Moistureproof and dustproof epoxy paint and preparation method thereof

Abstract

The invention discloses moisture-proof and dust-proof epoxy paint and a preparation method thereof, and belongs to the technical field of paint. The invention discloses moisture-proof and dust-proof epoxy paint which comprises the following raw material components in parts by weight: 100 parts of high-temperature-resistant epoxy resin, 0.8-1.2 parts of a curing agent, 8-12 parts of waterproof silicon resin, 4-6 parts of a defoaming agent, 5 parts of a flatting agent, 10-15 parts of a solvent and 1-3 parts of an antistatic agent, the high-temperature-resistant epoxy resin is obtained by reacting and grafting 1-bromine-4-(trifluorovinyloxy) benzene, cardanol and phosphonitrilic chloride trimer and then performing epoxidation; the waterproof silicon resin is obtained by carrying out polycondensation on 3-glycidyl ether oxypropyl triethoxy silane and tetraethyl orthosilicate and then carrying out end capping by adopting 4-[trifluorovinyl (oxygen) phenyl] dimethylsilane.

Description

Technical Field

[0001] The invention relates to moisture-proof and dust-proof epoxy paint and a preparation method thereof. Background Art

[0002] With the continuous advancement of industrial technology and the increasing awareness of environmental protection, the coating industry is also constantly developing and innovating. Among the many types of coatings, epoxy paint is widely used for corrosion protection of various metal surfaces due to its excellent adhesion, chemical resistance and mechanical strength. However, in specific application environments, such as outdoor equipment, underground pipelines, ships and marine engineering, the requirements for coating materials are more stringent. Not only must they have good anti-corrosion properties, but they must also have excellent waterproof and dustproof properties to ensure stability and reliability during long-term use.

[0003] Although traditional epoxy paint can provide a certain degree of protection, its waterproof and dustproof capabilities often fail to meet actual needs in extreme environments. Especially in areas with high humidity or frequent sandstorms, the coating easily absorbs moisture or accumulates dust, resulting in a decrease in physical properties, and even bubbling and shedding, which seriously affects the service life and protective effect of the coating. In addition, with the increasing environmental protection requirements, the development of environmentally friendly high-performance epoxy paint has also become one of the research hotspots in the industry.

[0004] In view of the above problems, the present invention provides a moisture-proof and dust-proof epoxy paint and a preparation method thereof. Summary of the invention

[0005] The purpose of the present invention is to provide a moisture-proof and dust-proof epoxy paint and a preparation method thereof, so as to solve the technical problems mentioned in the above background technology.

[0006] The technical solution for achieving the purpose of the present invention is:

[0007] A moisture-proof and dust-proof epoxy paint comprises raw material components, measured by weight: 100 parts by weight of high-temperature resistant epoxy resin, 0.8-1.2 parts by weight of curing agent, 8-12 parts by weight of waterproof silicone resin, 4-6 parts by weight of defoaming agent, 5 parts by weight of leveling agent, 10-15 parts by weight of solvent, and 1-3 parts by weight of antistatic agent.

[0008] Furthermore, the high temperature resistant epoxy resin is obtained by epoxidation after grafting reaction of 1-bromo-4-(trifluorovinyloxy)benzene, cardanol and hexachlorocyclotriphosphazene.

[0009] Furthermore, the waterproof silicone resin is obtained by polycondensing 3-glycidyloxypropyltriethoxysilane and tetraethyl orthosilicate and then end-capping with 4-[trifluorovinyl(oxy)phenyl]dimethylsilane.

[0010] The present invention also provides a method for preparing a moisture-proof and dust-proof epoxy paint, comprising the following preparation steps: 100 parts by mass of a high-temperature resistant epoxy resin, 0.8 to 1.2 parts by mass of a curing agent, 8 to 12 parts by mass of a waterproof silicone resin, 4 to 6 parts by mass of a defoaming agent, 5 parts by mass of a leveling agent, 10 to 15 parts by mass of a solvent, and 1 to 3 parts by mass of an antistatic agent are mixed evenly, heated at 58 to 62° C. and stirred for 28 to 32 minutes, and allowed to mature and defoam for 10 to 15 minutes. After the maturation is completed, the obtained varnish is filtered with a 200-mesh filter cloth, and then poured into a spray gun and waited for spraying.

[0011] Furthermore, the preparation method of the high temperature resistant epoxy resin is as follows: 38 to 42 parts by mass of cardanol cyclotriphosphazene, 6.6 to 7 parts by mass of formic acid, 0.3 to 0.5 parts by mass of p-toluenesulfonic acid, 0.1 to 0.3 parts by mass of stabilizer urea, and 172 to 176 parts by mass of toluene are added to a reactor in sequence, stirred to dissolve and heated to 48 to 52° C., and then 22 to 32 parts by mass of hydrogen peroxide solution are added dropwise, and the addition is completed within 1.5 to 2.5 hours. After the addition is completed, the temperature is raised to 58 to 62° C., and the reaction is continued for 3.5 to 4.5 hours to obtain a high temperature resistant epoxy resin.

[0012] Furthermore, the preparation method of the cardanol-based cyclotriphosphazene is as follows: 11 to 13 parts by mass of sodium hydride and 176 to 180 parts by mass of tetrahydrofuran are stirred and mixed, and then 28 to 32 parts by mass of 1-bromo-4-(trifluorovinyloxy)benzene and 38 to 42 parts by mass of cardanol are added dropwise at -1 to 1°C, and the temperature is raised to 58 to 62°C after the addition is completed, and the reaction is continued for 25 to 35 minutes, and then 13 to 15 parts by mass of a tetrahydrofuran solution of hexachlorocyclotriphosphazene is added dropwise, and the temperature is continued to be raised to 68 to 72°C after the addition is completed, and the reaction is reacted for 23 to 25 hours. After the reaction is completed, it is naturally cooled to room temperature to obtain cardanol-based cyclotriphosphazene.

[0013] Furthermore, the preparation method of the waterproof silicone resin is as follows: 3.3 to 3.5 parts by mass of water, 2.5 to 3.5 parts by mass of ethanol, 0.9 to 1.1 parts by mass of glacial acetic acid, 9.7 to 9.9 parts by mass of 3-glycidyloxypropyltriethoxysilane, and 5.1 to 5.3 parts by mass of tetraethyl orthosilicate are stirred and mixed evenly, heated to 68 to 72° C. for reaction for 2 to 3 hours, cooled to room temperature, and then rotary evaporated at 65 to 75° C. to remove small molecular compounds, and then added 6.9 to 7.1 parts by mass of 4-[trifluorovinyl (oxy)phenyl]dimethylsilane, 0.1 parts by mass of tris(pentafluorophenyl)boron, and 20 parts by mass of toluene, stirred and reacted at 58 to 62° C. for 11 to 13 hours, and after removing the solvent toluene under reduced pressure, purified by silica gel column chromatography using n-hexane as an eluent to obtain a waterproof silicone resin.

[0014] Furthermore, the preparation method of the 4-[trifluorovinyl (oxy) phenyl] dimethyl silane is as follows: 6.34 parts by mass of 50 mesh magnesium powder, 0.001 parts by mass of iodine, 45 parts by mass of chlorodimethylsilane, and 275 parts by mass of tetrahydrofuran are stirred and mixed, and then 60 parts by mass of 1-bromo-4-(trifluorovinyloxy) benzene are added at room temperature. After the mixture starts to release heat and darkens, it is cooled to 0-5°C in an ice bath. After the addition of 1-bromo-4-(trifluorovinyloxy) benzene is completed, it is slowly heated to room temperature within 4.5-5.5 hours, and then stirred at room temperature for 14-16 hours, and the reaction is quenched with 24-26 parts by mass of water and 130-132 parts by mass of hexane. After filtering through silica gel, it is distilled under reduced pressure to obtain 4-[trifluorovinyl (oxy) phenyl] dimethyl silane.

[0015] Furthermore, the solvent is obtained by mixing xylene and butanone in a mass ratio of 5 to 7:4.

[0016] The present invention also provides a method for using the moisture-proof and dust-proof epoxy paint, which comprises spraying the moisture-proof and dust-proof epoxy paint uniformly on the object to be painted, then heating the paint to 60-80°C in an inert gas environment and keeping the paint for 1.5-2.5 hours, then heating the paint to 170-190°C at a rate of 1-3°C / min and keeping the paint for 1.5-2.5 hours, then heating the paint to 190-210°C and keeping the paint for 2-4 hours, and cooling the paint to room temperature.

[0017] By adopting the above technical solution, the present invention has the following beneficial effects:

[0018] The moisture-proof and dust-proof epoxy paint disclosed by the invention comprises, by weight, raw material components: 100 parts by weight of high-temperature resistant epoxy resin, 0.8-1.2 parts by weight of curing agent, 8-12 parts by weight of waterproof silicone resin, 4-6 parts by weight of defoaming agent, 5 parts by weight of leveling agent, 10-15 parts by weight of solvent, and 1-3 parts by weight of antistatic agent; the high-temperature resistant epoxy resin is obtained by epoxidation after grafting reaction of 1-bromo-4-(trifluorovinyloxy)benzene, cardanol and hexachlorocyclotriphosphazene; the waterproof silicone resin is obtained by polycondensing 3-glycidyloxypropyltriethoxysilane and tetraethyl orthosilicate and then end-capping with 4-[trifluorovinyl (oxy)phenyl]dimethylsilane; wherein the high-temperature resistant epoxy resin is used as a substrate, and the resin is obtained by grafting reaction of 1-bromo-4-(trifluorovinyloxy)benzene, cardanol and hexachlorocyclotriphosphazene. The phosphazene is grafted by reaction and then epoxidized, which not only improves the temperature resistance and chemical stability of the resin, but also enhances the mechanical strength of the coating. At the same time, a waterproof silicone resin is added, and the silicone resin is polycondensed by 3-glycidyloxypropyltriethoxysilane and tetraethyl orthosilicate, and then end-capped with 4-[trifluorovinyl (oxy)phenyl]dimethylsilane to form a dense hydrophobic layer, which effectively blocks water penetration and reduces dust adsorption. In addition, an appropriate amount of defoamer, leveling agent and solvent ensures the uniformity and flatness of the coating during construction, while the antistatic agent can further reduce the electrostatic effect on the surface of the coating to prevent dust adhesion. The moisture-proof and dust-proof epoxy paint prepared by the present invention has excellent waterproof and dust-proof properties after curing, and the heat resistance and mechanical properties are also significantly improved, which is suitable for long-term protection in a variety of harsh environments.

[0019] Firstly, cardanol is derived from the natural product cashew nut shell oil, which gives the epoxy resin excellent mechanical properties and thermal stability, as well as excellent chemical resistance, high bonding strength, low shrinkage and biodegradability; hexachlorocyclotriphosphazene derivatives not only have good hydrolysis resistance, but the synergistic effect of phosphorus and nitrogen elements in their structure further improves the resin's heat resistance and halogen-free flame retardant properties; the introduction of 1-bromo-4-(trifluorovinyloxy)benzene, by increasing the rigidity of the molecular chain and the hydrophobic and oleophobic properties of the fluorine element, gives the resin better hydrophobicity and lower surface energy, reduces the adsorption of moisture and dust, and enhances the resin's weather resistance and waterproof properties; 1-bromo-4-(trifluorovinyloxy)benzene, cardanol and hexachlorocyclotriphosphazene are reacted and grafted and then epoxidized to form an epoxy resin with a branched structure with a phosphazene ring as the core. This branched structure significantly improves the crosslinking density of the resin and enhances the mechanical strength and chemical resistance of the coating.

[0020] Secondly, the waterproof silicone resin is prepared by polycondensing 3-glycidyloxypropyltriethoxysilane with tetraethyl orthosilicate and then end-capping with 4-[trifluorovinyl(oxy)phenyl]dimethylsilane; the introduction of 4-[trifluorovinyl(oxy)phenyl]dimethylsilane not only effectively prevents the explosion and gelation phenomena that may occur during the polycondensation process, but also gives the silicone resin excellent hydrophobicity and dustproofness; this is because the fluorocarbon chain in the end-capping group has an extremely low surface energy and can form a dense hydrophobic barrier to effectively prevent the intrusion of moisture and dust; in addition, the stability and chemical inertness of the end-capping group also enhance the overall weather resistance and aging resistance of the resin, ensuring the reliability and stability of the coating in long-term use.

[0021] Finally, during use, the moisture-proof and dust-proof epoxy paint undergoes multi-stage temperature-raising curing in an inert gas environment. The cross-linked high-temperature resistant epoxy resin and the trifluoroethylene in the waterproof silicone resin are cross-linked at high temperature to form a tighter three-dimensional network structure, which further improves the cross-linking density of the moisture-proof and dust-proof epoxy paint. This not only enhances the mechanical strength and chemical resistance of the coating, but also significantly improves the waterproof and dustproof properties of the coating. At the same time, the inert gas environment effectively avoids the influence of oxygen and other impurities, ensuring the uniformity and controllability of the curing process, thereby ensuring the quality and performance of the final coating. DETAILED DESCRIPTION

[0022] In order to better understand the above technical solution, the above technical solution will be described in detail below in conjunction with specific implementation methods.

[0023] Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without making any creative work shall fall within the scope of protection of the present invention.

[0024] The following embodiments are only used to more clearly illustrate the technical solutions of the present invention, and are not intended to limit the protection scope of the present invention.

[0025] The curing agent is DMP-30;

[0026] The defoamer is obtained by mixing BYK-141 of Guangzhou Daixun Trading Co., Ltd. and a solvent, wherein BYK-141 accounts for 10wt%;

[0027] The leveling agent is obtained by mixing BYK-306 of Guangzhou Daixun Trading Co., Ltd. and a solvent, wherein BYK-306 accounts for 10wt%;

[0028] The antistatic agent is sodium dodecylbenzene sulfonate.

[0029] Example 1

[0030] A method for using moisture-proof and dust-proof epoxy paint comprises spraying the moisture-proof and dust-proof epoxy paint evenly on a wooden board, then heating to 60°C in an inert gas environment and keeping the temperature for 1.5 hours, then heating to 170°C at a rate of 1°C / min and keeping the temperature for 1.5 hours, then heating to 190°C and keeping the temperature for 2 hours, and cooling to room temperature.

[0031] A method for preparing a moisture-proof and dust-proof epoxy paint comprises the following preparation steps: 100 parts by mass of a high-temperature resistant epoxy resin, 0.8 parts by mass of a curing agent, 8 parts by mass of a waterproof silicone resin, 4 parts by mass of a defoaming agent, 5 parts by mass of a leveling agent, 10 parts by mass of a solvent, and 1 part by mass of an antistatic agent are uniformly mixed, and then heated at 58°C and stirred for 28 minutes, and statically aged and defoamed for 10 minutes. After the aging is completed, the prepared varnish is filtered with a 200-mesh filter cloth, and then poured into a spray gun and waited for spraying.

[0032] The preparation method of the high temperature resistant epoxy resin is as follows: 38 parts by mass of cardanol cyclotriphosphazene, 6.6 parts by mass of formic acid, 0.3 parts by mass of p-toluenesulfonic acid, 0.1 parts by mass of stabilizer urea, and 172 parts by mass of toluene are added into a reactor in sequence, stirred to dissolve and heated to 48°C, then 22 parts by mass of 30% hydrogen peroxide solution is added dropwise, and the addition is completed within 1.5 hours. After the addition is completed, the temperature is raised to 58°C, and the reaction is continued for 3.5 hours. After the reaction is completed, it is naturally cooled to room temperature, an upper organic phase is taken, the upper organic phase is washed with distilled water until it is neutral, and finally the organic phase is dried with anhydrous sodium sulfate, and toluene is evaporated under reduced pressure to obtain a high temperature resistant epoxy resin.

[0033] The preparation method of the cardanol-based cyclotriphosphazene is as follows: 11 parts by mass of 60 wt% sodium hydride and 176 parts by mass of tetrahydrofuran are stirred and mixed, and then 28 parts by mass of 1-bromo-4-(trifluorovinyloxy)benzene and 38 parts by mass of cardanol are added dropwise at -1°C within 2 hours, and the temperature is raised to 58°C at 2°C / min after the addition is completed, and the reaction is continued for 25 minutes, and then 13 parts by mass of 1M tetrahydrofuran solution of hexachlorocyclotriphosphazene is added dropwise, and the addition is completed within 3.5 hours, and the temperature is continued to be raised to 68°C after the addition is completed, and the reaction is continued for 23 hours, and the reaction is naturally cooled to room temperature after the reaction is completed, and the THF solvent is first evaporated under reduced pressure, and unreacted cardanol and incompletely substituted by-products are washed with acetonitrile, and then dissolved in ethyl acetate, and washed with 5wt% NaOH three times, and then the organic phase is washed with distilled water until neutral; finally, the organic phase is dried with anhydrous sodium sulfate, and the ethyl acetate is evaporated under reduced pressure to obtain the cardanol-based cyclotriphosphazene.

[0034] The preparation method of the waterproof silicone resin is as follows: 3.3 parts by mass of water, 2.5 parts by mass of ethanol, 0.9 parts by mass of glacial acetic acid, 9.7 parts by mass of 3-glycidyloxypropyltriethoxysilane, and 5.1 parts by mass of tetraethyl orthosilicate are stirred and mixed evenly, heated to 68° C. for reaction for 2 hours, cooled to room temperature, and then rotary evaporated at 65° C. to remove solvents and other small molecular compounds, then added with 6.9 parts by mass of 4-[trifluorovinyl(oxy)phenyl]dimethylsilane, 0.1 parts by mass of tris(pentafluorophenyl)boron, and 20 parts by mass of toluene, stirred and reacted at 58° C. for 11 hours, and after removing the solvent toluene under reduced pressure, purified by silica gel column chromatography using n-hexane as an eluent to obtain the waterproof silicone resin.

[0035] The preparation method of the 4-[trifluorovinyl (oxy) phenyl] dimethyl silane is as follows: 6.34 parts by mass of 50-mesh magnesium powder, 0.001 parts by mass of iodine, 45 parts by mass of chlorodimethylsilane, and 275 parts by mass of tetrahydrofuran are stirred and mixed, and then 60 parts by mass of 1-bromo-4-(trifluorovinyloxy) benzene are added at room temperature. After the mixture starts to release heat and darkens, it is cooled to 0° C. in an ice bath. After the addition of 1-bromo-4-(trifluorovinyloxy) benzene is completed, the temperature is slowly raised to room temperature within 4.5 hours, and then stirring is continued at room temperature for 14 hours. The reaction is quenched with 24 parts by mass of water and 130 parts by mass of hexane, and filtered through silica gel and then distilled under reduced pressure to obtain 4-[trifluorovinyl (oxy) phenyl] dimethyl silane.

[0036] The solvent is obtained by mixing xylene and butanone in a mass ratio of 5:4.

[0037] Example 2

[0038] A method for using moisture-proof and dust-proof epoxy paint comprises spraying the moisture-proof and dust-proof epoxy paint evenly on a wooden board, then heating to 70°C in an inert gas environment for 2 hours, then heating to 180°C at a rate of 2°C / min for 2 hours, then heating to 200°C for 3 hours, and cooling to room temperature.

[0039] A method for preparing a moisture-proof and dust-proof epoxy paint comprises the following preparation steps: 100 parts by mass of a high-temperature resistant epoxy resin, 1 part by mass of a curing agent, 10 parts by mass of a waterproof silicone resin, 5 parts by mass of a defoaming agent, 5 parts by mass of a leveling agent, 13 parts by mass of a solvent, and 2 parts by mass of an antistatic agent are uniformly mixed, then heated at 60°C and stirred for 30 minutes, statically aged and defoamed for 13 minutes, and after the aging is completed, the prepared varnish is filtered with a 200-mesh filter cloth, and then poured into a spray gun and waited for spraying.

[0040] The preparation method of the high temperature resistant epoxy resin is as follows: 40 parts by mass of cardanol cyclotriphosphazene, 6.8 parts by mass of formic acid, 0.4 parts by mass of p-toluenesulfonic acid, 0.2 parts by mass of stabilizer urea, and 174 parts by mass of toluene are added into a reactor in sequence, stirred to dissolve and heated to 50° C., then 27 parts by mass of 30% hydrogen peroxide solution is added dropwise, and the addition is completed within 2 hours. After the addition is completed, the temperature is raised to 60° C. and the reaction is continued for 4 hours. After the reaction is completed, it is naturally cooled to room temperature, an upper organic phase is taken, the upper organic phase is washed with distilled water until it is neutral, and finally the organic phase is dried with anhydrous sodium sulfate, and the toluene is evaporated under reduced pressure to obtain a high temperature resistant epoxy resin.

[0041] The preparation method of the cardanol-based cyclotriphosphazene is as follows: 12 parts by mass of 60wt% sodium hydride and 178 parts by mass of tetrahydrofuran are stirred and mixed, and then 30 parts by mass of 1-bromo-4-(trifluorovinyloxy)benzene and 40 parts by mass of cardanol are added dropwise at 0°C within 2 hours, and the temperature is raised to 60°C at 3°C / min after the addition is completed, and the reaction is continued for 30 minutes, and then 14 parts by mass of 1M tetrahydrofuran solution of hexachlorocyclotriphosphazene is added dropwise for 4 hours, and the temperature is continued to be raised to 70°C after the addition is completed, and the reaction is carried out for 24 hours, and the reaction is naturally cooled to room temperature after the reaction is completed, and the THF solvent is first evaporated under reduced pressure, and unreacted cardanol and incompletely substituted by-products are washed with acetonitrile, and then dissolved in ethyl acetate, and washed with 5wt% NaOH three times, and then the organic phase is washed with distilled water until neutral; finally, the organic phase is dried with anhydrous sodium sulfate, and the ethyl acetate is evaporated under reduced pressure to obtain the cardanol-based cyclotriphosphazene.

[0042] The preparation method of the waterproof silicone resin is as follows: 3.4 parts by mass of water, 3 parts by mass of ethanol, 1 part by mass of glacial acetic acid, 9.8 parts by mass of 3-glycidyloxypropyltriethoxysilane, and 5.2 parts by mass of tetraethyl orthosilicate are stirred and mixed evenly, heated to 70°C for reaction for 2.5 hours, cooled to room temperature, and then evaporated at 70°C to remove solvents and other small molecular compounds, then added with 7 parts by mass of 4-[trifluorovinyl(oxy)phenyl]dimethylsilane, 0.1 parts by mass of tris(pentafluorophenyl)boron, and 20 parts by mass of toluene, stirred and reacted at 60°C for 12 hours, and after removing the solvent toluene under reduced pressure, purified by silica gel column chromatography using n-hexane as an eluent to obtain the waterproof silicone resin.

[0043] The preparation method of the 4-[trifluorovinyl (oxy) phenyl] dimethyl silane is as follows: 6.34 parts by mass of 50-mesh magnesium powder, 0.001 parts by mass of iodine, 45 parts by mass of chlorodimethylsilane, and 275 parts by mass of tetrahydrofuran are stirred and mixed, and then 60 parts by mass of 1-bromo-4-(trifluorovinyloxy) benzene are added at room temperature. After the mixture starts to release heat and darkens, it is cooled to 3° C. in an ice bath. After the addition of 1-bromo-4-(trifluorovinyloxy) benzene is completed, the temperature is slowly raised to room temperature within 5 hours, and then stirring is continued at room temperature for 15 hours. The reaction is quenched with 25 parts by mass of water and 131 parts by mass of hexane, and filtered through silica gel and then distilled under reduced pressure to obtain 4-[trifluorovinyl (oxy) phenyl] dimethyl silane.

[0044] The solvent is obtained by mixing xylene and butanone in a mass ratio of 6:4.

[0045] Example 3

[0046] A method for using moisture-proof and dust-proof epoxy paint comprises spraying the moisture-proof and dust-proof epoxy paint evenly on a wooden board, then heating to 80°C in an inert gas environment and keeping the temperature for 2.5 hours, then heating to 190°C at a rate of 3°C / min and keeping the temperature for 2.5 hours, then heating to 210°C and keeping the temperature for 4 hours, and cooling to room temperature.

[0047] A method for preparing a moisture-proof and dust-proof epoxy paint comprises the following preparation steps: 100 parts by mass of a high-temperature resistant epoxy resin, 1.2 parts by mass of a curing agent, 12 parts by mass of a waterproof silicone resin, 6 parts by mass of a defoaming agent, 5 parts by mass of a leveling agent, 15 parts by mass of a solvent, and 3 parts by mass of an antistatic agent are uniformly mixed, then heated at 62°C and stirred for 32 minutes, statically aged and defoamed for 15 minutes, and after the aging is completed, the prepared varnish is filtered with a 200-mesh filter cloth, and then poured into a spray gun and waited for spraying.

[0048] The preparation method of the high temperature resistant epoxy resin is as follows: 42 parts by mass of cardanol cyclotriphosphazene, 7 parts by mass of formic acid, 0.5 parts by mass of p-toluenesulfonic acid, 0.3 parts by mass of stabilizer urea, and 176 parts by mass of toluene are added into a reactor in sequence, stirred to dissolve and heated to 52° C., then 32 parts by mass of 30% hydrogen peroxide solution is added dropwise, and the addition is completed within 2.5 hours. After the addition is completed, the temperature is raised to 62° C. and the reaction is continued for 4.5 hours. After the reaction is completed, it is naturally cooled to room temperature, an upper organic phase is taken, the upper organic phase is washed with distilled water until it is neutral, and finally the organic phase is dried with anhydrous sodium sulfate, and toluene is evaporated under reduced pressure to obtain a high temperature resistant epoxy resin.

[0049] The preparation method of the cardanol-based cyclotriphosphazene is as follows: 13 parts by mass of 60wt% sodium hydride and 180 parts by mass of tetrahydrofuran are stirred and mixed, and then 32 parts by mass of 1-bromo-4-(trifluorovinyloxy)benzene and 42 parts by mass of cardanol are added dropwise at 1°C within 2 hours, and the temperature is raised to 62°C at 4°C / min after the addition is completed, and the reaction is continued for 35 minutes, and then 15 parts by mass of 1M tetrahydrofuran solution of hexachlorocyclotriphosphazene is added dropwise, and the addition is completed within 4.5 hours, and the temperature is continued to be raised to 72°C after the addition is completed, and the reaction is carried out for 25 hours, and the reaction is naturally cooled to room temperature after the reaction is completed, and the THF solvent is first evaporated under reduced pressure, and unreacted cardanol and incompletely substituted by-products are washed with acetonitrile, and then dissolved in ethyl acetate, and washed with 5wt% NaOH three times, and then the organic phase is washed with distilled water until neutral; finally, the organic phase is dried with anhydrous sodium sulfate, and the ethyl acetate is evaporated under reduced pressure to obtain the cardanol-based cyclotriphosphazene.

[0050] The preparation method of the waterproof silicone resin is as follows: 3.5 parts by mass of water, 3.5 parts by mass of ethanol, 1.1 parts by mass of glacial acetic acid, 9.9 parts by mass of 3-glycidyloxypropyltriethoxysilane, and 5.3 parts by mass of tetraethyl orthosilicate are stirred and mixed evenly, heated to 72° C. for reaction for 3 hours, cooled to room temperature, and then rotary evaporated at 75° C. to remove solvents and other small molecular compounds, then added with 7.1 parts by mass of 4-[trifluorovinyl(oxy)phenyl]dimethylsilane, 0.1 parts by mass of tris(pentafluorophenyl)boron, and 20 parts by mass of toluene, stirred and reacted at 62° C. for 13 hours, and after removing the solvent toluene under reduced pressure, purified by silica gel column chromatography using n-hexane as an eluent to obtain the waterproof silicone resin.

[0051] The preparation method of the 4-[trifluorovinyl (oxy) phenyl] dimethyl silane is as follows: 6.34 parts by mass of 50-mesh magnesium powder, 0.001 parts by mass of iodine, 45 parts by mass of chlorodimethylsilane, and 275 parts by mass of tetrahydrofuran are stirred and mixed, and then 60 parts by mass of 1-bromo-4-(trifluorovinyloxy) benzene are added at room temperature. After the mixture starts to release heat and darkens, it is cooled to 5° C. in an ice bath. After the addition of 1-bromo-4-(trifluorovinyloxy) benzene is completed, the temperature is slowly raised to room temperature within 5.5 hours, and then stirring is continued at room temperature for 16 hours. The reaction is quenched with 26 parts by mass of water and 132 parts by mass of hexane, and filtered through silica gel and then distilled under reduced pressure to obtain 4-[trifluorovinyl (oxy) phenyl] dimethyl silane.

[0052] The solvent is obtained by mixing xylene and butanone in a mass ratio of 7:4.

[0053] Comparative Example 1

[0054] The only difference between Comparative Example 1 and Example 2 is that the high temperature resistant epoxy resin is obtained by reacting and grafting cardanol with hexachlorocyclotriphosphazene and then epoxidizing it; the remaining steps and components are the same as those in Example 2.

[0055] Comparative Example 2

[0056] The only difference between Comparative Example 2 and Example 2 is that the high temperature resistant epoxy resin is obtained by reacting and grafting cardanol and then epoxidizing it; the remaining steps and components are the same as those in Example 2.

[0057] Comparative Example 3

[0058] The only difference between Comparative Example 3 and Example 2 is that the raw material components of the moisture-proof and dust-proof epoxy paint are different. The raw material components of the moisture-proof and dust-proof epoxy paint of Comparative Example 3 include: high temperature resistant epoxy resin, curing agent, defoaming agent, leveling agent, solvent, antistatic agent; the remaining steps and components are the same as Example 2.

[0059] Comparative Example 4

[0060] The only difference between Comparative Example 4 and Example 2 is the waterproof silicone resin. The waterproof silicone resin in this comparative example is obtained by polycondensing 3-glycidyloxypropyltriethoxysilane and tetraethyl orthosilicate and then capping with hexamethyldisiloxane; the remaining steps and components are the same as those in Example 2.

[0061] Comparative Example 5

[0062] The only difference between Comparative Example 5 and Example 2 is the method of using the moisture-proof and dust-proof epoxy paint. In this comparative example, the method of using the moisture-proof and dust-proof epoxy paint is to evenly spray the moisture-proof and dust-proof epoxy paint on the wooden board, then heat it to 70°C in an inert gas environment for 2 hours, cool it to room temperature, and dry it at room temperature for 24 hours.

[0063] Effect example

[0064] Dust prevention: Crush the carbon powder and pass it through a 300-mesh sieve and evenly spread 60 g on the painted wooden boards of the embodiments and comparative examples. Tilt the wooden boards 15 degrees, use a wind speed of 3 m / s, and blow the carbon powder on the coating parallel to the painted objects for 10 minutes. Then measure the residual amount of carbon powder on the painted objects.

[0065] Waterproofing: The contact angle of deionized water on the wood surface was measured using a contact angle meter for the wood boards sprayed with paint in the embodiments and comparative examples.

[0066] Thermal stability: The initial decomposition temperature T of the high temperature resistant epoxy resin after mixing with the curing agent was measured by a Pyrist TGA thermogravimetric analyzer from Perkin Elmer Instruments. 5％ ; Measurement parameters: nitrogen flow rate 50mL / min, temperature range room temperature ~ 850℃, heating rate 10℃ / min.

[0067] Mechanical properties: The tensile properties of the mixed and cured high temperature resistant epoxy resin, curing agent and waterproof silicone resin of the test examples and comparative examples were tested according to GB / T2569; the flexibility of the moisture-proof and dust-proof epoxy paint of the test examples and comparative examples was tested according to GB / T6742.

[0068] Table 1 below shows the performance data of moisture-proof and dust-proof epoxy paints prepared in Examples and Comparative Examples:

[0069] Table 1

[0070]

[0071]

[0072] As shown in Table 1 above, the moisture-proof and dust-proof epoxy paint prepared in the embodiment has good dust-proofness, thermal stability, water-proofness and mechanical properties.

[0073] Compared with Example 2, Comparative Example 1 performs poorly in dust resistance, thermal stability, water resistance and mechanical properties because the high temperature resistant epoxy resin in Comparative Example 1 lacks 1-bromo-4-(trifluorovinyloxy)benzene, which not only reduces surface energy, improves hydrophobicity and reduces dust adsorption, but also enhances the resin's temperature resistance, chemical stability and forms a tighter cross-linked structure, thereby comprehensively improving the performance of the coating of Example 2.

[0074] Compared with Example 2, Comparative Example 2 performs poorly in dust resistance, thermal stability, water resistance and mechanical properties because hexachlorocyclotriphosphazene is not added in Comparative Example 2. This ingredient can significantly improve the hydrophobicity of the coating, reduce surface energy, enhance heat resistance and halogen-free flame retardant properties, and promote the formation of a more stable cross-linked structure.

[0075] Compared with Example 2, Comparative Example 3 performs poorly in dust resistance, thermal stability, water resistance and mechanical properties because Comparative Example 3 lacks waterproof silicone resin. The hydrophobic layer formed by this component can effectively reduce dust adsorption, improve the water resistance of the coating, and at the same time improve the mechanical strength of the coating.

[0076] Compared with Example 2, Comparative Example 4 performs poorly in dustproofness, thermal stability, water resistance and mechanical properties. The main reason is that the hexamethyldisiloxane-terminated waterproof silicone resin used in Comparative Example 4 is not as good as the 4-[trifluorovinyl(oxy)phenyl]dimethylsilane-terminated waterproof silicone resin in Example 2, which has lower surface energy, better hydrophobicity, higher weather resistance and aging resistance, and can form a tighter three-dimensional network structure, thereby comprehensively improving the dustproofness, thermal stability, water resistance and mechanical properties of the coating.

[0077] The main difference between Comparative Example 5 and Example 2 is the different curing processes. Example 2 adopts a more complex multi-stage temperature-increasing curing process, which helps to form a tighter cross-linked network structure and improve the dustproofness, thermal stability, water resistance and mechanical properties of the coating.

[0078] The specific embodiments described above further illustrate the objectives, technical solutions and beneficial effects of the present invention in detail. It should be understood that the above description is only a specific embodiment of the present invention and is not intended to limit the present invention. Any modifications, equivalent substitutions, improvements, etc. made within the spirit and principles of the present invention should be included in the protection scope of the present invention.

Claims

1. A moisture-proof and dust-proof epoxy paint, characterized in that: In terms of weight, the raw material components include: 100 parts by weight of high temperature resistant epoxy resin, 0.8 to 1.2 parts by weight of curing agent, 8 to 12 parts by weight of waterproof silicone resin, 4 to 6 parts by weight of defoaming agent, 5 parts by weight of leveling agent, 10 to 15 parts by weight of solvent, and 1 to 3 parts by weight of antistatic agent.

2. The moisture-proof and dust-proof epoxy paint according to claim 1, characterized in that: The high temperature resistant epoxy resin is obtained by epoxidation after the reaction and grafting of 1-bromo-4-(trifluorovinyloxy)benzene, cardanol and hexachlorocyclotriphosphazene.

3. The moisture-proof and dust-proof epoxy paint according to claim 1, characterized in that: The waterproof silicone resin is obtained by polycondensing 3-glycidyloxypropyltriethoxysilane and tetraethyl orthosilicate and then end-capping with 4-[trifluorovinyl (oxy)phenyl]dimethylsilane.

4. A method for preparing a moisture-proof and dust-proof epoxy paint as claimed in any one of claims 1 to 3, characterized in that: The method comprises the following preparation steps: 100 parts by weight of high temperature resistant epoxy resin, 0.8 to 1.2 parts by weight of curing agent, 8 to 12 parts by weight of waterproof silicone resin, 4 to 6 parts by weight of defoaming agent, 5 parts by weight of leveling agent, 10 to 15 parts by weight of solvent and 1 to 3 parts by weight of antistatic agent are uniformly mixed, and then heated at 58 to 62° C. and stirred for 28 to 32 minutes, and subjected to static aging and defoaming for 10 to 15 minutes. After aging, the obtained varnish is filtered through a 200-mesh filter cloth, and then poured into a spray gun and waited for spraying.

5. The method for preparing moisture-proof and dust-proof epoxy paint according to claim 4, characterized in that: The preparation method of the high temperature resistant epoxy resin is as follows: 38 to 42 parts by weight of cardanol cyclotriphosphazene, 6.6 to 7 parts by weight of formic acid, 0.3 to 0.5 parts by weight of p-toluenesulfonic acid, 0.1 to 0.3 parts by weight of stabilizer urea, and 172 to 176 parts by weight of toluene are sequentially added into a reaction kettle, stirred to dissolve, and heated to 48 to 52° C., and then 22 to 32 parts by weight of hydrogen peroxide solution are dripped, and the dripping is completed within 1.5 to 2.5 hours. After the dripping is completed, the temperature is raised to 58 to 62° C., and the reaction is continued for 3.5 to 4.5 hours to obtain a high temperature resistant epoxy resin.

6. The method for preparing moisture-proof and dust-proof epoxy paint according to claim 5, characterized in that: The preparation method of the cardanol-based cyclotriphosphazene is as follows: 11 to 13 parts by weight of sodium hydride and 176 to 180 parts by weight of tetrahydrofuran are stirred and mixed, and then 28 to 32 parts by weight of 1-bromo-4-(trifluorovinyloxy)benzene and 38 to 42 parts by weight of cardanol are added dropwise at -1 to 1°C, and the temperature is raised to 58 to 62°C after the addition is completed, and the reaction is continued for 25 to 35 minutes, and then 13 to 15 parts by weight of a tetrahydrofuran solution of hexachlorocyclotriphosphazene is added dropwise, and the temperature is continued to be raised to 68 to 72°C after the addition is completed, and the reaction is carried out for 23 to 25 hours. After the reaction is completed, the cardanol-based cyclotriphosphazene is naturally cooled to room temperature to obtain the cardanol-based cyclotriphosphazene.

7. The method for preparing moisture-proof and dust-proof epoxy paint according to claim 4, characterized in that: The preparation method of the waterproof silicone resin is as follows: 3.3-3.5 parts by weight of water, 2.5-3.5 parts by weight of ethanol, 0.9-1.1 parts by weight of glacial acetic acid, 9.7-9.9 parts by weight of 3-glycidyloxypropyltriethoxysilane, and 5.1-5.3 parts by weight of tetraethyl orthosilicate are stirred and mixed evenly, heated to 68-72° C. for reaction for 2-3 hours, cooled to room temperature, and then evaporated at 65-75° C. to remove small molecular compounds, then added with 6.9-7.1 parts by weight of 4-[trifluorovinyl(oxy)phenyl]dimethylsilane, 0.1 parts by weight of tris(pentafluorophenyl)boron, and 20 parts by weight of toluene, stirred and reacted at 58-62° C. for 11-13 hours, and after removing the solvent toluene under reduced pressure, purified by silica gel column chromatography using n-hexane as an eluent to obtain the waterproof silicone resin.

8. The method for preparing moisture-proof and dust-proof epoxy paint according to claim 7, characterized in that: The preparation method of the 4-[trifluorovinyl (oxy) phenyl] dimethyl silane is as follows: 6.34 parts by mass of 50-mesh magnesium powder, 0.001 parts by mass of iodine, 45 parts by mass of chlorodimethylsilane, and 275 parts by mass of tetrahydrofuran are stirred and mixed, and then 60 parts by mass of 1-bromo-4-(trifluorovinyloxy) benzene are added at room temperature. After the mixture starts to release heat and darkens, it is cooled to 0-5° C. in an ice bath. After the addition of 1-bromo-4-(trifluorovinyloxy) benzene is completed, the temperature is slowly raised to room temperature within 4.5-5.5 hours, and then stirring is continued at room temperature for 14-16 hours. The reaction is quenched with 24-26 parts by mass of water and 130-132 parts by mass of hexane, and filtered through silica gel and then distilled under reduced pressure to obtain 4-[trifluorovinyl (oxy) phenyl] dimethyl silane.

9. The method for preparing moisture-proof and dust-proof epoxy paint according to claim 4, characterized in that: The solvent is obtained by mixing xylene and butanone in a mass ratio of 5 to 7:

4.

10. A method for using the moisture-proof and dust-proof epoxy paint according to any one of claims 1 to 3, characterized in that: Spray the moisture-proof and dust-proof epoxy paint evenly on the objects to be painted, then heat to 60-80℃ in an inert gas environment and keep it warm for 1.5-2.5h, then increase the temperature to 170-190℃ at a rate of 1-3℃ / min and keep it warm for 1.5-2.5h, continue to increase the temperature to 190-210℃ and keep it warm for 2-4h, and cool to room temperature.

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