CN114058248A - Epoxy resin anticorrosive paint and preparation method thereof - Google Patents
Epoxy resin anticorrosive paint and preparation method thereof Download PDFInfo
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- CN114058248A CN114058248A CN202111466669.6A CN202111466669A CN114058248A CN 114058248 A CN114058248 A CN 114058248A CN 202111466669 A CN202111466669 A CN 202111466669A CN 114058248 A CN114058248 A CN 114058248A
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- 239000003822 epoxy resin Substances 0.000 title claims abstract description 137
- 229920000647 polyepoxide Polymers 0.000 title claims abstract description 137
- 239000003973 paint Substances 0.000 title claims abstract description 83
- 238000002360 preparation method Methods 0.000 title claims abstract description 42
- 239000004593 Epoxy Substances 0.000 claims abstract description 96
- 229920000734 polysilsesquioxane polymer Polymers 0.000 claims abstract description 44
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 29
- 239000002904 solvent Substances 0.000 claims abstract description 22
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N phenol group Chemical group C1(=CC=CC=C1)O ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 claims abstract description 9
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical group CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 claims description 72
- 239000003513 alkali Substances 0.000 claims description 29
- 238000000034 method Methods 0.000 claims description 23
- 239000002689 soil Substances 0.000 claims description 20
- 239000000945 filler Substances 0.000 claims description 19
- 229920003986 novolac Polymers 0.000 claims description 19
- 238000002156 mixing Methods 0.000 claims description 14
- 125000003700 epoxy group Chemical group 0.000 claims description 13
- 230000007062 hydrolysis Effects 0.000 claims description 10
- 238000006460 hydrolysis reaction Methods 0.000 claims description 10
- 230000008569 process Effects 0.000 claims description 8
- 230000002194 synthesizing effect Effects 0.000 claims description 8
- 239000003085 diluting agent Substances 0.000 claims description 7
- 229910019142 PO4 Inorganic materials 0.000 claims description 6
- 239000012752 auxiliary agent Substances 0.000 claims description 6
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 claims description 6
- 239000010452 phosphate Substances 0.000 claims description 6
- IISBACLAFKSPIT-UHFFFAOYSA-N bisphenol A Chemical compound C=1C=C(O)C=CC=1C(C)(C)C1=CC=C(O)C=C1 IISBACLAFKSPIT-UHFFFAOYSA-N 0.000 claims description 4
- 125000003277 amino group Chemical group 0.000 claims description 3
- 239000004841 bisphenol A epoxy resin Substances 0.000 claims description 3
- 239000007787 solid Substances 0.000 claims description 3
- 238000012986 modification Methods 0.000 abstract description 2
- 230000004048 modification Effects 0.000 abstract description 2
- 238000012360 testing method Methods 0.000 description 42
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- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 33
- 238000000576 coating method Methods 0.000 description 22
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- 230000007797 corrosion Effects 0.000 description 12
- 238000005260 corrosion Methods 0.000 description 12
- 238000011156 evaluation Methods 0.000 description 12
- WGTYBPLFGIVFAS-UHFFFAOYSA-M tetramethylammonium hydroxide Chemical compound [OH-].C[N+](C)(C)C WGTYBPLFGIVFAS-UHFFFAOYSA-M 0.000 description 12
- 239000002253 acid Substances 0.000 description 10
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical class [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 9
- 230000007935 neutral effect Effects 0.000 description 8
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- 229910021641 deionized water Inorganic materials 0.000 description 6
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- 238000003756 stirring Methods 0.000 description 6
- 229910000831 Steel Inorganic materials 0.000 description 5
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- 230000009466 transformation Effects 0.000 description 5
- IAZDPXIOMUYVGZ-WFGJKAKNSA-N Dimethyl sulfoxide Chemical compound [2H]C([2H])([2H])S(=O)C([2H])([2H])[2H] IAZDPXIOMUYVGZ-WFGJKAKNSA-N 0.000 description 4
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 4
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- 238000001644 13C nuclear magnetic resonance spectroscopy Methods 0.000 description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- 238000005033 Fourier transform infrared spectroscopy Methods 0.000 description 2
- 238000001157 Fourier transform infrared spectrum Methods 0.000 description 2
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- 229910002808 Si–O–Si Inorganic materials 0.000 description 2
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
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- ZXEKIIBDNHEJCQ-UHFFFAOYSA-N isobutanol Chemical compound CC(C)CO ZXEKIIBDNHEJCQ-UHFFFAOYSA-N 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 239000011780 sodium chloride Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical group [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
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- 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 1
- 239000004615 ingredient Substances 0.000 description 1
- 238000007689 inspection Methods 0.000 description 1
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 1
- 230000002262 irrigation Effects 0.000 description 1
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- 125000000325 methylidene group Chemical group [H]C([H])=* 0.000 description 1
- GRVDJDISBSALJP-UHFFFAOYSA-N methyloxidanyl Chemical group [O]C GRVDJDISBSALJP-UHFFFAOYSA-N 0.000 description 1
- 244000005700 microbiome Species 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 238000000655 nuclear magnetic resonance spectrum Methods 0.000 description 1
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- 231100000419 toxicity Toxicity 0.000 description 1
- 239000002966 varnish Substances 0.000 description 1
Images
Classifications
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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
- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
- C09D7/40—Additives
- C09D7/65—Additives macromolecular
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/32—Phosphorus-containing compounds
- C08K2003/321—Phosphates
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/08—Stabilised against heat, light or radiation or oxydation
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2203/00—Applications
- C08L2203/20—Applications use in electrical or conductive gadgets
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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)
- Epoxy Resins (AREA)
Abstract
An epoxy resin anticorrosive paint and a preparation method thereof, which mainly relate to the field of power grid protection. According to the preparation method of the epoxy resin anticorrosive paint, epoxy polyhedral polysilsesquioxane is introduced into epoxy resin for modification to obtain polyhedral polysilsesquioxane covalent hybrid epoxy resin, and then the polyhedral polysilsesquioxane covalent hybrid epoxy resin is compounded with a phenolic epoxy curing agent and a solvent in a certain proportion to prepare the epoxy resin anticorrosive paint. Therefore, the epoxy resin anticorrosive paint and the preparation method thereof provided by the invention have important popularization and application values.
Description
Technical Field
The invention relates to the field of corrosion protection of power facilities and equipment, in particular to an epoxy resin anticorrosive paint and a preparation method thereof.
Background
Soil salinization is a worldwide problem. In China, the salinization area of soil is increased year by year due to unreasonable irrigation in partial areas, and the power transmission and transformation project is used as an infrastructure of power supply, one part of the power transmission and transformation project needs to be buried underground, and the part of the power transmission and transformation project is directly exposed in the environment with serious salinization of soil, moisture, microorganisms and the like, so that the corrosion problem of the power transmission and transformation project has serious influence on the aspects of power transmission cost, power transmission safety and the like. Therefore, an anticorrosive coating specially aiming at the saline-alkali soil environment is urgently needed to relieve the corrosion problem of the infrastructure related to the power transmission and transformation engineering.
Disclosure of Invention
The invention aims to provide an epoxy resin anticorrosive paint which has good acid and alkali resistance, cohesiveness, thermal stability and corrosion resistance, and has important significance for protecting infrastructure related to a power grid system in saline-alkali soil.
The invention also aims to provide a preparation method of the epoxy resin anticorrosive paint, which can prepare the epoxy resin anticorrosive paint with the functional effects.
The technical problem to be solved by the invention is realized by adopting the following technical scheme.
The invention provides a preparation method of an epoxy resin anticorrosive paint, which comprises the following steps:
synthesizing epoxy polyhedral polysilsesquioxane by a classical hydrolysis method;
mixing the epoxy polyhedral polysilsesquioxane, epoxy resin, a novolac epoxy curing agent and a solvent to prepare the epoxy polyhedral polysilsesquioxane, wherein the mass of the epoxy polyhedral polysilsesquioxane accounts for 1-5% of the total mass of the epoxy polyhedral polysilsesquioxane and the epoxy resin.
Further, in a preferred embodiment of the present invention, the mass of the epoxy polyhedral polysilsesquioxane is 3% to 5% of the total mass of the epoxy polyhedral polysilsesquioxane and the epoxy resin.
Further, in a preferred embodiment of the present invention, the epoxy polyhedral polysilsesquioxane is an octaepoxy polyhedral polysilsesquioxane; the epoxy resin is bisphenol A type epoxy resin; the solid content of the phenolic epoxy curing agent is 60-70%; the solvent is ethyl acetate.
Further, in a preferred embodiment of the present invention, the mixing and preparing process includes: adding the octa-epoxy polyhedral oligomeric silsesquioxane and the bisphenol A epoxy resin into the phenolic epoxy curing agent, and then adding the ethyl acetate for mixing; wherein the molar weight of the epoxy groups of the octa-epoxy polyhedral polysilsesquioxane is equal to the molar weight of the amino groups in the novolac epoxy curing agent.
Further, in a preferred embodiment of the present invention, the mass ratio of the novolac epoxy hardener to the ethyl acetate is 2: 1.
Further, in the preferred embodiment of the present invention, the epoxy resin is an E44 type epoxy resin.
The embodiment of the invention also provides the epoxy resin anticorrosive paint which is prepared according to the preparation method of the epoxy resin anticorrosive paint.
Further, in a preferred embodiment of the present invention, the epoxy resin anticorrosive paint further comprises an epoxy diluent, a filler and an auxiliary agent.
Further, in a preferred embodiment of the invention, the filler comprises a phosphate antirust filler and a system filler, and the mass ratio of the epoxy diluent to the phosphate antirust filler to the system filler to the auxiliary agent is 1-3: 20-25: 25-30: 1-2.
Further, in the preferred embodiment of the invention, the epoxy resin anticorrosive paint is prepared on the electric facility equipment in the saline-alkali soil area.
The epoxy resin anticorrosive paint and the preparation method thereof provided by the embodiment of the invention have the beneficial effects that:
the epoxy resin anticorrosive paint has good acid and alkali resistance, cohesiveness, thermal stability and corrosion resistance, has important significance for corrosion prevention in the process of power grid protection, and particularly has obvious advantages for power grid protection in saline-alkali soil areas.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings needed to be used in the embodiments will be briefly described below, it should be understood that the following drawings only illustrate some embodiments of the present invention and therefore should not be considered as limiting the scope, and for those skilled in the art, other related drawings can be obtained according to the drawings without inventive efforts.
FIG. 1 is a schematic diagram of the synthesis of an epoxy POSS in an embodiment of the present invention;
FIG. 2 shows KH560 and epoxy-based POSS in examples of the present invention1H NMR spectrum;
FIG. 3 is a representation of epoxy-based POSS in an embodiment of the present invention13C NMR spectrum;
FIG. 4 is an FT-IR spectrum of KH560 and epoxy-based POSS as starting materials for an example of the present invention;
FIG. 5 is a schematic diagram illustrating the synthesis of an epoxy resin anticorrosive paint provided by an embodiment of the present invention;
FIG. 6 is a photograph of different test samples soaked in a pH 2 sulfuric acid solution for 48 hours when performance evaluation is performed in test examples of the present invention;
FIG. 7 is a TGA curve for different test samples when evaluated for performance in accordance with a test example of the present invention;
FIG. 8a is a photograph of the salt spray resistance test of the coating layer when the performance evaluation is performed by using example 6 in the test examples of the present invention, wherein the test item corresponds to the conventional salt spray resistance test (3000 h);
FIG. 8b is a photograph of the salt spray resistance test of the coating layer when the performance evaluation is performed in example 6 selected in the test examples of the present invention, wherein the test item is the scratch salt spray resistance test (1000 h);
FIG. 9 is a photograph of a salt spray damp heat cycle test of the coating layer when the performance evaluation is performed by using example 6 in the test examples of the present invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below. The examples, in which specific conditions are not specified, were conducted under conventional conditions or conditions recommended by the manufacturer. The reagents or instruments used are not indicated by the manufacturer, and are all conventional products available commercially.
The epoxy resin anticorrosive paint and the preparation method thereof according to the embodiment of the present invention will be specifically described below.
The preparation method of the epoxy resin anticorrosive paint provided by the embodiment of the invention comprises the following steps:
s1, synthesizing the epoxy polyhedral polysilsesquioxane by a classical hydrolysis method.
In the preferred embodiment of the present invention, the epoxy polyhedral polysilsesquioxane (i.e. epoxy POSS) is an octaepoxy polyhedral polysilsesquioxane, and the synthetic route for preparing the octaepoxy polyhedral polysilsesquioxane is shown in fig. 1, and further specifically, the synthetic method is as follows: adding 4g KH560 and 6mL isopropanol into a 100mL three-neck flask, and magnetically stirring until the mixture is uniformly mixed; in N2Under protection, a mixture of 0.2g tetramethylammonium hydroxide (25% aqueous solution), 1mL deionized water, and 10mL isopropanol was added slowly and stirred at room temperature for 6 h. After the reaction is finished, the isopropanol is removed through decompression, viscous liquid is obtained, 10mL of methylbenzene is added to be dissolved again, the mixture reacts for 6 hours at the temperature of 90 ℃, the temperature is reduced to the room temperature, saturated NaCl aqueous solution is used for multiple times of extraction until the solution is neutral, and finally, the first is removedBenzene gave eight epoxy groups POSS in 78.9% yield as a viscous paste. It should be noted that, in the examples of the present invention, for convenience of explanation, specific amounts of various reagents and raw materials for preparing the epoxy polyhedral polysilsesquioxane are used, but in other examples of the present invention, the specific amounts defined in the present invention are not limited, as long as the corresponding proportional relationship is maintained, and the synthetic epoxy polyhedral polysilsesquioxane can be prepared.
It is further noted that the octa-epoxy POSS prepared by the method is prepared by utilizing1H NMR、13C NMR and FT-IR confirm the structure of the compound.1H NMR(400MHz,DMSO-d6,ppm):3.68(d,H),3.43(d,2H),3.32(d,H),3.11(s,H),3.57-3.76(d,2H),1.63(d,2H),0.60(d,2H)。13C NMR(400MHz,DMSO-d6,ppm):73.7(C3),71.5(C4),50.9(C2),44.3(C1),23.1(C5),8.9(C6)。FT-IR(KBr,v,cm-1):2936,2856(-CH2-),1250(C-Si),1119(Si-O-Si),901(epoxy group). As shown in fig. 2, 3 and 4, respectively. In particular, with reference to FIGS. 2 and 3, starting from KH560 and epoxy-based POSS1The comparison of H NMR spectrogram shows that the methyl peak of methoxyl at 3.50ppm of epoxy POSS chemical shift signal is completely disappeared1H NMR and13the C NMR spectra are well assigned, thus indicating that the epoxy POSS is successfully synthesized. In addition, of epoxy-based POSS1The 2.30ppm chemical shift signal in H NMR was attributable to the methyl peak of the solvent toluene; the FT-IR spectrum of the epoxy-based POSS is shown in FIG. 4 at 2936cm-1And 2856cm-1Stretching vibration of methylene was detected at 1250cm-1The peak at which the vibration is attributed to C-Si stretching vibration is 1119cm-1The peak at (a) is attributed to the Si-O-Si tensile vibration. 901cm-1The peaks in (a) are due to the characteristic absorption peaks of the epoxy groups, indicating that the epoxy groups remain intact and do not open rings when the hydrolysis process produces epoxy-based POSS. Compared with the spectrum of the raw material KH560, the epoxy group POSS is 1399cm-1The methyl peak at (a) disappeared, indicating that the hydrolysis was more complete. Combining the above results, the preparation of epoxy-based POSS was successful.
S2, mixing the epoxy polyhedral polysilsesquioxane with epoxy resin, a phenolic epoxy curing agent and a solvent to prepare the epoxy polyhedral polysilsesquioxane, wherein the mass of the epoxy polyhedral polysilsesquioxane accounts for 1% -5% of the total mass of the epoxy polyhedral polysilsesquioxane and the epoxy resin. Preferably, the mass of the epoxy polyhedral polysilsesquioxane accounts for 3 to 5 percent of the total mass of the epoxy polyhedral polysilsesquioxane and the epoxy resin.
Further preferably, the epoxy resin is a bisphenol a type epoxy resin; the solid content of the phenolic epoxy curing agent is 60-70%; the solvent is ethyl acetate. It should be noted that the bisphenol a type epoxy resin is selected because it has excellent stability and heat resistance, and particularly, the E44 type epoxy resin is preferably selected; the solvent is preferably selected to be ethyl acetate because the experiment can be started by optionally toluene, ethyl acetate, isobutanol and ethanol, but the toluene is too toxic to be used in a special scene and is not used as the preferable solvent, and the ethyl acetate has the best solubility and the lowest toxicity compared with the three solvents, so the ethyl acetate is preferably selected.
Further, referring to fig. 5, in the process of performing the mixing and preparing process, the method includes: adding the octa-epoxy polyhedral oligomeric silsesquioxane and the bisphenol A epoxy resin into the phenolic epoxy curing agent, and then adding the ethyl acetate for mixing; wherein the molar weight of the epoxy groups of the octa-epoxy polyhedral polysilsesquioxane is equal to the molar weight of the amino groups in the novolac epoxy curing agent.
Further, in the embodiment of the invention, the mass ratio of the novolac epoxy curing agent to the ethyl acetate is 2: 1. It should be noted that, in the embodiment of the present invention, the mass ratio of the novolac epoxy curing agent to the ethyl acetate is limited because too large or too small a ratio is not favorable for the adhesion of the coating, too large a ratio causes the coating to be too viscous and difficult to spread on the adhesion carrier, and too small a ratio causes the coating mixture to be too thin and easy to be smeared on the carrier plate, resulting in uneven thickness.
The embodiment of the invention also provides the epoxy resin anticorrosive paint which is prepared according to the preparation method of the epoxy resin anticorrosive paint.
Further, the epoxy resin anticorrosive paint provided in the embodiment of the present invention may further optionally include an epoxy diluent, a filler, and an auxiliary agent. Preferably, the filler comprises a phosphate antirust filler and a system filler, and the mass ratio of the epoxy diluent to the phosphate antirust filler to the system filler to the auxiliary agent is 1-3: 20-25: 25-30: 1-2.
In addition, the epoxy resin anticorrosive paint provided by the embodiment of the invention is prepared on power facility equipment in a saline-alkali soil area, namely, the epoxy resin anticorrosive paint provided by the embodiment of the invention is applied to the power facility equipment in the saline-alkali soil area for corrosion protection.
The features and properties of the present invention are described in further detail below with reference to examples.
Example 1
The embodiment provides a preparation method of an epoxy resin anticorrosive paint, which comprises the following preparation processes:
s1, synthesizing the octa-epoxy polyhedral polysilsesquioxane by a classical hydrolysis method. The synthetic route is shown in figure 1, and the specific synthetic method comprises the following steps: adding 4g KH560 and 6mL isopropanol into a 100mL three-neck flask, and magnetically stirring until the mixture is uniformly mixed; in N2Under protection, a mixture of 0.2g tetramethylammonium hydroxide (25% aqueous solution), 1mL deionized water, and 10mL isopropanol was added slowly and stirred at room temperature for 6 h. And (3) after the reaction is finished, decompressing and spinning out isopropanol to obtain viscous liquid, adding 10mL of methylbenzene to dissolve again, reacting for 6 hours at 90 ℃, cooling to room temperature, extracting for multiple times by using a saturated NaCl aqueous solution until the solution is neutral, and finally removing the methylbenzene to obtain viscous octa-epoxy group POSS.
S2, mixing octa-epoxy group POSS, epoxy resin, a novolac epoxy curing agent and a solvent to prepare, wherein the epoxy resin is specifically E44 type epoxy resin, and the solvent is ethyl acetate; the mass of the octa-epoxy group POSS accounts for 1 percent of the total mass of the octa-epoxy group POSS and the epoxy resin. Specifically, the mass of the E44 type epoxy resin is 9.9g, the mass of the octa epoxy group is POSS0.1g, the mass of the novolac epoxy curing agent is 10g, and the mass of the ethyl acetate is 5 g.
The embodiment also provides an epoxy resin anticorrosive paint which is prepared by the preparation method of the epoxy resin anticorrosive paint provided by the embodiment.
The embodiment also provides application of the epoxy resin anticorrosive paint, namely the epoxy resin anticorrosive paint and the preparation method thereof provided by the embodiment are applied to electric facility equipment in saline-alkali soil areas for anticorrosive protection.
Example 2
The embodiment provides a preparation method of an epoxy resin anticorrosive paint, which comprises the following preparation processes:
s1, synthesizing the octa-epoxy polyhedral polysilsesquioxane by a classical hydrolysis method. The synthetic route is shown in figure 1, and the specific synthetic method comprises the following steps: adding 4g KH560 and 6mL isopropanol into a 100mL three-neck flask, and magnetically stirring until the mixture is uniformly mixed; in N2Under protection, a mixture of 0.2g tetramethylammonium hydroxide (25% aqueous solution), 1mL deionized water, and 10mL isopropanol was added slowly and stirred at room temperature for 6 h. And (3) after the reaction is finished, decompressing and spinning out isopropanol to obtain viscous liquid, adding 10mL of methylbenzene to dissolve again, reacting for 6 hours at 90 ℃, cooling to room temperature, extracting for multiple times by using a saturated NaCl aqueous solution until the solution is neutral, and finally removing the methylbenzene to obtain viscous octa-epoxy group POSS.
S2, mixing octa-epoxy group POSS, epoxy resin, a novolac epoxy curing agent and a solvent to prepare, wherein the epoxy resin is specifically E44 type epoxy resin, and the solvent is ethyl acetate; the mass of the octa-epoxy group POSS accounts for 1 percent of the total mass of the octa-epoxy group POSS and the epoxy resin. Specifically, the mass of the E44 type epoxy resin is 9.8g, the mass of the octa epoxy group is POSS0.2g, the mass of the novolac epoxy curing agent is 10g, and the mass of the ethyl acetate is 5 g.
The embodiment also provides an epoxy resin anticorrosive paint which is prepared by the preparation method of the epoxy resin anticorrosive paint provided by the embodiment.
The embodiment also provides application of the epoxy resin anticorrosive paint, namely the epoxy resin anticorrosive paint and the preparation method thereof provided by the embodiment are applied to electric facility equipment in saline-alkali soil areas for anticorrosive protection.
Example 3
The embodiment provides a preparation method of an epoxy resin anticorrosive paint, which comprises the following preparation processes:
s1, synthesizing the octa-epoxy polyhedral polysilsesquioxane by a classical hydrolysis method. The synthetic route is shown in figure 1, and the specific synthetic method comprises the following steps: adding 4g KH560 and 6mL isopropanol into a 100mL three-neck flask, and magnetically stirring until the mixture is uniformly mixed; in N2Under protection, a mixture of 0.2g tetramethylammonium hydroxide (25% aqueous solution), 1mL deionized water, and 10mL isopropanol was added slowly and stirred at room temperature for 6 h. And (3) after the reaction is finished, decompressing and spinning out isopropanol to obtain viscous liquid, adding 10mL of methylbenzene to dissolve again, reacting for 6 hours at 90 ℃, cooling to room temperature, extracting for multiple times by using a saturated NaCl aqueous solution until the solution is neutral, and finally removing the methylbenzene to obtain viscous octa-epoxy group POSS.
S2, mixing octa-epoxy group POSS, epoxy resin, a novolac epoxy curing agent and a solvent to prepare, wherein the epoxy resin is specifically E44 type epoxy resin, and the solvent is ethyl acetate; the mass of the octa-epoxy group POSS accounts for 1 percent of the total mass of the octa-epoxy group POSS and the epoxy resin. Specifically, the mass of the E44 type epoxy resin is 9.7g, the mass of the octa epoxy group is POSS0.3g, the mass of the novolac epoxy curing agent is 10g, and the mass of the ethyl acetate is 5 g.
The embodiment also provides an epoxy resin anticorrosive paint which is prepared by the preparation method of the epoxy resin anticorrosive paint provided by the embodiment.
The embodiment also provides application of the epoxy resin anticorrosive paint, namely the epoxy resin anticorrosive paint and the preparation method thereof provided by the embodiment are applied to electric facility equipment in saline-alkali soil areas for anticorrosive protection.
Example 4
The embodiment provides a preparation method of an epoxy resin anticorrosive paint, which comprises the following preparation processes:
s1, synthesizing the octa-epoxy polyhedral polysilsesquioxane by a classical hydrolysis method. Synthetic pathwayThe line is shown in figure 1, and the specific synthesis method comprises the following steps: adding 4g KH560 and 6mL isopropanol into a 100mL three-neck flask, and magnetically stirring until the mixture is uniformly mixed; in N2Under protection, a mixture of 0.2g tetramethylammonium hydroxide (25% aqueous solution), 1mL deionized water, and 10mL isopropanol was added slowly and stirred at room temperature for 6 h. And (3) after the reaction is finished, decompressing and spinning out isopropanol to obtain viscous liquid, adding 10mL of methylbenzene to dissolve again, reacting for 6 hours at 90 ℃, cooling to room temperature, extracting for multiple times by using a saturated NaCl aqueous solution until the solution is neutral, and finally removing the methylbenzene to obtain viscous octa-epoxy group POSS.
S2, mixing octa-epoxy group POSS, epoxy resin, a novolac epoxy curing agent and a solvent to prepare, wherein the epoxy resin is specifically E44 type epoxy resin, and the solvent is ethyl acetate; the mass of the octa-epoxy group POSS accounts for 1 percent of the total mass of the octa-epoxy group POSS and the epoxy resin. Specifically, the mass of the E44 type epoxy resin is 9.6g, the mass of the octa epoxy group is POSS0.4g, the mass of the novolac epoxy curing agent is 10g, and the mass of the ethyl acetate is 5 g.
The embodiment also provides an epoxy resin anticorrosive paint which is prepared by the preparation method of the epoxy resin anticorrosive paint provided by the embodiment.
The embodiment also provides application of the epoxy resin anticorrosive paint, namely the epoxy resin anticorrosive paint and the preparation method thereof provided by the embodiment are applied to electric facility equipment in saline-alkali soil areas for anticorrosive protection.
Example 5
The embodiment provides a preparation method of an epoxy resin anticorrosive paint, which comprises the following preparation processes:
s1, synthesizing the octa-epoxy polyhedral polysilsesquioxane by a classical hydrolysis method. The synthetic route is shown in figure 1, and the specific synthetic method comprises the following steps: adding 4g KH560 and 6mL isopropanol into a 100mL three-neck flask, and magnetically stirring until the mixture is uniformly mixed; in N2Under protection, a mixture of 0.2g tetramethylammonium hydroxide (25% aqueous solution), 1mL deionized water, and 10mL isopropanol was added slowly and stirred at room temperature for 6 h. After the reaction is finished, the isopropanol is removed by decompression to obtain viscous liquid, 10mL of toluene is added for re-dissolution, and the mixture is dissolved at 90 DEG CReacting for 6 hours at the temperature, cooling to room temperature, extracting for multiple times by using a saturated NaCl aqueous solution until the solution is neutral, and finally removing toluene to obtain viscous octa-epoxy group POSS.
S2, mixing octa-epoxy group POSS, epoxy resin, a novolac epoxy curing agent and a solvent to prepare, wherein the epoxy resin is specifically E44 type epoxy resin, and the solvent is ethyl acetate; the mass of the octa-epoxy group POSS accounts for 1 percent of the total mass of the octa-epoxy group POSS and the epoxy resin. Specifically, the mass of the E44 type epoxy resin is 9.5g, the mass of the octa epoxy group is POSS0.5g, the mass of the novolac epoxy curing agent is 10g, and the mass of the ethyl acetate is 5 g.
The embodiment also provides an epoxy resin anticorrosive paint which is prepared by the preparation method of the epoxy resin anticorrosive paint provided by the embodiment.
The embodiment also provides an application of the epoxy resin anticorrosive paint, namely the epoxy resin anticorrosive paint and the preparation method thereof provided by the embodiment are applied to power grid electric facility equipment in saline-alkali soil areas for anticorrosive protection.
Example 6
The epoxy resin anticorrosive paint and the preparation method thereof provided by the embodiment are substantially the same as those in the embodiment 5, except that the epoxy resin anticorrosive paint further comprises epoxy diluent, filler, auxiliary agent and other paint-related agents, and the specific formula is shown in table 1:
table 1 the formulation of the saline-alkali resistant epoxy resin anticorrosive coating provided in example 6
The embodiment also provides application of the epoxy resin anticorrosive paint, namely the epoxy resin anticorrosive paint and the preparation method thereof provided by the embodiment are applied to electric facilities in saline-alkali soil areas for anticorrosive protection.
Test examples
In order to identify and verify the technical effects of the epoxy resin anticorrosive paint obtained in the embodiment of the invention, the epoxy resin anticorrosive paint in the embodiments 1 to 5 is selected as a sample of a test example, and a comparative example (namely when the content of epoxy POSS is zero) is added for carrying out multi-dimensional and all-directional protection performance evaluation, wherein the ingredients and contents of different groups in the test example are as shown in the following table 2:
TABLE 2 proportion of corresponding coatings with different epoxy POSS contents
a. Evaluation of salt and alkali resistance
To evaluate the corrosion protection performance of the coatings provided in the test examples in saline-alkaline environments, the applicant's project group designed accelerated simulation experiments. The aqueous solution comprises 1% KCl, 1% MgCl2，2％NaCl，5％Na2CO3(simulating the condition of real saline-alkali soil), the salt content of the solution is about 10 times (6 thousandths) higher than that of the saline-alkali soil, the pH value is 10, the pH value is higher than that of the high saline-alkali soil (9.5), and the temperature is 40 ℃. The specific operation method comprises the following steps: and (3) placing the steel plates coated with the POSS coatings with different contents into a water bath at 40 ℃ to perform a salt and alkali resistance test of the coatings, observing the steel plates at intervals of 24h at a part placed in the water bath of about 2/3, and recording the conditions of the steel plates (refer to GB/T9265-2009 to perform the salt and alkali resistance test of the coatings). Table 3 shows the test results of the corrosion-resistant coating after the saline-alkali accelerated soaking test. The evaluation result shows that the salt-base protection capability of the epoxy resin can be obviously improved by the covalent introduction of the epoxy POSS. When the POSS content reaches more than 3%, the saline-alkali resistance of the material is remarkably improved.
Table 37 days saline alkali resistance accelerated test result evaluation table
| Sample plate | Degree of destruction | Degree of color change | Degree of powdering | Grade of rust |
| EP-0 | 5 | 4 | 4 | 5 |
| EP-1 | 4 | 4 | 2 | 4 |
| EP-2 | 4 | 3 | 1 | 4 |
| EP-3 | 2 | 2 | 0 | 2 |
| EP-4 | 2 | 1 | 0 | 2 |
| EP-5 | 0 | 0 | 0 | 1 |
Note: referring to GB/T1766-.
b. Evaluation of acid resistance
In order to evaluate the protective capability of the epoxy resin anticorrosive paint in an acid environment, the acid resistance of the paint is evaluated. Preparing a sulfuric acid solution with the pH value of 2, putting the prepared sample into the solution, immersing 2/3, observing the condition of the steel plate at intervals of 24h and 48h, and observing whether the paint film has the phenomena of discoloration, bubbling, stripping, powdering, softening and the like. As can be seen from Table 4 and FIG. 6, none of the coatings with POSS added thereto was corroded, and the steel sheets without POSS added thereto showed small-area corrosion and were concentrated on the edges, indicating that the acid resistance was improved by the addition of POSS.
Table 448 h acid resistance test result evaluation table
Note: referring to GB/T1766-.
c. Evaluation of thermal stability
In order to evaluate the heat resistance of the POSS modified epoxy resin, the thermal stability test is carried out. FIG. 7 is a TGA graph of epoxy resins with different amounts of POSS and the atmosphere tested was nitrogen. Analysis can obtain: the thermal decomposition temperature of the epoxy resin is about 350 ℃, the residual mass of the coating is still more than 60% at 400 ℃, and the heat resistance of the coating added with POSS is better than that of the coating not added with POSS; the temperature of 5 percent of thermal weight loss is between 200 and 250 ℃, the temperature of 10 percent of thermal weight loss is about 315 ℃, the thermal decomposition temperature is about 341 ℃, and the final carbon residue rate is about 17 percent; the weight loss at the beginning is presumed to be caused by volatilization of a small amount of residual solvent in the sample and decomposition of a small amount of curing agent which does not participate in curing, and then the cured epoxy resin is decomposed and lost weight, and the quality tends to be stable at about 480 ℃. Therefore, the test result shows that the POSS modified epoxy resin anticorrosive paint prepared by the embodiment of the invention has excellent thermal stability and can meet the use requirement.
Furthermore, by combining the performance tests of saline-alkali resistance, acid resistance and thermal stability, the saline-alkali resistance, acid resistance and high-temperature resistance of the epoxy resin anticorrosive paint are remarkably improved and excellent when the content of the epoxy POSS is more than 3 wt%, and the performance reaches the best when the content of the epoxy POSS is 5 wt%. Thus, when an epoxy POSS content of 5 wt% is selected for use herein, further formulation and evaluation is conducted based on example 5. Specifically, the formulation, such as the coating formulation provided in example 6 of the present invention.
Further, in the evaluation process, the requirements and the treatment method of the substrate accord with the regulations of GB/T9271, and the surface treatment of the test panel reaches Sa2.5 grade regulated in GB/T8923; the test pattern size is about 150mm x 75mm x 1 mm; the thickness of the coating is controlled to be 200 +/-20 mu m; the salt spray resistance test standard is tested according to the GB1771-2007 color paint and varnish neutral salt spray resistance performance measurement. Specifically, the epoxy POSS modified epoxy resin anticorrosive coating is examined by adopting a conventional salt spray resistance test of 3000 hours and a scratch salt spray test of 1000 hours, whether a paint film is foamed, fallen off and rusted or not is mainly observed, and meanwhile, the scratch salt spray test also needs to examine the corrosion expansion condition at the scratch. The salt spray resistance test is carried out by entrusting the China ship industrial ship coating building door detection station, and the test results are shown in Table 5 and FIG. 8:
TABLE 5 salt spray resistance test results for coating systems
According to a table and a figure, the epoxy POSS modified epoxy resin anticorrosive coating has excellent salt spray resistance and corrosion resistance.
Furthermore, the present application further performs a salt spray resistance + damp-heat cycle test on the epoxy resin anticorrosive paint corresponding to the above example 6, in the test process, a 168h neutral salt spray test is performed according to the specification of GB/T1771, a 168h damp-heat test is performed according to the specification of GB/T1740, so that there are 12 cycle periods in total, and a salt spray resistance damp-heat cycle test is performed at a china ship industrial ship paint building door inspection station, and the test result is as shown in fig. 9, and it can be seen from the salt spray damp-heat cycle test result of fig. 9 that after the 12 cycle salt spray damp-heat cycle test is completed, the coating has no phenomena of blistering, cracking, rusting, and the like, which indicates that the coating has excellent anticorrosive performance.
In conclusion, in the preparation method of the epoxy resin anticorrosive paint provided by the embodiment of the invention, the epoxy polyhedral polysilsesquioxane is introduced into the epoxy resin for modification to obtain the polyhedral polysilsesquioxane covalent hybrid epoxy resin, and then the polyhedral polysilsesquioxane covalent hybrid epoxy resin is compounded with the phenolic epoxy curing agent and the solvent in a certain proportion to prepare the epoxy resin anticorrosive paint; the epoxy resin anticorrosive paint has good acid and alkali resistance, cohesiveness, thermal stability and corrosion resistance, and has the best performance at 5% of epoxy POSS content, so that the epoxy resin anticorrosive paint and the preparation method thereof provided by the embodiment of the invention have important significance for corrosion prevention in the power grid protection process, and especially have obvious advantages for power grid protection in saline-alkali soil areas.
The embodiments described above are some, but not all embodiments of the invention. The detailed description of the embodiments of the present invention is not intended to limit the scope of the invention as claimed, but is merely representative of selected embodiments of the invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Claims (10)
1. The preparation method of the epoxy resin anticorrosive paint is characterized by comprising the following steps of:
synthesizing epoxy polyhedral polysilsesquioxane by a classical hydrolysis method;
mixing the epoxy polyhedral polysilsesquioxane, epoxy resin, a novolac epoxy curing agent and a solvent to prepare the epoxy polyhedral polysilsesquioxane, wherein the mass of the epoxy polyhedral polysilsesquioxane accounts for 1-5% of the total mass of the epoxy polyhedral polysilsesquioxane and the epoxy resin.
2. The method for preparing the epoxy resin anticorrosive paint according to claim 1, wherein the mass of the epoxy polyhedral polysilsesquioxane is 3-5% of the total mass of the epoxy polyhedral polysilsesquioxane and the epoxy resin.
3. The method for preparing the epoxy resin anticorrosive paint according to claim 2, wherein the epoxy polyhedral polysilsesquioxane is an octaepoxy polyhedral polysilsesquioxane; the epoxy resin is bisphenol A type epoxy resin; the solid content of the phenolic epoxy curing agent is 60-70%; the solvent is ethyl acetate.
4. The method for preparing the epoxy resin anticorrosive paint according to claim 3, wherein the mixing and formulating process comprises:
adding the octa-epoxy polyhedral oligomeric silsesquioxane and the bisphenol A epoxy resin into the phenolic epoxy curing agent, and then adding the ethyl acetate for mixing; wherein the molar weight of the epoxy groups of the octa-epoxy polyhedral polysilsesquioxane is equal to the molar weight of the amino groups in the novolac epoxy curing agent.
5. The preparation method of the epoxy resin anticorrosive paint according to claim 4, wherein the mass ratio of the novolac epoxy curing agent to the ethyl acetate is 2: 1.
6. The preparation method of the epoxy resin anticorrosive paint according to claim 3, wherein the epoxy resin is E44 type epoxy resin.
7. An epoxy resin anticorrosive paint, characterized in that the epoxy resin anticorrosive paint is prepared according to the preparation method of the epoxy resin anticorrosive paint of any one of claims 1 to 6.
8. The epoxy resin anticorrosive paint according to claim 7, further comprising an epoxy diluent, a filler and an auxiliary.
9. The epoxy resin anticorrosive paint according to claim 8, wherein the filler comprises a phosphate antirust filler and a system filler, and the mass ratio of the epoxy diluent to the phosphate antirust filler to the system filler to the auxiliary agent is 1-3: 20-25: 25-30: 1-2.
10. The epoxy resin anticorrosive paint according to claim 9, wherein the epoxy resin anticorrosive paint is formulated on electric facilities in saline-alkali soil areas.
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