CN107955499A - A kind of anticorrosive paint and its preparation process - Google Patents

A kind of anticorrosive paint and its preparation process Download PDF

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Publication number
CN107955499A
CN107955499A CN201711357576.3A CN201711357576A CN107955499A CN 107955499 A CN107955499 A CN 107955499A CN 201711357576 A CN201711357576 A CN 201711357576A CN 107955499 A CN107955499 A CN 107955499A
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parts
anticorrosive paint
powder
small
includes following
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顾建强
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Suzhou Saiside Engineering Equipment Co Ltd
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Suzhou Saiside Engineering Equipment Co Ltd
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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
    • 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
    • C08K3/24—Acids; Salts thereof
    • C08K3/26—Carbonates; Bicarbonates
    • C08K2003/265—Calcium, strontium or barium carbonate
    • 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
    • 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
    • C08K2201/00—Specific properties of additives
    • C08K2201/011—Nanostructured additives
    • 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
    • C08K2201/00—Specific properties of additives
    • C08K2201/014—Additives containing two or more different additives of the same subgroup in C08K
    • 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
    • C08L2205/02—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
    • C08L2205/025—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group containing two or more polymers of the same hierarchy C08L, and differing only in parameters such as density, comonomer content, molecular weight, structure
    • 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
    • C08L2205/035—Polymer mixtures characterised by other features containing three or more polymers in a blend containing four or more polymers in a blend

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  • Chemical & Material Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Wood Science & Technology (AREA)
  • Organic Chemistry (AREA)
  • Paints Or Removers (AREA)

Abstract

The invention discloses a kind of anticorrosive paint, which includes first and second liang of components, counts first in mass ratio：Second=3:1 ratio mixing, first component include following components：Aqueous epoxy resins, water, graphene/polypyrrole polymers, filler, curing agent, dispersant, defoamer, levelling agent, compound rare-earth are silane coupling agent；Second component includes following components：20 epoxy resin of E, silicon carbide micro-powder, toluene diisocyanate vinegar prepolymer, nano-titanium dioxide, propylene glycol n-butyl ether, organotin catalysts, Intumescent Retardant System, dioctyl phthalate, SiO2Aeroge；The present invention also designs a kind of anticorrosive paint and its preparation process, and preparation is simple for this, and the coating prepared has good antiseptic property, extends its service life, reduces cost.

Description

A kind of anticorrosive paint and its preparation process
Technical field
The present invention relates to a kind of coating, and in particular to a kind of anticorrosive paint and its preparation process.
Background technology
With the progress and development of science and technology, one of the three big leading industries of new material as 21 century, it is clear that particularly Important, the industrial progress and development, coating that also represent country to a certain extent are mostly important as resistant material One of field.
Coating is to be coated on body surface to form film under certain conditions and play protection, decoration or other special work( Can, such as insulation, antirust, mould proof, heat-resisting a kind of liquid or solid material, the species of coating is very much, it is formulated different institute's energy The specific function reached is with regard to different.
Anticorrosive paint currently on the market is mainly used for steel industry and machinery industry, and anti-corrosion is frequently encountered in equipment Problem, for extending the service life of equipment, reduces cost, but anticorrosive paint antiseptic property of the prior art is weak, maintains Not how long.
The content of the invention
The technical problems to be solved by the invention are that the shortcoming existing in the prior art for more than, proposes that a kind of anti-corrosion applies Material and its preparation process, preparation is simple for this, and the coating prepared has good antiseptic property, extends it and uses the longevity Life, reduces cost.
The present invention solve above technical problem technical solution be：
A kind of anticorrosive paint, the anticorrosive paint include first and second liang of components, count first in mass ratio：Second=3:1 ratio mixing, wherein：
First component includes following components according to the mass fraction：
Aqueous epoxy resins：20-30 parts, water：25-30 parts, graphene/polypyrrole polymers：5-10 parts, filler：5-10 parts, Gu Agent：5-10 parts, dispersant：1-2 parts, defoamer：0.5-1 parts, levelling agent：0.5-1 parts, compound rare-earth is：0.1-0.3 parts, Silane coupling agent：2-5 parts；
Compound rare-earth includes following component by weight percentage： Y：13-15%, Sc：16-18%, Gd：9-11%, Sm：18-20%, Pr：The sum of 9-11%, surplus La, the above components are 100%；
Second component includes following components according to the mass fraction：
E-20 epoxy resin：10-15 parts, silicon carbide micro-powder：15-25 parts, toluene diisocyanate vinegar prepolymer：11-15 parts, nanometer Titanium dioxide：3-5 parts, propylene glycol n-butyl ether：3-5 parts, organotin catalysts：2-4 parts, Intumescent Retardant System：4-7 parts, adjacent benzene Diformazan dioctyl phthalate：1-2 parts, SiO2Aeroge：5-8 parts.
The technical solution that further limits of the present invention as：
In foregoing anticorrosive paint, filler is barium sulfate, talcum powder, the mixture of barium carbonate, is in mass ratio barium sulfate：Talcum Powder：Barium carbonate=1:1:1；Curing agent is m-phenylene diamine (MPD), one kind in diethylenetriamine, polyamide；Dispersant disperses for BYK190 Agent；Defoamer is dimethicone, one kind in organosilicon, polyvinyl acetate；Levelling agent is dimethyl silicone polymer, poly- first One kind in base phenyl siloxane or acrylic acid.
In foregoing anticorrosive paint, Intumescent Retardant System is in terms of mass fraction including following components：Ammonium polyphosphate：20-30 parts, Melamine：10-15 parts, pentaerythrite：5-10 parts.
In foregoing anticorrosive paint, toluene diisocyanate vinegar prepolymer is prepared according to the following steps：
Ethanedioic acid, trimethylolpropane, diglycol are uniformly mixed, dimethylbenzene is then added and continues to be uniformly mixing to obtain Linear polyester, by linear polyester and toluene di-isocyanate(TDI), butyl acetate, dimethylbenzene input reactor, counts line in mass ratio Property polyester：Toluene di-isocyanate(TDI)：Butyl acetate：Dimethylbenzene=20:13:14:5,15-20min is stirred, is to slowly warm up to 70-80 DEG C, 1-2h is reacted, is continuously heating to 85-90 DEG C, after keeping the temperature 1h, less than 50 DEG C is down to and obtains toluene diisocyanate vinegar prepolymer.
In foregoing anticorrosive paint, the preparation method of graphene/polypyrrole polymers is：
（1）By graphite powder, sodium nitrate, is added in the concentrated sulfuric acid and stirs, wherein the mass ratio of graphite powder and sodium nitrate For 1:1-3；
（2）Above-mentioned solution is transferred in ice-water bath, while stirring, while being slowly added to potassium permanganate and keeping solution temperature not More than 0 DEG C, and at 0 DEG C stand 2-3 it is small when；
（3）By above-mentioned steps（2）In mixture be transferred in reaction kettle, at 100-110 DEG C, reaction 2-3 it is small when, reaction knot Beam cooled to room temperature, supernatant liquor of going out, obtains viscous fluid, and stir 10-15 it is small when, obtain mixture of viscous form；
（4）To above-mentioned steps（3）Add water in mixture of viscous form, and instill 30% hydrogen peroxide under agitation until There is no bubble generation, stirring 20-30min centrifugations, then filter cake is washed 2-3 times with the hydrochloric acid solution of 1mol/L, finally with anhydrous Ethanol cleans filter cake repeatedly, and filter cake dries at 30-35 DEG C and obtains graphene oxide powder；
（5）By above-mentioned steps（4）In graphene oxide when being added to that ultrasonic disperse 2-3 is small in dilute hydrochloric acid, add polypyrrole Ketone, when continuation ultrasonic disperse 1-2 is small, obtains burgundy stably dispersing suspension, wherein graphene oxide and polypyrrole ketone quality Than for 1:1-1.5；
（6）By above-mentioned steps（5）In suspension be placed in ice bath, and pyrrole monomer is added dropwise into suspension, stirring reaction 1-2 Hour, obtain graphene oxide/pyrroles/mixed in hydrochloric acid liquid system；
（7）To above-mentioned steps（6）The aqueous solution of ammonium persulfate, stirring are added dropwise in graphene oxide/pyrroles/mixed in hydrochloric acid liquid system When reaction 20-25 is small；
（8）By above-mentioned steps（7）When the static 5-8 of mixed system is small, is washed repeatedly to filtrate using acetone, deionized water successively and be in It is colourless, obtain graphene oxide/polypyrrole；
（9）To above-mentioned steps（8）Middle graphene oxide/polypyrrole solution is added dropwise ammonium hydroxide and adjusts PH to 10-11, adds hydration Hydrazine, stirs 20-40min, is uniformly mixed solution, reflux is warming up to, when back flow reaction 20-24 is small；
（10）By above-mentioned steps（9）In reaction solution be cooled to room temperature suction filtration, with acetone and water washing filter cake, finally in 45 DEG C of bakings It is dry to obtain graphene/polypyrrole polymers.
Technique effect, graphene/polypyrrole polymers of the present invention can improve the dispersiveness of aqueous epoxy resins, improve water The antiseptic property of property epoxy resin；Polypyrrole even particulate dispersion spherical in shape is in graphene sheet layer and edge in the present invention, in stone Compound quantity bigger at the defects of black alkene lamella, the defects of compensate for graphene layer to a certain extent；Modified graphene asphalt mixtures modified by epoxy resin Grease coating material has relatively low corrosion rate and higher coating stability.
In foregoing anticorrosive paint, which includes first and second liang of components, counts first in mass ratio：Second=3:1 ratio is mixed Close, wherein：
First component includes following components according to the mass fraction：
Aqueous epoxy resins：20 parts, water：25 parts, graphene/polypyrrole polymers：5 parts, filler：5 parts, curing agent：5 parts, point Powder：1 part, defoamer：0.5 part, levelling agent：0.5 part, compound rare-earth is：0.1 part, silane coupling agent：2 parts；
Compound rare-earth includes following component by weight percentage： Y：13%, Sc：16%, Gd：9%, Sm：18%, Pr：9%, surplus is The sum of La, the above components is 100%；
Second component includes following components according to the mass fraction：
E-20 epoxy resin：10 parts, silicon carbide micro-powder：15 parts, toluene diisocyanate vinegar prepolymer：11 parts, nano-titanium dioxide： 3 parts, propylene glycol n-butyl ether：3 parts, organotin catalysts：2 parts, Intumescent Retardant System：4 parts, dioctyl phthalate：1 part, SiO2Aeroge：5 parts.
In foregoing anticorrosive paint, which includes first and second liang of components, counts first in mass ratio：Second=3:1 ratio is mixed Close, wherein：
First component includes following components according to the mass fraction：
Aqueous epoxy resins：30 parts, water：30 parts, graphene/polypyrrole polymers：10 parts, filler：10 parts, curing agent：10 parts, Dispersant：2 parts, defoamer：1 part, levelling agent：1 part, compound rare-earth is：0.3 part, silane coupling agent：5 parts；
Compound rare-earth includes following component by weight percentage： Y：15%, Sc：18%, Gd：11%, Sm：20%, Pr：11%, surplus For La, the sum of the above components are 100%；
Second component includes following components according to the mass fraction：
E-20 epoxy resin：15 parts, silicon carbide micro-powder：25 parts, toluene diisocyanate vinegar prepolymer：15 parts, nano-titanium dioxide： 5 parts, propylene glycol n-butyl ether：3-5 parts, organotin catalysts：4 parts, Intumescent Retardant System：7 parts, dioctyl phthalate：2 Part, SiO2Aeroge：8 parts.
In foregoing anticorrosive paint, which includes first and second liang of components, counts first in mass ratio：Second=3:1 ratio is mixed Close, wherein：
First component includes following components according to the mass fraction：
Aqueous epoxy resins：25 parts, water：28 parts, graphene/polypyrrole polymers：8 parts, filler：8 parts, curing agent：7 parts, point Powder：2 parts, defoamer：0.9 part, levelling agent：0.7 part, compound rare-earth is：0.2 part, silane coupling agent：3 parts；
Compound rare-earth includes following component by weight percentage： Y：14%, Sc：17%, Gd：10, Sm：19%, Pr：10%, surplus is The sum of La, the above components is 100%；
Second component includes following components according to the mass fraction：
E-20 epoxy resin：13 parts, silicon carbide micro-powder：19 parts, toluene diisocyanate vinegar prepolymer：13 parts, nano-titanium dioxide： 4 parts, propylene glycol n-butyl ether：4 parts, organotin catalysts：3 parts, Intumescent Retardant System：5 parts, dioctyl phthalate：1 part, SiO2Aeroge：7 parts.
The present invention also designs a kind of preparation process of anticorrosive paint, specifically includes following steps：
（One）The preparation of first component
Aqueous epoxy resins and water are uniformly mixed, when ultrasonic 2-3 is small, sequentially add filler and graphene/polypyrrole polymers, When ball mill ball milling 3-4 is small, filler is set fully to be uniformly dispersed in aqueous epoxy resins；
To the mixing species that prepare add curing agent stirring 1-1.5 it is small when, it is even sequentially adding dispersant, defoamer, silane Join agent, levelling agent and compound rare-earth, stirring is stand-by up to being uniformly mixed；
（Two）The preparation of second component
E-20 epoxy resin and dioctyl phthalate are sent to reactor, are warming up to 90-99 DEG C, is stirred evenly, Ran Houjia Enter to divide silicon carbide micro-powder, nano-titanium dioxide to be uniformly mixed, Intumescent Retardant System, SiO are added after being cooled to room temperature2Airsetting Glue stirs evenly, and adds propylene glycol n-butyl ether and continues to stir evenly, by toluene diisocyanate vinegar prepolymer with it is organotin catalyzed In agent input reactor, filtered after stirring evenly stand-by；
（Three）The preparation of finished product
By step（One）The first component and step being prepared（Two）The second component being prepared weighs uniformly mixed in mass ratio Curing obtains the finished product of anticorrosive paint.
The beneficial effects of the invention are as follows：
It with the addition of dispersant in the present invention, dispersant can increase the compatibility between base-material, can prevent that particle wadding is poly-, reduce finishing agent Viscosity, be firmly adsorbed on the surface of dispersed particle, and provide good space repulsion, particle is filled under high velocity agitation After scattered, it will not reunite again because of Van der Waals force, adsorption layer will not be shelled when being subject to external force to act on from particle surface From and cause the unstable of system, so as to optimize the physical and chemical properties of coating；
The present invention's adds compound rare-earth, since the metallic atomic radius of above rare earth element is big and rare earth has higher work Property, it is easy to the gap of storeroom is filled up, meanwhile, rare earth element is easily and the element compounds such as oxygen, sulphur generate the high compound of fusing point, The addition of compound rare-earth improves the dispersiveness and compatibility that prepare coating to a certain extent, product mix is uniformly also improved The anti-flammability of coating；The present invention is by adding dispersant, nano-titanium dioxide coating has good wear-resisting property.
Addition filler can increase the volume of coating, reduce cost, at the same can also improve the durability of filler, grinability, The performances such as hardness；Addition levelling agent can be obviously improved the feel of coating, to the wetability of base material, in addition to the resist blocking and that of paint film Property is helpful.
For the present invention by adding silicon carbide micro-powder, carborundum differential is a kind of ceramic material, and tool has good wearability, is excellent Different heat endurance, silicon carbide micro-powder and is evenly dispersed in coating so that the coating has good abrasion resistant effect.
Embodiment
Embodiment 1
The present embodiment provides a kind of anticorrosive paint, which includes first and second liang of components, counts first in mass ratio：Second=3:1 ratio Example mixing, wherein：
First component includes following components according to the mass fraction：
Aqueous epoxy resins：20 parts, water：25 parts, graphene/polypyrrole polymers：5 parts, filler：5 parts, curing agent：5 parts, point Powder：1 part, defoamer：0.5 part, levelling agent：0.5 part, compound rare-earth is：0.1 part, silane coupling agent：2 parts；
The compound rare-earth includes following component by weight percentage： Y：13%, Sc：16%, Gd：9%, Sm：18%, Pr：9%, Surplus is that the sum of La, the above components is 100%；
Filler is barium sulfate, talcum powder, the mixture of barium carbonate, is in mass ratio barium sulfate：Talcum powder：Barium carbonate=1:1:1； Curing agent is m-phenylene diamine (MPD)；Dispersant is BYK190 dispersants；Defoamer is dimethicone；Levelling agent is polydimethylsiloxanes Alkane；
Second component includes following components according to the mass fraction：
E-20 epoxy resin：10 parts, silicon carbide micro-powder：15 parts, toluene diisocyanate vinegar prepolymer：11 parts, nano-titanium dioxide： 3 parts, propylene glycol n-butyl ether：3 parts, organotin catalysts：2 parts, Intumescent Retardant System：4 parts, dioctyl phthalate：1 part, SiO2Aeroge：5 parts.
Intumescent Retardant System is in terms of mass fraction including following components：Ammonium polyphosphate：20 parts, melamine：10 parts, season penta Tetrol：5 parts.
The preparation method of above-mentioned graphene/polypyrrole polymers is：
（1）By graphite powder, sodium nitrate, is added in the concentrated sulfuric acid and stirs, wherein the mass ratio of graphite powder and sodium nitrate For 1:1；
（2）Above-mentioned solution is transferred in ice-water bath, while stirring, while being slowly added to potassium permanganate and keeping solution temperature not More than 0 DEG C, and at 0 DEG C stand 2 it is small when；
（3）By above-mentioned steps（2）In mixture be transferred in reaction kettle, at 100 DEG C, reaction 2 it is small when, reaction terminate nature Be cooled to room temperature, supernatant liquor of going out, obtain viscous fluid, and stir 10 it is small when, obtain mixture of viscous form；
（4）To above-mentioned steps（3）Add water in mixture of viscous form, and instill 30% hydrogen peroxide under agitation until There is no bubble generation, stirring 20min centrifugations, then filter cake is washed 2 times with the hydrochloric acid solution of 1mol/L, it is finally anti-with absolute ethyl alcohol Filter cake is cleaned again, and filter cake dries at 30 DEG C and obtains graphene oxide powder；
（5）By above-mentioned steps（4）In graphene oxide when being added to that ultrasonic disperse 2 is small in dilute hydrochloric acid, add polypyrrole ketone, When continuation ultrasonic disperse 1 is small, burgundy stably dispersing suspension is obtained, wherein graphene oxide and polypyrrole ketone mass ratio is 1: 1；
（6）By above-mentioned steps（5）In suspension be placed in ice bath, and pyrrole monomer is added dropwise into suspension, stirring reaction 1 is small When, obtain graphene oxide/pyrroles/mixed in hydrochloric acid liquid system；
（7）To above-mentioned steps（6）The aqueous solution of ammonium persulfate, stirring are added dropwise in graphene oxide/pyrroles/mixed in hydrochloric acid liquid system React 20 it is small when；
（8）By above-mentioned steps（7）When mixed system static 5 is small, it is in nothing to be washed repeatedly to filtrate using acetone, deionized water successively Color, obtains graphene oxide/polypyrrole；
（9）To above-mentioned steps（8）Middle graphene oxide/polypyrrole solution is added dropwise ammonium hydroxide and adjusts PH to 10, adds hydrazine hydrate, stirs 20min is mixed, is uniformly mixed solution, reflux is warming up to, when back flow reaction 20 is small；
（10）By above-mentioned steps（9）In reaction solution be cooled to room temperature suction filtration, with acetone and water washing filter cake, finally in 45 DEG C of bakings It is dry to obtain graphene/polypyrrole polymers.
Above-mentioned toluene diisocyanate vinegar prepolymer is prepared according to the following steps：
Ethanedioic acid, trimethylolpropane, diglycol are uniformly mixed, dimethylbenzene is then added and continues to be uniformly mixing to obtain Linear polyester, by linear polyester and toluene di-isocyanate(TDI), butyl acetate, dimethylbenzene input reactor, counts line in mass ratio Property polyester：Toluene di-isocyanate(TDI)：Butyl acetate：Dimethylbenzene=20:13:14:5,15min is stirred, is to slowly warm up to 70 DEG C, instead 1h is answered, is continuously heating to 85 DEG C, after keeping the temperature 1h, less than 50 DEG C is down to and obtains toluene diisocyanate vinegar prepolymer.
The preparation process of above-mentioned anticorrosive paint, specifically includes following steps：
（One）The preparation of first component
Aqueous epoxy resins and water are uniformly mixed, when ultrasound 2 is small, sequentially add filler and graphene/polypyrrole polymers, When ball mill ball milling 3 is small, filler is set fully to be uniformly dispersed in aqueous epoxy resins；
To the mixing species that prepare add curing agent stirring 1 it is small when, sequentially add dispersant, defoamer, silane coupling agent, Levelling agent and compound rare-earth, stirring are stand-by up to being uniformly mixed；
（Two）The preparation of second component
E-20 epoxy resin and dioctyl phthalate are sent to reactor, 90 DEG C is warming up to, stirs evenly, then adds and divides Silicon carbide micro-powder, nano-titanium dioxide are uniformly mixed, and Intumescent Retardant System, SiO are added after being cooled to room temperature2Aeroge stirs Mix uniformly, add propylene glycol n-butyl ether and continue to stir evenly, toluene diisocyanate vinegar prepolymer and organotin catalysts are thrown Enter in reactor, filtered after stirring evenly stand-by；
（Three）The preparation of finished product
By step（One）The first component and step being prepared（Two）The second component being prepared weighs uniformly mixed in mass ratio Curing obtains the finished product of anticorrosive paint.
Embodiment 2
The present embodiment provides a kind of anticorrosive paint, which includes first and second liang of components, counts first in mass ratio：Second=3:1 ratio Example mixing, wherein：
First component includes following components according to the mass fraction：
Aqueous epoxy resins：30 parts, water：30 parts, graphene/polypyrrole polymers：10 parts, filler：10 parts, curing agent：10 parts, Dispersant：2 parts, defoamer：1 part, levelling agent：1 part, compound rare-earth is：0.3 part, silane coupling agent：5 parts；
Compound rare-earth includes following component by weight percentage： Y：15%, Sc：18%, Gd：11%, Sm：20%, Pr：11%, surplus For La, the sum of the above components are 100%；
Filler is barium sulfate, talcum powder, the mixture of barium carbonate, is in mass ratio barium sulfate：Talcum powder：Barium carbonate=1:1:1； Curing agent is diethylenetriamine；Dispersant is BYK190 dispersants；Defoamer is organosilicon；Levelling agent is polymethyl-benzene base silica Alkane；
Second component includes following components according to the mass fraction：
E-20 epoxy resin：15 parts, silicon carbide micro-powder：25 parts, toluene diisocyanate vinegar prepolymer：15 parts, nano-titanium dioxide： 5 parts, propylene glycol n-butyl ether：3-5 parts, organotin catalysts：4 parts, Intumescent Retardant System：7 parts, dioctyl phthalate：2 Part, SiO2Aeroge：8 parts；
Intumescent Retardant System is in terms of mass fraction including following components：Ammonium polyphosphate：25 parts, melamine：13 parts, Ji Wusi Alcohol：8 parts.
The preparation method of above-mentioned graphene/polypyrrole polymers is：
（1）By graphite powder, sodium nitrate, is added in the concentrated sulfuric acid and stirs, wherein the mass ratio of graphite powder and sodium nitrate For 1:2；
（2）Above-mentioned solution is transferred in ice-water bath, while stirring, while being slowly added to potassium permanganate and keeping solution temperature not More than 0 DEG C, and at 0 DEG C stand 2 it is small when；
（3）By above-mentioned steps（2）In mixture be transferred in reaction kettle, at 105 DEG C, reaction 2 it is small when, reaction terminate nature Be cooled to room temperature, supernatant liquor of going out, obtain viscous fluid, and stir 12 it is small when, obtain mixture of viscous form；
（4）To above-mentioned steps（3）Add water in mixture of viscous form, and instill 30% hydrogen peroxide under agitation until There is no bubble generation, stirring 25min centrifugations, then filter cake is washed 2 times with the hydrochloric acid solution of 1mol/L, it is finally anti-with absolute ethyl alcohol Filter cake is cleaned again, and filter cake dries at 33 DEG C and obtains graphene oxide powder；
（5）By above-mentioned steps（4）In graphene oxide when being added to that ultrasonic disperse 3 is small in dilute hydrochloric acid, add polypyrrole ketone, When continuation ultrasonic disperse 1 is small, burgundy stably dispersing suspension is obtained, wherein graphene oxide and polypyrrole ketone mass ratio is 1: 1.2；
（6）By above-mentioned steps（5）In suspension be placed in ice bath, and pyrrole monomer is added dropwise into suspension, stirring reaction 1.5 Hour, obtain graphene oxide/pyrroles/mixed in hydrochloric acid liquid system；
（7）To above-mentioned steps（6）The aqueous solution of ammonium persulfate, stirring are added dropwise in graphene oxide/pyrroles/mixed in hydrochloric acid liquid system React 22 it is small when；
（8）By above-mentioned steps（7）When mixed system static 6 is small, it is in nothing to be washed repeatedly to filtrate using acetone, deionized water successively Color, obtains graphene oxide/polypyrrole；
（9）To above-mentioned steps（8）Middle graphene oxide/polypyrrole solution is added dropwise ammonium hydroxide and adjusts PH to 11, adds hydrazine hydrate, stirs 30min is mixed, is uniformly mixed solution, reflux is warming up to, when back flow reaction 22 is small；
（10）By above-mentioned steps（9）In reaction solution be cooled to room temperature suction filtration, with acetone and water washing filter cake, finally in 45 DEG C of bakings It is dry to obtain graphene/polypyrrole polymers.
Above-mentioned toluene diisocyanate vinegar prepolymer is prepared according to the following steps：
Ethanedioic acid, trimethylolpropane, diglycol are uniformly mixed, dimethylbenzene is then added and continues to be uniformly mixing to obtain Linear polyester, by linear polyester and toluene di-isocyanate(TDI), butyl acetate, dimethylbenzene input reactor, counts line in mass ratio Property polyester：Toluene di-isocyanate(TDI)：Butyl acetate：Dimethylbenzene=20:13:14:5,18min is stirred, is to slowly warm up to 75 DEG C, instead 4h is answered, is continuously heating to 88 DEG C, after keeping the temperature 1h, less than 50 DEG C is down to and obtains toluene diisocyanate vinegar prepolymer.
The preparation process of above-mentioned anticorrosive paint, specifically includes following steps：
（One）The preparation of first component
Aqueous epoxy resins and water are uniformly mixed, when ultrasound 2 is small, sequentially add filler and graphene/polypyrrole polymers, When ball mill ball milling 3 is small, filler is set fully to be uniformly dispersed in aqueous epoxy resins；
To the mixing species that prepare add curing agent stirring 1.2 it is small when, sequentially adding dispersant, defoamer, silane coupled Agent, levelling agent and compound rare-earth, stirring are stand-by up to being uniformly mixed；
（Two）The preparation of second component
E-20 epoxy resin and dioctyl phthalate are sent to reactor, 95 DEG C is warming up to, stirs evenly, then adds and divides Silicon carbide micro-powder, nano-titanium dioxide are uniformly mixed, and Intumescent Retardant System, SiO are added after being cooled to room temperature2Aeroge stirs Mix uniformly, add propylene glycol n-butyl ether and continue to stir evenly, toluene diisocyanate vinegar prepolymer and organotin catalysts are thrown Enter in reactor, filtered after stirring evenly stand-by；
（Three）The preparation of finished product
By step（One）The first component and step being prepared（Two）The second component being prepared weighs uniformly mixed in mass ratio Curing obtains the finished product of anticorrosive paint.
Embodiment 3
The present embodiment provides a kind of anticorrosive paint, which includes first and second liang of components, counts first in mass ratio：Second=3:1 ratio Example mixing, wherein：
First component includes following components according to the mass fraction：
Aqueous epoxy resins：25 parts, water：28 parts, graphene/polypyrrole polymers：8 parts, filler：8 parts, curing agent：7 parts, point Powder：2 parts, defoamer：0.9 part, levelling agent：0.7 part, compound rare-earth is：0.2 part, silane coupling agent：3 parts；
Compound rare-earth includes following component by weight percentage： Y：14%, Sc：17%, Gd：10, Sm：19%, Pr：10%, surplus is The sum of La, the above components is 100%；
Filler is barium sulfate, talcum powder, the mixture of barium carbonate, is in mass ratio barium sulfate：Talcum powder：Barium carbonate=1:1:1； Curing agent is polyamide；Dispersant is BYK190 dispersants；Defoamer is polyvinyl acetate；Levelling agent is acrylic acid；
Second component includes following components according to the mass fraction：
E-20 epoxy resin：13 parts, silicon carbide micro-powder：19 parts, toluene diisocyanate vinegar prepolymer：13 parts, nano-titanium dioxide： 4 parts, propylene glycol n-butyl ether：4 parts, organotin catalysts：3 parts, Intumescent Retardant System：5 parts, dioctyl phthalate：1 part, SiO2Aeroge：7 parts；
Intumescent Retardant System is in terms of mass fraction including following components：Ammonium polyphosphate：30 parts, melamine：15 parts, Ji Wusi Alcohol：10 parts.
The preparation method of above-mentioned graphene/polypyrrole polymers is：
（1）By graphite powder, sodium nitrate, is added in the concentrated sulfuric acid and stirs, wherein the mass ratio of graphite powder and sodium nitrate For 1:3；
（2）Above-mentioned solution is transferred in ice-water bath, while stirring, while being slowly added to potassium permanganate and keeping solution temperature not More than 0 DEG C, and at 0 DEG C stand 3 it is small when；
（3）By above-mentioned steps（2）In mixture be transferred in reaction kettle, at 110 DEG C, reaction 3 it is small when, reaction terminate nature Be cooled to room temperature, supernatant liquor of going out, obtain viscous fluid, and stir 15 it is small when, obtain mixture of viscous form；
（4）To above-mentioned steps（3）Add water in mixture of viscous form, and instill 30% hydrogen peroxide under agitation until There is no bubble generation, stirring 30min centrifugations, then filter cake is washed 3 times with the hydrochloric acid solution of 1mol/L, it is finally anti-with absolute ethyl alcohol Filter cake is cleaned again, and filter cake dries at 35 DEG C and obtains graphene oxide powder；
（5）By above-mentioned steps（4）In graphene oxide when being added to that ultrasonic disperse 3 is small in dilute hydrochloric acid, add polypyrrole ketone, When continuation ultrasonic disperse 2 is small, burgundy stably dispersing suspension is obtained, wherein graphene oxide and polypyrrole ketone mass ratio is 1: 1.5；
（6）By above-mentioned steps（5）In suspension be placed in ice bath, and pyrrole monomer is added dropwise into suspension, stirring reaction 2 is small When, obtain graphene oxide/pyrroles/mixed in hydrochloric acid liquid system；
（7）To above-mentioned steps（6）The aqueous solution of ammonium persulfate, stirring are added dropwise in graphene oxide/pyrroles/mixed in hydrochloric acid liquid system React 25 it is small when；
（8）By above-mentioned steps（7）When mixed system static 8 is small, it is in nothing to be washed repeatedly to filtrate using acetone, deionized water successively Color, obtains graphene oxide/polypyrrole；
（9）To above-mentioned steps（8）Middle graphene oxide/polypyrrole solution is added dropwise ammonium hydroxide and adjusts PH to 11, adds hydrazine hydrate, stirs 40min is mixed, is uniformly mixed solution, reflux is warming up to, when back flow reaction 24 is small；
（10）By above-mentioned steps（9）In reaction solution be cooled to room temperature suction filtration, with acetone and water washing filter cake, finally in 45 DEG C of bakings It is dry to obtain graphene/polypyrrole polymers.
Above-mentioned toluene diisocyanate vinegar prepolymer is prepared according to the following steps：
Ethanedioic acid, trimethylolpropane, diglycol are uniformly mixed, dimethylbenzene is then added and continues to be uniformly mixing to obtain Linear polyester, by linear polyester and toluene di-isocyanate(TDI), butyl acetate, dimethylbenzene input reactor, counts line in mass ratio Property polyester：Toluene di-isocyanate(TDI)：Butyl acetate：Dimethylbenzene=20:13:14:5,20min is stirred, is to slowly warm up to 80 DEG C, instead 2h is answered, is continuously heating to 90 DEG C, after keeping the temperature 1h, less than 50 DEG C is down to and obtains toluene diisocyanate vinegar prepolymer.
The preparation process of above-mentioned anticorrosive paint, specifically includes following steps：
（One）The preparation of first component
Aqueous epoxy resins and water are uniformly mixed, when ultrasound 3 is small, sequentially add filler and graphene/polypyrrole polymers, When ball mill ball milling 4 is small, filler is set fully to be uniformly dispersed in aqueous epoxy resins；
To the mixing species that prepare add curing agent stirring 1.5 it is small when, sequentially adding dispersant, defoamer, silane coupled Agent, levelling agent and compound rare-earth, stirring are stand-by up to being uniformly mixed；
（Two）The preparation of second component
E-20 epoxy resin and dioctyl phthalate are sent to reactor, 99 DEG C is warming up to, stirs evenly, then adds and divides Silicon carbide micro-powder, nano-titanium dioxide are uniformly mixed, and Intumescent Retardant System, SiO are added after being cooled to room temperature2Aeroge stirs Mix uniformly, add propylene glycol n-butyl ether and continue to stir evenly, toluene diisocyanate vinegar prepolymer and organotin catalysts are thrown Enter in reactor, filtered after stirring evenly stand-by；
（Three）The preparation of finished product
By step（One）The first component and step being prepared（Two）The second component being prepared weighs uniformly mixed in mass ratio Curing obtains the finished product of anticorrosive paint.
In addition to the implementation, the present invention can also have other embodiment.It is all to use equivalent substitution or equivalent transformation shape Into technical solution, all fall within the protection domains of application claims.

Claims (9)

  1. A kind of 1. anticorrosive paint, it is characterised in that：The anticorrosive paint includes first and second liang of components, counts first in mass ratio：Second=3:1 Ratio mixes, wherein：
    The first component includes following components according to the mass fraction：
    Aqueous epoxy resins：20-30 parts, water：25-30 parts, graphene/polypyrrole polymers：5-10 parts, filler：5-10 parts, Gu Agent：5-10 parts, dispersant：1-2 parts, defoamer：0.5-1 parts, levelling agent：0.5-1 parts, compound rare-earth is：0.1-0.3 parts, Silane coupling agent：2-5 parts；
    The compound rare-earth includes following component by weight percentage： Y：13-15%, Sc：16-18%, Gd：9-11%, Sm： 18-20%, Pr：The sum of 9-11%, surplus La, the above components are 100%；
    The second component includes following components according to the mass fraction：
    E-20 epoxy resin：10-15 parts, silicon carbide micro-powder：15-25 parts, toluene diisocyanate vinegar prepolymer：11-15 parts, nanometer Titanium dioxide：3-5 parts, propylene glycol n-butyl ether：3-5 parts, organotin catalysts：2-4 parts, Intumescent Retardant System：4-7 parts, adjacent benzene Diformazan dioctyl phthalate：1-2 parts, SiO2Aeroge：5-8 parts.
  2. 2. anticorrosive paint according to claim 1, it is characterised in that：The filler is barium sulfate, talcum powder, barium carbonate Mixture, be in mass ratio barium sulfate：Talcum powder：Barium carbonate=1:1:1；Curing agent for m-phenylene diamine (MPD), diethylenetriamine, One kind in polyamide；The dispersant is BYK190 dispersants；The defoamer is dimethicone, organosilicon, gathers One kind in vinylacetate；The levelling agent is in dimethyl silicone polymer, polymethylphenylsiloxane or acrylic acid It is a kind of.
  3. 3. anticorrosive paint according to claim 1, it is characterised in that：The Intumescent Retardant System in terms of mass fraction including Following components：Ammonium polyphosphate：20-30 parts, melamine：10-15 parts, pentaerythrite：5-10 parts.
  4. 4. anticorrosive paint according to claim 1, it is characterised in that：The preparation side of the graphene/polypyrrole polymers Method is：
    （1）By graphite powder, sodium nitrate, is added in the concentrated sulfuric acid and stirs, wherein the graphite powder and sodium nitrate Mass ratio is 1:1-3；
    （2）Above-mentioned solution is transferred in ice-water bath, while stirring, while being slowly added to potassium permanganate and keeping solution temperature not More than 0 DEG C, and at 0 DEG C stand 2-3 it is small when；
    （3）By above-mentioned steps（2）In mixture be transferred in reaction kettle, at 100-110 DEG C, reaction 2-3 it is small when, reaction knot Beam cooled to room temperature, supernatant liquor of going out, obtains viscous fluid, and stir 10-15 it is small when, obtain mixture of viscous form；
    （4）To above-mentioned steps（3）Add water in mixture of viscous form, and instill 30% hydrogen peroxide under agitation until There is no bubble generation, stirring 20-30min centrifugations, then filter cake is washed 2-3 times with the hydrochloric acid solution of 1mol/L, finally with anhydrous Ethanol cleans filter cake repeatedly, and filter cake dries at 30-35 DEG C and obtains graphene oxide powder；
    （5）By above-mentioned steps（4）In graphene oxide when being added to that ultrasonic disperse 2-3 is small in dilute hydrochloric acid, add polypyrrole Ketone, when continuation ultrasonic disperse 1-2 is small, obtains burgundy stably dispersing suspension, wherein the graphene oxide and polypyrrole Ketone mass ratio is 1:1-1.5；
    （6）By above-mentioned steps（5）In suspension be placed in ice bath, and pyrrole monomer is added dropwise into suspension, stirring reaction 1-2 Hour, obtain graphene oxide/pyrroles/mixed in hydrochloric acid liquid system；
    （7）To above-mentioned steps（6）The aqueous solution of ammonium persulfate, stirring are added dropwise in graphene oxide/pyrroles/mixed in hydrochloric acid liquid system When reaction 20-25 is small；
    （8）By above-mentioned steps（7）When the static 5-8 of mixed system is small, is washed repeatedly to filtrate using acetone, deionized water successively and be in It is colourless, obtain graphene oxide/polypyrrole；
    （9）To above-mentioned steps（8）Middle graphene oxide/polypyrrole solution is added dropwise ammonium hydroxide and adjusts PH to 10-11, adds hydration Hydrazine, stirs 20-40min, is uniformly mixed solution, reflux is warming up to, when back flow reaction 20-24 is small；
    （10）By above-mentioned steps（9）In reaction solution be cooled to room temperature suction filtration, with acetone and water washing filter cake, finally in 45 DEG C of bakings It is dry to obtain graphene/polypyrrole polymers.
  5. 5. anticorrosive paint according to claim 1, it is characterised in that：The toluene diisocyanate vinegar prepolymer presses following step It is rapid to prepare：
    Ethanedioic acid, trimethylolpropane, diglycol are uniformly mixed, dimethylbenzene is then added and continues to be uniformly mixing to obtain Linear polyester, by linear polyester and toluene di-isocyanate(TDI), butyl acetate, dimethylbenzene input reactor, counts line in mass ratio Property polyester：Toluene di-isocyanate(TDI)：Butyl acetate：Dimethylbenzene=20:13:14:5,15-20min is stirred, is to slowly warm up to 70-80 DEG C, 1-2h is reacted, is continuously heating to 85-90 DEG C, after keeping the temperature 1h, less than 50 DEG C is down to and obtains toluene diisocyanate vinegar prepolymer.
  6. 6. anticorrosive paint according to claim 1, it is characterised in that：The anticorrosive paint includes first and second liang of components, by quality Than counting first：Second=3:1 ratio mixing, wherein：
    The first component includes following components according to the mass fraction：
    Aqueous epoxy resins：20 parts, water：25 parts, graphene/polypyrrole polymers：5 parts, filler：5 parts, curing agent：5 parts, point Powder：1 part, defoamer：0.5 part, levelling agent：0.5 part, compound rare-earth is：0.1 part, silane coupling agent：2 parts；
    The compound rare-earth includes following component by weight percentage： Y：13%, Sc：16%, Gd：9%, Sm：18%, Pr：9%, Surplus is that the sum of La, the above components is 100%；
    The second component includes following components according to the mass fraction：
    E-20 epoxy resin：10 parts, silicon carbide micro-powder：15 parts, toluene diisocyanate vinegar prepolymer：11 parts, nano-titanium dioxide： 3 parts, propylene glycol n-butyl ether：3 parts, organotin catalysts：2 parts, Intumescent Retardant System：4 parts, dioctyl phthalate：1 part, SiO2Aeroge：5 parts.
  7. 7. anticorrosive paint according to claim 1, it is characterised in that：The anticorrosive paint includes first and second liang of components, by quality Than counting first：Second=3:1 ratio mixing, wherein：
    The first component includes following components according to the mass fraction：
    Aqueous epoxy resins：30 parts, water：30 parts, graphene/polypyrrole polymers：10 parts, filler：10 parts, curing agent：10 parts, Dispersant：2 parts, defoamer：1 part, levelling agent：1 part, compound rare-earth is：0.3 part, silane coupling agent：5 parts；
    The compound rare-earth includes following component by weight percentage： Y：15%, Sc：18%, Gd：11%, Sm：20%, Pr： The sum of 11%, surplus La, the above components are 100%；
    The second component includes following components according to the mass fraction：
    E-20 epoxy resin：15 parts, silicon carbide micro-powder：25 parts, toluene diisocyanate vinegar prepolymer：15 parts, nano-titanium dioxide： 5 parts, propylene glycol n-butyl ether：3-5 parts, organotin catalysts：4 parts, Intumescent Retardant System：7 parts, dioctyl phthalate：2 Part, SiO2Aeroge：8 parts.
  8. 8. anticorrosive paint according to claim 1, it is characterised in that：The anticorrosive paint includes first and second liang of components, by quality Than counting first：Second=3:1 ratio mixing, wherein：
    The first component includes following components according to the mass fraction：
    Aqueous epoxy resins：25 parts, water：28 parts, graphene/polypyrrole polymers：8 parts, filler：8 parts, curing agent：7 parts, point Powder：2 parts, defoamer：0.9 part, levelling agent：0.7 part, compound rare-earth is：0.2 part, silane coupling agent：3 parts；
    The compound rare-earth includes following component by weight percentage： Y：14%, Sc：17%, Gd：10, Sm：19%, Pr：10%, Surplus is that the sum of La, the above components is 100%；
    The second component includes following components according to the mass fraction：
    E-20 epoxy resin：13 parts, silicon carbide micro-powder：19 parts, toluene diisocyanate vinegar prepolymer：13 parts, nano-titanium dioxide： 4 parts, propylene glycol n-butyl ether：4 parts, organotin catalysts：3 parts, Intumescent Retardant System：5 parts, dioctyl phthalate：1 part, SiO2Aeroge：7 parts.
  9. 9. the preparation process of anticorrosive paint according to claim 1, it is characterised in that specifically include following steps：
    （One）The preparation of first component
    Aqueous epoxy resins and water are uniformly mixed, when ultrasonic 2-3 is small, sequentially add filler and graphene/polypyrrole polymers, When ball mill ball milling 3-4 is small, filler is set fully to be uniformly dispersed in aqueous epoxy resins；
    To the mixing species that prepare add curing agent stirring 1-1.5 it is small when, it is even sequentially adding dispersant, defoamer, silane Join agent, levelling agent and compound rare-earth, stirring is stand-by up to being uniformly mixed；
    （Two）The preparation of second component
    E-20 epoxy resin and dioctyl phthalate are sent to reactor, are warming up to 90-99 DEG C, is stirred evenly, Ran Houjia Enter to divide silicon carbide micro-powder, nano-titanium dioxide to be uniformly mixed, Intumescent Retardant System, SiO are added after being cooled to room temperature2Airsetting Glue stirs evenly, and adds propylene glycol n-butyl ether and continues to stir evenly, by toluene diisocyanate vinegar prepolymer with it is organotin catalyzed In agent input reactor, filtered after stirring evenly stand-by；
    （Three）The preparation of finished product
    By step（One）The first component and step being prepared（Two）The second component being prepared weighs uniformly mixed in mass ratio Curing obtains the finished product of anticorrosive paint.
CN201711357576.3A 2017-12-16 2017-12-16 A kind of anticorrosive paint and its preparation process Pending CN107955499A (en)

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Application publication date: 20180424