A bottom-surface integrated thick-layer glass flake anticorrosive coating and a preparation method thereof

By combining glass flakes, nano-silica, and tertiary amine accelerators into a two-component thick-layer glass flake anti-corrosion coating, an organic-inorganic hybrid network is formed, solving the problems of limited thickness, easy cracking, and slow drying speed of existing coatings in complex corrosive environments, and achieving high density and fast drying anti-corrosion effect.

CN122188485APending Publication Date: 2026-06-12SUZHOU DACHENG ENVIRONMENTAL PROTECTION NEW MATERIAL CO LTD

Patent Information

Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
SUZHOU DACHENG ENVIRONMENTAL PROTECTION NEW MATERIAL CO LTD
Filing Date
2026-05-08
Publication Date
2026-06-12
Patent Text Reader

Abstract

This application relates to a combined base and surface thick-layer glass flake anti-corrosion coating and its preparation method, belonging to the field of coating technology. It includes component A and component B. The raw materials for preparing component A include the following components in parts by weight: 30-60 parts hydrogenated epoxy resin, 5-15 parts aluminum tripolyphosphate, 5-15 parts zinc phosphate, 10-30 parts glass flakes, 3-8 parts functional composite additives, 1-5 parts anti-flash rust agent, 0.5-2 parts dispersant, 0.5-2 parts defoamer, 1-5 parts thickener, and 10-20 parts solvent. The raw materials for preparing component B include the following components in parts by weight: 12-18 parts fatty amine curing agent and 2-8 parts solvent. The functional composite additives include nano-silica and tertiary amine accelerators. The coating prepared by this application can achieve thick coating without cracking, has a stable coating structure, fast drying speed, and good anti-corrosion performance.
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Description

Technical Field

[0001] This application relates to the field of coating technology, and in particular to a base-and-surface integrated thick-layer glass flake anti-corrosion coating and its preparation method. Background Technology

[0002] In many industrial sectors such as chemical engineering, marine engineering, and power, equipment and facilities are exposed to highly corrosive environments for extended periods. Corrosion not only severely shortens the service life of equipment and increases maintenance costs, but may also lead to safety hazards. Therefore, the demand for long-lasting anti-corrosion coatings is becoming increasingly urgent.

[0003] In existing technologies, traditional anti-corrosion coatings often fall short when facing complex and harsh corrosive environments. Ordinary coatings cannot withstand the erosion of strong media such as acids and alkalis for a long time, and the process of applying primer and topcoat separately is cumbersome and costly. Although glass flake anti-corrosion coatings improve the coating's impermeability to some extent due to their unique flake structure, they still have many limitations in practical applications. For example, the coating thickness is limited, and cracking is prone to occur when applying thick coatings exceeding 300μm. In addition, some products have insufficient flash rust inhibition and slow drying speed, making it difficult to meet the heavy-duty anti-corrosion requirements under extreme working conditions. Summary of the Invention

[0004] To address the aforementioned issues, this application provides a bottom-and-surface integrated thick-layer glass flake anti-corrosion coating and its preparation method.

[0005] This application provides a bottom-and-surface integrated thick-layer glass flake anti-corrosion coating and its preparation method, which adopts the following technical solution: In a first aspect, this application provides a base-surface integrated thick-layer glass flake anti-corrosion coating, employing the following technical solution: A thick-layer glass flake anti-corrosion coating integrating the base and surface layers, comprising component A and component B, wherein the raw materials for preparing component A include the following components in parts by weight: 30-60 parts of hydrogenated epoxy resin 5-15 parts aluminum tripolyphosphate 5-15 parts zinc phosphate 10-30 pieces of glass flakes 3-8 parts of functional compound additives Anti-flash rust agent 1-5 parts Dispersant 0.5-2 parts 0.5-2 parts of defoamer Thickener 1-5 parts Solvent 10-20 parts; The raw materials for preparing component B include the following components in parts by weight: 12-18 parts of fatty amine curing agent and 2-8 parts of solvent; The functional composite additives include nano-silica and tertiary amine accelerators.

[0006] This integrated thick-layer glass flake anti-corrosion coating employs a two-component design. Component A uses hydrogenated epoxy resin as the main film-forming substance, providing the coating with good adhesion and basic mechanical protection. Component B contains a fatty amine curing agent that undergoes a cross-linking reaction with the resin to form a three-dimensional network structure, giving the coating basic density and hardness. The glass flakes in component A are arranged in parallel within the coating, extending the penetration path of corrosive media and enhancing the physical barrier effect of the coating. Aluminum tripolyphosphate and zinc phosphate work synergistically to form a chemical passivation film at the metal interface, improving the coating's chemical corrosion resistance. The anti-flash rust agent inhibits electrochemical oxidation on the steel surface during the initial coating application. The corrosion reaction is controlled, ensuring the quality of the interface bonding between the coating and the substrate. The functional composite additive uses a combination of nano-silica and tertiary amine accelerators. The tertiary amine accelerators accelerate the cross-linking reaction rate between epoxy resin and curing agent, improving the drying speed of the coating. The nano-silica is uniformly dispersed in the coating and forms a tight organic-inorganic hybrid network with the resin matrix, absorbing and dispersing the internal stress generated during curing shrinkage, thus improving the crack resistance of the coating. At the same time, the filling effect of nanoparticles makes the coating structure more compact. Together with the shielding effect of glass flakes and the passivation effect of anti-rust pigments, they jointly improve the overall corrosion resistance of the coating.

[0007] Preferably, the mass ratio of component A to component B is (3-5):1.

[0008] By controlling the mass ratio of component A to component B within a reasonable range, the hydrogenated epoxy resin and the fatty amine curing agent can form a stoichiometric curing reaction system after mixing, ensuring that the crosslinking reaction proceeds fully, improving the drying speed and crosslinking density of the coating. At the same time, the nano-silica is uniformly dispersed in the reaction system, effectively absorbing and releasing the internal stress generated by curing shrinkage, thus improving the coating's crack resistance. On this basis, the physical shielding layer formed by glass flakes and the chemical passivation film constructed by aluminum tripolyphosphate and zinc phosphate can work synergistically to improve the overall corrosion resistance of the coating.

[0009] Preferably, the tertiary amine accelerator includes 2,4,6-tris(dimethylaminomethyl)phenol.

[0010] 2,4,6-Tris(dimethylaminomethyl)phenol was selected as a tertiary amine accelerator. The tertiary amine group in its molecular structure has lone pairs of electrons, which can catalyze and accelerate the crosslinking reaction between the aliphatic amine curing agent and the hydrogenated epoxy resin. While ensuring the complete formation of the crosslinking network, it also improves the drying speed of the coating. The presence of benzene rings in the molecular structure enhances the compatibility with the epoxy resin system, allowing nano-silica to be uniformly dispersed in the rapidly curing reaction system and effectively absorb the internal stress generated during curing shrinkage, thereby improving the crack resistance of the coating. Under the combined effect of increased crosslinking density and denser coating structure, the physical shielding effect of glass flakes and the chemical passivation effect of aluminum tripolyphosphate and zinc phosphate work together to improve the overall corrosion resistance of the coating.

[0011] Preferably, the mass ratio of nano-silica to tertiary amine accelerator in the functional composite additive is (1.8-2.2):1.

[0012] By controlling the mass ratio of nano-silica to tertiary amine accelerator within a suitable range, the tertiary amine accelerator can effectively catalyze the crosslinking reaction between the aliphatic amine curing agent and the hydrogenated epoxy resin at this ratio, resulting in a faster drying speed for the coating. The nano-silica remains uniformly dispersed in this system, and its rigid nanoparticles absorb and disperse internal stress during the coating curing shrinkage process, improving the coating's crack resistance. At the same time, the filling effect of nano-silica makes the coating structure more compact, which, together with the physical shielding effect of glass flakes and the chemical passivation effect of aluminum tripolyphosphate and zinc phosphate, enhances the overall corrosion resistance of the coating.

[0013] Preferably, the anti-flash rust agent comprises ammonium benzoate.

[0014] Ammonium benzoate was selected as the anti-flash rust agent. In the early stage of coating, it can adsorb onto the surface of the steel substrate and form a dense organic salt protective film at the interface. This effectively inhibits the occurrence of electrochemical corrosion reaction and prevents the formation of flash rust, thus ensuring the quality of the interface bonding between the coating and the substrate. Good interface adhesion allows the coating to maintain its structural integrity during the curing shrinkage process, improving the coating's crack resistance. At the same time, a clean metal surface is conducive to the uniformity of the subsequent curing reaction, enabling the complete formation of the cross-linked network and improving the coating's drying speed. Under the combined effect of interface protection and coating densification, along with the physical shielding effect of glass flakes and the chemical passivation effect of aluminum tripolyphosphate and zinc phosphate, the overall corrosion resistance of the coating is improved.

[0015] Preferably, the raw materials for preparing component A further include a synergistic modifier, which is prepared by the following steps: mixing 1,4-butanediol diglycidyl ether, γ-butyrolactone, trimethylolpropane monoallyl ether, zirconium acetylacetonate and toluene, heating and stirring under a protective atmosphere and refluxing, and removing toluene by vacuum distillation after the reaction is completed to obtain the synergistic modifier.

[0016] The synergistic modifier molecule contains both flexible aliphatic segments and active epoxy groups, which can chemically bond with the hydrogenated epoxy resin matrix to form a uniform organic-inorganic hybrid network. Its flexible segments effectively absorb and disperse internal stress during the coating curing process, complementing the rigid toughening effect of nano-silica, further improving the coating's crack resistance. At the same time, the residual tertiary amine structure in the modifier molecule has a synergistic catalytic effect on the epoxy-amine curing reaction, accelerating the coating's drying speed. With the combined effect of a denser coating structure and effective release of internal stress, along with the physical shielding effect of glass flakes and the chemical passivation effect of aluminum tripolyphosphate and zinc phosphate, the overall corrosion resistance of the coating is further improved.

[0017] Preferably, the amount of the synergistic modifier added is 3-5 parts.

[0018] The amount of synergistic modifier added is controlled within a reasonable range to ensure uniform dispersion in the system and full chemical bonding with the hydrogenated epoxy resin matrix. The flexible segments in the modifier molecule effectively absorb and disperse internal stress during coating curing, complementing the rigid toughening effect of nano-silica and improving the crack resistance of the coating. At the same time, the residual tertiary amine structure in the modifier plays a synergistic catalytic role in the epoxy-amine curing reaction, accelerating the drying speed of the coating. Within this addition range, the synergistic modifier will not excessively dilute the crosslinking density of the main resin, allowing the physical shielding effect of glass flakes and the chemical passivation effect of aluminum tripolyphosphate and zinc phosphate to be fully utilized, thereby improving the overall corrosion resistance of the coating.

[0019] Preferably, the mass ratio of 1,4-butanediol diglycidyl ether, γ-butyrolactone and trimethylolpropane monoallyl ether is 1:0.85:(0.11-0.13).

[0020] By optimizing the mass ratio of the three monomers, flexible segments, tertiary amine catalytic active centers, and reactive groups are simultaneously introduced into the molecular structure, enabling them to be uniformly dispersed in the system and form stable chemical bonds with the resin matrix.

[0021] Secondly, this application provides a method for preparing a base-surface integrated thick-layer glass flake anti-corrosion coating, employing the following technical solution: A method for preparing a thick-layer glass flake anti-corrosion coating that integrates the base and surface layers includes the following steps: Hydrogenated epoxy resin, aluminum tripolyphosphate, zinc phosphate, glass flakes, functional composite additives, anti-flash rust agent, dispersant, defoamer, thickener and solvent are mixed and stirred to obtain component A; fatty amine curing agent and solvent are mixed and stirred to obtain component B; component A and component B are packaged separately to obtain a base-top integrated thick-layer glass flake anti-corrosion coating.

[0022] The functional components are thoroughly mixed and dispersed with the resin matrix, ensuring the uniform distribution of nano-silica and the synergistic effect of the additives, laying the foundation for the coating performance. During use, after component A and component B are mixed, the aliphatic amine curing agent undergoes a cross-linking reaction with the hydrogenated epoxy resin, achieving rapid curing under the synergistic catalysis of the tertiary amine accelerator. At the same time, the nano-silica absorbs internal stress, improving crack resistance, and works together with the physical shielding of glass flakes and the chemical passivation of aluminum tripolyphosphate and zinc phosphate to give the coating excellent corrosion resistance.

[0023] In summary, this application includes at least one of the following beneficial technical effects: 1. The combined base and topcoat thick-layer glass flake anti-corrosion coating adopts a two-component design. Component A uses hydrogenated epoxy resin as the main film-forming substance, providing good adhesion and basic mechanical protection for the coating. The fatty amine curing agent in component B undergoes a cross-linking reaction with the resin to form a three-dimensional network structure, giving the coating basic density and hardness. The glass flakes in component A are arranged in parallel in the coating, extending the penetration path of corrosive media and improving the physical shielding effect of the coating. Aluminum tripolyphosphate and zinc phosphate work synergistically to form a chemical passivation film at the metal interface, improving the chemical anti-corrosion capability of the coating. The anti-flash rust agent inhibits the electrical conductivity of the steel surface in the early stage of coating. Chemical corrosion reaction ensures the quality of the interface bonding between the coating and the substrate. The functional composite additive uses a combination of nano-silica and tertiary amine accelerators. The tertiary amine accelerators accelerate the crosslinking reaction rate between epoxy resin and curing agent, improving the drying speed of the coating. Nano-silica is uniformly dispersed in the coating and forms a tight organic-inorganic hybrid network with the resin matrix, absorbing and dispersing the internal stress generated during curing shrinkage, thus improving the crack resistance of the coating. At the same time, the filling effect of nanoparticles makes the coating structure more compact. Together with the shielding effect of glass flakes and the passivation effect of anti-rust pigments, they jointly improve the overall corrosion resistance of the coating.

[0024] 2. The synergistic modifier molecule contains both flexible aliphatic segments and active epoxy groups, which can chemically bond with the hydrogenated epoxy resin matrix to form a uniform organic-inorganic hybrid network. Its flexible segments effectively absorb and disperse internal stress during the coating curing process, complementing the rigid toughening effect of nano-silica, further improving the coating's crack resistance. At the same time, the residual tertiary amine structure in the modifier molecule has a synergistic catalytic effect on the epoxy-amine curing reaction, accelerating the coating's drying speed. With the combined effect of a denser coating structure and effective release of internal stress, along with the physical shielding effect of glass flakes and the chemical passivation effect of aluminum tripolyphosphate and zinc phosphate, the overall corrosion resistance of the coating is further improved. Detailed Implementation

[0025] This application discloses a combined base and surface thick-layer glass flake anti-corrosion coating and its preparation method. Unless otherwise specified, all raw materials used in this application are commercially available. The following detailed description, in conjunction with embodiments, further illustrates this application: Raw material specifications: Hydrogenated epoxy resin EP-4080E was purchased from Adico (China) Investment Co., Ltd.; aluminum tripolyphosphate and zinc phosphate were purchased from Guangzhou Runzhan Chemical Co., Ltd.; glass flakes were purchased from Lingshou Rongbang Mineral Products Processing Plant; nano silica was purchased from Shanghai Huijingya Nanomaterials Co., Ltd.; Ancamine K54 was purchased from Evonik; ammonium benzoate (CAS No.: 1863-63-4); dispersant BYK-P104S and defoamer BYK-141 were purchased from BYK Additives (Shanghai) Co., Ltd.; thickener AKN-7010 was purchased from Foshan Qianyou Chemical Co., Ltd.; butyl acetate (CAS No.: 123-86-4); and fatty amine curing agent Kingcure. 260A was purchased from Fujian Wangpai New Materials Co., Ltd., containing triethanolamine (CAS No.: 102-71-6), ammonium formate (CAS No.: 540-69-2), 1,4-butanediol diglycidyl ether (CAS No.: 2425-79-8), γ-butyrolactone (CAS No.: 96-48-0), trimethylolpropane monoallyl ether (CAS No.: 682-11-1), and zirconium acetylacetonate (CAS No.: 17501-44-9). Example 1

[0026] Weigh component A: 30 parts hydrogenated epoxy resin, 5 parts aluminum tripolyphosphate, 5 parts zinc phosphate, 10 parts glass flakes, 3 parts functional composite additive, 1 part anti-flash rust agent, 0.5 parts dispersant, 0.5 parts defoamer, 1 part thickener, and 10 parts solvent; weigh component B: 12 ​​parts fatty amine curing agent and 2 parts solvent; the hydrogenated epoxy resin is model EP-4080E, and the functional composite additive consists of nano-silica and tertiary amine accelerator in a mass ratio of 1.8:1. The nano-silica has a particle size of 10-50 nm, and the tertiary amine accelerator is 2,4,6-tris(dimethylaminomethyl)phenol (model Ancamine). K54), glass flakes thickness 2-5μm, particle size 40-50μm, anti-flash rust agent is ammonium benzoate, dispersant model is BYK-P104S, defoamer model is BYK-141, thickener model is AKN-7010, solvent is butyl acetate, fatty amine curing agent model is Kingcure 260A.

[0027] Hydrogenated epoxy resin, aluminum tripolyphosphate, zinc phosphate, glass flakes, functional composite additives, anti-flash rust agent, dispersant, defoamer, thickener, and solvent were added to a mixing tank and stirred at 1400 rpm for 50 min to obtain component A. Fatty amine curing agent and solvent were added to the mixing tank and stirred at 600 rpm for 20 min to obtain component B. Components A and B were packaged separately to obtain a combined thick-layer glass flake anti-corrosion coating. In use, components A and B were mixed evenly at a mass ratio of 3:1 and applied to the substrate surface to form a coating with a dry film thickness of 600 μm. Example 2

[0028] Weigh component A: 60 parts hydrogenated epoxy resin, 15 parts aluminum tripolyphosphate, 15 parts zinc phosphate, 30 parts glass flakes, 8 parts functional composite additives, 5 parts anti-flash rust agent, 2 parts dispersant, 2 parts defoamer, 5 parts thickener, and 20 parts solvent; weigh component B: 18 parts fatty amine curing agent and 8 parts solvent; the hydrogenated epoxy resin is model EP-4080E, and the functional composite additives consist of nano-silica and tertiary amine accelerators in a mass ratio of 2.2:1. The particle size of the nano-silica is 10-50 nm, and the tertiary amine accelerator is 2,4,6-tris(dimethylaminomethyl)phenol (model Ancamine). K54), glass flakes thickness 2-5μm, particle size 40-50μm, anti-flash rust agent is ammonium benzoate, dispersant model is BYK-P104S, defoamer model is BYK-141, thickener model is AKN-7010, solvent is butyl acetate, fatty amine curing agent model is Kingcure 260A.

[0029] Hydrogenated epoxy resin, aluminum tripolyphosphate, zinc phosphate, glass flakes, functional composite additives, anti-flash rust agent, dispersant, defoamer, thickener, and solvent were added to a mixing tank and stirred at 1400 rpm for 50 min to obtain component A. Fatty amine curing agent and solvent were added to the mixing tank and stirred at 600 rpm for 20 min to obtain component B. Components A and B were packaged separately to obtain a combined thick-layer glass flake anti-corrosion coating. In use, components A and B were mixed evenly at a mass ratio of 5:1 and applied to the substrate surface to form a coating with a dry film thickness of 600 μm. Example 3

[0030] Weigh component A: 45 parts hydrogenated epoxy resin, 10 parts aluminum tripolyphosphate, 10 parts zinc phosphate, 20 parts glass flakes, 5.5 parts functional composite additive, 3 parts anti-flash rust agent, 1.25 parts dispersant, 1.25 parts defoamer, 3 parts thickener, and 15 parts solvent; weigh component B: 15 parts fatty amine curing agent and 5 parts solvent; the hydrogenated epoxy resin is model EP-4080E, and the functional composite additive consists of nano-silica and tertiary amine accelerator in a mass ratio of 2:1. The nano-silica has a particle size of 10-50 nm, and the tertiary amine accelerator is 2,4,6-tris(dimethylaminomethyl)phenol (model Ancamine). K54), glass flakes thickness 2-5μm, particle size 40-50μm, anti-flash rust agent is ammonium benzoate, dispersant model is BYK-P104S, defoamer model is BYK-141, thickener model is AKN-7010, solvent is butyl acetate, fatty amine curing agent model is Kingcure 260A.

[0031] Hydrogenated epoxy resin, aluminum tripolyphosphate, zinc phosphate, glass flakes, functional composite additives, anti-flash rust agent, dispersant, defoamer, thickener, and solvent were added to a mixing tank and stirred at 1400 rpm for 50 min to obtain component A. Fatty amine curing agent and solvent were added to the mixing tank and stirred at 600 rpm for 20 min to obtain component B. Components A and B were packaged separately to obtain a combined thick-layer glass flake anti-corrosion coating. In use, components A and B were mixed evenly at a mass ratio of 4:1 and applied to the substrate surface to form a coating with a dry film thickness of 600 μm. Example 4

[0032] Example 4 is based on Example 3. The only difference between Example 4 and Example 3 is that in Example 4, component A and component B are mixed at a mass ratio of 2:1. Example 5

[0033] Example 5 is based on Example 3. The only difference between Example 5 and Example 3 is that in Example 5, component A and component B are mixed at a mass ratio of 6:1. Example 6

[0034] Example 6 is based on Example 3. The only difference between Example 6 and Example 3 is that the mass ratio of nano-silica to tertiary amine accelerator in the functional composite additive in Example 6 is 1.5:1. Example 7

[0035] Example 7 is based on Example 3. The only difference between Example 7 and Example 3 is that the mass ratio of nano-silica to tertiary amine accelerator in the functional composite additive in Example 7 is 2.5:1. Example 8

[0036] Example 8 is based on Example 3. The only difference between Example 8 and Example 3 is that in Example 8, the tertiary amine accelerator 2,4,6-tris(dimethylaminomethyl)phenol is replaced with triethanolamine. Example 9

[0037] Example 9 is based on Example 3. The only difference between Example 9 and Example 3 is that in Example 9, the anti-flash rust agent ammonium benzoate is replaced with ammonium formate. Example 10

[0038] Example 10 is based on Example 3. The only difference between Example 10 and Example 3 is that the raw materials for preparing component A in Example 10 also include 3 parts of synergistic modifier.

[0039] Preparation of synergistic modifiers The mass ratio of 1,4-butanediol diglycidyl ether, γ-butyrolactone and trimethylolpropane monoallyl ether is 1:0.85:0.11, and the amount of zirconium acetylacetonate accounts for 1.5% of the total mass of the monomers.

[0040] 1,4-Butanediol diglycidyl ether, γ-butyrolactone, trimethylolpropane monoallyl ether, zirconium acetylacetonate, and anhydrous toluene were added to a reaction flask (solid content 50%). The mixture was stirred and refluxed at 110°C and 200 rpm for 16 h under nitrogen protection. After the reaction was completed, toluene was removed by vacuum distillation to obtain the synergistic modifier.

[0041] Preparation of a thick-layer glass flake anti-corrosion coating that integrates the base and surface Weigh component A: 45 parts hydrogenated epoxy resin, 10 parts aluminum tripolyphosphate, 10 parts zinc phosphate, 20 parts glass flakes, 5.5 parts functional composite additive, 3 parts anti-flash rust agent, 1.25 parts dispersant, 1.25 parts defoamer, 3 parts thickener, 3 parts synergistic modifier, and 15 parts solvent; weigh component B: 15 parts fatty amine curing agent and 5 parts solvent; the hydrogenated epoxy resin is model EP-4080E, and the functional composite additive consists of nano-silica and tertiary amine accelerator in a mass ratio of 2:1. The nano-silica has a particle size of 10-50 nm, and the tertiary amine accelerator is 2,4,6-tris(dimethylaminomethyl)phenol (model Ancamine). K54), glass flakes thickness 2-5μm, particle size 40-50μm, anti-flash rust agent is ammonium benzoate, dispersant model is BYK-P104S, defoamer model is BYK-141, thickener model is AKN-7010, solvent is butyl acetate, fatty amine curing agent model is Kingcure 260A.

[0042] Hydrogenated epoxy resin, aluminum tripolyphosphate, zinc phosphate, glass flakes, functional composite additives, anti-flash rust agent, dispersant, defoamer, thickener, synergistic modifier, and solvent were added to a mixing tank and stirred at 1400 rpm for 50 min to obtain component A. Fatty amine curing agent and solvent were added to the mixing tank and stirred at 600 rpm for 20 min to obtain component B. Components A and B were packaged separately to obtain a combined thick-layer glass flake anti-corrosion coating. In use, components A and B are mixed evenly at a mass ratio of 4:1 and applied to the substrate surface to form a coating with a dry film thickness of 600 μm. Example 11

[0043] Example 11 is based on Example 3. The only difference between Example 11 and Example 3 is that the raw materials for preparing component A in Example 11 also include 5 parts of synergistic modifier.

[0044] Preparation of synergistic modifiers The mass ratio of 1,4-butanediol diglycidyl ether, γ-butyrolactone and trimethylolpropane monoallyl ether is 1:0.85:0.13, and the amount of zirconium acetylacetonate accounts for 1.5% of the total mass of the monomers.

[0045] 1,4-Butanediol diglycidyl ether, γ-butyrolactone, trimethylolpropane monoallyl ether, zirconium acetylacetonate, and anhydrous toluene were added to a reaction flask (solid content 50%). The mixture was stirred and refluxed at 110°C and 200 rpm for 16 h under nitrogen protection. After the reaction was completed, toluene was removed by vacuum distillation to obtain the synergistic modifier.

[0046] Preparation of a thick-layer glass flake anti-corrosion coating that integrates the base and surface Weigh component A: 45 parts hydrogenated epoxy resin, 10 parts aluminum tripolyphosphate, 10 parts zinc phosphate, 20 parts glass flakes, 5.5 parts functional composite additive, 3 parts anti-flash rust agent, 1.25 parts dispersant, 1.25 parts defoamer, 3 parts thickener, 5 parts synergistic modifier, and 15 parts solvent; weigh component B: 15 parts fatty amine curing agent and 5 parts solvent; the hydrogenated epoxy resin is model EP-4080E, and the functional composite additive consists of nano-silica and tertiary amine accelerator in a mass ratio of 2:1. The nano-silica has a particle size of 10-50 nm, and the tertiary amine accelerator is 2,4,6-tris(dimethylaminomethyl)phenol (model Ancamine). K54), glass flakes thickness 2-5μm, particle size 40-50μm, anti-flash rust agent is ammonium benzoate, dispersant model is BYK-P104S, defoamer model is BYK-141, thickener model is AKN-7010, solvent is butyl acetate, fatty amine curing agent model is Kingcure 260A.

[0047] Hydrogenated epoxy resin, aluminum tripolyphosphate, zinc phosphate, glass flakes, functional composite additives, anti-flash rust agent, dispersant, defoamer, thickener, synergistic modifier, and solvent were added to a mixing tank and stirred at 1400 rpm for 50 min to obtain component A. Fatty amine curing agent and solvent were added to the mixing tank and stirred at 600 rpm for 20 min to obtain component B. Components A and B were packaged separately to obtain a combined thick-layer glass flake anti-corrosion coating. In use, components A and B are mixed evenly at a mass ratio of 4:1 and applied to the substrate surface to form a coating with a dry film thickness of 600 μm. Example 12

[0048] Example 12 is based on Example 3. The only difference between Example 12 and Example 3 is that the raw materials for preparing component A in Example 12 also include 4 parts of synergistic modifier.

[0049] Preparation of synergistic modifiers The mass ratio of 1,4-butanediol diglycidyl ether, γ-butyrolactone and trimethylolpropane monoallyl ether is 1:0.85:0.12, and the amount of zirconium acetylacetonate accounts for 1.5% of the total mass of the monomers.

[0050] 1,4-Butanediol diglycidyl ether, γ-butyrolactone, trimethylolpropane monoallyl ether, zirconium acetylacetonate, and anhydrous toluene were added to a reaction flask (solid content 50%). The mixture was stirred and refluxed at 110°C and 200 rpm for 16 h under nitrogen protection. After the reaction was completed, toluene was removed by vacuum distillation to obtain the synergistic modifier.

[0051] Preparation of a thick-layer glass flake anti-corrosion coating that integrates the base and surface Weigh component A: 45 parts hydrogenated epoxy resin, 10 parts aluminum tripolyphosphate, 10 parts zinc phosphate, 20 parts glass flakes, 5.5 parts functional composite additive, 3 parts anti-flash rust agent, 1.25 parts dispersant, 1.25 parts defoamer, 3 parts thickener, 4 parts synergistic modifier, and 15 parts solvent; weigh component B: 15 parts fatty amine curing agent and 5 parts solvent; the hydrogenated epoxy resin is model EP-4080E, and the functional composite additive consists of nano-silica and tertiary amine accelerator in a mass ratio of 2:1. The nano-silica has a particle size of 10-50 nm, and the tertiary amine accelerator is 2,4,6-tris(dimethylaminomethyl)phenol (model Ancamine). K54), glass flakes thickness 2-5μm, particle size 40-50μm, anti-flash rust agent is ammonium benzoate, dispersant model is BYK-P104S, defoamer model is BYK-141, thickener model is AKN-7010, solvent is butyl acetate, fatty amine curing agent model is Kingcure 260A.

[0052] Hydrogenated epoxy resin, aluminum tripolyphosphate, zinc phosphate, glass flakes, functional composite additives, anti-flash rust agent, dispersant, defoamer, thickener, synergistic modifier, and solvent were added to a mixing tank and stirred at 1400 rpm for 50 min to obtain component A. Fatty amine curing agent and solvent were added to the mixing tank and stirred at 600 rpm for 20 min to obtain component B. Components A and B were packaged separately to obtain a combined thick-layer glass flake anti-corrosion coating. In use, components A and B are mixed evenly at a mass ratio of 4:1 and applied to the substrate surface to form a coating with a dry film thickness of 600 μm. Example 13

[0053] Example 13 is based on Example 12. The only difference between Example 13 and Example 12 is that the amount of synergistic modifier added in Example 13 is 1 part. Example 14

[0054] Example 14 is based on Example 12. The only difference between Example 14 and Example 12 is that the amount of synergistic modifier added in Example 14 is 7 parts. Example 15

[0055] Example 15 is based on Example 12. The only difference between Example 15 and Example 12 is that in Example 15, the mass ratio of 1,4-butanediol diglycidyl ether, γ-butyrolactone and trimethylolpropane monoallyl ether is 1:0.85:0.08 when preparing the synergistic modifier. Example 16

[0056] Example 16 is based on Example 12. The only difference between Example 16 and Example 12 is that the mass ratio of 1,4-butanediol diglycidyl ether, γ-butyrolactone and trimethylolpropane monoallyl ether is 1:0.85:0.15 when preparing the synergistic modifier in Example 16. Example 17

[0057] Example 17 is based on Example 12. The only difference between Example 17 and Example 12 is that in Example 17, trimethylolpropane monoallyl ether is not added when preparing the synergistic modifier.

[0058] Comparative Example 1 Comparative Example 1 is based on Example 3. The only difference between Comparative Example 1 and Example 3 is that in Comparative Example 1, only nano-silica is added as the functional composite additive.

[0059] Comparative Example 2 Comparative Example 2 is based on Example 3. The only difference between Comparative Example 2 and Example 3 is that in Comparative Example 2, only tertiary amine accelerators are added to the functional composite additive.

[0060] Comparative Example 3 Comparative Example 3 is based on Example 3. The only difference between Comparative Example 3 and Example 3 is that no functional compound additives are added in Comparative Example 3. Performance testing experiment

[0061] (1) The standard was selected as GB / T30789.4-2015 Evaluation of the number and size of defects and the identification of uniform changes in appearance of paint and varnish coatings - Part 4: Evaluation of cracking grade. The sample was coated on a tinplate, the dry film thickness was controlled at 600 μm, and it was cured at 23℃ and 50% relative humidity for 7 days. The coating surface was observed and the cracking grade was evaluated. The results were recorded in Table 1.

[0062] (2) The standard GB / T 1728-2020 Determination of Drying Time of Paint Film and Putty Film was selected. The surface drying time of the sample was tested by the finger touch method and the actual drying time of the sample was tested by the filter paper pressing method. The results are recorded in Table 1.

[0063] (3) The standard ISO 9227:2022 / Amd 1:2024 Corrosion test in artificial atmosphere: salt spray test was selected. The sample was coated on a carbon steel test plate and the dry film thickness was controlled to be 600 μm. It was cured at 23℃ and 50% relative humidity for 7 days. The edges were sealed with a mixture of paraffin and rosin. A scratch parallel to the long side (through the coating to the substrate) was made in the middle of the test plate with a sharp knife. Then the test plate was placed in a salt spray test chamber. The test conditions were: the spray solution was 5% sodium chloride solution, pH value 7.0, temperature in the spray chamber 35℃, continuous spraying for 1000h, and average spray collection rate of 2mL / h per 80cm² area. The unidirectional corrosion width at the scratch was detected and the results were recorded in Table 1.

[0064] Table 1. Test results of crack resistance, drying performance, and corrosion resistance. Test results Crack grade (level) Surface work (h) / Actual work (h) Erosion width (mm) Example 1 0 2.0 / 11.0 1.6 Example 2 0 1.5 / 9.0 1.5 Example 3 0 1.5 / 10.0 1.4 Example 4 0 2.5 / 14.0 1.8 Example 5 2 1.0 / 7.0 2.5 Example 6 0 2.0 / 12.0 1.5 Example 7 1 1.0 / 8.0 1.9 Example 8 0 1.5 / 11.0 1.5 Example 9 0 1.5 / 10.0 1.8 Example 10 0 1.2 / 8.5 0.9 Example 11 0 1.2 / 8.5 1.0 Example 12 0 1.0 / 7.5 0.8 Example 13 0 1.4 / 9.5 1.1 Example 14 1 1.0 / 7.0 1.6 Example 15 0 1.4 / 9.5 1.4 Example 16 1 0.9 / 7.0 1.5 Example 17 0 1.5 / 10.0 1.4 Comparative Example 1 0 3.5 / 20.0 2.2 Comparative Example 2 Level 3 1.0 / 7.0 3.0 Comparative Example 3 Level 5 3.0 / 18.0 4.5 As shown in Table 1, the cracking grade of Examples 1-3 is 0, the surface drying time is less than 2 hours, the actual drying time is less than 11 hours, and the corrosion diffusion width is less than 1.6 mm. This shows that the anti-corrosion coating prepared in this application has good crack resistance, fast drying speed and good corrosion resistance.

[0065] As shown in Table 1, the only difference between Examples 4 and 5 and Example 3 is that the mixing ratio of component A and component B was changed in Examples 4 and 5, which affected the curing performance of the coating.

[0066] As shown in Table 1, the only difference between Examples 6-8 and Example 3 is that the ratio of functional composite additives was changed in Examples 6 and 7, which affected the synergistic effect of the two and the performance decreased; in Example 8, the tertiary amine accelerator was replaced with triethanolamine, which resulted in a decrease in performance.

[0067] As shown in Table 1, the only difference between Example 9 and Example 3 is that ammonium benzoate was replaced with ammonium formate in Example 9, which reduced the interface protection and increased the corrosion width.

[0068] As shown in Table 1, the differences between Examples 10-17 and Example 3 are only as follows: Examples 10-12 added a synergistic modifier, which effectively improved the performance of the coating; Examples 13 and 14 violated the limited dosage, as too little dosage had limited performance improvement, while too much dosage would lead to a soft coating with unbalanced internal stress and decreased performance; Examples 15 and 16 changed the synthesis ratio of the synergistic modifier, and too much or too little allyl ether would affect the balance of catalytic performance; Example 17 did not add allyl ether when preparing the synergistic modifier, only linear toughening, and the effect on performance improvement was not obvious.

[0069] As shown in Table 1, the only difference between Comparative Examples 1-3 and Example 3 is that: Comparative Examples 1-2 use a single functional composite additive component, which affects the synergistic effect of the two components. A single component cannot simultaneously achieve the performance of fast drying and thick coating without cracking; Comparative Example 3 does not add a composite functional additive, and the performance is further reduced.

[0070] This specific embodiment is merely an explanation of this application and is not intended to limit it. Based on the above description, those skilled in the art can make various changes and modifications without departing from the technical concept of this application. The technical scope of this application is not limited to the contents of the specification but must be determined according to the scope of the claims.

Claims

1. A thick-layer glass flake anti-corrosion coating integrating the bottom and surface layers, characterized in that: It includes component A and component B, wherein the raw materials for preparing component A include the following components in parts by mass: 30-60 parts of hydrogenated epoxy resin 5-15 parts aluminum tripolyphosphate 5-15 parts zinc phosphate 10-30 pieces of glass flakes 3-8 parts of functional compound additives Anti-flash rust agent 1-5 parts Dispersant 0.5-2 parts 0.5-2 parts of defoamer Thickener 1-5 parts Solvent 10-20 parts; The raw materials for preparing component B include the following components in parts by weight: 12-18 parts of fatty amine curing agent and 2-8 parts of solvent; The functional composite additives include nano-silica and tertiary amine accelerators.

2. The bottom-surface integrated thick-layer glass flake anti-corrosion coating according to claim 1, characterized in that: The mass ratio of component A to component B is (3-5):

1.

3. The bottom-and-surface integrated thick-layer glass flake anti-corrosion coating according to claim 1, characterized in that: The tertiary amine accelerators include 2,4,6-tris(dimethylaminomethyl)phenol.

4. The bottom-and-surface integrated thick-layer glass flake anti-corrosion coating according to claim 1, characterized in that: The mass ratio of nano-silica to tertiary amine accelerator in the functional composite additive is (1.8-2.2):

1.

5. The bottom-and-surface integrated thick-layer glass flake anti-corrosion coating according to claim 1, characterized in that: The anti-flash rust agent includes ammonium benzoate.

6. The bottom-and-surface integrated thick-layer glass flake anti-corrosion coating according to claim 1, characterized in that: The raw materials for preparing component A also include a synergistic modifier, which is prepared by the following steps: 1,4-butanediol diglycidyl ether, γ-butyrolactone, trimethylolpropane monoallyl ether, zirconium acetylacetonate and toluene are mixed and heated and stirred under a protective atmosphere under reflux. After the reaction is completed, toluene is removed by vacuum distillation to obtain the synergistic modifier.

7. The bottom-and-surface integrated thick-layer glass flake anti-corrosion coating according to claim 6, characterized in that: The amount of the synergistic modifier added is 3-5 parts.

8. The bottom-and-surface integrated thick-layer glass flake anti-corrosion coating according to claim 7, characterized in that: The mass ratio of 1,4-butanediol diglycidyl ether, γ-butyrolactone, and trimethylolpropane monoallyl ether is 1:0.85:(0.11-0.13).

9. A method for preparing a bottom-and-surface integrated thick-layer glass flake anti-corrosion coating as described in any one of claims 1-8, characterized in that: Includes the following steps: Hydrogenated epoxy resin, aluminum tripolyphosphate, zinc phosphate, glass flakes, functional composite additives, anti-flash rust agent, dispersant, defoamer, thickener and solvent are mixed and stirred to obtain component A; fatty amine curing agent and solvent are mixed and stirred to obtain component B; component A and component B are packaged separately to obtain a base-top integrated thick-layer glass flake anti-corrosion coating.