CN107880776A - It is a kind of that the scattered method for preparing graphene anticorrosive paint is carried by dendritic macromole - Google Patents

It is a kind of that the scattered method for preparing graphene anticorrosive paint is carried by dendritic macromole Download PDF

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CN107880776A
CN107880776A CN201711120382.1A CN201711120382A CN107880776A CN 107880776 A CN107880776 A CN 107880776A CN 201711120382 A CN201711120382 A CN 201711120382A CN 107880776 A CN107880776 A CN 107880776A
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graphene
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anticorrosive paint
dendritic macromole
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陈庆
昝航
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Chengdu New Keli Chemical Science Co Ltd
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    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09DCOATING 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
    • C09D187/00Coating compositions based on unspecified macromolecular compounds, obtained otherwise than by polymerisation reactions only involving unsaturated carbon-to-carbon bonds
    • C09D187/005Block or graft polymers not provided for in groups C09D101/00 - C09D185/04
    • CCHEMISTRY; METALLURGY
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    • C08GMACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G83/00Macromolecular compounds not provided for in groups C08G2/00 - C08G81/00
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    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
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    • C09D5/00Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
    • C09D5/08Anti-corrosive paints
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    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
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    • C08K2003/2241Titanium dioxide
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    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00Use of inorganic substances as compounding ingredients
    • C08K3/32Phosphorus-containing compounds
    • C08K2003/321Phosphates
    • C08K2003/327Aluminium phosphate
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    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
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    • C08K3/34Silicon-containing compounds
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    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K5/00Use of organic ingredients
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    • C08K5/10Esters; Ether-esters

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Abstract

The present invention provides a kind of by the scattered method for preparing graphene anticorrosive paint of dendritic macromole carrying.It is proposed to carry dispersed graphite alkene using dendritic macromole and be configured in coating, because a variety of groups are contained on dendritic macromole surface, it can effectively adsorb, carry graphene, it is good with cold coating compatibility, the dispersiveness of graphene is improved, avoids its own reunion.Relative to the general process for dispersing of graphene in coating, the inventive method dispersion effect is more preferable, and can significantly lift graphene incorporation, preferably utilizes the excellent properties of graphene.

Description

It is a kind of that the scattered method for preparing graphene anticorrosive paint is carried by dendritic macromole
Technical field
The present invention relates to paint field, and in particular to a kind of carried by dendritic macromole disperses to prepare the painting of graphene anti-corrosion The method of material.
Background technology
Metal material is damaged by the effect of surrounding medium, referred to as metal erosion.The corrosion of metal is most common corrosion Form.During corrosion, there occurs chemistry or electrochemistry heterogeneous reaction on the interface of metal, metal is set to be transferred to oxidation (ion) shape State.This can significantly reduce the mechanical properties such as the intensity, plasticity, toughness of metal material, destroy the geometry of hardware, increase Add the abrasion between part, deteriorate the physical property such as electrical and optical, shorten the service life of equipment.Corrosion of metal phenomenon is very Generally, the corrosion of the wherein maximum metal-ironwork of dosage is most commonly seen.Causing the corrosion factor of metal material has a lot, its Include, salinity, temperature, pH value and microbiologic(al) corrosion in air or liquid.Conventional anti-corrosion measure is, in metallic surface One layer of anticorrosive paint is smeared, by metal and air insulated, reaches corrosion-resistant effect.
Anticorrosive paint, conventional anticorrosive paint and anticorrosive paint are generally divided into, are one kind essential in paint Coating.Conventional anticorrosive paint is under general condition, etch-proof effect, the longevity that protection non-ferrous metal uses to be played to metal etc. Life;It for anticorrosive paint refers to relatively conventional anticorrosive paint, can be applied in relatively harsh corrosive environment, and have and can reach A kind of anticorrosive paint of protection period longer than conventional anticorrosive paint.Anticorrosive paint is always one of important branch of coating, in work Using quite varied in industry production.In national economy production, the using of a large amount of metallic articles causes the requirement of equipment anticorrosion very Height, the market demand of anticorrosive paint, which is presented, persistently rises situation.
Graphene is thickness minimum, the species of maximum intensity in nano material.Because absorptance is very low, only 2.3%, institute It is almost fully transparent with outward appearance.Graphene excellent physical properties, heat conductivility are also higher than CNT and diamond, room temperature Its electron mobility exceedes CNT or silicon crystal under environment.Graphene is that electric conductivity is best in known materials on our times Material, resistivity is less than copper or silver.Graphene have concurrently specific surface area is big, good conductivity, chemical stability are strong, mechanical property and The advantages that excellent thermal conductivity, once appearance, just by the extensive concern of countries in the world.Graphene application is very wide, Coating is an important component in the numerous application fields of current graphene.Graphene has hydrophobic and lyophobic property in itself, its Lamellar structure has " labyrinth " effect, has excellent anti-corrosion barrier property, can hinder water, corrosive ion etc. to metal base Infiltration, delay the corrosion rate of metal base, so ground is played corrosion-resistant effect.Graphene leads to various coating resins It is compound to cross the methods such as physical blending, in-situ polymerization and sol-gel technique;Or modified with coupling agent, or using works such as in-situ polymerizations Skill.These techniques confirm feasible in modified aqueous paint, and performance improvement has certain effect.Nonetheless, graphene exists Apply to exist in anticorrosive paint and be difficult to the defects of scattered, itself can be produced and reunited, its scattered uniformity, compactness is destroyed, lead The obtained anticorrosion with coat effect of cause is poor, and barrier property is undesirable, and antiseptic property declines on the contrary.
Dendritic macromole is a kind of high regularity, three-dimensional structure, a kind of macromolecular with nanoscale.Branch Shape macromolecular is different from traditional polymer freely wound, and three parts are divided into structure:Kernel is originated, is connected in and originates kernel On the last layer functionalization group that is referred to as the repetitive structure in generation, is connected on dendritic macromole outermost layer repeat unit.Dendroid Macromolecular is a kind of real nanoscale molecular, its diameter range from G0 generations to G10 on behalf of 1~13 nm, dendritic macromole Structure, size, accurate size are controllable, and dendritic macromole can be grafted on graphenic surface by chemical bond, and this is graphene material Being greatly improved for dispersive property of material provides possibility with application extension.
Currently, carry out a series of research work for scattering problem of the graphene in coating, achieve some achievements, But graphene dispersion is improved and addition in coating is still limited, does not reach the requirement of modified anti-corrosive coating, stone Scattering problem of the black alkene in high incorporation is that one of key technology of graphene performance is played in anticorrosive paint.
The content of the invention
Excellent properties and graphene for graphene are applied to exist in anticorrosive paint is difficult to the defects of scattered, Yi Jishi The layer of black alkene easily again overlapping aggregation the defects of, technology art means are to carry graphene using carrier to be disperseed at present, but Carry less efficient, obtained properties of product are unstable.Based on this, the present invention proposes that a kind of carried by dendritic macromole is disperseed Graphene anticorrosive paint is prepared, realizes fine dispersion of the graphene in anticorrosive paint, lifts graphene incorporation, lifts anti-corrosion The performance of coating.
A kind of to carry the scattered method for preparing graphene anticorrosive paint by dendritic macromole, concrete technology step is as follows:
(1)Carboxylated processing
72% concentrated sulfuric acid is put 0 ~ 3 DEG C is cooled in ice water tank, be placed in ice-water bath in there-necked flask and sequentially add graphite powder, NaNO3 With the concentrated sulfuric acid, 10 ~ 30min of mechanic whirl-nett reaction;Potassium permanganate is slowly added to, control there-necked flask interior reaction temperature is at 10 ~ 15 DEG C Between, 1 ~ 2h of mechanic whirl-nett reaction;Then there-necked flask heating water bath is slowly dropped into distilled water and H to 80 ~ 95 DEG C2O2, machinery Stir 30 ~ 120min;After solution colour is changed into glassy yellow from burgundy, filters, washed with 5% hydrochloric acid solution while hot;Centrifugation Separate and be washed to solution by weakly acidic pH with distillation, 50 ~ 80 DEG C are dried in vacuo to obtain graphite oxide;The graphite powder, 72% dense sulphur Acid, NaNO3, potassium permanganate, H2O2, distilled water addition part by weight be:1:35~45:0.4~0.7:3~5:2~5:90~150;
Graphite oxide is dispersed in water, 10 ~ 30min of ultrasonic disperse, into uniform aaerosol solution, adds NaOH and monoxone Sodium, 1 ~ 2h of water bath sonicator, then neutralized with dilute HCl solution, the hydroxyl on graphene oxide and epoxy radicals is converted into carboxyl;Spend Ion is washed to neutrality, 50 ~ 80 DEG C of vacuum drying, obtains carboxylated graphene(CO-GOOH);The graphite oxide, H2O、 NaOH, the addition part by weight of sodium chloroacetate are:1:1000:40~50:45~60;
(2)Prepare Polyamidoamine Dendrimers-graphene
Ethylenediamine and methanol are added dropwise in the three-necked flask of nitrogen protection, magnetic agitation is uniform in ice-water bath;Add step Suddenly(1)Obtained carboxylated graphene, then be added dropwise to the methanol solution of methyl acrylate, 20 ~ 30 DEG C of reactions 6 stirred below ~ 24h;Then, solvent methanol and excessive raw material propylene acid methyl esters are removed at 50 DEG C, obtain Polyamidoamine Dendrimers- Graphene;
(3)The preparation of graphene anticorrosive paint
By step(2)Obtained Polyamidoamine Dendrimers-graphene 3-10 parts by weight, titanium dioxide 5-10 parts by weight, talcum Powder 10-15 parts by weight, different monooctyl ester 20-30 parts by weight, aluminium triphosphate 5-10 parts, Ludox 3-5 parts, 1.5 ~ 2.5 parts of propane diols, Water 20-30 parts by weight add sand mill 120 ~ 240min of sanded treatment, obtain graphene anticorrosive paint.
Preferably, step(2)The ethylenediamine, methanol, methyl acrylate, the addition part by weight of carboxylated graphene For:1:3~4:10~15:1.
Polyamidoamine Dendrimers are a kind of three-dimensional, novel macromolecules of high-sequential.Dendrimer with it is traditional Linear polymer has very big difference in structure, brings characteristics much different from linear polymer, and these characteristics all can not Explained with traditional polymer theoretical, thus the appearance of dendrimer is supplemented traditional polymer theoretical.Knot Close the chemical property of graphene, the dendritic polyamide-amide (PAMAM) and carboxylic of present invention selection polyamines active function groups Base graphite alkene reaction, polyamide-amide (PAMAM) are one of most ripe, most deep dendrimers of current research, and it both had There is the general character of dendrimer, there is the characteristic of itself again, be first tree with 3 D stereo spherical structure being reported Dendritic macromolecule.It is by initially triggering the internal layer that core, repeat unit form, the surface region three parts structure containing a large amount of functional groups Into because there is highly branched, high degree of symmetry and surface to contain unique design feature such as a large amount of functional groups for it.Due to dendroid Macromolecular surface contains a variety of groups, can effectively adsorb, carry graphene, so as to prevent graphene from reuniting in coating.
The present invention is a kind of to carry the scattered method for preparing graphene anticorrosive paint by dendritic macromole, with prior art phase Than, its protrude the characteristics of and excellent effect be:
1st, propose to carry dispersed graphite alkene using dendritic macromole first and be configured in coating, due to dendritic macromole table A variety of groups are contained in face, can effectively adsorb, carry graphene, good with cold coating compatibility, improve point of graphene Property is dissipated, avoids its own reunion.Relative to the general process for dispersing of graphene in coating, the inventive method dispersion effect is more preferable, and Graphene incorporation can be significantly lifted, preferably utilizes the excellent properties of graphene.
2nd, the present invention proposes a kind of graphene anticorrosive paint, has nontoxic, non-ignitable, easy for construction, fast drying, paint film machinery Intensity is high, adhesive force is strong, antiseptic property is excellent, the advantages that coating excellent storage stability.The coating train, automobile, ship, There is good applicability in terms of anticorrosion in the air of ferrous materials in the facilities such as bridge, pipeline, container, basin.
Embodiment
Below by way of embodiment, the present invention is described in further detail, but this should not be interpreted as to the present invention Scope be only limitted to following example.In the case where not departing from above method thought of the present invention, according to ordinary skill The various replacements or change that knowledge and customary means are made, should be included in the scope of the present invention.
Embodiment 1
A kind of to carry the scattered method for preparing graphene anticorrosive paint by dendritic macromole, concrete technology step is as follows:
(1)Carboxylated processing
72% concentrated sulfuric acid is put 0 ~ 3 DEG C is cooled in ice water tank, be placed in ice-water bath in there-necked flask and sequentially add graphite powder, NaNO3 With the concentrated sulfuric acid, mechanic whirl-nett reaction 10min;Be slowly added to potassium permanganate, control there-necked flask interior reaction temperature 10 ~ 15 DEG C it Between, mechanic whirl-nett reaction 1h;Then there-necked flask heating water bath is slowly dropped into distilled water and H to 80 DEG C2O2, mechanical agitation 30min;After solution colour is changed into glassy yellow from burgundy, filters, washed with 5% hydrochloric acid solution while hot;Centrifuge and be used in combination Distillation is washed to solution by weakly acidic pH, and 50 DEG C are dried in vacuo to obtain graphite oxide;The graphite powder, 72% concentrated sulfuric acid, NaNO3, Gao Meng Sour potassium, H2O2, distilled water addition part by weight be:1:35:0.4:3:2:90;
Graphite oxide is dispersed in water, 10 ~ 30min of ultrasonic disperse, into uniform aaerosol solution, adds NaOH and monoxone Sodium, 1 ~ 2h of water bath sonicator, then neutralized with dilute HCl solution, the hydroxyl on graphene oxide and epoxy radicals is converted into carboxyl;Spend Ion is washed to neutrality, 50 DEG C of vacuum drying, obtains carboxylated graphene(CO-GOOH);The graphite oxide, H2O、NaOH、 The addition part by weight of sodium chloroacetate is:1:1000:40:45;
(2)Prepare Polyamidoamine Dendrimers-graphene
Ethylenediamine and methanol are added dropwise in the three-necked flask of nitrogen protection, magnetic agitation is uniform in ice-water bath;Add step Suddenly(1)Obtained carboxylated graphene, then the methanol solution of methyl acrylate is added dropwise to, in 20 ~ 30 DEG C of reaction 6h stirred below; Then, solvent methanol and excessive raw material propylene acid methyl esters are removed at 50 DEG C, obtains Polyamidoamine Dendrimers-graphite Alkene;The ethylenediamine, methanol, methyl acrylate, the addition part by weight of carboxylated graphene are:1:3:10:1;
(3)The preparation of graphene anticorrosive paint
By step(2)Obtained parts by weight of Polyamidoamine Dendrimers-graphene 5, the parts by weight of titanium dioxide 5, the weight of talcum powder 10 Measure part, the parts by weight of different monooctyl ester 20,5 parts of aluminium triphosphate, 3 parts of Ludox, 1.55 parts of propane diols, the parts by weight of water 20 addition sand mill Sanded treatment 120min, obtain graphene anticorrosive paint.
It is manufactured in the present embodiment a kind of by dendritic macromole carrying dispersed graphite alkene anticorrosive paint, its performance test such as table Shown in 1.
Embodiment 2
A kind of to carry the scattered method for preparing graphene anticorrosive paint by dendritic macromole, concrete technology step is as follows:
(1)Carboxylated processing is same as Example 1;
(2)Prepare Polyamidoamine Dendrimers-graphene
Ethylenediamine and methanol are added dropwise in the three-necked flask of nitrogen protection, magnetic agitation is uniform in ice-water bath;Add step Suddenly(1)Obtained carboxylated graphene, then the methanol solution of methyl acrylate is added dropwise to, in 20 ~ 30 DEG C of reactions stirred below 10h;Then, solvent methanol and excessive raw material propylene acid methyl esters are removed at 50 DEG C, obtain Polyamidoamine Dendrimers- Graphene;The ethylenediamine, methanol, methyl acrylate, the addition part by weight of carboxylated graphene are:1:4:15:1;
(3)The preparation of graphene anticorrosive paint
By step(2)Obtained parts by weight of Polyamidoamine Dendrimers-graphene 10, the parts by weight of titanium dioxide 10, talcum powder 15 Parts by weight, the parts by weight of different monooctyl ester 30,10 parts of aluminium triphosphate, 5 parts of Ludox, 2.5 parts of propane diols, the parts by weight of water 30, which add, to be sanded Machine sanded treatment 240min, obtains graphene anticorrosive paint.
It is manufactured in the present embodiment a kind of by dendritic macromole carrying dispersed graphite alkene anticorrosive paint, its performance test such as table Shown in 1.
Embodiment 3
A kind of to carry the scattered method for preparing graphene anticorrosive paint by dendritic macromole, concrete technology step is as follows:
(1)Carboxylated processing is same as Example 1
(2)It is same as Example 2 to prepare Polyamidoamine Dendrimers-graphene
(3)The preparation of graphene anticorrosive paint
By step(2)Obtained parts by weight of Polyamidoamine Dendrimers-graphene 10, the parts by weight of titanium dioxide 5, talcum powder 10 Parts by weight, the parts by weight of different monooctyl ester 25,10 parts of aluminium triphosphate, 5 parts of Ludox, 2.5 parts of propane diols, the parts by weight of water 30, which add, to be sanded Machine sanded treatment 120min, obtains graphene anticorrosive paint.
It is manufactured in the present embodiment a kind of by dendritic macromole carrying dispersed graphite alkene anticorrosive paint, its performance test such as table Shown in 1.
Embodiment 4
A kind of to carry the scattered method for preparing graphene anticorrosive paint by dendritic macromole, concrete technology step is as follows:
(1)Carboxylated processing
72% concentrated sulfuric acid is put 0 ~ 3 DEG C is cooled in ice water tank, be placed in ice-water bath in there-necked flask and sequentially add graphite powder, NaNO3 With the concentrated sulfuric acid, 10 ~ 30min of mechanic whirl-nett reaction;Potassium permanganate is slowly added to, control there-necked flask interior reaction temperature is at 10 ~ 15 DEG C Between, mechanic whirl-nett reaction 2h;Then there-necked flask heating water bath is slowly dropped into distilled water and H to 80 ~ 95 DEG C2O2, machinery stirs Mix 120min;After solution colour is changed into glassy yellow from burgundy, filters, washed with 5% hydrochloric acid solution while hot;Centrifuge And solution is washed to by weakly acidic pH with distillation, 80 DEG C are dried in vacuo to obtain graphite oxide;The graphite powder, 72% concentrated sulfuric acid, NaNO3、 Potassium permanganate, H2O2, distilled water addition part by weight be:1:45:0.7:5:2:90;
Graphite oxide is dispersed in water, 10 ~ 30min of ultrasonic disperse, into uniform aaerosol solution, adds NaOH and monoxone Sodium, water bath sonicator 2h, then neutralized with dilute HCl solution, the hydroxyl on graphene oxide and epoxy radicals is converted into carboxyl;Spend from Son is washed to neutrality, 50 ~ 80 DEG C of vacuum drying, obtains carboxylated graphene(CO-GOOH);The graphite oxide, H2O、NaOH、 The addition part by weight of sodium chloroacetate is:1:1000:50:60;
(2)Prepare Polyamidoamine Dendrimers-graphene
Ethylenediamine and methanol are added dropwise in the three-necked flask of nitrogen protection, magnetic agitation is uniform in ice-water bath;Add step Suddenly(1)Obtained carboxylated graphene, then the methanol solution of methyl acrylate is added dropwise to, in 20 ~ 30 DEG C of reactions stirred below 24h;Then, solvent methanol and excessive raw material propylene acid methyl esters are removed at 50 DEG C, obtain Polyamidoamine Dendrimers- Graphene;The ethylenediamine, methanol, methyl acrylate, the addition part by weight of carboxylated graphene are:1:3:15:1;
(3)The preparation of graphene anticorrosive paint
By step(2)Obtained parts by weight of Polyamidoamine Dendrimers-graphene 10, the parts by weight of titanium dioxide 10, talcum powder 105 parts by weight, the parts by weight of different monooctyl ester 20, the parts by weight of aluminium triphosphate 10, the parts by weight of Ludox 5, the parts by weight of propane diols 1.5, water 20 parts by weight add sand mill 120 ~ 240min of sanded treatment, obtain graphene anticorrosive paint.
It is manufactured in the present embodiment a kind of by dendritic macromole carrying dispersed graphite alkene anticorrosive paint, its performance test such as table Shown in 1.
Comparative example 1
A kind of method for preparing graphene anticorrosive paint, concrete technology step are as follows:
(1)Carboxylated processing
72% concentrated sulfuric acid is put 0 ~ 3 DEG C is cooled in ice water tank, be placed in ice-water bath in there-necked flask and sequentially add graphite powder, NaNO3 With the concentrated sulfuric acid, 10 ~ 30min of mechanic whirl-nett reaction;Potassium permanganate is slowly added to, control there-necked flask interior reaction temperature is at 10 ~ 15 DEG C Between, mechanic whirl-nett reaction 2h;Then there-necked flask heating water bath is slowly dropped into distilled water and H to 80 ~ 95 DEG C2O2, machinery stirs Mix 120min;After solution colour is changed into glassy yellow from burgundy, filters, washed with 5% hydrochloric acid solution while hot;Centrifuge And solution is washed to by weakly acidic pH with distillation, 80 DEG C are dried in vacuo to obtain graphite oxide;The graphite powder, 72% concentrated sulfuric acid, NaNO3、 Potassium permanganate, H2O2, distilled water addition part by weight be:1:45:0.7:5:2:90;
Graphite oxide is dispersed in water, 10 ~ 30min of ultrasonic disperse, into uniform aaerosol solution, adds NaOH and monoxone Sodium, water bath sonicator 2h, then neutralized with dilute HCl solution, the hydroxyl on graphene oxide and epoxy radicals is converted into carboxyl;Spend from Son is washed to neutrality, 50 ~ 80 DEG C of vacuum drying, obtains carboxylated graphene(CO-GOOH);The graphite oxide, H2O、NaOH、 The addition part by weight of sodium chloroacetate is:1:1000:50:60;
(2)The preparation of graphene anticorrosive paint
By step(1)Obtained parts by weight of carboxylated graphene 10, the parts by weight of titanium dioxide 10, the parts by weight of talcum powder 105, different monooctyl ester 20 parts by weight, the parts by weight of aluminium triphosphate 10, the parts by weight of Ludox 5, the parts by weight of propane diols 1.5, the parts by weight of water 20, which add, to be sanded Machine 120 ~ 240min of sanded treatment, obtains graphene anticorrosive paint.
The anticorrosive paint that embodiment 1-4, comparative example 1 are obtained applies test, is analyzed, as shown in table 1.
Table 1:
As seen from Table 1, a kind of graphene anticorrosive paint by the scattered preparation of dendritic macromole carrying has good resist Acid and alkali corrosion, salt fog resistance burn into is water-fast, and heat resistance is good.

Claims (2)

1. a kind of carry the scattered method for preparing graphene anticorrosive paint by dendritic macromole, concrete technology step is as follows:
(1)Carboxylated processing
72% concentrated sulfuric acid is put 0 ~ 3 DEG C is cooled in ice water tank, be placed in ice-water bath in there-necked flask and sequentially add graphite powder, NaNO3 With the concentrated sulfuric acid, 10 ~ 30min of mechanic whirl-nett reaction;Potassium permanganate is slowly added to, control there-necked flask interior reaction temperature is at 10 ~ 15 DEG C Between, 1 ~ 2h of mechanic whirl-nett reaction;Then there-necked flask heating water bath is slowly dropped into distilled water and H to 80 ~ 95 DEG C2O2, machinery Stir 30 ~ 120min;After solution colour is changed into glassy yellow from burgundy, filters, washed with 5% hydrochloric acid solution while hot;Centrifugation Separate and be washed to solution by weakly acidic pH with distillation, 50 ~ 80 DEG C are dried in vacuo to obtain graphite oxide;The graphite powder, 72% dense sulphur Acid, NaNO3, potassium permanganate, H2O2, distilled water addition part by weight be:1:35~45:0.4~0.7:3~5:2~5:90~150;
Graphite oxide is dispersed in water, 10 ~ 30min of ultrasonic disperse, into uniform aaerosol solution, adds NaOH and monoxone Sodium, 1 ~ 2h of water bath sonicator, then neutralized with dilute HCl solution, the hydroxyl on graphene oxide and epoxy radicals is converted into carboxyl;Spend Ion is washed to neutrality, 50 ~ 80 DEG C of vacuum drying, obtains carboxylated graphene(CO-GOOH);The graphite oxide, H2O、 NaOH, the addition part by weight of sodium chloroacetate are:1:1000:40~50:45~60;
(2)Prepare Polyamidoamine Dendrimers-graphene
Ethylenediamine and methanol are added dropwise in the three-necked flask of nitrogen protection, magnetic agitation is uniform in ice-water bath;Add step Suddenly(1)Obtained carboxylated graphene, then be added dropwise to the methanol solution of methyl acrylate, 20 ~ 30 DEG C of reactions 6 stirred below ~ 24h;Then, solvent methanol and excessive raw material propylene acid methyl esters are removed at 50 DEG C, obtain Polyamidoamine Dendrimers- Graphene;
(3)The preparation of graphene anticorrosive paint
By step(2)Obtained Polyamidoamine Dendrimers-graphene 3-10 parts by weight, titanium dioxide 5-10 parts by weight, talcum Powder 10-15 parts by weight, different monooctyl ester 20-30 parts by weight, aluminium triphosphate 5-10 parts, Ludox 3-5 parts, 1.5 ~ 2.5 parts of propane diols, Water 20-30 parts by weight add sand mill 120 ~ 240min of sanded treatment, obtain graphene anticorrosive paint.
2. a kind of according to claim 1 carry the scattered method for preparing graphene anticorrosive paint by dendritic macromole, its It is characterised by:Step(2)The ethylenediamine, methanol, methyl acrylate, the addition part by weight of carboxylated graphene are:1:3~ 4:10~15:1.
CN201711120382.1A 2017-11-14 2017-11-14 It is a kind of that the scattered method for preparing graphene anticorrosive paint is carried by dendritic macromole Withdrawn CN107880776A (en)

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CN110903506A (en) * 2019-12-19 2020-03-24 哈尔滨工业大学 Preparation method of dendritic macromolecule reinforced porous graphene oxide paper
CN112625647A (en) * 2020-12-18 2021-04-09 北京创盈光电医疗科技有限公司 High-heat-resistance LED packaging adhesive and preparation method thereof
CN112646624A (en) * 2020-11-30 2021-04-13 青岛科技大学 Method for promoting efficient generation of methane hydrate by graphene composite hydrogel
CN112979208A (en) * 2021-03-29 2021-06-18 鸡西瀚宇石墨烯科技有限公司 Preparation method and preparation device of graphene cement additive
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CN114990898A (en) * 2022-06-09 2022-09-02 王正文 High-elasticity wear-resistant fabric and preparation method thereof
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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110903506A (en) * 2019-12-19 2020-03-24 哈尔滨工业大学 Preparation method of dendritic macromolecule reinforced porous graphene oxide paper
CN112646624A (en) * 2020-11-30 2021-04-13 青岛科技大学 Method for promoting efficient generation of methane hydrate by graphene composite hydrogel
CN112625647A (en) * 2020-12-18 2021-04-09 北京创盈光电医疗科技有限公司 High-heat-resistance LED packaging adhesive and preparation method thereof
CN112979208A (en) * 2021-03-29 2021-06-18 鸡西瀚宇石墨烯科技有限公司 Preparation method and preparation device of graphene cement additive
CN114990898A (en) * 2022-06-09 2022-09-02 王正文 High-elasticity wear-resistant fabric and preparation method thereof
CN114889282A (en) * 2022-06-16 2022-08-12 启明新材料股份有限公司 Antibacterial high-barrier multilayer co-extrusion BOPP (biaxially-oriented polypropylene) optical film
CN114889282B (en) * 2022-06-16 2024-05-10 启明新材料股份有限公司 Antibacterial high-barrier multilayer co-extrusion BOPP light film
CN116487090A (en) * 2023-02-23 2023-07-25 深圳市贝加电子材料有限公司 Graphene conductive solution and preparation method and application thereof

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