High-temperature-resistant single-component epoxy resin coating and preparation method thereof

By combining phenolic resin and silicone epoxy copolymer, a single-component epoxy resin coating is prepared, which solves the problem of softening and deformation of traditional coatings at high temperatures, and improves heat resistance and structural stability.

CN120536045AActive Publication Date: 2025-08-26深圳市深赛尔股份有限公司 +1
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Patent Information

Application Number
CN202510946591.X
Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Filing Date
2025-07-09
Publication Date
2025-08-26
Estimated Expiration
2045-07-09

AI Technical Summary

Technical Problem

Traditional epoxy resin coatings are prone to softening, deforming and aging in high temperature environments, and cannot meet the long-term and stable use needs. The high fluorine content and silica addition will affect transparency and material brittleness.

Method used

A single-component epoxy resin is prepared by mixing phenolic resin and silicone epoxy copolymer by controlling the viscosity of the coating and adding functional components to form a tight three-dimensional network structure to enhance heat resistance.

Benefits of technology

While reducing the fluorine content and coating thickness, the heat resistance and structural stability of the coating are improved, thermal expansion and deformation are avoided, and the stability of the coating is ensured in a high-temperature environment.

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Abstract

The invention belongs to the technical field of composite materials, and discloses a high-temperature-resistant single-component epoxy resin coating and a preparation method thereof.The preparation method comprises the following steps that phenolic resin, an epoxy compound and a catalyst are mixed, stirred and heated, and a resin monomer is obtained; the preparation method comprises the following steps: mixing a resin monomer with an organosilicon epoxy copolymer to obtain an epoxy resin prepolymer, detecting the viscosity of the epoxy resin prepolymer, and adjusting the viscosity of the epoxy resin prepolymer until the viscosity of the epoxy resin prepolymer reaches a preset viscosity; adding functional components into the epoxy resin prepolymer to obtain resin slurry, and then adding a latent curing agent to obtain the single-component epoxy resin coating. Therefore, the heat resistance of the resin coating can be improved while the fluorine content and the thickness of the resin coating are reduced.
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Description

Technical Field

[0001] The present application relates to the technical field of composite materials, and in particular to a high-temperature resistant single-component epoxy resin coating and a preparation method thereof. Background Art

[0002] With the advancement of industrialization, various equipment and components are increasingly used in high-temperature environments, placing higher demands on the high-temperature resistance of coatings. Traditional epoxy resin coatings, while offering excellent adhesion and corrosion resistance, are prone to softening, deformation, and aging in high-temperature environments, making them unable to meet the requirements for long-term stable use under these conditions. Therefore, developing epoxy resin coatings with excellent high-temperature resistance has become a pressing technical challenge.

[0003] In order to improve the heat resistance of epoxy resin, the performance of fluorine-containing epoxy resin can be improved by using epoxy resin with higher fluorine content in combination with silica. However, due to the excessive fluorine content in the resin, it is easy to cause potential harm to the environment and human body, and the addition of silica will also affect the overall transparency or processability of the resin, and may even cause the brittleness of the material to increase; or by thickly applying epoxy resin, the cross-linking structure of the resin is enhanced and the thermal expansion stress of the resin is relieved, thereby improving its heat resistance. However, thickly applied epoxy resin is prone to "skinning" on the resin surface and incomplete internal curing. Summary of the Invention

[0004] The technical problem that the present application actually aims to solve is to provide a high-temperature resistant one-component epoxy resin coating and a preparation method thereof, aiming to solve the problem of how to reduce the fluorine content and coating thickness while still improving the heat resistance of the resin coating.

[0005] To solve the above problems, the present invention proposes a method for preparing a one-component epoxy resin coating, which comprises the following steps: S1, mixing a phenolic resin, an epoxy compound, and a catalyst, stirring, and heating to obtain a resin monomer; S2. mixing the resin monomer and the organosilicon epoxy copolymer to obtain an epoxy resin prepolymer, detecting the viscosity of the epoxy resin prepolymer, and adjusting the viscosity of the epoxy resin prepolymer until the viscosity of the epoxy resin prepolymer reaches a preset viscosity; S3. Add functional components to the epoxy resin prepolymer to obtain a resin slurry, and then add a latent curing agent to obtain a single-component epoxy resin coating.

[0006] In some embodiments, the phenolic resin in step S1 includes at least one of phenolic resin, bisphenol A resin, and bisphenol F resin; the epoxy compound includes at least one of epichlorohydrin, epoxy propane, and epoxypropylene; and the catalyst includes at least one of triethylamine, sodium hydroxide, and benzoic acid.

[0007] In some embodiments, the organosilicon epoxy copolymer in step S2 includes at least one of polydimethylsiloxane elastomer and / or polyether-modified polysiloxane.

[0008] In some embodiments, the functional component in step S3 is at least one of a toughening agent and a leveling agent; the toughening agent includes at least one of carboxyl-terminated nitrile-acrylonitrile liquid rubber and polyetherimide, the leveling agent includes polyether-modified polydimethylsiloxane and / or polyacrylate, and the latent curing agent includes at least one of 2-phenyl-4-methylimidazole benzoate, microencapsulated dicyandiamide curing agent, and polyesteramine curing agent.

[0009] In some embodiments, step S1 includes: S1.1. Mix a phenolic resin, an epoxy compound, and a catalyst at room temperature, place the mixture in a heated reactor, introduce nitrogen, heat, and stir to react for 2-4 hours, and cool to room temperature to obtain a primary product, wherein the mass ratio of the phenolic resin to the epoxy compound is 1.1-1.2:1, the mass of the catalyst is 0.5-1% of the total mass of the reactants, the nitrogen flow rate is 50-200 mL / min, and the reaction temperature is 100-130°C; S1.2. Wash, stir, and filter the primary product with a solvent to obtain a resin monomer, wherein the solvent includes at least one of methanol, ethanol, and isopropanol, the volume ratio of the solvent to the primary product is 1:3-5, and the stirring time is 30-60 min.

[0010] In some embodiments, step S2 includes: S2.1. Add the resin monomer and the silicone epoxy copolymer to a reactor, introduce nitrogen, and heat and stir under vacuum for 2-6 hours to obtain an epoxy resin prepolymer, wherein the mass ratio of the resin monomer to the silicone epoxy copolymer is 5.5-6.5:1, the reaction pressure is -0.08 MPa, the reaction temperature is 80-120°C, and the stirring speed is 200-400 rpm; S2.2. Use a viscometer to detect the viscosity of the epoxy resin prepolymer, and adjust the viscosity of the epoxy resin prepolymer until the viscosity of the epoxy resin prepolymer reaches a preset viscosity.

[0011] Adjusting the viscosity of epoxy resin prepolymer includes adding viscosity-adjusting ingredients and adjusting reaction conditions, including stirring time and reaction temperature. The steps of adjusting the viscosity of the epoxy resin prepolymer until the viscosity of the epoxy resin prepolymer reaches a preset viscosity range include: Determine whether the viscosity of the epoxy resin prepolymer reaches the preset viscosity range; If yes, proceed to step S3; If not, adding a viscosity adjusting component to the epoxy resin prepolymer, performing the steps of using a viscometer to detect the viscosity of the epoxy resin prepolymer and determining whether the viscosity of the epoxy resin prepolymer reaches a preset viscosity range; If the viscosity of the epoxy resin prepolymer is lower than the preset viscosity range, the coating may be too thin and prone to flow after application, resulting in an uneven coating and insufficient coating strength. If it is higher than the preset viscosity range, the coating will have poor leveling properties, resulting in brush marks, bubbles, and other problems, affecting the quality of the coating surface and causing uneven coating during the curing process, which in turn affects the coating's hardness, durability and other properties. In some embodiments, the viscosity adjusting component includes a thickener and a diluent; the thickener includes at least one of acrylate, urethane, and polyether-modified silane, and the diluent includes at least one of ethyl acetate, methyl ethyl ketone, and cyclohexane.

[0012] In some embodiments, step S3 includes: S3.1. Transfer the epoxy resin prepolymer to a shear disperser, heat, and add the functional ingredients at the same material temperature while stirring. Continue stirring for 20-40 minutes to obtain a resin slurry, wherein the mass of the functional ingredients is 1-10% of the total mass of the epoxy resin prepolymer. The material temperature is 55-60°C and the stirring speed is 1000-2000 rpm. S3.2. Place the resin slurry in a planetary vacuum degassing machine, cool it to 40°C, add a latent curing agent, and stir it with a planetary mixer for 8-12 minutes. Then, let it stand at 45°C and -0.09 MPa for 20 minutes to eliminate microbubbles, thereby obtaining a single-component epoxy resin coating. The mass of the latent curing agent is 5-10% of the mass of the resin slurry.

[0013] The present invention provides a one-component epoxy resin coating, which is prepared by the above-mentioned preparation method of the one-component epoxy resin coating.

[0014] The beneficial effects of the present invention are: The phenolic backbone in phenolic resins provides a rigid structure. Through the combination of aromatic rings and stable chemical bonds, it enhances the resin's resistance to high-temperature oxidation and thermal decomposition, ensuring that it maintains structural integrity even at extreme temperatures. Multifunctional epoxy groups can react with curing agents to form more cross-linking points, thereby generating a tighter three-dimensional network structure. This not only improves the structural stability of the resin, but also effectively enhances its tolerance to high temperatures, avoiding problems with thermal expansion and thermal deformation. The strong silicon-oxygen bond (Si-O) binding energy in silicone-epoxy copolymers makes the backbone less susceptible to breakage or degradation at high temperatures, maintaining good structural stability. At the same time, the silicone-oxygen backbone itself has a low thermal expansion coefficient, which can reduce the thermal stress of the resin during temperature changes and avoid deformation or cracking caused by uneven thermal expansion. The synergistic effect of phenolic resin and silicone-epoxy copolymer effectively improves the heat resistance of single-component epoxy resin coatings. DETAILED DESCRIPTION

[0015] In the description of this application, it should be noted that if specific conditions are not specified in the examples, the experiments were carried out according to conventional conditions or the conditions recommended by the manufacturer. The reagents or instruments used, if the manufacturer is not specified, are all conventional products that can be purchased commercially.

[0016] The present invention provides a method for preparing a one-component epoxy resin coating, which comprises the following steps: S1, mixing a phenolic resin, an epoxy compound, and a catalyst, stirring, and heating to obtain a resin monomer; In step S1, the phenolic resin includes at least one of phenolic resin, bisphenol A resin, and bisphenol F resin; the epoxy compound includes at least one of epichlorohydrin, epoxy propane, and epoxypropylene; and the catalyst includes at least one of triethylamine, sodium hydroxide, and benzoic acid.

[0017] The phenolic skeleton in phenolic resins provides a rigid structure. Through the combination of aromatic rings and stable chemical bonds, it enhances the resin's resistance to high-temperature oxidation and thermal decomposition, ensuring that it can maintain its structural integrity even at extreme temperatures. The multifunctional epoxy groups can react with the curing agent to form more cross-linking points, thereby generating a tighter three-dimensional network structure, which not only improves the structural stability of the resin, but also effectively enhances its tolerance to high temperatures, avoiding the problems of thermal expansion and thermal deformation.

[0018] Triethylamine acts as a basic catalyst, providing nitrogen lone pair electrons to react with the epoxy group in the epoxy compound to produce a nucleophilic reaction, thereby promoting the ring opening of the epoxy compound to generate a more reactive intermediate, thereby enhancing the reactivity with the phenolic resin; sodium hydroxide acts as a strong base to provide hydroxide ions (OH -), by increasing the negative charge of the oxygen atom of the epoxy compound, enhancing its nucleophilicity, and further accelerating the reaction of the epoxy compound with the phenolic resin; benzoic acid, as an acidic catalyst, by providing protons (H + ) imparts a positive charge to the oxygen atoms in epoxy compounds, increasing their nucleophilicity and thus promoting reaction with phenolic resins. These catalysts enable the reaction to proceed smoothly at lower temperatures and times, improving reaction efficiency and product yield.

[0019] S1.1. Mix the phenolic resin, epoxy compound and catalyst at room temperature, put them into a heated reactor, introduce nitrogen, heat and stir to react for 2-4 hours, cool to room temperature to obtain a primary product, wherein the mass ratio of phenolic resin to epoxy compound is 1.1-1.2:1, the mass of the catalyst is 0.5-1% of the total mass of reactants, the flow rate of nitrogen is 50-200 mL / min, and the reaction temperature is 100-130°C.

[0020] Mixing the phenolic resin with the epoxy compound and catalyst at room temperature and heating and stirring in a nitrogen atmosphere for 2-4 hours prevents oxidation and maintains a reducing reaction environment, helping to promote the chemical reaction between the phenolic resin and the epoxy compound, resulting in a high-quality and pure initial product. Carrying out the reaction within a controlled temperature range (100-130°C) effectively increases the reaction rate and promotes the cross-linking reaction between the epoxy compound and the phenolic resin, thereby enhancing the structural stability and physical properties of the initial product.

[0021] S1.2. Wash, stir, and filter the primary product with a solvent to obtain a resin monomer, wherein the solvent includes at least one of methanol, ethanol, and isopropanol, the volume ratio of the solvent to the primary product is 1:3-5, and the stirring time is 30-60 min.

[0022] Methanol, ethanol and isopropanol are all highly polar solvents that can promote the dissolution and dispersion of impurities. Under stirring, impurities are fully removed to ensure the purity of the resin monomer; and the volume ratio of solvent to primary product is controlled within the range of 1:3~5, which can ensure that there is sufficient solvent for washing, effectively remove impurities, thereby improving the quality of the resin monomer and avoiding the negative impact of catalyst residues on subsequent reactions or product performance.

[0023] S2. Mixing the resin monomer and the silicone epoxy copolymer to obtain an epoxy resin prepolymer, detecting the viscosity of the epoxy resin prepolymer, and adjusting the viscosity of the epoxy resin prepolymer until the viscosity of the epoxy resin prepolymer reaches a preset viscosity.

[0024] The organosilicon epoxy copolymer in step S2 includes polydimethylsiloxane elastomer and / or polyether-modified polysiloxane.

[0025] The strong silicon-oxygen bond (Si-O) in silicone-epoxy copolymers makes the skeleton less prone to breakage or degradation at high temperatures, maintaining good structural stability. At the same time, the silicone-oxygen skeleton itself has a low coefficient of thermal expansion, which can reduce the thermal stress of the resin during temperature changes and avoid deformation or cracking caused by uneven thermal expansion.

[0026] Step S2 includes: S2.1. Add the resin monomer and the silicone epoxy copolymer to a reactor, introduce nitrogen, and heat and stir under vacuum for 2-6 hours to obtain an epoxy resin prepolymer. The mass ratio of the resin monomer to the silicone epoxy copolymer is 5.5-6.5:1. The nitrogen flow rate is 50-200 mL / min, the reaction pressure is -0.08 MPa, the reaction temperature is 80-120°C, and the stirring speed is 200-400 rpm. The nitrogen flow rate is controlled at 50~200 A flow rate of 100 mL / min effectively excludes oxygen and prevents oxidation reactions, ensuring the reaction takes place in an inert atmosphere and improving product purity and reaction efficiency. A negative pressure of -0.08 MPa helps remove volatile byproducts, reduces side reactions, and further promotes reaction completeness. A temperature between 80°C and 120°C maintains a moderate reaction rate, avoiding degradation or incomplete reaction caused by excessive temperatures, thereby ensuring the quality of the epoxy resin. Furthermore, a reaction time of 2 to 6 hours ensures full reaction of the reactants, avoiding the risk of incomplete reaction due to a short reaction time or the risk of side reactions due to a long reaction time. Finally, the mass ratio of the resin monomer to the silicone-epoxy copolymer is 5.5 to 6.5:1. This ratio ensures the integrity of the epoxy resin's backbone structure while providing the silicone portion with appropriate flexibility and heat resistance, thereby optimizing the properties of the final product. A stirring speed of 200 to 400 rpm ensures uniform mixing of the reactants, improves reaction efficiency, and avoids excessive bubbles caused by excessive stirring, which can affect reaction quality.

[0027] S2.2. Use a viscometer to detect the viscosity of the epoxy resin prepolymer, and adjust the viscosity of the epoxy resin prepolymer until the viscosity of the epoxy resin prepolymer reaches a preset viscosity.

[0028] If the preset viscosity range of the epoxy resin prepolymer is lower than this viscosity range, the coating may be too thin and easily flow after application, forming an uneven coating and resulting in insufficient coating strength; if it is higher than this viscosity range, the coating will have poor leveling properties, resulting in brush marks, bubbles and other problems, affecting the quality of the coating surface and also causing uneven coating during the curing process, thereby affecting the hardness, durability and other properties of the coating.

[0029] Adjusting the viscosity of epoxy resin prepolymer includes adding viscosity-adjusting ingredients and adjusting reaction conditions, including stirring time and reaction temperature. The steps of adjusting the viscosity of the epoxy resin prepolymer until the viscosity of the epoxy resin prepolymer reaches a preset viscosity range include: Determine whether the viscosity of the epoxy resin prepolymer reaches the preset viscosity range; If yes, proceed to step S3; If not, adding a viscosity adjusting component to the epoxy resin prepolymer, performing the steps of using a viscometer to detect the viscosity of the epoxy resin prepolymer and determining whether the viscosity of the epoxy resin prepolymer reaches a preset viscosity range; The viscosity adjusting components include a thickener and a diluent; the thickener includes at least one of acrylate, urethane, and polyether-modified silane, and the diluent includes at least one of ethyl acetate, methyl ethyl ketone, and cyclohexane.

[0030] In one embodiment, when the viscosity of the epoxy resin prepolymer is too low, acrylate is used as a thickener because the unsaturated double bonds in the acrylate molecules can react with the epoxy resin during the cross-linking process to form a three-dimensional network structure. This cross-linking effect not only enhances the adhesion and durability of the resin, but also improves the thickness uniformity and rheological properties of the coating, making the coating easier to control during the coating process and avoiding uneven coating or sagging. When the viscosity of the epoxy resin prepolymer is too high, ethyl acetate is used as a diluent. By interacting with the polar functional groups (such as epoxy groups) in the epoxy resin, it destroys the hydrogen bonds between the resin molecules, reduces the viscosity of the resin, and provides a better dispersion medium for the toughening agent. As a result, the cyano or carboxyl groups in the toughening agent can chemically react with the epoxy groups of the epoxy resin to form a cross-linked structure, thereby enhancing the toughness of the resin.

[0031] In one embodiment, in order to calculate the accurate preset viscosity range, the following formula is proposed: in: a0 (in mPa·s), a1 (in mPa·s / K), a2 (in mPa·s / K²), and a3 (in mPa·s·K) are temperature coefficients, which are obtained by performing isothermal scanning tests using a rotational rheometer and then fitting the experimental data of different temperature sections. In this embodiment, T can be 360K, 370K, 380K, and 390K. It can be calculated that the value range of a0 is -200~500, the value range of a1 is -5.0~0.5, the value range of a2 is -0.02~0.005, and the value range of a3 is 2.0×10 3 ~1.0×10 5 .

[0032] ‌b0 (unit: ‌mPa·s ^0.5 )、b1(unit is mPa·s -1 ), ‌b2 (unit: mPa·s -2 )‌ is the time coefficient. The crosslinking degree is monitored by differential scanning calorimetry and the viscosity change is recorded simultaneously. In this embodiment, the value of t can be 2h, 3h, 4h, 5h, or 6h (the unit needs to be converted to seconds for calculation). Then, the crosslinking degree is calculated according to the quantitative formula of thermal analysis. The value range of ‌b0 is 0-0.2, the value range of b1 is 0-0.001, and the value range of ‌b2 is -1×10 -8 ~1×10 -7 ‌; c0 (mPa·s / rad), c1 (mPa·s / rad²), and c2 (mPa·s·rad) are shear coefficients, which were measured using a cone-plate rheometer for 0.1-1000s. -1 Shear rate scanning is performed to record the shear stress τ and shear rate ω data. In this embodiment, the value of ω can be 200 rpm, 250 rpm, 300 rpm, 350 rpm, and 400 rpm. Then, by calculation, the value range of c0 is -0.8~0.2, and the value range of c1 is -1×10 -4 ~5×10 -5 , the value range of ‌c2 is 1×10 4 ~1×10 5 ; ‌k1, k2, and ‌k3‌ are dimensionless weight coefficients. The contribution of each factor is obtained by orthogonal experimental design around reaction temperature, reaction time, and stirring rate. That is, the value range of ‌k1 is ‌0.42~0.58, the value range of k2 is ‌0.25~0.38, and the value range of ‌k3 is 0.08~0.18 (Σk n =1, that is, k1+k2+k3=1); ‌ε‌ is the correction term (‌mPa·s). In this case, the resin is an epoxy resin system. The residuals between the model prediction value and the measured value are collected and calculated. The value range of ‌ε‌ is 7–70. η1 represents the viscosity component determined by temperature (mPa·s), η2 represents the viscosity component determined by time (mPa·s), and η3 represents the viscosity component determined by shear rate (mPa·s); T is temperature (unit K), t is reaction time (s), ω is stirring speed (rpm); η is final viscosity (mPa·s).

[0033] In one embodiment, a0=50 mPa·s, a1=-1.2 mPa·s / K, a2=-0.015 mPa·s / K², a3=1.5×104 mPa·s / K²,‌b0=0.1‌mPa·s ^0.5 , b1=0.0005mPa·s -1 , ‌b2=0.5×10 -7 mPa·s -2 , c0=0.05‌mPa·s / rad, c1=3×10 -5 mPa·s / rad²,‌c²=5×10 4 mPa·s·rad, ‌k1=0.50, k2=0.32, ‌k3=0.18, ‌ε=35‌mPa·s. By adjusting the reaction temperature, reaction time, and stirring speed within the range, the maximum / minimum value of the preset viscosity range can be obtained, thereby determining how to adjust the state of the epoxy resin prepolymer.

[0034] S3. Add functional components to the epoxy resin prepolymer to obtain a resin slurry, and then add a latent curing agent to obtain a single-component epoxy resin coating.

[0035] Plasticizers lower the resin's glass transition temperature (Tg), improving its flexibility and workability. This results in a cured coating with improved impact and flex resistance. They also improve the resin's fluidity, helping the coating spread evenly during application. Leveling agents enhance the coating's surface smoothness, preventing bubbles, scratches, and unevenness during application, ensuring a high-quality coating appearance. Latent curing agents activate under appropriate temperature and conditions to promote the curing reaction of epoxy resins. Due to their low reactivity, latent curing agents prevent premature curing at room temperature, allowing the coating to have a longer working life during storage and application. Upon heating or under specific conditions, the curing agent initiates the cross-linking reaction of the epoxy resin, ultimately forming a hard and durable film. By adding plasticizers, leveling agents, and latent curing agents, epoxy resin coatings can achieve excellent workability, coating quality, and long-term stable storage, meeting the needs of various coating applications.

[0036] The functional component in step S3 is at least one of a toughening agent and a leveling agent; the toughening agent includes at least one of carboxyl-terminated nitrile-acrylonitrile liquid rubber and polyetherimide, and the leveling agent includes polyether-modified polydimethylsiloxane and / or polyacrylate; the latent curing agent includes at least one of 2-phenyl-4-methylimidazole benzoate, microencapsulated dicyandiamide curing agent, and polyesteramine curing agent.

[0037] Step S3 includes: S3.1. Transfer the epoxy resin prepolymer to a shear disperser, heat, and add the functional ingredients at the same material temperature while stirring. Continue stirring for 20-40 minutes to obtain a resin slurry, wherein the mass of the functional ingredients is 1-10% of the total mass of the epoxy resin prepolymer. The material temperature is 55-60°C and the stirring speed is 1000-2000 rpm. During the preparation of the resin slurry, a material temperature of 55~60°C can not only promote the effective reaction between the epoxy group and the functional components, but also avoid side reactions caused by high temperature; high-speed shear stirring of 1000~2000rpm ensures the uniform dispersion of the functional components and strengthens the interface bonding; the addition ratio of 1~10% of the functional components can achieve the modification effect and maintain the stability of the system; the reaction time of 20~40min ensures sufficient bonding. These conditions work synergistically to form a resin slurry with uniform structure and stable performance.

[0038] S3.2. Place the resin slurry in a planetary vacuum degassing machine, cool it to 40°C, add a latent curing agent, and stir it with a planetary mixer for 8-12 minutes. Then, let it stand at 45°C and -0.09 MPa for 20 minutes to eliminate microbubbles, thereby obtaining a single-component epoxy resin coating. The mass of the latent curing agent is 5-10% of the mass of the resin slurry.

[0039] By removing microbubbles through vacuum degassing, the mechanical properties of epoxy resin coatings can be improved, and the formation of stress concentration points after the bubbles solidify, which leads to a decrease in strength, can be avoided. At the same time, the surface quality of epoxy resin coatings can be guaranteed, and surface defects such as pinholes and fisheyes can be prevented from occurring in the coating.

[0040] The above embodiments are preferred implementation modes of the present application, but the implementation modes of the present application are not limited to the above embodiments. Any other changes, modifications, substitutions, combinations, and simplifications made without departing from the spirit and principles of the present application shall be considered as equivalent replacement methods and shall be included in the scope of protection of the present application.

Claims

1. A method for preparing a one-component epoxy resin coating, characterized in that: The preparation method comprises the following steps: S1, mixing a phenolic resin, an epoxy compound, and a catalyst, stirring, and heating to obtain a resin monomer; S2. mixing the resin monomer and the organosilicon epoxy copolymer to obtain an epoxy resin prepolymer, detecting the viscosity of the epoxy resin prepolymer, and adjusting the viscosity of the epoxy resin prepolymer until the viscosity of the epoxy resin prepolymer reaches a preset viscosity; S3. Add functional components to the epoxy resin prepolymer to obtain a resin slurry, and then add a latent curing agent to obtain a single-component epoxy resin coating.

2. The method for preparing a one-component epoxy resin coating according to claim 1, wherein: The phenolic resin in step S1 includes at least one of phenolic resin, bisphenol A resin, and bisphenol F resin; the epoxy compound includes at least one of epichlorohydrin, ethylene oxide, and propylene oxide; and the catalyst includes at least one of triethylamine, sodium hydroxide, and benzoic acid.

3. The method for preparing a one-component epoxy resin coating according to claim 1, wherein: The organosilicon epoxy copolymer in step S2 includes polydimethylsiloxane elastomer and / or polyether-modified polysiloxane.

4. The method for preparing a one-component epoxy resin coating according to claim 1, wherein: The functional component in step S3 is at least one of a toughening agent and a leveling agent; the toughening agent includes at least one of carboxyl-terminated nitrile-acrylonitrile liquid rubber and polyetherimide, the leveling agent includes polyether-modified polydimethylsiloxane and / or polyacrylate, and the latent curing agent includes at least one of 2-phenyl-4-methylimidazole benzoate, microencapsulated dicyandiamide curing agent, and polyesteramine curing agent.

5. The method for preparing a one-component epoxy resin coating according to claim 1, wherein: Step S1 includes: S1.

1. Mix a phenolic resin, an epoxy compound, and a catalyst at room temperature, place the mixture in a heated reactor, introduce nitrogen, heat, and stir to react for 2-4 hours, and cool to room temperature to obtain a primary product, wherein the mass ratio of the phenolic resin to the epoxy compound is 1.1-1.2:1, the mass of the catalyst is 0.5-1% of the total mass of the reactants, the nitrogen flow rate is 50-200 mL / min, and the reaction temperature is 100-130°C; S1.

2. Wash, stir, and filter the primary product with a solvent to obtain a resin monomer, wherein the solvent includes at least one of methanol, ethanol, and isopropanol, the volume ratio of the solvent to the primary product is 1:3-5, and the stirring time is 30-60 min.

6. The method for preparing a one-component epoxy resin coating according to claim 1, wherein: Step S2 includes: S2.

1. Add the resin monomer and the silicone epoxy copolymer to a reactor, introduce nitrogen, and heat and stir under vacuum for 2-6 hours to obtain an epoxy resin prepolymer, wherein the mass ratio of the resin monomer to the silicone epoxy copolymer is 5.5-6.5:1, the reaction pressure is -0.08 MPa, the reaction temperature is 80-120°C, and the stirring speed is 200-400 rpm; S2.

2. Use a viscometer to detect the viscosity of the epoxy resin prepolymer, and adjust the viscosity of the epoxy resin prepolymer until the viscosity of the epoxy resin prepolymer reaches a preset viscosity.

7. The method for preparing a one-component epoxy resin coating according to claim 6, characterized in that: Adjusting the viscosity of epoxy resin prepolymer includes adding viscosity-adjusting components and adjusting reaction conditions, including stirring time and reaction temperature; The steps of adjusting the viscosity of the epoxy resin prepolymer until the viscosity of the epoxy resin prepolymer reaches a preset viscosity range include: Determine whether the viscosity of the epoxy resin prepolymer reaches the preset viscosity range; If yes, proceed to step S3; If not, a viscosity adjusting component is added to the epoxy resin prepolymer, and the viscosity of the epoxy resin prepolymer is detected using a viscometer and the step of determining whether the viscosity of the epoxy resin prepolymer reaches a preset viscosity range is performed.

8. The method for preparing a one-component epoxy resin coating according to claim 7, characterized in that: The viscosity adjusting component includes a thickener and a diluent; the thickener includes at least one of acrylate, urethane, and polyether modified silane; the diluent includes at least one of ethyl acetate, methyl ethyl ketone, and cyclohexane.

9. The method for preparing a one-component epoxy resin coating according to claim 1, characterized in that: Step S3 includes: S3.

1. Transfer the epoxy resin prepolymer to a shear disperser, heat, and add the functional ingredients at the same material temperature while stirring. Continue stirring for 20-40 minutes to obtain a resin slurry, wherein the mass of the functional ingredients is 1-10% of the total mass of the epoxy resin prepolymer. The material temperature is 55-60°C and the stirring speed is 1000-2000 rpm. S3.

2. Place the resin slurry in a planetary vacuum degassing machine, cool it to 40°C, add a latent curing agent, and stir it with a planetary mixer for 8-12 minutes. Then, let it stand at 45°C and -0.09 MPa for 20 minutes to eliminate microbubbles, thereby obtaining a single-component epoxy resin coating. The mass of the latent curing agent is 5-10% of the mass of the resin slurry.

10. A one-component epoxy resin coating, characterized in that: The single-component epoxy resin coating is prepared by the preparation method of any one of claims 1 to 9.

Citation Information

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