CN109957308A - A kind of corrosion-inhibiting coating and its processing technology based on graphene - Google Patents

A kind of corrosion-inhibiting coating and its processing technology based on graphene Download PDF

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CN109957308A
CN109957308A CN201910254076.XA CN201910254076A CN109957308A CN 109957308 A CN109957308 A CN 109957308A CN 201910254076 A CN201910254076 A CN 201910254076A CN 109957308 A CN109957308 A CN 109957308A
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corrosion
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inhibiting coating
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CN109957308B (en
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刘小龙
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GUANGDONG JULAN NOVEL MATERIAL TECHNOLOGY Co.,Ltd.
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刘小龙
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    • C—CHEMISTRY; METALLURGY
    • 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
    • C—CHEMISTRY; METALLURGY
    • 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
    • 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
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
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    • C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
    • C09D7/40—Additives
    • C09D7/60—Additives non-macromolecular
    • C09D7/61—Additives non-macromolecular inorganic
    • C—CHEMISTRY; METALLURGY
    • 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
    • C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
    • C09D7/40—Additives
    • C09D7/60—Additives non-macromolecular
    • C09D7/61—Additives non-macromolecular inorganic
    • C09D7/62—Additives non-macromolecular inorganic modified by treatment with other compounds
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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
    • C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
    • C09D7/40—Additives
    • C09D7/65—Additives macromolecular
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • 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
    • C08K2003/2248—Oxides; Hydroxides of metals of copper
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00—Use of inorganic substances as compounding ingredients
    • C08K3/30—Sulfur-, selenium- or tellurium-containing compounds
    • C08K2003/3045—Sulfates
    • C08K2003/3081—Aluminum sulfate
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00—Use of inorganic substances as compounding ingredients
    • C08K3/32—Phosphorus-containing compounds
    • C08K2003/329—Phosphorus containing acids
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2205/00—Polymer mixtures characterised by other features
    • C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend

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Abstract

The invention discloses a kind of raw materials such as corrosion-inhibiting coating and its processing technology based on graphene, including epoxy resin, polyaniline, modified graphene oxide, aluminum sulfate, selfreparing micro-capsule；Wherein using epoxy resin as film forming matter, using aluminum sulfate and polyaniline as additive, aluminum sulfate can prevent the immersion of corrosive medium, play the role of physical protection as inorganic filler；There are conjugated double bonds in the molecular structure of polyaniline, can form a kind of protective oxide in metal surface, be passivated metal, to reduce corrosion of metal effect；The present invention devises a kind of corrosion-inhibiting coating and its processing technology based on graphene, and reasonable mixture ratio of components realizes the selfreparing effect of corrosion-inhibiting coating, improve the service life of corrosion-inhibiting coating, Optimal Parameters technique, so that the anti-corrosion effect of coating is more outstanding, practicability with higher.

Description

A kind of corrosion-inhibiting coating and its processing technology based on graphene
Technical field
The present invention relates to corrosion-inhibiting coating field, specifically a kind of corrosion-inhibiting coating and its processing technology based on graphene.
Background technique
The interfacial reactions such as physics, chemistry, biology, electrochemistry, gold occur for the finger metal and surrounding medium of metal erosion Belong to original attribute change and caused by destruction；According to statistics, the annual whole world is produced because the steel that corrosion is scrapped accounts for about year steel The 20%-40% of amount, metal erosion will also result in the consumption of mass energy and resource while leading to direct economic loss, because This, becomes the hot spot that we pay close attention to always about metal erosion.
With research deeply and development, we start to coat erosion shield in metal surface, improve metal with this Corrosion-resistance properties, people have found again after this, and the metal for being coated with corrosion-inhibiting coating uses in the high temperature environment, due to water steam The presence of the factors such as gas, corrosive ions, corrosion-inhibiting coating are easy to that the local corrosions such as blistering, perforation, filiform corrosion occur, and use the longevity It orders short.
And the appearance of self-healing coating efficiently solves the problems, such as this, self-healing coating refers to the shielding effect in common coating On the basis of answering, coating is set to have the function of biological modeling self-healing by technological improvement.
In view of the above-mentioned problems, this patent devises a kind of corrosion-inhibiting coating and its processing technology based on graphene, Neng Gou Coating occurs to be automatically repaired coating when local corrosion, improves the service life of coating, this is our urgent problems to be solved.
Summary of the invention
The purpose of the present invention is to provide a kind of corrosion-inhibiting coating and its processing technology based on graphene, to solve existing skill The problems in art.
To achieve the above object, the invention provides the following technical scheme:
A kind of corrosion-inhibiting coating based on graphene, the corrosion-inhibiting coating each raw material component are as follows: by weight, epoxy resin 20- 80 parts, 6-18 parts of modified graphene oxide, 40-140 parts of solvent, 10-25 parts of selfreparing micro-capsule, 3-10 parts of additive.
More optimally, the modified graphene oxide is prepared by graphene oxide by modifier modification, the oxidation Graphene is aoxidized by graphene and is prepared.
More optimally, the selfreparing micro-capsule each raw material component is as follows: by weight, 2-5 parts of alkylbenzene sulfonate, phosphorus 3-6 parts sour, 20-40 parts of phenolic resin, 30-70 parts of tetraethyl orthosilicate.
More optimally, the modifying agent each raw material component is as follows: by weight, 10-20 parts of sodium borohydride, tetrahydrofuran 40-100 parts, 3-8 parts of iodine, 15-60 parts of dilute hydrochloric acid.
More optimally, the additive each raw material component is as follows: 5-15 parts of polyaniline, 3-10 parts of aluminum sulfate, pyridine 2-6 Part, 5-10 parts of copper oxide.
More optimally, the solvent includes toluene and n-butanol, and the mass ratio of the toluene and n-butanol is 1:(1- 1.5).
A kind of corrosion-inhibiting coating and its processing technology based on graphene, including epoxy resin, polyphenyl are devised in the present invention The raw materials such as amine, modified graphene oxide, aluminum sulfate, selfreparing micro-capsule；Wherein using epoxy resin as film forming matter, with sulfuric acid Aluminium and polyaniline are additive, and aluminum sulfate can prevent the immersion of corrosive medium as inorganic filler, play the work of physical protection With.
There are conjugated double bonds in the molecular structure of polyaniline, can form a kind of protective oxide in metal surface, make Metal passivation, to reduce corrosion of metal effect, while polyaniline small molecule structure can be filled into the hole of coating and lack Among falling into, enhance the compactness of coating, polyaniline draw ratio with higher is conducive to the evenly dispersed of conducting polymer, mentions The service life of high coating；The hydroxyl on polyaniline surface can be cross-linked with each other with the polar group in epoxy coating simultaneously, increase The strong adhesive force and bonding force of coating.
It is prepared for modified graphene oxide in the present invention, is aoxidized using graphene by strong oxidizer, obtained oxidation stone More hydroxyl, carboxyl and epoxy group are contained in black alkene surface, prepare modified graphene oxide by modifying agent in the present invention, modification Agent includes that the raw materials such as sodium borohydride, tetrahydrofuran, iodine, dilute hydrochloric acid using tetrahydrofuran as solvent pass through NaBH4/I2Reduction system Surface group reduction to graphene oxide, by the carboxyl of surface of graphene oxide, carbonyl reduction at alcohol radical, so that modified oxidized Graphene surface is flooded with a large amount of-OH group；The preparation of modified graphene oxide, not only can be improved coating in the present invention Mechanical property and wearability, while selfreparing micro-capsule can be cooperateed with to swash and realize self-repair procedure, that improves corrosion-inhibiting coating uses the longevity Life and Corrosion Protection.
It is added to selfreparing micro-capsule in the present invention, cyst wall is prepared using tetraethyl orthosilicate hydrolysate, by phenolic resin It is wrapped in phosphoric acid intracapsular, the selfreparing micro-capsule being prepared has preferable thermal stability and storage leakproofness, and selfreparing is micro- Capsule disperses in the epoxy, on the one hand to can effectively improve the wearability of coating, on the other hand, in metal coating by part When corrosion, selfreparing micro-capsule is damaged, and internal phenolic resin and phosphoric acid overflow, and corrosion-inhibiting coating is influenced by vapor, at this time Aluminum sulfate in coating can hydrolyze, and the aluminium hydroxide for hydrolyzing generation can generate Al (H with phosphatase reaction2PO4)3, simultaneously Aluminium hydroxide can decompose at high temperature generates Al2O3, at this time in the Al (H of copper oxide and generation2PO4)3It is modified oxidized under effect The hydroxyl of graphene surface is oxidized to aldehyde radical, and aldehyde radical can further reset generation enol structure, and the enol structure of generation can be with Al2O3, copper oxide, Al (H2PO4)3It is copolymerized generation macromolecular；Simultaneous oxidation copper, Al2O3It is also used as curing agent, with Al (H2PO4)3Reaction, the mix products of generation can be used as adhesive, carry out self-regeneration in the position of coating damage, improve The corrosion resistance of coating, service life are higher.
Meanwhile after selfreparing micro-capsule is broken, copper oxide, Al2O3As curing agent and Al (H2PO4)3During reaction, The organosilicon cyst wall of selfreparing micro-capsule can be dispersed in entire coating system, with the epoxy in the adhesive and coating of formation Resin is combined closely, and plays toughening effect to entire coating, improves the compression strength and wearability of coating.
Reaction mechanism are as follows: Al (OH)3+3H3PO4= Al (H2PO4)3+3H2O；
2Al(OH)3 = Al2O3 + 3H2O
More optimally, a kind of processing technology of the corrosion-inhibiting coating based on graphene, comprising the following steps:
1) prepare raw material；
2) modified graphene oxide is prepared；
3) selfreparing micro-capsule is prepared；
4) it is mixed, obtains the corrosion-inhibiting coating.
More optimally, comprising the following steps:
1) prepare raw material:
A) sodium borohydride, tetrahydrofuran, iodine, dilute hydrochloric acid, alkylbenzene sulfonate, phosphoric acid, phenolic resin, positive silicic acid are weighed in proportion Tetra-ethyl ester, epoxy resin, polyaniline, aluminum sulfate, pyridine and copper oxide, it is spare；
B) graphene is weighed in proportion, is dried, it is spare；
C) toluene, n-butanol are weighed in proportion, are uniformly mixed, solvent is prepared, it is spare；
2) modified graphene oxide is prepared:
A) prepare graphene oxide: the graphene for taking step 1) to prepare, strong oxidizer oxidation obtain graphene oxide；
B) graphene oxide for taking step a) to prepare is placed in a beaker, tetrahydrofuran dissolution, then the hydroboration for taking step 1) to prepare Sodium is put into beaker in batches, is quickly stirred, until gas stops evolution；It is again heated to 95-105 DEG C, tetrahydrofuran is slowly added dropwise Continue to stir, be slow added into dilute hydrochloric acid, mentioned after reaction with ether until gas stops evolution with the mixing liquid of iodine It takes, dry filter obtains modified graphene oxide；
3) selfreparing micro-capsule is prepared:
A) alkylbenzene sulfonate for taking step 1) to prepare, is placed in a beaker, adds phosphoric acid and phenolic resin, heating stirring is stirred Distilled water is slowly added dropwise after mixing uniformly, obtains material A；
B) tetraethyl orthosilicate for taking step 1) to prepare, is placed in hydrochloric acid solution, and heating water bath hydrolysis obtains material B；
C) material A for taking step 1) to prepare, the material B of addition step 2 preparation, hydrochloric acid adjust PH, are heated to 60-100 DEG C, it is stirred to react 2-4h, it is cooling, obtain the selfreparing micro-capsule；
4) preparation of coating:
A) polyaniline for taking step 1) to prepare, is placed in a beaker, and the solvent that step 1) prepares is added, stirring, then is placed in ultrasonic machine Middle ultrasonic disperse 2-3h, obtains material C；
B) epoxy resin for taking step 1) to prepare, is added the solvent dissolution that step 1) prepares, and stirring adds step a) preparation Material C, stirring, then the successively modified graphene oxide of investment step 2 preparation, the selfreparing micro-capsule of step 3) preparation, step 1) Aluminum sulfate, copper oxide, the pyridine of preparation, stirring, place into baking oven, vacuumize, obtain the corrosion-inhibiting coating.
More optimally, comprising the following steps:
1) prepare raw material:
A) sodium borohydride, tetrahydrofuran, iodine, dilute hydrochloric acid, alkylbenzene sulfonate, phosphoric acid, phenolic resin, positive silicic acid are weighed in proportion Tetra-ethyl ester, epoxy resin, polyaniline, aluminum sulfate, pyridine and copper oxide, it is spare；
B) graphene is weighed in proportion, and 70-80 DEG C of drying is spare；
C) toluene, n-butanol are weighed in proportion, are uniformly mixed, solvent is prepared, it is spare；In step 1), the present invention prepares The material that needs simultaneously carries out pre-processing work, convenient for the progress of subsequent step；
2) modified graphene oxide is prepared:
A) prepare graphene oxide: the graphene for taking step 1) to prepare, strong oxidizer oxidation obtain graphene oxide；This technology Graphene oxide is prepared first with the graphene of drying in scheme, is aoxidized using strong oxidizer, surface of graphene oxide With groups such as numerous hydroxyls, carboxyls, it is modified convenient for later use modifying agent；
B) graphene oxide for taking step a) to prepare is placed in a beaker, tetrahydrofuran dissolution, then the hydroboration for taking step 1) to prepare Sodium puts into beaker in batches, quickly stirs 20-30min, until gas stops evolution；It is again heated to 95-105 DEG C, is slowly added dropwise The mixing liquid of tetrahydrofuran and iodine continues to stir 2-3h until gas stops evolution, is slow added into dilute hydrochloric acid, reaction knot Shu Houyong extracted by ether, dry filter obtain modified graphene oxide；NaBH is utilized in the technical program4/I2Reduction system pair Graphene oxide is modified, and the groups such as the carboxyl of surface of graphene oxide, carbonyl are restored, alcoholic extract hydroxyl group is obtained；It is modified The alcoholic extract hydroxyl group of surface of graphene oxide can cooperate with oneself of the common progress coating of selfreparing micro-capsule effect in coating damage Repair；
3) selfreparing micro-capsule is prepared:
A) alkylbenzene sulfonate for taking step 1) to prepare, is placed in a beaker, adds phosphoric acid and phenolic resin, heating stirring 30- Distilled water is slowly added dropwise in 40min after mixing evenly, obtains material A；First with alkylbenzene sulfonate conduct in the technical program Surfactant prepares the capsule-core based on phenolic resin, phosphoric acid；
B) tetraethyl orthosilicate for taking step 1) to prepare, is placed in hydrochloric acid solution, and heating water bath hydrolysis obtains material B；
C) material A for taking step 1) to prepare, the material B of addition step 2 preparation, hydrochloric acid adjust PH to 2-4, are heated to 60- 100 DEG C, it is stirred to react 2-4h, it is cooling, obtain the selfreparing micro-capsule；Tetraethyl orthosilicate is placed in acid condition by the present invention Middle prehydrolysis, the organic alkane being prepared are coated on capsule-core surface as micro-capsule wall, selfreparing micro-capsule are prepared；
4) preparation of coating:
A) polyaniline for taking step 1) to prepare, is placed in a beaker, and the solvent that step 1) prepares is added, and stirs 15-20min, then set The ultrasonic disperse 2-3h in ultrasonic machine obtains material C；
B) epoxy resin for taking step 1) to prepare is added the solvent dissolution that step 1) prepares, stirs 20-25min, add step A) the material C prepared stirs 50-60min, then successively prepared by the modified graphene oxide of investment step 2 preparation, step 3) Aluminum sulfate, the copper oxide, pyridine that selfreparing micro-capsule, step 1) prepare, stir 40-50min, place into baking oven, vacuumize 15- 25min obtains the corrosion-inhibiting coating.The materials such as selfreparing micro-capsule, modified graphene oxide are put into epoxy in the technical program In resin, using epoxy resin as filmogen, corrosion-inhibiting coating is prepared.
Compared with prior art, the beneficial effects of the present invention are:
The invention firstly uses strong oxidizer graphene oxides, prepare graphene oxide, recycle reducing agent by graphene surface The groups such as carboxyl, carbonyl restored, the hydroxyl for restoring generation can cooperate selfreparing micro-capsule to realize coating selfreparing effect； Then ethyl orthosilicate hydrolyzed under acidic conditions is utilized in the technical program, the organosilicon of formation utilizes phenolic aldehyde tree as cyst wall Rouge and phosphoric acid mixing are used as capsule-core, and organosilicon is wrapped in capsule-core surface, when local corrosion occurs for coating, in selfreparing micro-capsule Phosphoric acid can be acted on components such as aluminum sulfate, modified graphene oxide, copper oxide in coating, realized selfreparing effect, improved The service life of coating.
The present invention devises a kind of corrosion-inhibiting coating and its processing technology based on graphene, and reasonable mixture ratio of components realizes The selfreparing effect of corrosion-inhibiting coating improves the service life of corrosion-inhibiting coating, Optimal Parameters technique, so that the anti-corrosion effect of coating is more Add outstanding, practicability with higher.
Specific embodiment
The technical scheme in the embodiments of the invention will be clearly and completely described below, it is clear that described implementation Example is only a part of the embodiment of the present invention, instead of all the embodiments.Based on the embodiments of the present invention, this field is common Technical staff's every other embodiment obtained without making creative work belongs to the model that the present invention protects It encloses.
Embodiment 1:
Prepare raw material first, weighs sodium borohydride, tetrahydrofuran, iodine, dilute hydrochloric acid, alkylbenzene sulfonate, phosphoric acid, phenolic aldehyde in proportion Resin, tetraethyl orthosilicate, epoxy resin, polyaniline, aluminum sulfate, pyridine and copper oxide, it is spare；Graphene is weighed in proportion, 70 DEG C of drying, it is spare；Toluene, n-butanol are weighed in proportion, are uniformly mixed, solvent is prepared, it is spare；
Modified graphene oxide is prepared again, takes graphene, and strong oxidizer oxidation obtains graphene oxide；Graphene oxide is taken to set In beaker, tetrahydrofuran dissolution, then sodium borohydride is taken, it puts into beaker in batches, quickly stirs 20min, until gas stops Evolution；95 DEG C are again heated to, the mixing liquid of tetrahydrofuran and iodine is slowly added dropwise, until gas stops evolution, continues to stir 2h, It is slow added into dilute hydrochloric acid, uses extracted by ether after reaction, dry filter obtains modified graphene oxide；
Then selfreparing micro-capsule is prepared, alkylbenzene sulfonate is taken, is placed in a beaker, phosphoric acid and phenolic resin are added, heating is stirred 30min is mixed, distilled water is slowly added dropwise after mixing evenly, obtains material A；Tetraethyl orthosilicate is taken, is placed in hydrochloric acid solution, water-bath Heating hydrolysis, obtains material B；Material A is taken, add materials B, and hydrochloric acid adjusts PH to 2, and 60 DEG C are heated to, 2h is stirred to react, It is cooling, obtain the selfreparing micro-capsule；
The preparation for finally carrying out coating, takes polyaniline, is placed in a beaker, and solvent is added, and stirs 15min, then be placed in ultrasonic machine Ultrasonic disperse 2h obtains material C；Extracting epoxy resin is added solvent dissolution, stirs 20min, add material C, stirs 50min, Modified graphene oxide, selfreparing micro-capsule, aluminum sulfate, copper oxide, pyridine are successively put into again, are stirred 40min, are placed into baking oven In, 15min is vacuumized, the corrosion-inhibiting coating is obtained.
In the present embodiment, corrosion-inhibiting coating each raw material component is as follows: by weight, 20 parts of epoxy resin, modified graphite oxide 6 parts of alkene, 40 parts of solvent, 10 parts of selfreparing micro-capsule, 3 parts of additive.
Wherein selfreparing micro-capsule each raw material component is as follows: by weight, 2 parts of alkylbenzene sulfonate, 3 parts of phosphoric acid, phenolic aldehyde tree 20 parts of rouge, 30 parts of tetraethyl orthosilicate；Modifying agent each raw material component is as follows: by weight, 10 parts of sodium borohydride, tetrahydrofuran 40 Part, 3 parts of iodine, 15 parts of dilute hydrochloric acid；Additive each raw material component is as follows: 5 parts of polyaniline, 3 parts of aluminum sulfate, 2 parts of pyridine, copper oxide 5 Part；Solvent includes toluene and n-butanol, and the mass ratio of the toluene and n-butanol is 1:1.
Embodiment 2:
Prepare raw material first, weighs sodium borohydride, tetrahydrofuran, iodine, dilute hydrochloric acid, alkylbenzene sulfonate, phosphoric acid, phenolic aldehyde in proportion Resin, tetraethyl orthosilicate, epoxy resin, polyaniline, aluminum sulfate, pyridine and copper oxide, it is spare；Graphene is weighed in proportion, 75 DEG C of drying, it is spare；Toluene, n-butanol are weighed in proportion, are uniformly mixed, solvent is prepared, it is spare；
Modified graphene oxide is prepared again, takes graphene, and strong oxidizer oxidation obtains graphene oxide；Graphene oxide is taken to set In beaker, tetrahydrofuran dissolution, then sodium borohydride is taken, it puts into beaker in batches, quickly stirs 25min, until gas stops Evolution；100 DEG C are again heated to, the mixing liquid of tetrahydrofuran and iodine is slowly added dropwise, until gas stops evolution, continues to stir 2.5h is slow added into dilute hydrochloric acid, uses extracted by ether after reaction, and dry filter obtains modified graphene oxide；
Then selfreparing micro-capsule is prepared, alkylbenzene sulfonate is taken, is placed in a beaker, phosphoric acid and phenolic resin are added, heating is stirred 35min is mixed, distilled water is slowly added dropwise after mixing evenly, obtains material A；Tetraethyl orthosilicate is taken, is placed in hydrochloric acid solution, water-bath Heating hydrolysis, obtains material B；Material A is taken, add materials B, and hydrochloric acid adjusts PH to 3, and 80 DEG C are heated to, 3h is stirred to react, It is cooling, obtain the selfreparing micro-capsule；
The preparation for finally carrying out coating, takes polyaniline, is placed in a beaker, and solvent is added, and stirs 18min, then be placed in ultrasonic machine Ultrasonic disperse 2.5h obtains material C；Extracting epoxy resin is added solvent dissolution, stirs 23min, add material C, stirs 55min, then modified graphene oxide, selfreparing micro-capsule, aluminum sulfate, copper oxide, pyridine are successively put into, 45min is stirred, is placed into In baking oven, 20min is vacuumized, obtains the corrosion-inhibiting coating.
In the present embodiment, corrosion-inhibiting coating each raw material component is as follows: by weight, 50 parts of epoxy resin, modified graphite oxide 10 parts of alkene, 60 parts of solvent, 20 parts of selfreparing micro-capsule, 5 parts of additive.
Wherein selfreparing micro-capsule each raw material component is as follows: by weight, 4 parts of alkylbenzene sulfonate, phosphatase 24 part, phenolic aldehyde tree 30 parts of rouge, 55 parts of tetraethyl orthosilicate；Modifying agent each raw material component is as follows: by weight, 15 parts of sodium borohydride, tetrahydrofuran 60 Part, 5 parts of iodine, 35 parts of dilute hydrochloric acid；Additive each raw material component is as follows: 5-15 parts of polyaniline, 8 parts of aluminum sulfate, 5 parts of pyridine, oxidation 8 parts of copper；Solvent includes toluene and n-butanol, and the mass ratio of the toluene and n-butanol is 1:1.2.
Embodiment 3:
Prepare raw material first, weighs sodium borohydride, tetrahydrofuran, iodine, dilute hydrochloric acid, alkylbenzene sulfonate, phosphoric acid, phenolic aldehyde in proportion Resin, tetraethyl orthosilicate, epoxy resin, polyaniline, aluminum sulfate, pyridine and copper oxide, it is spare；Graphene is weighed in proportion, 80 DEG C of drying, it is spare；Toluene, n-butanol are weighed in proportion, are uniformly mixed, solvent is prepared, it is spare；
Modified graphene oxide is prepared again, takes graphene, and strong oxidizer oxidation obtains graphene oxide；Graphene oxide is taken to set In beaker, tetrahydrofuran dissolution, then sodium borohydride is taken, it puts into beaker in batches, quickly stirs 30min, until gas stops Evolution；105 DEG C are again heated to, the mixing liquid of tetrahydrofuran and iodine is slowly added dropwise, until gas stops evolution, continues to stir 3h is slow added into dilute hydrochloric acid, uses extracted by ether after reaction, and dry filter obtains modified graphene oxide；
Then selfreparing micro-capsule is prepared, alkylbenzene sulfonate is taken, is placed in a beaker, phosphoric acid and phenolic resin are added, heating is stirred 40min is mixed, distilled water is slowly added dropwise after mixing evenly, obtains material A；Tetraethyl orthosilicate is taken, is placed in hydrochloric acid solution, water-bath Heating hydrolysis, obtains material B；Material A is taken, add materials B, and hydrochloric acid adjusts PH to 4, is heated to 100 DEG C, is stirred to react 4h, it is cooling, obtain the selfreparing micro-capsule；
The preparation for finally carrying out coating, takes polyaniline, is placed in a beaker, and solvent is added, and stirs 20min, then be placed in ultrasonic machine Ultrasonic disperse 3h obtains material C；Extracting epoxy resin is added solvent dissolution, stirs 25min, add material C, stirs 60min, Modified graphene oxide, selfreparing micro-capsule, aluminum sulfate, copper oxide, pyridine are successively put into again, are stirred 50min, are placed into baking oven In, 25min is vacuumized, the corrosion-inhibiting coating is obtained.
In the present embodiment, corrosion-inhibiting coating each raw material component is as follows: by weight, 80 parts of epoxy resin, modified graphite oxide 18 parts of alkene, 140 parts of solvent, 25 parts of selfreparing micro-capsule, 10 parts of additive.
Wherein selfreparing micro-capsule each raw material component is as follows: by weight, 5 parts of alkylbenzene sulfonate, 6 parts of phosphoric acid, phenolic aldehyde tree 40 parts of rouge, 70 parts of tetraethyl orthosilicate；Modifying agent each raw material component is as follows: by weight, 20 parts of sodium borohydride, tetrahydrofuran 100 parts, 8 parts of iodine, 60 parts of dilute hydrochloric acid；Additive each raw material component is as follows: 15 parts of polyaniline, 10 parts of aluminum sulfate, 6 parts of pyridine, oxygen Change 10 parts of copper；Solvent includes toluene and n-butanol, and the mass ratio of the toluene and n-butanol is 1:1.5.
Embodiment 4:
Prepare raw material first, weighs sodium borohydride, tetrahydrofuran, iodine, dilute hydrochloric acid, alkylbenzene sulfonate, phosphoric acid, phenolic aldehyde in proportion Resin, tetraethyl orthosilicate, epoxy resin, polyaniline, aluminum sulfate, pyridine and copper oxide, it is spare；Graphene is weighed in proportion, 75 DEG C of drying, it is spare；Toluene, n-butanol are weighed in proportion, are uniformly mixed, solvent is prepared, it is spare；
Selfreparing micro-capsule is prepared again, takes alkylbenzene sulfonate, is placed in a beaker, and phosphoric acid and phenolic resin, heating stirring are added Distilled water is slowly added dropwise in 35min after mixing evenly, obtains material A；Tetraethyl orthosilicate is taken, is placed in hydrochloric acid solution, water-bath adds Pyrohydrolysis obtains material B；Material A is taken, add materials B, and hydrochloric acid adjusts PH to 3, is heated to 80 DEG C, is stirred to react 3h, cold But, the selfreparing micro-capsule is obtained；
The preparation for finally carrying out coating, takes polyaniline, is placed in a beaker, and solvent is added, and stirs 18min, then be placed in ultrasonic machine Ultrasonic disperse 2.5h obtains material C；Extracting epoxy resin is added solvent dissolution, stirs 23min, add material C, stirs 55min, then graphene, selfreparing micro-capsule, aluminum sulfate, copper oxide, pyridine are successively put into, 45min is stirred, is placed into baking oven, 20min is vacuumized, the corrosion-inhibiting coating is obtained.
In the present embodiment, corrosion-inhibiting coating each raw material component is as follows: by weight, 50 parts of epoxy resin, 10 parts of graphene, molten 60 parts of agent, 20 parts of selfreparing micro-capsule, 5 parts of additive.
Wherein selfreparing micro-capsule each raw material component is as follows: by weight, 4 parts of alkylbenzene sulfonate, phosphatase 24 part, phenolic aldehyde tree 30 parts of rouge, 55 parts of tetraethyl orthosilicate；Additive each raw material component is as follows: 5-15 parts of polyaniline, 8 parts of aluminum sulfate, 5 parts of pyridine, 8 parts of copper oxide；Solvent includes toluene and n-butanol, and the mass ratio of the toluene and n-butanol is 1:1.2.
Embodiment 5:
Prepare raw material first, weighs sodium borohydride, tetrahydrofuran, iodine, dilute hydrochloric acid, alkylbenzene sulfonate, phosphoric acid, phenolic aldehyde in proportion Resin, tetraethyl orthosilicate, epoxy resin, polyaniline, aluminum sulfate, pyridine and copper oxide, it is spare；Graphene is weighed in proportion, 75 DEG C of drying, it is spare；Toluene, n-butanol are weighed in proportion, are uniformly mixed, solvent is prepared, it is spare；
The preparation for carrying out coating again, takes polyaniline, is placed in a beaker, and solvent is added, and stirs 18min, then is placed in ultrasonic machine and surpasses Sound disperses 2.5h, obtains material C；Extracting epoxy resin is added solvent dissolution, stirs 23min, add material C, stirs 55min, Graphene, aluminum sulfate, copper oxide, pyridine are successively put into again, are stirred 45min, are placed into baking oven, vacuumize 20min, obtain institute State corrosion-inhibiting coating.
In the present embodiment, corrosion-inhibiting coating each raw material component is as follows: by weight, 50 parts of epoxy resin, 10 parts of graphene, molten 60 parts of agent, 5 parts of additive.
Additive each raw material component is as follows: 5-15 parts of polyaniline, 8 parts of aluminum sulfate, 5 parts of pyridine, 8 parts of copper oxide；Solvent packet Include toluene and n-butanol, the mass ratio of the toluene and n-butanol is 1:1.2.
Experiment: the corrosion-inhibiting coating sample that Example 1-5 is prepared is respectively coated on aluminium sheet, and drying obtains sample 1-5。
Embodiment 1-3 is technical solution of the present invention, and graphene is not aoxidized and is modified in embodiment 4, is only prepared Selfreparing micro-capsule；Both modified graphene oxide is not prepared in embodiment 5, also without preparation selfreparing micro-capsule, wherein implementing In contrast example 1-3 is tested with embodiment 4, embodiment 5 respectively, from data in upper table:
Salt spray resistance, resistance to distilled water, resistance to 3%NaCl, the resistance to 10%H of the corrosion-inhibiting coating prepared in embodiment 1-32SO4, resistance to 5%NaOH Performance is better, and the service life of relatively conventional corrosion-inhibiting coating, coating is significantly improved, this is absolutely proved Rationally, process parameter optimizing can effectively improve the service life of corrosion-inhibiting coating for the formula design of technical solution of the present invention.
Graphene is not aoxidized and is modified in embodiment 4, is only prepared for selfreparing micro-capsule, remaining affecting parameters is not Become；In contrast embodiment 4 is tested with embodiment 1-3, compare data it is found that the corrosion-inhibiting coating of the preparation of embodiment 4 is in acid, alkali Property, the service life in neutral liquid be below the data in embodiment 1-3, this absolutely proved modified graphene oxide with from Repairing micro-capsule has synergistic effect, plays promotion to the repairing effect of selfreparing micro-capsule, further improves making for corrosion-inhibiting coating Use the service life.
Both modified graphene oxide is not prepared in embodiment 5, without preparation selfreparing micro-capsule, remaining affecting parameters is not yet Become；It is found that the service life of 5 floating coat of embodiment is significantly lower than the data in embodiment 1-4, this is absolutely proved correlation data Selfreparing micro-capsule, modified graphene oxide have an impact to the service life of coating, and anticorrosion of the selfreparing micro-capsule to coating The influence of performance is bigger.
It is obvious to a person skilled in the art that invention is not limited to the details of the above exemplary embodiments, Er Qie In the case where without departing substantially from spirit or essential attributes of the invention, the present invention can be realized in other specific forms.Therefore, no matter From the point of view of which point, the present embodiments are to be considered as illustrative and not restrictive, and the scope of the present invention is by appended power Benefit requires rather than above description limits, it is intended that all by what is fallen within the meaning and scope of the equivalent elements of the claims Variation is included within the present invention.

Claims (9)

1. a kind of corrosion-inhibiting coating based on graphene, it is characterised in that: the corrosion-inhibiting coating each raw material component is as follows: with weight Meter, 20-80 parts of epoxy resin, 6-18 parts of modified graphene oxide, 40-140 parts of solvent, 10-25 parts of selfreparing micro-capsule, additive 3-10 parts.
2. a kind of corrosion-inhibiting coating based on graphene according to claim 1, it is characterised in that: the modified graphite oxide Alkene is prepared by graphene oxide by modifier modification, and the graphene oxide is aoxidized by graphene and prepared.
3. a kind of corrosion-inhibiting coating based on graphene according to claim 2, it is characterised in that: the selfreparing micro-capsule is each Raw material components are as follows: by weight, 2-5 parts of alkylbenzene sulfonate, 3-6 parts of phosphoric acid, 20-40 parts of phenolic resin, positive silicic acid tetrem 30-70 parts of ester.
4. a kind of corrosion-inhibiting coating based on graphene according to claim 3, it is characterised in that: each raw material of modifying agent Component is as follows: by weight, 10-20 parts of sodium borohydride, 40-100 parts of tetrahydrofuran, 3-8 parts of iodine, 15-60 parts of dilute hydrochloric acid.
5. a kind of corrosion-inhibiting coating based on graphene according to claim 4, it is characterised in that: each raw material of additive Component is as follows: 5-15 parts of polyaniline, 3-10 parts of aluminum sulfate, 2-6 parts of pyridine, 5-10 parts of copper oxide.
6. a kind of corrosion-inhibiting coating based on graphene according to claim 5, it is characterised in that: the solvent includes toluene And n-butanol, the mass ratio of the toluene and n-butanol are 1:(1-1.5).
7. a kind of processing technology of the corrosion-inhibiting coating based on graphene, it is characterised in that: the following steps are included:
1) prepare raw material；
2) modified graphene oxide is prepared；
3) selfreparing micro-capsule is prepared；
4) it is mixed, obtains the corrosion-inhibiting coating.
8. a kind of processing technology of corrosion-inhibiting coating based on graphene according to claim 7, it is characterised in that: including with Lower step:
1) prepare raw material:
A) sodium borohydride, tetrahydrofuran, iodine, dilute hydrochloric acid, alkylbenzene sulfonate, phosphoric acid, phenolic resin, positive silicic acid are weighed in proportion Tetra-ethyl ester, epoxy resin, polyaniline, aluminum sulfate, pyridine and copper oxide, it is spare；
B) graphene is weighed in proportion, is dried, it is spare；
C) toluene, n-butanol are weighed in proportion, are uniformly mixed, solvent is prepared, it is spare；
2) modified graphene oxide is prepared:
A) prepare graphene oxide: the graphene for taking step 1) to prepare, strong oxidizer oxidation obtain graphene oxide；
B) graphene oxide for taking step a) to prepare is placed in a beaker, tetrahydrofuran dissolution, then the hydroboration for taking step 1) to prepare Sodium is put into beaker in batches, is quickly stirred, until gas stops evolution；It is again heated to 95-105 DEG C, tetrahydrofuran is slowly added dropwise Continue to stir, be slow added into dilute hydrochloric acid, mentioned after reaction with ether until gas stops evolution with the mixing liquid of iodine It takes, dry filter obtains modified graphene oxide；
3) selfreparing micro-capsule is prepared:
A) alkylbenzene sulfonate for taking step 1) to prepare, is placed in a beaker, adds phosphoric acid and phenolic resin, heating stirring is stirred Distilled water is slowly added dropwise after mixing uniformly, obtains material A；
B) tetraethyl orthosilicate for taking step 1) to prepare, is placed in hydrochloric acid solution, and heating water bath hydrolysis obtains material B；
C) material A for taking step 1) to prepare, the material B of addition step 2 preparation, hydrochloric acid adjust PH, are heated to 60-100 DEG C, it is stirred to react 2-4h, it is cooling, obtain the selfreparing micro-capsule；
4) preparation of coating:
A) polyaniline for taking step 1) to prepare, is placed in a beaker, and the solvent that step 1) prepares is added, stirring, then is placed in ultrasonic machine Middle ultrasonic disperse 2-3h, obtains material C；
B) epoxy resin for taking step 1) to prepare, is added the solvent dissolution that step 1) prepares, and stirring adds step a) preparation Material C, stirring, then the successively modified graphene oxide of investment step 2 preparation, the selfreparing micro-capsule of step 3) preparation, step 1) Aluminum sulfate, copper oxide, the pyridine of preparation, stirring, place into baking oven, vacuumize, obtain the corrosion-inhibiting coating.
9. a kind of processing technology of corrosion-inhibiting coating based on graphene according to claim 8, it is characterised in that: including with Lower step:
1) prepare raw material:
D) sodium borohydride, tetrahydrofuran, iodine, dilute hydrochloric acid, alkylbenzene sulfonate, phosphoric acid, phenolic resin, positive silicic acid are weighed in proportion Tetra-ethyl ester, epoxy resin, polyaniline, aluminum sulfate, pyridine and copper oxide, it is spare；
E) graphene is weighed in proportion, and 70-80 DEG C of drying is spare；
F) toluene, n-butanol are weighed in proportion, are uniformly mixed, solvent is prepared, it is spare；
2) modified graphene oxide is prepared:
C) prepare graphene oxide: the graphene for taking step 1) to prepare, strong oxidizer oxidation obtain graphene oxide；
D) graphene oxide for taking step a) to prepare is placed in a beaker, tetrahydrofuran dissolution, then the hydroboration for taking step 1) to prepare Sodium puts into beaker in batches, quickly stirs 20-30min, until gas stops evolution；It is again heated to 95-105 DEG C, is slowly added dropwise The mixing liquid of tetrahydrofuran and iodine continues to stir 2-3h until gas stops evolution, is slow added into dilute hydrochloric acid, reaction knot Shu Houyong extracted by ether, dry filter obtain modified graphene oxide；
3) selfreparing micro-capsule is prepared:
D) alkylbenzene sulfonate for taking step 1) to prepare, is placed in a beaker, adds phosphoric acid and phenolic resin, heating stirring 30- Distilled water is slowly added dropwise in 40min after mixing evenly, obtains material A；
E) tetraethyl orthosilicate for taking step 1) to prepare, is placed in hydrochloric acid solution, and heating water bath hydrolysis obtains material B；
F) material A for taking step 1) to prepare, the material B of addition step 2 preparation, hydrochloric acid adjust PH to 2-4, are heated to 60- 100 DEG C, it is stirred to react 2-4h, it is cooling, obtain the selfreparing micro-capsule；
4) preparation of coating:
C) polyaniline for taking step 1) to prepare, is placed in a beaker, and the solvent that step 1) prepares is added, and stirs 15-20min, then set The ultrasonic disperse 2-3h in ultrasonic machine obtains material C；
D) epoxy resin for taking step 1) to prepare is added the solvent dissolution that step 1) prepares, stirs 20-25min, add step A) the material C prepared stirs 50-60min, then successively prepared by the modified graphene oxide of investment step 2 preparation, step 3) Aluminum sulfate, the copper oxide, pyridine that selfreparing micro-capsule, step 1) prepare, stir 40-50min, place into baking oven, vacuumize 15- 25min obtains the corrosion-inhibiting coating.
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