and used for enhancing the coating performance. The prepared coating has excellent anticorrosive performance, the production process is mature and simple to operate, no complex equipment is required, and large-scale industrial production is facilitated.
Description
Technical field
The present invention relates to a kind of protective system, particularly relate to a kind of polyaniline/silicon carbide/Graphene composite anticorrosion coating and preparation method thereof, belong to advanced composite material and field of functional coatings.
Background technology
Metallic corrosion is that metallic substance is subject to surrounding environment effect that chemistry or electrochemical reaction occur, thus the phenomenon causing metallic substance performance destroyed.Therefore even stop metallic corrosion to reduce, people adopt cathode protection method, coating to protect metal.At present one of the most common, the most convenient, most effective means applies one deck anticorrosive coating, and isolated external environment contacts with metallic surface, thus reaches the object of anti-corrosion of metal.Growing for protective system demand in fields such as petroleum industry, power industry and capital constructions at present.
The polyaniline of one of conducting polymer, as a kind of novel anticorrosion material, can improve metal corrosion potential, the electronics formed in conduction corrosion process, hinders electronics to oxidizing substance transmission, forms passivation layer, slow down corrosion of metal in metallic surface.Graphene is two-dimensional material the thinnest in the world at present, and its Heat stability is good, excellent electric conductivity, hardness advantages of higher make it can be applied in coating.Chinese invention patent application CN102604533A and CN104910752A discloses protective system based on polyaniline and graphene composite material and preparation method.Two inventions all think that Graphene is conducive to improving paint film physical preservation performance, and load can provide electrochemical anti-corrosive at the polyaniline of Graphene, and the synergy of the two makes this coating have good anti-corrosion of metal performance.But in above-mentioned patent, Graphene is not further processed, it easily reunites in dispersion process, the heavy stacking performance affecting self performance.These coating are in routine use process on the other hand, and various frictional wear inevitably occurs, and cause the destruction of metal substrate surface coating and come off.Therefore existing protective system effect is general, is necessary very much to develop a kind of new anti-corrosion coating.
Summary of the invention
The object of the present invention is to provide and a kind of there is polyaniline/silicon carbide/Graphene composite anticorrosion coating of physics and electrochemistry dual anticorrosion, good physical performance, high comprehensive performance and preparation method thereof.
To achieve these goals, technical scheme of the present invention is: a kind of polyaniline/silicon carbide/Graphene composite anticorrosion coating, is made up of following component,
Epoxy resin 40-60, polyaniline/silicon carbide/graphene composite material 5-10, solidifying agent 10-30, softening agent 1-5, defoamer 1-5, solvent 20-40, by mass percentage.
By such scheme, the preparation method of described polyaniline/silicon carbide/graphene composite material is:
1) add in sodium dodecyl benzene sulfonate aqueous solution by 0.5-1g silicon carbide, add aniline, be uniformly mixed at 0-4 DEG C after ultrasonic disperse 5-30 minute, Sodium dodecylbenzene sulfonate concentration is 20-50mg/mL, and concentration of aniline is 0.1-0.5mol/L;
2) configure the aqueous solution containing oxygenant of pH=1-4, be cooled to 0-4 DEG C, described oxygenant is iron(ic) chloride, iron nitrate or ammonium persulphate, and the mol ratio of oxygenant and aniline is 3:1-1:2;
3) by step 1) with step 2) solution mix, stirring reaction 4-12 hour at 0-4 DEG C, filters, washing, dry, obtains polyaniline/composite material of silicon carbide;
4) polyaniline/composite material of silicon carbide is dispersed in water, preparation polyaniline/composite material of silicon carbide weight content is the suspension of 0.5-10%, suspension is under agitation added drop-wise to the graphene oxide water solution that concentration is 0.5-5mg/mL, is added dropwise to complete rear filtration, be drying to obtain the coated polyaniline/carbofrax material of graphene oxide;
5) coated for graphene oxide polyaniline/carbofrax material is placed in hydrazine hydrate, reduction reaction 12-24 hour at 70-95 DEG C, filtration, washing, drying, obtain polyaniline/silicon carbide/graphene composite material.
The preparation method of described polyaniline/silicon carbide/Graphene composite anticorrosion coating, is characterized in that:
1) add in sodium dodecyl benzene sulfonate aqueous solution by 0.5-1g silicon carbide, add aniline, be uniformly mixed at 0-4 DEG C after ultrasonic disperse 5-30 minute, Sodium dodecylbenzene sulfonate concentration is 20-50mg/mL, and concentration of aniline is 0.1-0.5mol/L;
2) configure the aqueous solution containing oxygenant of pH=1-4, be cooled to 0-4 DEG C, described oxygenant is iron(ic) chloride, iron nitrate or ammonium persulphate, and the mol ratio of oxygenant and aniline is 3:1-1:2;
3) by step 1) with step 2) solution mix, stirring reaction 4-12 hour at 0-4 DEG C, filters, washing, dry, obtains polyaniline/composite material of silicon carbide;
4) polyaniline/composite material of silicon carbide is dispersed in water, preparation polyaniline/composite material of silicon carbide weight content is the suspension of 0.5-10%, suspension is under agitation added drop-wise to the graphene oxide water solution that concentration is 0.5-5mg/mL, is added dropwise to complete rear filtration, be drying to obtain the coated polyaniline/carbofrax material of graphene oxide;
5) coated for graphene oxide polyaniline/carbofrax material is placed in hydrazine hydrate, reduction reaction 12-24 hour at 70-95 DEG C, filtration, washing, drying, obtain polyaniline/silicon carbide/graphene composite material;
6) polyaniline/silicon carbide/graphene composite material is added in the solvent containing epoxy resin, dispersed with stirring is even, and then stir 10-30 minute again after adding solidifying agent, softening agent and defoamer, obtain polyaniline/silicon carbide/Graphene composite anticorrosion coating.
By such scheme, described epoxy resin is epoxy resin E51, epoxy resin E44, epoxy resin E42, epoxy resin E35 or epoxy resin E31.
By such scheme, described solidifying agent is polyamide curing agent or polyetheramine solidifying agent.
By such scheme, described softening agent is dibutyl phthalate or dioctyl phthalate (DOP).
By such scheme, described defoamer is fluorosilicone class Airex931, fluorosilicone class Airex932 or organic modified polyorganosiloxane Airex962.
By such scheme, described solvent be toluene, dimethylbenzene, propyl carbinol or N ?methyl-2-pyrrolidone.
Compared with prior art, the present invention has following outstanding effect:
1) sodium dodecyl benzene sulfonate aqueous solution is conducive to the dispersion of silicon carbide, thus realizes the effective embedding of polyaniline to silicon carbide; 2) aniline group of polyaniline/carbon/silicon carbide composite material surface presents positive polarity, assembling can be conigenous with issuing at electrostatic interaction with electronegative graphene oxide, realize graphene oxide and be tightly coated on polyaniline/carbon/silicon carbide composite material surface, obtain polyaniline/silicon carbide/graphene composite material after final reduction, solve the difficult problem that Graphene is difficult to process dispersion in matrix material preparation; 3) polyaniline in matrix material and Graphene have good electroconductibility, can play rot-resistant effect, and silicon carbide hardness is high, thermostability is high, can strengthen coating property, and three's synergy makes this coating have excellent antiseptic property; 4) mature production technology, simple to operate, without the need to complex apparatus, be easy to large-scale industrial and produce.
Embodiment
For a better understanding of the present invention, illustrate content of the present invention further below in conjunction with embodiment, but content of the present invention is not only confined to the following examples.
Embodiment 1:
Percentages is made up of following component in mass ratio, and epoxy resin E51 is 50, and polyaniline/silicon carbide/graphene composite material is 5, polyamide curing agent is 15, plasticizer phthalic acid dibutylester is 2, and defoamer fluorosilicone class Airex931 is 1, solvent N ?methyl-2-pyrrolidone be 27.
1) add in sodium dodecyl benzene sulfonate aqueous solution by 0.5g silicon carbide, ultrasonic disperse added aniline after 10 minutes, was uniformly mixed at 0 DEG C, and Sodium dodecylbenzene sulfonate concentration is 20mg/mL, and concentration of aniline is 0.15mol/L;
2) configure the aqueous solution containing iron(ic) chloride of pH=1, be cooled to 0 DEG C, the mol ratio of iron(ic) chloride and aniline is 1.5:1;
3) by step 1) with step 2) solution mix, stirring reaction 8 hours at 0 DEG C, filters, washing, dry, obtains polyaniline/composite material of silicon carbide;
4) polyaniline/composite material of silicon carbide is dispersed in water, preparation polyaniline/composite material of silicon carbide weight content is the suspension of 1%, suspension is under agitation added drop-wise to the graphene oxide water solution that concentration is 0.5mg/mL, is added dropwise to complete rear filtration, be drying to obtain the coated polyaniline/carbofrax material of graphene oxide;
5) coated for graphene oxide polyaniline/carbofrax material is placed in hydrazine hydrate, reduction reaction 12 hours at 95 DEG C, filtration, washing, drying, obtain polyaniline/silicon carbide/graphene composite material.
6) polyaniline/silicon carbide/graphene composite material is added N containing epoxy resin E51 ?in methyl-2-pyrrolidone, dispersed with stirring is even, and then stir 15 minutes again after adding polyamide curing agent, plasticizer phthalic acid dibutylester and defoamer fluorosilicone class Airex931, obtain polyaniline/silicon carbide/Graphene composite anticorrosion coating.
Embodiment 2:
Count in mass ratio and be made up of following component, epoxy resin E44 is 45, and polyaniline/silicon carbide/graphene composite material is 8, and polyamide curing agent is 18, and plasticizer phthalic acid dibutylester is 5, and defoamer fluorosilicone class Airex932 is 1, and solvent, n-butanol is 23.
1) add in sodium dodecyl benzene sulfonate aqueous solution by 0.6g silicon carbide, ultrasonic disperse added aniline after 15 minutes, was uniformly mixed at 2 DEG C, Sodium dodecylbenzene sulfonate concentration 30mg/mL, and concentration of aniline is 0.3mol/L;
2) configure the aqueous solution containing iron nitrate of pH=2, be cooled to 2 DEG C, the mol ratio of iron nitrate and aniline is 1:1;
3) by step 1) with step 2) solution mix, stirring reaction 12 hours at 2 DEG C, filters, washing, dry, obtains polyaniline/composite material of silicon carbide;
4) polyaniline/composite material of silicon carbide is dispersed in water, preparation polyaniline/composite material of silicon carbide weight content is the suspension of 5%, suspension is under agitation added drop-wise to the graphene oxide water solution that concentration is 4mg/mL, is added dropwise to complete rear filtration, be drying to obtain the coated polyaniline/carbofrax material of graphene oxide;
5) coated for graphene oxide polyaniline/carbofrax material is placed in hydrazine hydrate, reduction reaction 18 hours at 90 DEG C, filtration, washing, drying, obtain polyaniline/silicon carbide/graphene composite material.
6) polyaniline/silicon carbide/graphene composite material is added in the solvent containing epoxy resin E44, dispersed with stirring is even, and then stir 20 minutes again after adding polyamide curing agent, plasticizer phthalic acid dibutylester and defoamer fluorosilicone class Airex932, obtain polyaniline/silicon carbide/Graphene composite anticorrosion coating.
Embodiment 3:
Count in mass ratio and be made up of following component, epoxy resin E42 is 60, and polyaniline/silicon carbide/graphene composite material is 8, polyetheramine solidifying agent is 10, plasticizer phthalic acid dioctyl ester is 4, and defoamer organic modified polyorganosiloxane Airex962 is 1, and solvent xylene is 17.
1) add in sodium dodecyl benzene sulfonate aqueous solution by 0.8g silicon carbide, ultrasonic disperse added aniline after 30 minutes, was uniformly mixed at 4 DEG C, and Sodium dodecylbenzene sulfonate concentration is 40mg/mL, and concentration of aniline is 0.4mol/L;
2) configure the aqueous solution containing oxygenant of pH=4, be cooled to 4 DEG C, described oxygenant is iron(ic) chloride, iron nitrate or ammonium persulphate, and the mol ratio of oxygenant and aniline is 2:1;
3) by step 1) with step 2) solution mix, stirring reaction 12 hours at 4 DEG C, filters, washing, dry, obtains polyaniline/composite material of silicon carbide;
4) polyaniline/composite material of silicon carbide is dispersed in water, preparation polyaniline/composite material of silicon carbide weight content is the suspension of 4%, suspension is under agitation added drop-wise to the graphene oxide water solution that concentration is 2mg/mL, is added dropwise to complete rear filtration, be drying to obtain the coated polyaniline/carbofrax material of graphene oxide;
5) coated for graphene oxide polyaniline/carbofrax material is placed in hydrazine hydrate, reduction reaction 24 hours at 70 DEG C, filtration, washing, drying, obtain polyaniline/silicon carbide/graphene composite material.
6) polyaniline/silicon carbide/graphene composite material is added in the dimethylbenzene containing epoxy resin E42, dispersed with stirring is even, and then stir 20 minutes again after adding polyetheramine solidifying agent, plasticizer phthalic acid dioctyl ester and defoamer organic modified polyorganosiloxane Airex962, obtain polyaniline/silicon carbide/Graphene composite anticorrosion coating.
Embodiment 4:
Count in mass ratio and be made up of following component, epoxy resin E35 is 45, and polyaniline/silicon carbide/graphene composite material is 10, and polyetheramine solidifying agent is 15, and plasticizer phthalic acid dibutylester is 3, and defoamer fluorosilicone class Airex931 is 1, and solvent xylene is 26.
1) add in sodium dodecyl benzene sulfonate aqueous solution by 0.7g silicon carbide, ultrasonic disperse added aniline after 15 minutes, was uniformly mixed at 0 DEG C, and Sodium dodecylbenzene sulfonate concentration is 30mg/mL, and concentration of aniline is 0.5mol/L;
2) configure the aqueous solution containing ammonium persulphate of pH=3, but to 0 DEG C, the mol ratio of ammonium persulphate and aniline is 1:1;
3) by step 1) with step 2) solution mix, stirring reaction 10 hours at 0 DEG C, filters, washing, dry, obtains polyaniline/composite material of silicon carbide;
4) polyaniline/composite material of silicon carbide is dispersed in water, preparation polyaniline/composite material of silicon carbide weight content is the suspension of 6%, suspension is under agitation added drop-wise to the graphene oxide water solution that concentration is 1mg/mL, is added dropwise to complete rear filtration, be drying to obtain the coated polyaniline/carbofrax material of graphene oxide;
5) coated for graphene oxide polyaniline/carbofrax material is placed in hydrazine hydrate, reduction reaction 16 hours at 85 DEG C, filtration, washing, drying, obtain polyaniline/silicon carbide/graphene composite material.
6) polyaniline/silicon carbide/graphene composite material is added in the dimethylbenzene containing epoxy resin, dispersed with stirring is even, and then stir 10 minutes again after adding polyetheramine solidifying agent, plasticizer phthalic acid dibutylester and defoamer fluorosilicone class Airex931, obtain polyaniline/silicon carbide/Graphene composite anticorrosion coating.
Embodiment 5:
Count in mass ratio and be made up of following component, epoxy resin E31 is 40, and polyaniline/silicon carbide/graphene composite material is 8, polyamide curing agent is 15, plasticizer phthalic acid dioctyl ester is 5, and defoamer fluorosilicone class Airex932 is 1, solvent N ?methyl-2-pyrrolidone be 31.
1) add in sodium dodecyl benzene sulfonate aqueous solution by 0.9g silicon carbide, ultrasonic disperse added aniline after 30 minutes, was uniformly mixed at 4 DEG C, and Sodium dodecylbenzene sulfonate concentration is 35mg/mL, and concentration of aniline is 0.25mol/L;
2) configure the aqueous solution containing iron(ic) chloride of pH=1, be cooled to 4 DEG C, the mol ratio of iron(ic) chloride and aniline is 1:2;
3) by step 1) with step 2) solution mix, stirring reaction 12 hours at 4 DEG C, filters, washing, dry, obtains polyaniline/composite material of silicon carbide;
4) polyaniline/composite material of silicon carbide is dispersed in water, preparation polyaniline/composite material of silicon carbide weight content is the suspension of 8%, suspension is under agitation added drop-wise to the graphene oxide water solution that concentration is 4mg/mL, is added dropwise to complete rear filtration, be drying to obtain the coated polyaniline/carbofrax material of graphene oxide;
5) coated for graphene oxide polyaniline/carbofrax material is placed in hydrazine hydrate, reduction reaction 12 hours at 90 DEG C, filtration, washing, drying, obtain polyaniline/silicon carbide/graphene composite material.
6) polyaniline/silicon carbide/graphene composite material is added N containing epoxy resin ?in methyl-2-pyrrolidone, dispersed with stirring is even, and then stir 15 minutes again after adding polyamide curing agent, plasticizer phthalic acid dioctyl ester and defoamer fluorosilicone class Airex932, obtain polyaniline/silicon carbide/Graphene composite anticorrosion coating.
Polyaniline/silicon carbide/Graphene composite anticorrosion coating that Example 1-5 obtains is coated on carbon steel electrode, and coat-thickness is about 300 μm, is immersed in the NaCl aqueous solution of massfraction 3.5%, uses CHI-660 electrochemical workstation to carry out performance test.
Table 1 contrasts the physicals of corrosion potential, corrosion current and the coating applying matrix material of the present invention and uncoated carbon steel.
From table 1, polyaniline/silicon carbide/Graphene composite coating prepared by the present invention has excellent antiseptic property and physicals.Silicon carbide and Graphene add the compactness enhancing coating, and improve the adhesive power of polyaniline to metallic surface.Therefore, polyaniline/silicon carbide/Graphene composite coating has good preservative effect.
Each raw material cited by the present invention can realize the present invention, and the bound value of each raw material, interval value can realize the present invention; Embodiment is not enumerated at this.Bound value, the interval value of processing parameter of the present invention (as temperature, time etc.) can realize the present invention, do not enumerate embodiment at this.
Claims (8)
1. polyaniline/silicon carbide/Graphene composite anticorrosion coating, is made up of following component,
Epoxy resin 40-60, polyaniline/silicon carbide/graphene composite material 5-10, solidifying agent 10-30, softening agent 1-5, defoamer 1-5, solvent 20-40, by mass percentage.
2. polyaniline/silicon carbide/Graphene composite anticorrosion coating according to claim 1, is characterized in that the preparation method of described polyaniline/silicon carbide/graphene composite material is:
1) add in sodium dodecyl benzene sulfonate aqueous solution by 0.5-1g silicon carbide, add aniline, be uniformly mixed at 0-4 DEG C after ultrasonic disperse 5-30 minute, Sodium dodecylbenzene sulfonate concentration is 20-50mg/mL, and concentration of aniline is 0.1-0.5mol/L;
2) configure the aqueous solution containing oxygenant of pH=1-4, be cooled to 0-4 DEG C, described oxygenant is iron(ic) chloride, iron nitrate or ammonium persulphate, and the mol ratio of oxygenant and aniline is 3:1-1:2;
3) by step 1) with step 2) solution mix, stirring reaction 4-12 hour at 0-4 DEG C, filters, washing, dry, obtains polyaniline/composite material of silicon carbide;
4) polyaniline/composite material of silicon carbide is dispersed in water, preparation polyaniline/composite material of silicon carbide weight content is the suspension of 0.5-10%, suspension is under agitation added drop-wise to the graphene oxide water solution that concentration is 0.5-5mg/mL, is added dropwise to complete rear filtration, be drying to obtain the coated polyaniline/carbofrax material of graphene oxide;
5) coated for graphene oxide polyaniline/carbofrax material is placed in hydrazine hydrate, reduction reaction 12-24 hour at 70-95 DEG C, filtration, washing, drying, obtain polyaniline/silicon carbide/graphene composite material.
3. the preparation method of polyaniline/silicon carbide/Graphene composite anticorrosion coating according to claim 1, is characterized in that:
1) add in sodium dodecyl benzene sulfonate aqueous solution by 0.5-1g silicon carbide, add aniline, be uniformly mixed at 0-4 DEG C after ultrasonic disperse 5-30 minute, Sodium dodecylbenzene sulfonate concentration is 20-50mg/mL, and concentration of aniline is 0.1-0.5mol/L;
2) configure the aqueous solution containing oxygenant of pH=1-4, be cooled to 0-4 DEG C, described oxygenant is iron(ic) chloride, iron nitrate or ammonium persulphate, and the mol ratio of oxygenant and aniline is 3:1-1:2;
3) by step 1) with step 2) solution mix, stirring reaction 4-12 hour at 0-4 DEG C, filters, washing, dry, obtains polyaniline/composite material of silicon carbide;
4) polyaniline/composite material of silicon carbide is dispersed in water, preparation polyaniline/composite material of silicon carbide weight content is the suspension of 0.5-10%, suspension is under agitation added drop-wise to the graphene oxide water solution that concentration is 0.5-5mg/mL, is added dropwise to complete rear filtration, be drying to obtain the coated polyaniline/carbofrax material of graphene oxide;
5) coated for graphene oxide polyaniline/carbofrax material is placed in hydrazine hydrate, reduction reaction 12-24 hour at 70-95 DEG C, filtration, washing, drying, obtain polyaniline/silicon carbide/graphene composite material;
6) polyaniline/silicon carbide/graphene composite material is added in the solvent containing epoxy resin, dispersed with stirring is even, and then stir 10-30 minute again after adding solidifying agent, softening agent and defoamer, obtain polyaniline/silicon carbide/Graphene composite anticorrosion coating.
4. the preparation method of polyaniline/silicon carbide/Graphene composite anti-corrosion material according to claim 3, is characterized in that: described epoxy resin is epoxy resin E51, epoxy resin E44, epoxy resin E42, epoxy resin E35 or epoxy resin E31.
5. the preparation method of polyaniline/silicon carbide/Graphene composite anti-corrosion material according to claim 3, is characterized in that: described solidifying agent is polyamide curing agent or polyetheramine solidifying agent.
6. the preparation method of polyaniline/silicon carbide/Graphene composite anti-corrosion material according to claim 3, is characterized in that: described softening agent is dibutyl phthalate or dioctyl phthalate (DOP).
7. the preparation method of polyaniline/silicon carbide/Graphene composite anti-corrosion material according to claim 3, is characterized in that: described defoamer is fluorosilicone class Airex931, fluorosilicone class Airex932 or organic modified polyorganosiloxane Airex962.
8. the preparation method of polyaniline/silicon carbide/Graphene composite anti-corrosion material according to claim 3, is characterized in that: described solvent be toluene, dimethylbenzene, propyl carbinol or N ?methyl-2-pyrrolidone.
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