CN106398206B - The preparation method of graphene oxide/polyaniline/titanium dioxide nanocomposite and polyaniline nano anticorrosive paint - Google Patents
The preparation method of graphene oxide/polyaniline/titanium dioxide nanocomposite and polyaniline nano anticorrosive paint Download PDFInfo
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- CN106398206B CN106398206B CN201610814953.0A CN201610814953A CN106398206B CN 106398206 B CN106398206 B CN 106398206B CN 201610814953 A CN201610814953 A CN 201610814953A CN 106398206 B CN106398206 B CN 106398206B
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K9/00—Use of pretreated ingredients
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- C08G73/00—Macromolecular compounds obtained by reactions forming a linkage containing nitrogen with or without oxygen or carbon in the main chain of the macromolecule, not provided for in groups C08G12/00 - C08G71/00
- C08G73/02—Polyamines
- C08G73/026—Wholly aromatic polyamines
- C08G73/0266—Polyanilines or derivatives thereof
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- 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
- C09D163/00—Coating compositions based on epoxy resins; Coating compositions based on derivatives of epoxy resins
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- 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
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2237—Oxides; Hydroxides of metals of titanium
- C08K2003/2241—Titanium dioxide
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Abstract
The invention discloses the preparation methods of a kind of graphene oxide/polyaniline/titanium dioxide nanocomposite and polyaniline nano anticorrosive paint, the preparation method of nanocomposite includes: (1) using sodium hydroxide solution or ammonia spirit as dispersing agent, and graphite oxide ultrasound is removed to obtain graphene oxide；(2) graphene oxide is added to the organic sulfonic acid solution of aniline, stirring 10h ~ 16h obtains graphene oxide/polyaniline nano-composite material；(3) nano-titanium dioxide is added in the organic sulfonic acid solution of the resulting graphene oxide/polyaniline nano-composite material of step (2), stir 10h ~ 16h, successively through centrifugation, washing, dry to obtain graphene oxide/polyaniline/titanium dioxide nanocomposite.Raw material of the present invention is cheap and easy to get, and simple process is easily-controllable, and the antiseptic property of gained polyaniline nano anticorrosive paint is excellent and environmental-friendly.
Description
Technical field
The invention belongs to the technical field of metal anti-corrosion such as aluminium alloy, and in particular to a kind of graphene oxide/polyaniline/dioxy
Change the preparation method of titanium nanometer composite material and polyaniline nano anticorrosive paint.
Background technique
The metal materials such as aluminium alloy have high intensity, high rigidity, good electrical and thermal conductivity and excellent mechanical performance etc.
Feature, thus have important in modern society and be widely applied, but loss and harm brought by the corrosion of metal material
It is also difficult to the appraisal.Alloy product is mostly used greatly at present using dichromic acid surface oxidation as the pretreatment of representative, with epoxy zinc
Yellow class paint is the priming paint of representative, is aided with the anticorrosion process of the finishing coats such as alkyd paint, acrylic polyurethane coating.But above-mentioned technique is using
It has the following problems in the process: (1) as the use environment of metal material the next complicated, traditional dichromic acid surface oxidation treatment
Method is not able to satisfy the requirement of alloy surface complete passivation gradually, and a large amount of extremely toxic substance such as Cr VI is generated in passivating solution,
It cannot meet environmental requirements；(2) epoxy zinc yellow class priming paint generates a large amount of poisonous and hazardous volatile in coating and use process
Organic matter VOC generates side effect to environment, does not meet the Green Development trend in epoch and science and technology；(3) traditional priming paint film layer exists
It cannot be to Cl in cargo sweat environment-Equal harmful ions play permanently effective insulating effect；(4) by this body structure of organic molecule
It is limited, the long-term weatherability of epoxylite substrate in the environment is insufficient, is easy to happen aging, falls off.To sum up, existing
The anticorrosion treatment technology of the metal materials such as aluminium alloy is no longer satisfied the use demand of modern product.
Although polyaniline anti-corrosion coating has unique anti-spot corrosion and scratch resistant performance, there are dissolubilities, shielding
And film forming it is poor, should not directly as coating use the problems such as.Result of study shows through organic acid doped or inorganic nano
After material modification, dissolubility, shielding, film forming and adhesive force of polyaniline anti-corrosion coating etc. can be improved.Doping
Organic acid is mostly organic sulfonic acid.The fusing point and boiling point of organic sulfonic acid are compared with inorganic acid height, and environmental stability is more excellent, both contain polar group
Group, and contain non-polar group, so the electric conductivity of polyaniline not only can be improved after doping, but also the environment of polyaniline can be improved
Stability and dissolubility.In addition, inorganic nano material has preferable dispersibility in polyaniline, can fill up in polyaniline structure
Hole enhances shielding action, while the thermal stability and mechanical performance of coating, such as impact resistance, resistance to marring also can be improved.
Inorganic lamellar material such as montmorillonite, graphene etc. can interact on a molecular scale with organic component, and the performance of compound is more
Easy to control and modulation.
Since discovery graphene in 2004, graphene relies on its superior performance, such as good thermal conductivity and conduction
Property, big specific surface area, powerful mechanical strength and chemical stability have attracted the attention of numerous researchers.Graphite oxide
Alkene is the graphene film by chemical modification, and the edge of skeleton and lamella contains a large amount of oxygen-containing group, such as epoxy group,
Hydroxyl, carboxyl etc..Therefore for graphene oxide is compared to graphene, electric conductivity is reduced, but dispersibility greatly improves, especially
It is the dispersibility in water, and the properties such as big specific surface area and chemical stability still retain.
Nano material is due to unique small-size effect, quantum size effect, surface and interfacial effect and macroscopic view
Quantum tunneling effect shows superiority more more than traditional coating, and the application in coating is also increasingly taken seriously.Small ruler
Very little effect enables nano material to be filled into the hole and defect of coating, to effectively improve the antiseptic property of coating.Surface
Effect enables nano material to have very high surface, is easy in conjunction with atom in coating, improves coating compactness.Nano material
Other special effects it is also possible to improving the levelability of coating, hardness, adhesive force and the performances such as anti-aging.For example, nanometer two
Titanium oxide has the function of absorbing ultraviolet light, can carry out photocatalysis Decomposition to organic matter in environment in addition coating, realize surface
Automatically cleaning, to effectively improve the function of the anti-aging and antiultraviolet of coating.
Summary of the invention
Graphene oxide/polyaniline/titanium dioxide nanometer that an object of the present invention is to provide a kind of simple process is multiple
The preparation method of condensation material, gained nanocomposite can be used as paint filler.
The second object of the present invention is to provide a kind of preparation method of the polyaniline nano anticorrosive paint of simple process, gained
The antiseptic property of polyaniline nano anticorrosive paint is excellent and environmental-friendly.
To reach first purpose, the preparation of graphene oxide of the invention/polyaniline/titanium dioxide nanocomposite
Method, comprising steps of
(1) using sodium hydroxide solution or ammonia spirit as dispersing agent, graphite oxide ultrasound is removed into obtain graphene oxide；
(2) graphene oxide is added to the organic sulfonic acid solution of aniline, stirring 10h ~ 16h obtains graphene oxide/polyphenyl
Amine nanocomposite；
(3) nano-titanium dioxide is added to having for step (2) resulting graphene oxide/polyaniline nano-composite material
In machine sulfonic acid solutions, stir 10h ~ 16h, successively through centrifugation, washing, dry to obtain graphene oxide/polyaniline/titanium dioxide nanometer
Composite material.
Preferably, the concentration of sodium hydroxide solution or ammonia spirit is 0.01mol/L ~ 0.1mol/L.
Preferably, the organic sulfonic acid solution of aniline is the sulfosalisylic acid solution of aniline.
Preferably, the mass ratio of graphene oxide and aniline is (1 ~ 5): 1, and graphene oxide/polyaniline/titanium dioxide
The mass percent of nano-titanium dioxide is 5% ~ 20% in titanium nanometer composite material.
To reach second purpose, the preparation method of polyaniline nano anticorrosive paint of the invention, comprising:
Above-mentioned gained graphene oxide/polyaniline/titanium dioxide nanocomposite is added to resin, it is agitated to gather
Aniline nano anticorrosive paint.
Preferably, graphene oxide/polyaniline/titanium dioxide nanocomposite in polyaniline nano anticorrosive paint
Mass percent is 1% ~ 10%.
Preferably, resin is aqueous epoxy resins.There is very strong cohesive force between aqueous epoxy resins and metallic matrix, together
Thing is also with good stability, good dispersion, and environmentally protective.
The present invention mixes the organic sulfonic acid solution of graphene oxide and aniline with bigger serface and excellent hydrophilic
Reaction is closed, graphene oxide/polyaniline nano-composite material is prepared by situ aggregation method；Nano-titanium dioxide is added to again
Stirred in graphene oxide/polyaniline nano-composite material organic sulfonic acid solution, successively through centrifugation, washing, dry to obtain oxidation
Graphene/polyaniline/titanic oxide nano compound material；By gained graphene oxide/nano combined material of polyaniline/titanium dioxide
Material is used as paint filler, can sufficiently improve the antiseptic property of polyaniline paint.
The present invention utilizes the Large ratio surface and polymolecularity of graphene oxide, to promote aniline molecule to carry out original on its surface
Position polymerization, thus effectively solve polyaniline paint present in film forming, shielding and dispersibility it is poor the problems such as, so as to abundant
Play the excellent antiseptic property of polyaniline.
The present invention will have the active nano-titanium dioxide of light degradation and graphene oxide/polyaniline nano-composite material into
Row nanometer level it is compound, graphene oxide/polyaniline/titanium dioxide nanocomposite is obtained, with graphene oxide/polyphenyl
Amine/titanic oxide nano compound material is the functional filler of coating, can not only improve film forming, shielding and the attachment of coating
Power further increases the antiseptic property of coating；It also can get self-cleaning surface function, to improve the environment resistant of coating.
Compared to the prior art, the invention has the advantages that and the utility model has the advantages that
(1) raw material is cheap and easy to get, and graphene oxide/polyaniline/titanium dioxide nanocomposite and polyaniline nano are anti-
The preparation process of rotten coating is simple and easy to control；
(2) present invention gained anticorrosive paint is water paint, environmental-friendly, can be used for the anti-corrosion of the metal materials such as aluminium alloy
Coating；
(3) graphene oxide can improve film forming, shielding and the dispersibility of polyaniline paint, poly- to give full play of
The excellent antiseptic property of aniline；
(4) nano-titanium dioxide can improve film forming, shielding and the adhesion of polyaniline paint, may additionally facilitate coating pair
The light degradation of water environment microorganism, to improve the antiseptic property of polyaniline paint and environment resistant.
Detailed description of the invention
Fig. 1 is the XRD spectrum of 1 gained nanocomposite of embodiment；
Fig. 2 is the SEM figure of 1 gained nanocomposite of embodiment；
Fig. 3 is that 1 gained nanocomposite of embodiment is degraded the efficiency chart of rhodamine B solution under full spectrum；
Fig. 4 is the EIS spectrum of 1 gained nanometer anticorrosive coating of embodiment；
Fig. 5 is the Tafel figure of 1 gained nanometer anticorrosive coating of embodiment；
Fig. 6 is the XRD spectrum of 2 gained nanocomposite of embodiment；
Fig. 7 is the SEM figure of 2 gained nanocomposite of embodiment；
Fig. 8 is that 2 gained nanocomposite of embodiment is degraded the efficiency chart of rhodamine B solution under full spectrum；
Fig. 9 is the EIS spectrum of 2 gained nanometer anticorrosive coating of embodiment；
Figure 10 is the Tafel figure of 2 gained nanometer anticorrosive coating of embodiment；
Figure 11 is the XRD spectrum of 3 gained nanocomposite of embodiment；
Figure 12 is the SEM figure of 3 gained nanocomposite of embodiment；
Figure 13 is that 3 gained nanocomposite of embodiment is degraded the efficiency chart of rhodamine B solution under full spectrum；
Figure 14 is the EIS spectrum of 3 gained nanometer anticorrosive coating of embodiment；
Figure 15 is the Tafel figure of 3 gained nanometer anticorrosive coating of embodiment.
Specific embodiment
Embodiment 1
By the 2.5 g graphite powders mixed solution oxygen of the 58 mL concentrated sulfuric acids, 1.25 g sodium nitrate and 7.5 g potassium permanganate
It is melted into graphite oxide.0.5 g graphite oxide is taken to use 0.01mol/L sodium hydroxide solution as dispersing agent, ultrasound 8 h of removing are obtained
The preferable graphene oxide of peeling effect.It is 1:1 according to the mass ratio of graphene oxide and aniline, graphene oxide is added to
10 h are stirred to react in the sulfosalisylic acid solution of aniline, obtain graphene oxide/polyaniline nano-composite material.Again by nanometer two
Titanium oxide, which is added in graphene oxide/polyaniline nano-composite material sulfosalisylic acid solution, stirs 10 h, successively through from
The heart, washing, drying obtain graphene oxide/polyaniline/titanium dioxide nanocomposite.By gained graphene oxide/polyphenyl
Amine/titanic oxide nano compound material is added to aqueous epoxy resins, and homogeneous latex emulsion is sufficiently stirred into get polyaniline nano
Anticorrosive paint, wherein graphene oxide/polyaniline/titanium dioxide nanocomposite mass percent is 1%.
The quality hundred of titanium dioxide in graphene oxide/polyaniline/titanium dioxide nanocomposite obtained by the present embodiment
Point than be that X-ray diffraction powder diffraction (XRD) that 5%, Fig. 1 be the present embodiment nanocomposite is composed, it can be seen that in contain it is aerobic
Graphite alkene, polyaniline and titanium dioxide.Fig. 2 is scanning electron microscope (SEM) figure of the present embodiment nanocomposite, can
See that titanium dioxide granule is distributed in graphene oxide/polyaniline nano on piece.Fig. 3 is the present embodiment nanocomposite in xenon
To the degradation efficiency figure for the rhodamine B solution that concentration is 10 mg/L under the full spectral illumination of lamp, 2 h degradation efficiencies are up to 55.4%.Fig. 4
For the electrochemical impedance spectroscopy (EIS) of nanometer anticorrosive coating obtained by the present embodiment, Fig. 5 is nanometer anticorrosive coating obtained by the present embodiment
Tafel polarization curve (Tafel) figure, corrosion electric current density are 1.01 μ A/cm2。
Embodiment 2
By the 2.5 g graphite powders mixed solution oxygen of the 58 mL concentrated sulfuric acids, 1.25 g sodium nitrate and 7.5 g potassium permanganate
It is melted into graphite oxide.0.5 g graphite oxide is taken to use 0.05 mol/L sodium hydroxide solution as dispersing agent, ultrasound 8 h of removing are obtained
The preferable graphene oxide of peeling effect.It is 2.3:1 according to the mass ratio of graphene oxide and aniline, graphene oxide is added
It is stirred to react 12h into the sulfosalisylic acid solution of aniline, obtains graphene oxide/polyaniline nano-composite material.Again by nanometer
Titanium dioxide, which is added in graphene oxide/polyaniline nano-composite material sulfosalisylic acid solution, stirs 12 h, successively passes through
Centrifugation, washing, drying, obtain graphene oxide/polyaniline/titanium dioxide nanocomposite.By gained graphene oxide/polyphenyl
Amine/titanic oxide nano compound material is added to aqueous epoxy resins, and homogeneous latex emulsion is sufficiently stirred into get polyaniline nano
Anticorrosive paint, wherein graphene oxide/polyaniline/titanium dioxide nanocomposite mass percent is 5%.
The quality hundred of titanium dioxide in graphene oxide/polyaniline/titanium dioxide nanocomposite obtained by the present embodiment
Divide than being that the X-ray diffraction powder diffraction (XRD) that 15%, Fig. 6 is the present embodiment nanocomposite is composed, Fig. 7 is the present embodiment
Scanning electron microscope (SEM) figure of nanocomposite, Fig. 8 are the present embodiment nanocomposite in the full spectral illumination of xenon lamp
Under to concentration be 10 mg/L rhodamine B solution degradation efficiency figure, 2 h degradation efficiencies up to 99.1%, Fig. 9 be the present embodiment institute
The electrochemical impedance spectroscopy (EIS) of nanometer anticorrosive coating is obtained, Figure 10 is the Ta Feier polarization of nanometer anticorrosive coating obtained by the present embodiment
Curve (Tafel) figure, corrosion electric current density are 0.37 μ A/cm2。
Embodiment 3
By the 2.5 g graphite powders mixed solution oxygen of the 58 mL concentrated sulfuric acids, 1.25 g sodium nitrate and 7.5 g potassium permanganate
It is melted into graphite oxide.0.5 g graphite oxide is taken to use 0.1 mol/L sodium hydroxide solution as dispersing agent, ultrasound 8 h of removing are obtained
The preferable graphene oxide of peeling effect.It is 5:1 according to the mass ratio of graphene oxide and aniline, graphene oxide is added to
It is stirred to react 16h in the sulfosalisylic acid solution of aniline, obtains graphene oxide/polyaniline nano-composite material.Again by nanometer two
Titanium oxide, which is added in graphene oxide/polyaniline nano-composite material sulfosalisylic acid solution, stirs 16 h, successively through from
The heart, washing, drying obtain graphene oxide/polyaniline/titanium dioxide nanocomposite.By gained graphene oxide/polyphenyl
Amine/titanic oxide nano compound material is added to aqueous epoxy resins, and homogeneous latex emulsion is sufficiently stirred into get polyaniline nano
Anticorrosive paint, wherein graphene oxide/polyaniline/titanium dioxide nanocomposite mass percent is 10%,
The quality hundred of titanium dioxide in graphene oxide/polyaniline/titanium dioxide nanocomposite obtained by the present embodiment
Divide than being that the X-ray diffraction powder diffraction (XRD) that 20%, Figure 11 is the present embodiment nanocomposite is composed, Figure 12 is this implementation
Scanning electron microscope (SEM) figure of example nanocomposite, Figure 13 are under the full spectrum of the present embodiment nanocomposite to sieve
The degradation efficiency figure of red bright B solution (10 mg/L), 2 h degradation efficiencies up to 77.1%, Figure 14 be nano anti-corrosive obtained by the present embodiment
Electrochemical impedance spectroscopy (EIS) figure of coating, Figure 15 are the Tafel polarization curve of nanometer anticorrosive coating obtained by the present embodiment
(Tafel) figure, corrosion electric current density are 0.52 μ A/cm2。
In above-described embodiment, graphene oxide/polyaniline/titanium dioxide nanometer that the mass fraction of titanium dioxide is 15%
Composite material has best photocatalytic degradation effect under full spectrum, and prepares by filler of the nanocomposite of the ratio
Water-repellent preservation nano paint be coated in aluminum alloy surface formation corrosion-inhibiting coating have best antiseptic property.
Claims (7)
1. graphene oxide/polyaniline/titanium dioxide nanocomposite preparation method, characterized in that comprising steps of
(1) using sodium hydroxide solution or ammonia spirit as dispersing agent, graphite oxide ultrasound is removed into obtain graphene oxide；
(2) graphene oxide is added to the organic sulfonic acid solution of aniline, stirring 10h ~ 16h obtains graphene oxide/polyaniline and receives
Nano composite material；
(3) nano-titanium dioxide is added to organic sulphur of the resulting graphene oxide/polyaniline nano-composite material of step (2)
In acid solution, stir 10h ~ 16h, successively through centrifugation, washing, dry graphene oxide/polyaniline/titanium dioxide is nano combined
Material.
2. graphene oxide as described in claim 1/polyaniline/titanium dioxide nanocomposite preparation method, special
Sign is:
The concentration of the sodium hydroxide solution or ammonia spirit is 0.01mol/L ~ 0.1mol/L.
3. graphene oxide as described in claim 1/polyaniline/titanium dioxide nanocomposite preparation method, special
Sign is:
The organic sulfonic acid solution of the aniline is the sulfosalisylic acid solution of aniline.
4. graphene oxide as described in claim 1/polyaniline/titanium dioxide nanocomposite preparation method, special
Sign is:
The mass ratio of the graphene oxide and aniline is (1 ~ 5): 1, and graphene oxide/polyaniline/titanium dioxide nanometer
The mass percent of nano-titanium dioxide is 5% ~ 20% in composite material.
5. the preparation method of polyaniline nano anticorrosive paint, characterized in that include:
Claim 1 gained graphene oxide/polyaniline/titanium dioxide nanocomposite is added to resin, it is agitated to obtain
Polyaniline nano anticorrosive paint.
6. the preparation method of polyaniline nano anticorrosive paint as claimed in claim 5, it is characterized in that:
Graphene oxide/polyaniline/titanium dioxide nanocomposite quality hundred in the polyaniline nano anticorrosive paint
Divide than being 1% ~ 10%.
7. the preparation method of polyaniline nano anticorrosive paint as claimed in claim 5, it is characterized in that:
The resin is aqueous epoxy resins.
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| CN110872457B (en) * | 2018-08-29 | 2022-04-08 | 中国石油化工股份有限公司 | Graphene and nano titanium dioxide composite coating and preparation method and application thereof |
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| CN110305565A (en) * | 2019-08-05 | 2019-10-08 | 大洋电力科技集团有限公司 | A kind of anticorrosive paint and preparation method thereof of defecation just pipeline |
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| CN112852260B (en) * | 2021-01-12 | 2022-06-10 | 江南大学 | Durable epoxy resin anticorrosive paint and preparation method and application thereof |
| CN114874437A (en) * | 2021-02-05 | 2022-08-09 | 贵州电网有限责任公司 | Preparation method of polyaniline graphene oxide composite material |
| CN113637386A (en) * | 2021-08-13 | 2021-11-12 | 贵州电网有限责任公司 | Anticorrosive paint for electric power iron tower and preparation method thereof |
| CN113773643A (en) * | 2021-08-13 | 2021-12-10 | 贵州电网有限责任公司 | Graphene oxide/polyaniline/titanium dioxide ternary nanocomposite, anticorrosive paint and preparation method |
| CN113549387A (en) * | 2021-08-13 | 2021-10-26 | 贵州电网有限责任公司 | Modified epoxy resin coating and preparation method thereof |
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