CN102604533A - Polyaniline-graphene composite based anticorrosive paint and preparation method thereof - Google Patents
Polyaniline-graphene composite based anticorrosive paint and preparation method thereof Download PDFInfo
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Abstract
The invention provides polyaniline-graphene composite based anticorrosive paint and a preparation method thereof. The polyaniline-graphene composite based anticorrosive paint comprises, by weight, 20-90 parts of film former, 0.1-20 parts of polyaniline-graphene composite, 1-10 parts of pigment, 1-10 parts of filler, 0.1-3 parts of sag-proof agent, 0.1-4 parts of dispersant, 0.01-2 parts of flatting agent, 0.01-2 parts of defoaming agent, and 1-50 parts of solvent. The paint has good physical anticorrosion as graphene is high in radius-thickness ratio and high in flexibility and has electromechanical anticorrosion by the aid of polyaniline loaded on the surface of the graphene, and under synergism of the polyaniline and the graphene, the paint has fine metal corrosion resistance. The anticorrosive paint achieves passivation and corrosion inhibition of metal substrates, avoids use of heavy metals causing environmental pollution, such as chromium and the like, and is simple to prepare, low in cost and easy in industrial batch production.
Description
Technical field
What the present invention relates to is a kind of protective system.The present invention also relates to a kind of preparation method of protective system.
Background technology
Have the mica powder, aluminium powder, glass flake etc. of flaky texture because the penetrating quality of corrosion protection coating is reduced; Thereby play the effect of physics rot-resistant; Therefore often be used as applying filler in protective system, for example (Chinese patent ZL91111830.6) proposed the preparation method of glass flake anticorrosion paint.Yet because this lamellar structure only can provide physics anticorrosion, do not reach the ideal preservative effect, the pigment that therefore normal and chromic salt etc. has electrochemical anti-corrosive makes the preservative activity that is used for improving coating simultaneously.In the last few years; Having the redox potential polyaniline comes to light and can make metal surface passivation; Therefore can replace chromium system and lead is that anticorrosive packing adds to and realizes electrochemical anti-corrosive in the protective system, people such as Liu Fuchun (Chinese patent number: 101643619B) with aluminium powder, glass flake etc. through polyaniline-modified, prepared the protective system that has the anticorrosion and electrochemical anti-corrosive function of physics simultaneously; Not only significantly improve the antiseptic property of coating, and avoided the use of deleterious chromic salt.
Graphene (graphene) is the newfound in recent years a kind of carbonaceous novel material with two-dimentional laminated structure by the tightly packed one-tenth of monolayer carbon atom; Graphene have excellent electric performance and high radius-thickness ratio (＞200) and thin laminated structure (＜1nm), therefore it is contemplated that to have to have better physics preservative activity than mica powder commonly used at present, aluminium powder, glass flake etc.If therefore with polyaniline load on the Graphene surface and with its as filler with providing good physics anticorrosion and Chemical Preservation simultaneously, thereby significantly improve the antiseptic property of coating, the research of related fields is not seen in report as yet.
Summary of the invention
The object of the invention provides a kind of protective system based on polyaniline and graphene composite material with good metallic corrosion barrier propterty.The present invention also aims to provide that a kind of preparation technology is simple, cost is low, be easy to realize the preparation method based on the protective system of polyaniline and graphene composite material of suitability for industrialized production.
The objective of the invention is to realize like this:
Protective system based on polyaniline and graphene composite material of the present invention is made up of following component in weight fraction: filmogen 20-90; Polyaniline and graphene composite material 0.1-20; Pigment 1-10; Filler 1-10; Anti-sagging agent 0.1-3; Dispersion agent 0.1-4; Flow agent 0.01-2; Skimmer 0.01-2; Solvent 1-50.
Described filmogen is any one in Synolac, resol, epoxy resin, fluorocarbon resin, chlorinated rubber, ethylene chloride, supervinyi chloride resin or the urethane resin.
Described pigment is coating pigment commonly used, like wherein any one such as white titanium pigment, zinc oxide, red iron oxide or phthalocyanine green.
Described filler is a coating filler commonly used, like wherein any one such as lime carbonate, talcum powder, silica sand ground barium sulfate.
Described solvent is a solvent commonly used in the preparation coating, like toluene, YLENE, butanols, butanone or pimelinketone or the like any one or two or more mixtures.
Described polyaniline and graphene composite material are that a kind of centre is Graphene or graphene oxide, and the surface is the lamella sandwich structure of polyaniline nano particulate, and the mass ratio of polyaniline and Graphene or graphene oxide is 0.1-500: 1.
Described anti-sagging agent is to cover one of holder soil, wilkinite, kaolin, aerosil or both above arbitrary proportion mixtures.
Said dispersion agent, flow agent, skimmer are coating auxiliary agents commonly used.The Disperbyk163 of dispersion agent such as German Bi Ke chemical company, Disperbyk 111, and Disperbyk 115, and Disperbyk 192; Disperbyk 191, Disperbyk 190 etc., the BYK-353 of flow agent such as German Bi Ke chemical company, BYK-354; BYK-355, BYK-331 etc., the BYK-053 of skimmer such as German Bi Ke chemical company; BYK-065, BYK-055, BYK-053 etc.
The preparation method of the protective system based on polyaniline and graphene composite material of the present invention carries out as follows:
(1) preparation of polyaniline and graphene composite material
1) preparation contains the graphene oxide of aniline, hydrochloric acid or the dispersion liquid of Graphene; Wherein aniline concentration is 0.01-1mol/L; Concentration of hydrochloric acid is 0.01-0.2mol/L, and the concentration of graphene oxide or Graphene is 0.01-10mg/mL, and the back precooling that stirs is to 0-10 ℃;
2) preparation contains the aqueous solution of oxygenant of hydrochloric acid, and wherein the concentration of the oxygenant in the solution is 0.01-1mol/L, and with its precooling to 0-10 ℃, concentration of hydrochloric acid is 0.01-0.2mol/L, oxygenant is ammonium persulphate or Potassium Persulphate;
The aqueous solution that 3) will contain the oxygenant of hydrochloric acid under agitation slowly splashes in the dispersion liquid of the graphene oxide that contains aniline, hydrochloric acid or Graphene; At 0-10 ℃ of reaction 0.5-10h; Be ground to less than 200 orders after centrifugal, filtration, the washing and drying, the volume ratio of dispersion liquid and the aqueous solution of the oxygenant that contains hydrochloric acid that wherein contains graphene oxide or the Graphene of aniline, hydrochloric acid is 1: 1;
(2) dispersion agent, flow agent, skimmer, anti-sagging agent, pigment, filler are joined in filmogen and the solvent, stir 10-120min, grind then, fineness is less than discharging after 60 microns;
(3) under agitation join polyaniline and graphene composite material in the filmogen mixture that step (2) obtains, carry out homodisperse, obtain polyaniline and Graphene protective system;
Wherein each component constitutes in weight fraction: filmogen 20-90; Polyaniline and graphene composite material 0.1-20; Pigment 1-10; Filler 1-10; Anti-sagging agent 0.1-3; Dispersion agent 0.1-4; Flow agent 0.01-2; Skimmer 0.01-2; Solvent 1-50.
Preparing method based on polyaniline and the protective system of graphene composite material of the present invention is different according to filmogen, selects corresponding curing agent and consumption, and some filmogen does not use the solidifying agent can film forming yet; Under normal temperature condition, solidify and form polyaniline and Graphene protective system after 7-15 days.
Graphene in the resulting coating of the present invention is because radius-thickness ratio is high; Snappiness can provide good physics preservative activity well; And the polyaniline that loads on the Graphene surface can provide the electrochemical anti-corrosive effect, and the synergy mechanism of the two makes this coating have good metallic corrosion barrier propterty.
Protective system of the present invention can be realized the passivation and the inhibition of metal base, has avoided causing the use of the heavy metals such as chromium of environmental pollution simultaneously, and preparation is simple, cost is low, be easy to industrialized mass production.
Embodiment
The comparative example 1
0.6 part of dispersion agent (Disperbyk191), 1.2 parts of flow agents (BYK 331), 1 part of skimmer (BYK 053), 0.6 part of anti-sagging agent (covering holder soil), 2 parts of pigment (white titanium pigment), 2 parts of fillers (lime carbonate), 20 parts of polyanilines (the commodity polyaniline that the Changchun applied chemistry is produced); Add 60 parts of epoxy resin (double A type epoxy resin E-44) and 30 parts of solvents (toluene); Stirred 20 minutes; In sand mill, grind then; Fineness is less than discharging after 45 microns, prepares protective system component one, 591 type solidifying agent and is dissolved in and is prepared into 50% solution in the butanols as component two.By weight component one: component two equals to mix two components at 100: 40, on No. 45 steel plates of 150mm * 75mm * 2mm that commercial blast was handled, films, and Air drying 15 days, paint film build are 400 μ m.Be immersed in concentration filming and be in 3.5% the NaCl aqueous solution, with its Ta Feier curve of CHI-660 electrochemical workstation test.
Embodiment 1
Prepare polyaniline/graphene composite material by following method
A) preparation contains the dispersion liquid of Graphene of aniline, hydrochloric acid, and wherein aniline concentration is 0.5mol/L, and concentration of hydrochloric acid is 0.2mol/L, and the concentration of Graphene be (10mg/mL), and precooling to 5 afterwards ℃ stirs.
B) preparation contains the ammonium persulfate aqueous solution of hydrochloric acid, and wherein the ammonium persulphate concentration in the solution is 0.5mol/L, and with its precooling to 5 ℃, concentration of hydrochloric acid is 0.2mol/L.
C) (b) solution is under agitation slowly splashed in (a) solution, wherein (a) solution is 1: 1 with (b) volume ratio of solution, at 5 ℃ of reaction 1h, is ground to less than 200 orders after centrifugal, filtration, the washing and drying, makes polyaniline/graphene composite material.
0.6 part of dispersion agent (Disperbyk191), 1.2 parts of flow agents (BYK 331), 1 part of skimmer (BYK 053), 0.6 part of anti-sagging agent (covering holder soil), 2 parts of pigment (white titanium pigment), 2 parts of fillers (lime carbonate), 20 parts of polyaniline/graphene composite materials; Add 60 parts of epoxy resin (double A type epoxy resin E-44) and 30 parts of solvents (toluene); Stirred 20 minutes; In sand mill, grind then; Fineness is less than discharging after 45 microns, prepares protective system component one, 591 type solidifying agent and is dissolved in and is prepared into 50% solution in the butanols as component two.By weight component one: component two equals to mix two components at 100: 40, on No. 45 steel plates of 150mm * 75mm * 2mm that commercial blast was handled, films, and Air drying 15 days, paint film build are 400 μ m.Be immersed in concentration filming and be in 3.5% the NaCl aqueous solution, with its Ta Feier curve of CHI-660 electrochemical workstation test.
Embodiment 2
Prepare polyaniline/graphene composite material by following method
A) preparation contains the graphene oxide dispersion liquid of aniline, hydrochloric acid, and wherein aniline concentration is 1mol/L, and concentration of hydrochloric acid is 0.01mol/L, and the concentration of graphene oxide or Graphene be (5mg/mL), and precooling to 10 afterwards ℃ stirs.
B) preparation contains the persulfate aqueous solution of hydrochloric acid, and wherein the Potassium Persulphate concentration in the solution is 1mol/L, and concentration of hydrochloric acid is 0.01mol/L, and with its precooling to 10 ℃.
C) (b) solution is under agitation slowly splashed in (a) solution, wherein (a) solution is 1: 1 with (b) volume ratio of solution, at 10 ℃ of reaction 1h, is ground to less than 200 orders the polyaniline of system/graphene oxide matrix material after centrifugal, filtration, the washing and drying.
20 parts of 0.6 part of 0.6 part of dispersion agents (Disperbyk191), 1.2 parts of flow agents (BYK331), 1 part of skimmer (BYK 053), anti-sagging agent (covering holder soil), 2 parts of pigment (white titanium pigment), 2 parts of fillers (lime carbonate), polyaniline/graphene oxide matrix material; Add 60 parts of epoxy resin (double A type epoxy resin E-44) and 30 parts of solvents (toluene); Stirred 20 minutes; In sand mill, grind then; Fineness is less than discharging after 45 microns, prepares protective system component one, 591 type solidifying agent and is dissolved in and is prepared into 50% solution in the butanols as component two.By weight component one: component two equals to mix two components at 100: 40, on No. 45 steel plates of 150mm * 75mm * 2mm that commercial blast was handled, films, and Air drying 15 days, paint film build are 400 μ m.Being immersed in concentration to film is in 3.5% the NaCl aqueous solution, with its Ta Feier curve of CHI-660 electrochemical workstation test.The corrosion potential result that table 1 has provided comparative example and embodiment 1,2 can be known that by table 1 this polyaniline/graphene composite material has been given the coating good corrosion prevention performance, compares its antiseptic property with simple polyaniline and significantly improves.
The corrosion potential result of table 1 comparative example and embodiment 1,2
| Embodiment | Corrosion potential (V) |
| The comparative example 1 | -0.523 |
| Embodiment 1 | -0.247 |
| Embodiment 2 | -0.209 |
Claims (4)
1. the protective system based on polyaniline and graphene composite material is characterized in that: be made up of following component in weight fraction: filmogen 20-90; Polyaniline and graphene composite material 0.1-20; Pigment 1-10; Filler 1-10; Anti-sagging agent 0.1-3; Dispersion agent 0.1-4; Flow agent 0.01-2; Skimmer 0.01-2; Solvent 1-50.
2. the protective system based on polyaniline and graphene composite material according to claim 1 is characterized in that described filmogen is any one in Synolac, resol, epoxy resin, fluorocarbon resin, chlorinated rubber, ethylene chloride, supervinyi chloride resin or the urethane resin.
3. the protective system based on polyaniline and graphene composite material according to claim 1; It is characterized in that described polyaniline and graphene composite material are that a kind of centre that obtains according to following method is Graphene or graphene oxide; The surface is the lamella sandwich structure of polyaniline nano particulate, and the mass ratio of polyaniline and Graphene or graphene oxide is 0.1-500: 1 matrix material:
1) preparation contains the graphene oxide of aniline, hydrochloric acid or the dispersion liquid of Graphene; Wherein aniline concentration is 0.01-1mol/L; Concentration of hydrochloric acid is 0.01-0.2mol/L, and the concentration of graphene oxide or Graphene is 0.01-10mg/mL, and the back precooling that stirs is to 0-10 ℃;
2) preparation contains the aqueous solution of oxygenant of hydrochloric acid, and wherein the concentration of the oxygenant in the solution is 0.01-1mol/L, and with its precooling to 0-10 ℃, concentration of hydrochloric acid is 0.01-0.2mol/L, oxygenant is ammonium persulphate or Potassium Persulphate;
The aqueous solution that 3) will contain the oxygenant of hydrochloric acid under agitation slowly splashes in the dispersion liquid of the graphene oxide that contains aniline, hydrochloric acid or Graphene; At 0-10 ℃ of reaction 0.5-10h; Be ground to less than 200 orders after centrifugal, filtration, the washing and drying, the volume ratio of dispersion liquid and the aqueous solution of the oxygenant that contains hydrochloric acid that wherein contains graphene oxide or the Graphene of aniline, hydrochloric acid is 1: 1.
4. preparation method based on the protective system of polyaniline and graphene composite material is characterized in that carrying out as follows:
(1) preparation of polyaniline and graphene composite material
1) preparation contains the graphene oxide of aniline, hydrochloric acid or the dispersion liquid of Graphene; Wherein aniline concentration is 0.01-1mol/L; Concentration of hydrochloric acid is 0.01-0.2mol/L, and the concentration of graphene oxide or Graphene is 0.01-10mg/mL, and the back precooling that stirs is to 0-10 ℃;
2) preparation contains the aqueous solution of oxygenant of hydrochloric acid, and wherein the concentration of the oxygenant in the solution is 0.01-1mol/L, and with its precooling to 0-10 ℃, concentration of hydrochloric acid is 0.01-0.2mol/L, oxygenant is ammonium persulphate or Potassium Persulphate;
The aqueous solution that 3) will contain the oxygenant of hydrochloric acid under agitation slowly splashes in the dispersion liquid of the graphene oxide that contains aniline, hydrochloric acid or Graphene; At 0-10 ℃ of reaction 0.5-10h; Be ground to less than 200 orders after centrifugal, filtration, the washing and drying, the volume ratio of dispersion liquid and the aqueous solution of the oxygenant that contains hydrochloric acid that wherein contains graphene oxide or the Graphene of aniline, hydrochloric acid is 1: 1;
(2) dispersion agent, flow agent, skimmer, anti-sagging agent, pigment, filler are joined in filmogen and the solvent, stir 10-120min, grind then, fineness is less than discharging after 60 microns;
(3) under agitation join polyaniline and graphene composite material in the filmogen mixture that step (2) obtains, carry out homodisperse, obtain polyaniline and Graphene protective system;
Wherein each component constitutes in weight fraction: filmogen 20-90; Polyaniline and graphene composite material 0.1-20; Pigment 1-10; Filler 1-10; Anti-sagging agent 0.1-3; Dispersion agent 0.1-4; Flow agent 0.01-2; Skimmer 0.01-2; Solvent 1-50.
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