CN113355005A - Anticorrosive flame-retardant difunctional epoxy resin coating and preparation method thereof - Google Patents
Anticorrosive flame-retardant difunctional epoxy resin coating and preparation method thereof Download PDFInfo
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- CN113355005A CN113355005A CN202110532266.0A CN202110532266A CN113355005A CN 113355005 A CN113355005 A CN 113355005A CN 202110532266 A CN202110532266 A CN 202110532266A CN 113355005 A CN113355005 A CN 113355005A
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- RNFJDJUURJAICM-UHFFFAOYSA-N 2,2,4,4,6,6-hexaphenoxy-1,3,5-triaza-2$l^{5},4$l^{5},6$l^{5}-triphosphacyclohexa-1,3,5-triene Chemical compound N=1P(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP=1(OC=1C=CC=CC=1)OC1=CC=CC=C1 RNFJDJUURJAICM-UHFFFAOYSA-N 0.000 title claims abstract description 77
- 239000003063 flame retardant Substances 0.000 title claims abstract description 77
- 239000003822 epoxy resin Substances 0.000 title claims abstract description 73
- 229920000647 polyepoxide Polymers 0.000 title claims abstract description 73
- 238000000576 coating method Methods 0.000 title claims abstract description 67
- 239000011248 coating agent Substances 0.000 title claims abstract description 62
- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- 230000001588 bifunctional effect Effects 0.000 claims abstract description 25
- 239000000945 filler Substances 0.000 claims abstract description 20
- 239000003431 cross linking reagent Substances 0.000 claims abstract description 14
- 239000000839 emulsion Substances 0.000 claims abstract description 13
- 239000002904 solvent Substances 0.000 claims abstract description 9
- 239000006185 dispersion Substances 0.000 claims description 34
- 239000007788 liquid Substances 0.000 claims description 21
- 239000004593 Epoxy Substances 0.000 claims description 15
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 13
- 238000004132 cross linking Methods 0.000 claims description 11
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 10
- 238000005303 weighing Methods 0.000 claims description 10
- 238000002156 mixing Methods 0.000 claims description 7
- 238000009210 therapy by ultrasound Methods 0.000 claims description 7
- -1 black phosphorus alkene Chemical class 0.000 claims description 6
- 239000000126 substance Substances 0.000 claims description 6
- IAZDPXIOMUYVGZ-UHFFFAOYSA-N Dimethylsulphoxide Chemical compound CS(C)=O IAZDPXIOMUYVGZ-UHFFFAOYSA-N 0.000 claims description 4
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 4
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 claims description 4
- 239000007787 solid Substances 0.000 claims description 4
- AHDSRXYHVZECER-UHFFFAOYSA-N 2,4,6-tris[(dimethylamino)methyl]phenol Chemical compound CN(C)CC1=CC(CN(C)C)=C(O)C(CN(C)C)=C1 AHDSRXYHVZECER-UHFFFAOYSA-N 0.000 claims description 3
- 239000003795 chemical substances by application Substances 0.000 claims description 3
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims description 2
- SECXISVLQFMRJM-UHFFFAOYSA-N N-Methylpyrrolidone Chemical compound CN1CCCC1=O SECXISVLQFMRJM-UHFFFAOYSA-N 0.000 claims description 2
- 150000001412 amines Chemical class 0.000 claims description 2
- PZYDAVFRVJXFHS-UHFFFAOYSA-N n-cyclohexyl-2-pyrrolidone Chemical compound O=C1CCCN1C1CCCCC1 PZYDAVFRVJXFHS-UHFFFAOYSA-N 0.000 claims description 2
- 229920002994 synthetic fiber Polymers 0.000 claims description 2
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 claims description 2
- 150000008064 anhydrides Chemical class 0.000 claims 1
- 230000000694 effects Effects 0.000 abstract description 5
- 238000000034 method Methods 0.000 abstract description 4
- 238000009776 industrial production Methods 0.000 abstract description 2
- 238000001132 ultrasonic dispersion Methods 0.000 description 10
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 9
- 238000005260 corrosion Methods 0.000 description 7
- WEVYAHXRMPXWCK-UHFFFAOYSA-N Acetonitrile Chemical compound CC#N WEVYAHXRMPXWCK-UHFFFAOYSA-N 0.000 description 6
- 238000012360 testing method Methods 0.000 description 6
- JHYNEQNPKGIOQF-UHFFFAOYSA-N 3,4-dihydro-2h-phosphole Chemical compound C1CC=PC1 JHYNEQNPKGIOQF-UHFFFAOYSA-N 0.000 description 5
- 230000007797 corrosion Effects 0.000 description 5
- 229920006334 epoxy coating Polymers 0.000 description 5
- 229910052698 phosphorus Inorganic materials 0.000 description 5
- 239000011574 phosphorus Substances 0.000 description 5
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 4
- 230000004888 barrier function Effects 0.000 description 4
- 239000013078 crystal Substances 0.000 description 4
- 239000008367 deionised water Substances 0.000 description 4
- 229910021641 deionized water Inorganic materials 0.000 description 4
- 230000009977 dual effect Effects 0.000 description 4
- 229920005989 resin Polymers 0.000 description 4
- 239000011347 resin Substances 0.000 description 4
- 238000004786 cone calorimetry Methods 0.000 description 3
- 239000000243 solution Substances 0.000 description 3
- 238000005406 washing Methods 0.000 description 3
- 238000005336 cracking Methods 0.000 description 2
- 238000001723 curing Methods 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 238000000157 electrochemical-induced impedance spectroscopy Methods 0.000 description 2
- LNEPOXFFQSENCJ-UHFFFAOYSA-N haloperidol Chemical compound C1CC(O)(C=2C=CC(Cl)=CC=2)CCN1CCCC(=O)C1=CC=C(F)C=C1 LNEPOXFFQSENCJ-UHFFFAOYSA-N 0.000 description 2
- 238000009830 intercalation Methods 0.000 description 2
- 230000002687 intercalation Effects 0.000 description 2
- 230000007774 longterm Effects 0.000 description 2
- 239000002135 nanosheet Substances 0.000 description 2
- 239000003973 paint Substances 0.000 description 2
- 238000011056 performance test Methods 0.000 description 2
- 239000010453 quartz Substances 0.000 description 2
- 238000001878 scanning electron micrograph Methods 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- 239000011780 sodium chloride Substances 0.000 description 2
- JRMUNVKIHCOMHV-UHFFFAOYSA-M tetrabutylammonium bromide Chemical compound [Br-].CCCC[N+](CCCC)(CCCC)CCCC JRMUNVKIHCOMHV-UHFFFAOYSA-M 0.000 description 2
- UWFRVQVNYNPBEF-UHFFFAOYSA-N 1-(2,4-dimethylphenyl)propan-1-one Chemical compound CCC(=O)C1=CC=C(C)C=C1C UWFRVQVNYNPBEF-UHFFFAOYSA-N 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 229910000975 Carbon steel Inorganic materials 0.000 description 1
- 238000003917 TEM image Methods 0.000 description 1
- 150000008065 acid anhydrides Chemical class 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 239000010962 carbon steel Substances 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 238000005119 centrifugation Methods 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 238000005536 corrosion prevention Methods 0.000 description 1
- 230000003111 delayed effect Effects 0.000 description 1
- 238000006392 deoxygenation reaction Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 125000003700 epoxy group Chemical group 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- PBZROIMXDZTJDF-UHFFFAOYSA-N hepta-1,6-dien-4-one Chemical compound C=CCC(=O)CC=C PBZROIMXDZTJDF-UHFFFAOYSA-N 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 238000002791 soaking Methods 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
- 238000001291 vacuum drying Methods 0.000 description 1
- 230000004580 weight loss Effects 0.000 description 1
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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
- 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
- C09D5/18—Fireproof paints including high temperature resistant 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
- C08K3/02—Elements
- C08K2003/026—Phosphorus
-
- 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
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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)
- Application Of Or Painting With Fluid Materials (AREA)
Abstract
The invention discloses an anticorrosive flame-retardant bifunctional epoxy resin coating which is prepared from the following components in percentage by mass: 20-40% of epoxy resin emulsion, 40-70% of solvent, 5-15% of cross-linking agent and 0.1-5% of anticorrosive flame-retardant filler. The invention also discloses a preparation method of the anticorrosive flame-retardant bifunctional epoxy resin coating. The invention has good anticorrosion effect and obvious flame retardant effect, is environment-friendly, has high adhesion and excellent comprehensive performance; the preparation method is simple, the process is mature, the industrial production is convenient, the coating can be used for preparing the anticorrosive flame-retardant dual-function epoxy resin coating, and the coating has a good application prospect in the field of anticorrosive flame-retardant functional coatings.
Description
Technical Field
The invention relates to the technical field of epoxy resin coatings, in particular to an anticorrosive flame-retardant bifunctional epoxy resin coating and a preparation method thereof.
Background
In all organic coatings, epoxy resins have been widely used due to their good adhesion to the substrate, excellent chemical inertness, and electrical insulating properties. Has become the most representative high-performance anticorrosive paint variety with the largest dosage. The molecular structure of the epoxy resin is characterized in that the macromolecular chain contains epoxy groups, more than 40 percent of the epoxy resin is used for manufacturing epoxy paint every year all over the world, and most of the epoxy resin is used in the field of corrosion prevention. However, the existing epoxy resin coating has the defect of poor barrier property, gaps among macromolecular chains are large after the resin is dried, water, oxygen and corrosive ions are difficult to prevent from permeating, and the long-term anticorrosion performance is poor.
Disclosure of Invention
Aiming at the defects of the epoxy resin coating, the invention provides the anticorrosive flame-retardant bifunctional epoxy resin coating which is relatively stable functional resin, and the prepared coating has good film forming property, heat resistance and chemical corrosion resistance by introducing the two-dimensional lamellar nano material phospholene with thermal stability and barrier property, and the formed film is colorless and transparent, can be used for preparing the anticorrosive flame-retardant bifunctional epoxy resin coating and can meet the requirements of people on the functional coating.
The second purpose of the invention is to provide a preparation method of the anticorrosive and flame-retardant bifunctional epoxy resin coating.
In order to achieve the above object, the present invention is realized by: an anticorrosive flame-retardant bifunctional epoxy resin coating is prepared from the following components in percentage by mass:
the epoxy resin includes but is not limited to one or more mixed epoxy resins of traditional solvent type epoxy resin and epoxy resin, and can be solid epoxy resin solution with the model number DER 660-X80 of Dow chemical company in America or water-based epoxy emulsion with the model number BC2060 of Huangshan Pont and synthetic materials company Limited, and the like.
The crosslinking agent is one or more of amine and acid anhydride curing agents, and may be XZ 92441.01 available from Dow chemical company, EPIKURE 8538-Y-68 available from Hexion corporation, or DMP30(2, 4, 6 tris (dimethylaminomethyl) phenol).
The solvent may be one or more of water, acetone, N-dimethylformamide, tetrahydrofuran, N-cyclohexylpyrrolidone, N-methylpyrrolidone, dimethyl sulfoxide and isopropanol.
The anticorrosive flame-retardant filler is black phosphorus alkene with a nano single-sheet or multi-sheet layer structure. The black phosphorus alkene can be prepared by stripping black phosphorus crystals.
The preparation method of the anticorrosive flame-retardant bifunctional epoxy resin coating comprises the following steps:
(1) dispersing the anticorrosive flame-retardant filler into a solvent to form a uniform dispersion liquid with the concentration of 0.1-10mg/mL
(2) Weighing the epoxy resin emulsion and the solvent according to the proportion, mixing and dispersing uniformly to form epoxy dispersion liquid;
(3) weighing the cross-linking agent and the anticorrosive flame-retardant filler dispersion according to the proportion, and uniformly mixing and dispersing to form cross-linking dispersion;
(4) and (3) mixing the epoxy dispersion liquid obtained in the step (2) and the crosslinking dispersion liquid obtained in the step (3), and performing ultrasonic treatment for dispersing uniformly, wherein the ultrasonic treatment time is 10-30 minutes.
In the step (1), the step (2) and the step (3), ultrasonic treatment is adopted to treat the dispersion liquid, wherein ultrasonic dispersion is carried out, the ultrasonic frequency is 20-60kHz, the power is 50-500W, and the ultrasonic time is 20-120 minutes.
In the step (4), the ultrasonic treatment frequency is 20-60kHz, and the power is 50-500W.
The phospholene is obtained by stripping black phosphorus.
According to the invention, the anticorrosive flame-retardant filler with flame retardant property is added into the coating, and the phospholene in the anticorrosive flame-retardant filler has a two-dimensional nanosheet structure, so that the anticorrosive property and the flame retardant property of the epoxy resin can be improved, and the anticorrosive flame-retardant coating has the advantages of low addition amount, high flame retardant efficiency and the like. The phosphorus alkene modified epoxy resin coating has good compatibility among the components and has a synergistic effect, so that the corrosion resistance of the coating is effectively improved, and the heat resistance and the flame retardance of the coating are improved. In general, the invention also has the advantages of low addition amount, high adhesion, heat resistance, flame retardance and the like, and can obviously improve the salt resistance (3.5 percent NaCl solution) and the flame retardance (cone calorimetry analysis).
Compared with the prior art, the invention has the following outstanding effects:
1) in the invention, the method of directly adding the anticorrosive flame-retardant filler for ultrasonic mixing and dispersion at room temperature is adopted, the addition amount is small, the process is simple and mature, the operation is easy, and the large-scale industrial production is easy;
2) in the invention, the epoxy resin is used as commercial finished resin, has wide universality and can be popularized and applied to the field of other polymer coatings;
3) the resin of the invention introduces the anticorrosive flame-retardant filler, so as to improve the barrier property and the heat resistance of the epoxy resin, effectively improve the anticorrosive and flame-retardant properties of the coating, and can be widely applied to the field of functional coatings.
Drawings
FIG. 1 is a TEM image of a black phosphorus allyl ketone dispersion;
FIG. 2 is an SEM image of an epoxy coating;
FIG. 3 is an SEM image of an anticorrosive flame retardant dual function epoxy coating of the present invention;
FIG. 4 is a graph of the total heat release of epoxy (WEP) and anticorrosive flame retardant dual function epoxy coating (0.2% BP);
FIG. 5 is a graph of heat release rate for an anti-corrosive flame retardant dual function epoxy coating;
FIG. 6 is a semi-circle plot of the electrochemical impedance of the epoxy and the anti-corrosive flame retardant dual function epoxy coating (BP/WEP).
Detailed Description
The present invention is further described with reference to the following specific examples, which should be construed as limiting the scope of the invention as claimed.
The anticorrosive flame-retardant bifunctional epoxy resin coating prepared by the invention can be characterized by the following method: the stripping condition of the phospholene is analyzed by a Transmission Electron Microscope (TEM); analyzing the microscopic morphology of the coating inside by using a Scanning Electron Microscope (SEM); the flame retardant property of the coating is analyzed by cone calorimetry; the corrosion resistance of the coating was analyzed by Electrochemical Impedance Spectroscopy (EIS).
Example 1
The anticorrosive and flame-retardant difunctional epoxy resin coating comprises an epoxy resin emulsion, a crosslinking agent, an anticorrosive and flame-retardant filler and water, and comprises the following specific components:
the preparation method of the anticorrosive flame-retardant bifunctional epoxy resin coating comprises the following steps:
a. preparing the anticorrosive flame-retardant filler: placing the black phosphorus crystal in acetonitrile at room temperature, performing electrochemical intercalation stripping by using tetrabutylammonium bromide, then performing ultrasonic dispersion, performing centrifugal deoxygenation and deionized water washing, and taking the dispersion liquid after centrifugation at the rotating speed of 3000 rpm;
b. preparing the anticorrosive flame-retardant coating: weighing epoxy resin emulsion and deionized water according to mass percentage at room temperature, and performing ultrasonic dispersion uniformly to form epoxy dispersion liquid; respectively weighing the anticorrosive flame-retardant filler aqueous dispersion and the crosslinking agent with different mass fractions, and uniformly dispersing by ultrasonic to form a crosslinking dispersion; and pouring the epoxy dispersion liquid into the cross-linking dispersion liquid for uniform ultrasonic dispersion to obtain the anticorrosive flame-retardant bifunctional epoxy resin coating. Wherein the ultrasonic wave is dispersed, the ultrasonic frequency is 30kHz, the power is 100W, and the ultrasonic time is 30 minutes.
Pouring the anticorrosive flame-retardant bifunctional epoxy resin coating into a conical calorimetric sample preparation grinding tool, carrying out vacuum drying at room temperature until the moisture is completely dried, and carrying out performance test on the sample without weight loss.
The anticorrosive flame-retardant bifunctional epoxy resin coating sample has the advantages of smooth surface, uniform thickness, uniform color, no bubbles and no cracking. And (3) testing the flame retardant property: the samples were cut into 10 x 10cm standards and cone calorimetry was performed using a PX-07-007 cone calorimeter. The test results were as follows:
the test results were analyzed to obtain: the anticorrosive flame-retardant dual-function epoxy resin coating (BP/WEP) is added with 0.12% of the phosphorus in the mass fraction of the system, the phosphorus accounts for 0.2% of the solid content of the system, the ignition time is delayed by 32s compared with that of pure epoxy resin (WEP), the peak value of the heat release rate is reduced by 41.1%, the total heat release amount is reduced by 30.2%, and the thermal stability and the flame retardant property are both greatly improved.
Example 2
The anticorrosive and flame-retardant difunctional epoxy resin coating comprises an epoxy resin emulsion, a crosslinking agent, an anticorrosive and flame-retardant filler and water, and comprises the following specific components:
the preparation method of the anticorrosive flame-retardant bifunctional epoxy resin coating comprises the following steps:
a. preparing the anticorrosive flame-retardant filler: dispersing the black phosphorus crystal in acetone in an ice bath, firstly carrying out cell crushing for 2 hours (the power is 800W), then carrying out ultrasonic dispersion for 12 hours, finally centrifuging and washing repeatedly, and taking the dispersion liquid centrifugally collected at more than 3000 rpm;
b. preparing the anticorrosive flame-retardant coating: weighing epoxy resin emulsion and deionized water according to mass percentage at room temperature, and performing ultrasonic dispersion uniformly to form epoxy dispersion liquid; respectively weighing the anticorrosive flame-retardant filler aqueous dispersion and the crosslinking agent with different mass fractions, and uniformly dispersing by ultrasonic to form a crosslinking dispersion; and pouring the epoxy dispersion liquid into the cross-linking dispersion liquid for uniform ultrasonic dispersion to obtain the anticorrosive flame-retardant bifunctional epoxy resin coating. Wherein the ultrasonic wave is dispersed, the ultrasonic frequency is 50kHz, the power is 200W, and the ultrasonic time is 25 minutes.
Example 3:
the anticorrosive and flame-retardant difunctional epoxy resin coating comprises an epoxy resin emulsion, a cross-linking agent, an anticorrosive and flame-retardant filler, acetone and ethylene glycol diglycidyl ether, and comprises the following specific components:
the preparation method of the anticorrosive flame-retardant bifunctional epoxy resin coating comprises the following steps:
a. preparing the anticorrosive flame-retardant filler: at room temperature, placing the black phosphorus crystal in acetonitrile, performing electrochemical intercalation stripping by using tetrabutylammonium bromide, then dispersing the electrochemically expanded black phosphorus in acetone for ultrasonic dispersion, repeatedly centrifuging and washing, and taking a dispersion liquid centrifugally collected at more than 3000 rpm;
b. preparing the anticorrosive flame-retardant coating: weighing epoxy resin emulsion and deionized water according to mass percentage at room temperature, and performing ultrasonic dispersion uniformly to form epoxy dispersion liquid; respectively weighing the anticorrosive flame-retardant filler aqueous dispersion and the crosslinking agent with different mass fractions, and uniformly dispersing by ultrasonic to form a crosslinking dispersion; and pouring the epoxy dispersion liquid into the cross-linking dispersion liquid for uniform ultrasonic dispersion to obtain the anticorrosive flame-retardant bifunctional epoxy resin coating. Wherein the ultrasonic wave is dispersed, the ultrasonic frequency is 40kHz, the power is 250W, and the ultrasonic time is 40 minutes.
Respectively coating the surface-treated Q235A carbon steel with 150 mu m of coating by using an QTG film coater on the anticorrosive flame-retardant bifunctional epoxy resin coating of the embodiments 1 to 3, naturally evaporating water at room temperature for drying, curing and crosslinking at 100 ℃ for 120-180 min, and cooling to room temperature for carrying out an anticorrosive performance test.
The anticorrosive flame-retardant bifunctional epoxy resin coating composite coating has the advantages of smooth surface, no bubbles and no cracking. And (3) testing the long-term corrosion resistance: and adhering a quartz tube on the surface of the coating, soaking the quartz tube in a solution with the mass fraction of 3.5% of NaCl for 40 days, and periodically carrying out electrochemical impedance test. And (3) testing results: after 40 days, the impedance values of the anticorrosive and flame-retardant dual-function epoxy resin coating with the system mass percent of 0.04%, 0.08% and 0.12% of the phosphorus alkene are added, wherein the mass fractions of the phosphorus alkene in the solid epoxy resin are 0.1%, 0.2% and 0.4%, which are respectively improved by about 7 times, 17 times and 3 times compared with a pure epoxy resin coating, and the anticorrosive performance is obviously improved.
The performance of the anti-corrosion and flame-retardant dual-function epoxy resin coating in the embodiment 1 is shown in fig. 1-6. The invention introduces the phospholene nano-sheet material with a two-dimensional lamellar structure, has good barrier property and has an anti-corrosion effect; has good heat resistance, gas-phase flame retardance and catalytic carbon performance, and has flame retardance effect. Other embodiments of the invention specifically demonstrate similar experimental results to those of example 1 above and are not meant to be redundant herein.
The above examples are only some examples of the present invention, and the corrosion resistance, heat resistance and flame retardant property of the anticorrosive flame retardant dual-function epoxy resin coating prepared in the examples are significantly improved, and the examples are not intended to limit the scope of the present invention, and all equivalent changes and modifications made by using the contents of the present invention are covered by the scope of the present invention claimed in the claims.
Claims (10)
1. The anticorrosive flame-retardant difunctional epoxy resin coating is characterized by being prepared from the following components in percentage by mass:
2. the anticorrosive flame-retardant dual-function epoxy resin coating as claimed in claim 1, wherein the epoxy resin emulsion comprises but is not limited to solvent type epoxy resin and one or more mixed epoxy resin of epoxy resin.
3. The anticorrosive flame-retardant dual-function epoxy resin coating as claimed in claim 2, wherein the epoxy resin emulsion is a solid epoxy resin solution of DER 660-X80 manufactured by Dow chemical company or a water-based epoxy emulsion of BC2060 manufactured by Nippon Huangshang and synthetic materials Co.
4. The anticorrosive flame-retardant bifunctional epoxy resin coating as claimed in claim 1, wherein the crosslinking agent is one or more of amine curing agent and anhydride curing agent.
5. The anticorrosive flame-retardant dual-function epoxy resin coating as claimed in claim 1, wherein the cross-linking agent is a cross-linking agent of type XZ 92441.01 from Dow chemical company, a cross-linking agent of type EPIKURE 8538-Y-68 from Vast Van der USA or DMP 30.
6. The anticorrosive flame-retardant bifunctional epoxy resin coating as claimed in claim 1, wherein the solvent is one or more of water, acetone, N-dimethylformamide, tetrahydrofuran, N-cyclohexylpyrrolidone, N-methylpyrrolidone, dimethyl sulfoxide and isopropanol.
7. The anticorrosive flame-retardant bifunctional epoxy resin coating as claimed in claim 1, wherein the anticorrosive flame-retardant filler is black phosphorus alkene with a nano single-sheet or multi-sheet structure.
8. The preparation method of the anticorrosive flame-retardant bifunctional epoxy resin coating according to any one of claims 1 to 7, characterized by comprising the following steps:
(1) dispersing the anticorrosive flame-retardant filler into a solvent to form a uniform dispersion liquid with the concentration of 0.1-10mg/mL
(2) Weighing the epoxy resin emulsion and the solvent according to the proportion, mixing and dispersing uniformly to form epoxy dispersion liquid;
(3) weighing the cross-linking agent and the anticorrosive flame-retardant filler dispersion according to the proportion, and uniformly mixing and dispersing to form cross-linking dispersion;
(4) and (3) mixing the epoxy dispersion liquid obtained in the step (2) and the crosslinking dispersion liquid obtained in the step (3), and performing ultrasonic treatment for dispersing uniformly, wherein the ultrasonic treatment time is 10-30 minutes.
9. The preparation method of the anticorrosive and flame-retardant bifunctional epoxy resin coating as claimed in claim 8, wherein in the steps (1), (2) and (3), the dispersion is treated by ultrasonic waves, wherein the ultrasonic waves are dispersed at an ultrasonic frequency of 20-60kHz and a power of 50-500W for 20-120 minutes.
10. The preparation method of the anticorrosive flame-retardant bifunctional epoxy resin coating according to claim 8, wherein in the step (4), the ultrasonic treatment frequency is 20-60kHz, and the power is 50-500W.
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| CN111699222A (en) * | 2018-02-06 | 2020-09-22 | 应用石墨烯材料英国有限公司 | Corrosion protection of metal substrates |
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| Title |
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| CE LI: "《Electrochemically prepared black phosphorene micro-powder as flame retardant for epoxy resin》", 《COMPOSITE INTERFACES》 * |
| 孙旗: "《黑磷烯纳米阻燃剂研究进展》", 《中国塑料》 * |
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