A method for preparing an anticorrosive coating, and products and applications thereof
By mixing and heating an aqueous solution of IVB group element ceramic agent with a polysilazane solution, an anti-corrosion coating was prepared under zinc powder-free conditions. This solved the corrosion resistance problem of thin coatings in neutral salt spray tests and achieved corrosion resistance and surface uniformity of more than 2000 hours.
Patent Information
- Application Number
- CN202510383811.2
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- Filing Date
- 2025-03-28
- Publication Date
- 2025-11-04
- Estimated Expiration
- 2045-03-28
AI Technical Summary
Existing anti-corrosion coatings struggle to achieve ideal corrosion resistance in neutral salt spray tests under thin-film conditions, especially without the addition of zinc powder. Traditional methods are insufficient to meet the corrosion resistance requirements of ultra-thin coatings.
An anti-corrosion coating is prepared by mixing an aqueous solution of IVB group element ceramic agent with a polysilazane solution, heating and stirring under a protective gas to form a mixed solution, and then combining it with anti-rust pigments, resins, reinforcing agents, additives and other components.
Without the need to add zinc powder, the anti-corrosion coating achieves over 2000 hours of corrosion resistance in neutral salt spray tests, avoiding localized pitting corrosion and exhibiting good surface uniformity.
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Abstract
Description
TECHNICAL FIELD
[0001] The present application relates to the technical field of anticorrosive coatings, in particular to a preparation method of an anticorrosive coating, a product thereof and application. BACKGROUND
[0002] For the anticorrosive coating applied to Q235 carbon steel, zinc powder is often added to the anticorrosive coating. When zinc powder and Q235 carbon steel form a primary cell in a corrosive environment, due to the existence of potential difference, zinc as an anode will lose electrons and undergo oxidation reaction first, thereby protecting the carbon steel as a cathode, so that the carbon steel is not corroded. Chinese invention patent CN116515371B (January 5, 2024) discloses an epoxy zinc-rich system coating obtained by taking phenolic epoxy resin and zinc powder as main raw materials, which improves the corrosion resistance and durability of the coating formed by the coating. The coating thickness is 60-80 μm; but in some application scenarios where the coating thickness is extremely strict and ultra-thin coating is required, the epoxy zinc-rich system coating is difficult to achieve ideal neutral salt spray test results. Based on this situation, in the aspect of coating use in some application fields, Dacromet process is used; Chinese invention patent CN114456711B (March 10, 2023) discloses a chromium-free Dacromet coating liquid, which discloses that zinc-aluminum alloy powder is added to the chromium-free Dacromet coating liquid. The method for implementing corrosion prevention by using Dacromet zinc-aluminum coating process on the surface of carbon steel can achieve a salt spray corrosion resistance of up to 1500 hours in neutral salt spray test.
[0003] When the anticorrosive coating forms a coating thickness of 20-30 μm, and the anticorrosive coating does not contain zinc powder and has excellent corrosion resistance, the existing technical solutions cannot meet this requirement.
[0004] Therefore, it is a main technical problem to be solved at present to provide an anticorrosive coating without zinc powder and forming a thin coating. SUMMARY
[0005] In order to solve the above technical problems, the first aspect of the present application provides a preparation method of an anticorrosive coating, comprising the following steps:
[0006] S1. Dissolving a ceram agent aqueous solution in DMF to obtain a ceram agent / DMF solution;
[0007] S2. Adding a water absorber to the ceram agent / DMF solution to obtain a ceram agent / DMF solution with a water content of <0.1%, and then adding a polysilazane solution for mixing. The mixture is heated and stirred under a protective gas to obtain a mixed solution;
[0008] S3. Mixing and grinding the mixed solution, anti-rust pigment, resin, reinforcing agent, additive, and solvent to obtain an anticorrosive coating;
[0009] The aqueous ceramizer solution is an aqueous Group IVB element ceramizer solution.
[0010] The inventors found in the experiment that the mixed solution obtained by mixing the aqueous Group IVB element ceramizer solution and the polysilazane solution can achieve a neutral salt spray test of more than 2000 hours without adding zinc powder under thin coating conditions, but the inventors encountered technical difficulties in the experiment that the anticorrosive coating appeared local pitting corrosion when applied by spraying. The inventors found in the experiment that when the ceramizer / DMF solution was not treated by water removal and the anticorrosive coating prepared by mixing the ceramizer / DMF solution and the polysilazane solution without obtaining a mixed solution appeared pitting corrosion defects earlier when subjected to a neutral salt spray test. When the ceramizer / DMF solution with a water content of less than 0.1% and the polysilazane solution were mixed and heated and stirred under a protective gas to obtain a mixed solution, the salt spray resistance of the anticorrosive coating prepared therefrom reached 2000 hours and did not appear irregular local pitting corrosion. The possible reason is that when the water content in the ceramizer / DMF solution is high, the polysilazane is hydrolyzed after being exposed to water, forming a small amount of silicon oxide gel, which causes the anticorrosive coating to appear local pitting corrosion when applied by spraying.
[0011] In one embodiment, the aqueous Group IVB element ceramizer solution comprises a combination of one or more of an aqueous hafnium fluoride solution, an aqueous titanium fluoride solution, and an aqueous zirconium fluoride solution.
[0012] In one embodiment, the reaction that can occur during preparation of the anticorrosive coating is as follows:
[0013]
[0014] The X is any one of Ti, Zr, and Hf elements.
[0015] In one embodiment, the mass concentration of the ceramizer in the ceramizer / DMF solution is 2-10%.
[0016] In one embodiment, the aqueous ceramizer solution is an aqueous hafnium fluoride solution.
[0017] In one embodiment, the aqueous ceramizer solution is an aqueous titanium fluoride solution.
[0018] In one embodiment, the aqueous ceramizer solution is an aqueous zirconium fluoride solution.
[0019] In one embodiment, a water absorbing agent is added to the ceramizer / DMF solution in S2 to obtain a ceramizer / DMF solution with a water content of less than 0.1%.
[0020] In an embodiment, the water absorbent in S2 includes one or more of a combination of anhydrous calcium chloride, water-absorbing silica gel, and molecular sieve.
[0021] The inventors found in the experiment that when the ceramist / DMF solution with a water content of <0.1% and the polysilazane solution are used together, the salt spray test time of the anti-corrosion coating can be improved, and large-area corrosion can be avoided within 1700h. When the ceramist / DMF solution with a water content of >0.1% and the polysilazane solution are used together, local pitting corrosion occurs in the salt spray performance test of the anti-corrosion coating. The possible reason is that the commercially available ceramist usually exists in the form of an aqueous solution, and the polysilazane used contains a large amount of active Si-N bonds, which are extremely easy to react with water to form a small amount of silicon oxide gel, resulting in local pitting corrosion in the salt spray performance of the anti-corrosion coating when applied by spraying.
[0022] In an embodiment, the water absorbent in S2 includes one or more of a combination of anhydrous calcium chloride, water-absorbing silica gel, and molecular sieve.
[0023] In an embodiment, the water absorbent is anhydrous calcium chloride.
[0024] In an embodiment, the water absorbent is water-absorbing silica gel.
[0025] In an embodiment, the water absorbent is molecular sieve.
[0026] In an embodiment, the polysilazane in S2 includes one or more of a combination of methyl polysilazane ammoniated with ammonia gas, perhydropolysilazane, vinyl polysilazane, or polysilazane ammoniated with long-chain primary amine.
[0027] In an embodiment, the methyl polysilazane ammoniated with ammonia gas in S2 is commercially available methyl polysilazane.
[0028] In an embodiment, the commercially available methyl polysilazane includes methyl silicon hydrogen polysilazane.
[0029] In an embodiment, the model of the commercially available methyl polysilazane includes YCP05 from Hangzhou Yuanqi High-tech Materials Co., Ltd.
[0030] In an embodiment, the polysilazane in S2 is perhydropolysilazane.
[0031] In an embodiment, the polysilazane in S2 is vinyl polysilazane.
[0032] In one embodiment, the vinyl polysilazane is commercially available from Merck Durazane TM 1800.
[0033] The inventors found in the experiment that when the ceramifying agent / DMF solution and the polysilazane solution with water content <0.1% were mixed, the obtained anticorrosion coating could avoid corrosion for 2000 hours of salt spray resistance; but the inventors also found in the experiment that when the ceramifying agent / DMF solution with water content <0.1% and the polysilazane were directly mixed, the obtained anticorrosion coating appeared partial pitting corrosion state for 2000 hours of salt spray resistance, and the possible reason was that at room temperature, part of the acidic ceramifying agent would randomly combine with the amino group in the polysilazane, and the obtained anticorrosion coating after spraying appeared local unevenness problem, and after long-term neutral salt spray test, although no large area corrosion appeared, irregular local pitting corrosion appeared; in order to solve the problem of irregular local pitting corrosion, the inventors found in the experiment that the ceramifying agent / DMF solution and the polysilazane solution were first mixed to obtain a mixed solution, the acidic ceramifying agent and the amino group in the polysilazane were pre-reacted and pre-combined, so that the ceramifying agent could react with the polysilazane, and then the anticorrosion pigment and the additive were combined to obtain the anticorrosion coating, and the ceramifying agent of the anticorrosion coating after spraying was uniformly distributed, and when the anticorrosion coating was sprayed on the sandblasted Q235 carbon steel and then subjected to salt spray test, the obtained anticorrosion coating reached 2000h of salt spray resistance, and no irregular pitting corrosion appeared.
[0034] In one embodiment, the polysilazane in S2 is a polysilazane ammonolyzed by a long-chain primary amine.
[0035] In one embodiment, the preparation method of the polysilazane ammonolyzed by a long-chain primary amine comprises the following steps:
[0036] A1. Dissolving methylhydrodichlorosilane in a solvent to form solution a;
[0037] A2. Adding a primary amine to solution a for stirring reaction to obtain a product;
[0038] A3. After filtering out the solid from the product, polysilazane oligomers are obtained by distillation under reduced pressure, and the polysilazane ammonolyzed by a long-chain primary amine is obtained by heating under nitrogen protection;
[0039] The CAS number of the methylhydrodichlorosilane is 75-54-7.
[0040] The number of carbon atoms in the primary amine is greater than 10.
[0041] In one embodiment, the molar ratio of the methylsilane and the primary amine is 1:(3-3.2);
[0042] In an embodiment, the molar ratio of the methylsilane and the primary amine is 1:3.1.
[0043] In an embodiment, the primary amine comprises undecylamine, dodecylamine, octadecylamine.
[0044] In an embodiment, the method for preparing the polysilazane ammonolysed by long-chain primary amine comprises the following steps:
[0045] A1. Dissolve methylhydrogen dichlorosilane in n-hexane to form solution a, the mass concentration of methylhydrogen dichlorosilane in the solution a is 10%;
[0046] A2. Slowly drop a dodecylamine n-hexane solution with a mass concentration of 10% into solution a for stirring reaction, and control the reaction temperature below 25°C to obtain a product, the molar ratio of methylhydrogen dichlorosilane and dodecylamine is 1:3.1;
[0047] A3. After filtering out the solid from the product, distill under reduced pressure to obtain polysilazane oligomers, heat the polysilazane oligomers to 150°C under nitrogen protection to obtain polysilazane ammonolysed by long-chain primary amine.
[0048] The inventors found in the experiment that although the coating prepared by the polysilazane prepared by the ammonia gas ammonolysis method has high level of zinc-free corrosion resistance, the short-chain amine group is very active and easily reacts with H2XF6 to form salt precipitation, and the special polysilazane ammonolysed by long-chain primary amine can improve the salt spray resistance of the anti-corrosion coating.
[0049] In an embodiment, the mass ratio of the ceramifying agent / DMF solution and the polysilazane solution in S2 is 1:(20-40).
[0050] In an embodiment, the polysilazane solution is composed of polysilazane and solvent, and the mass ratio of the polysilazane and the solvent is 1:1.
[0051] In an embodiment, the solvent comprises xylene.
[0052] In an embodiment, S2 is heated and stirred at 80°C under a protective gas for 2h.
[0053] In an embodiment, the protective gas in S2 comprises argon, nitrogen.
[0054] In an embodiment, the protective gas in S2 is argon.
[0055] In an embodiment, the protective gas in S2 is nitrogen.
[0056] In an embodiment, the anti-rust pigment in S3 comprises a combination of one or more of zinc phosphomolybdate, aluminum phosphate, zinc phosphate, aluminum phosphomolybdate.
[0057] In an embodiment, the anti-rust pigment in S3 is zinc phosphomolybdate.
[0058] In an embodiment, the anti-rust pigment in S3 is aluminum phosphate.
[0059] In an embodiment, the anti-rust pigment in S3 is zinc phosphate.
[0060] In an embodiment, the anti-rust pigment in S3 is aluminum phosphomolybdate.
[0061] In an embodiment, the mass ratio of the mixed solution, anti-rust pigment, resin, reinforcing agent, auxiliary agent, solvent in S3 is 100: (10-20): (8-12): (5-9): (2-5): (10-20).
[0062] In an embodiment, the mass ratio of the mixed solution, anti-rust pigment, resin, reinforcing agent, auxiliary agent, solvent in S3 is 100:15:10:7:3.4:15.
[0063] In an embodiment, the resin in S3 comprises chlorinated rubber xylene solution with a mass concentration of 30%.
[0064] In an embodiment, the reinforcing agent in S3 comprises carbon black and mica.
[0065] In an embodiment, the reinforcing agent in S3 consists of carbon black and mica, and the mass ratio of the carbon black and mica is 1:2.5.
[0066] In an embodiment, the auxiliary agent in S3 comprises an anti-settling agent, a thixotropic agent, a dispersing agent, a defoaming agent, and a leveling agent.
[0067] In an embodiment, the auxiliary agent in S3 consists of an anti-settling agent, a thixotropic agent, a dispersing agent, a defoaming agent, and a leveling agent.
[0068] In an embodiment, the mass ratio of the anti-settling agent, the thixotropic agent, the dispersing agent, the defoaming agent, and the leveling agent is 1.5:1:0.3:0.3:0.3.
[0069] In an embodiment, the anti-settling agent is fumed nano-silica, and the available manufacturers and models of the fumed nano-silica include WACKER Fumed Nano-Silica R972.
[0070] In an embodiment, the available manufacturers and models of the thixotropic agent include BYK 410 from Germany.
[0071] In an embodiment, the commercially available model of the dispersant includes BYK 163 from BYK, Germany.
[0072] In an embodiment, the commercially available model of the defoamer includes WSS980 from Wusishixin Material Co., Ltd., Hangzhou, China.
[0073] In an embodiment, the commercially available model of the leveling agent includes TEGO 410 from DEGUKON, Germany.
[0074] In an embodiment, the solvent in S3 includes ethyl acetate.
[0075] The inventors found in the experiment that in order to prolong the salt spray resistance of the anti-corrosion coating, the inventors found in the experiment that after forming a mixed solution of the ceram agent / DMF solution and the polysilazane solution, and then compounding with the anti-rust pigment and the additive, the salt spray resistance of the anti-corrosion coating can be improved to 2300h when the amount of the ceram agent / DMF solution is increased.
[0076] The inventors found in the experiment that the use of the aqueous solution of the IVB group element ceram agent and the polysilazane in the anti-corrosion coating can form a coating layer with excellent performance of more than 2000 hours in the neutral salt spray test without adding zinc powder; but the inventors found that the anti-corrosion coating obtained by mixing the ceram agent and the polysilazane and other raw materials can greatly improve the salt spray resistance test, but the inventors proposed a better solution; the reason is that the commonly used ceram agent on the market is usually in the form of an aqueous solution, and the polysilazane contains a large number of active Si-N bonds, which are easy to react with water; in view of this technical difficulty, the inventors found in the experiment that the ceram agent / DMF solution is dehydrated to reduce the water content, and then mixed with the polysilazane solution to obtain a mixed solution, which can ensure that the Si-N bond is not damaged at room temperature and is not easy to produce gel components; but the inventors found in the experiment that even if the Si-N bond is effectively protected, but in the case of continuing to improve the salt spray test results, new problems have emerged one after another, some acidic ceram agents will randomly combine with the amino groups in the polysilazane at room temperature, so that the ceram agent can react with the polysilazane, and after the anti-corrosion coating prepared by the ceram agent and the polysilazane is sprayed, local unevenness will appear, which may be the formation of ammonium salt precipitates; after long-term neutral salt spray test, although the coating layer does not appear large area corrosion, but irregular local pitting corrosion problem occurs. Based on the above problems, the inventors found that the dehydrated acidic ceram agent and the amino groups in the polysilazane are pre-reacted and pre-bound, which can promote the ceram agent to uniformly react with the polysilazane, and then the anti-corrosion coating formed by compounding the anti-rust pigment and the additive can make the ceram agent uniformly distributed after spraying, solving the above problems.
[0077] The second aspect of the present application provides an anti-corrosion coating prepared by the preparation method of the anti-corrosion coating.
[0078] The third aspect of the present application provides an application of the anti-corrosion coating, which is applied to the fields of petrochemical industry, traffic engineering, hardware tools, and power engineering technology.
[0079] Advantages
[0080] 1. In the present application, the aqueous solution of IVB element ceramifying agent and the polysilazane solution are mixed to obtain a mixed solution, and the anti-corrosion coating can reach more than 2000 hours of neutral salt spray test without adding zinc powder, and a thin coating is obtained.
[0081] 2. In the present application, when the ceramifying agent / DMF solution with a water content of less than 0.1% and the polysilazane solution are mixed and heated and stirred under a protective gas, the salt spray resistance of the anti-corrosion coating prepared by the mixed solution reaches 2000 hours.
[0082] 3. In the present application, when the ceramifying agent / DMF solution with a water content of less than 0.1% and the polysilazane solution are used together, the salt spray test time of the anti-corrosion coating can be improved, and large-area corrosion can be avoided within 1700 hours.
[0083] 4. In the present application, when the ceramifying agent / DMF solution, the polysilazane solution, the anti-rust pigment, and the additive are used together after forming a mixed solution, the salt spray performance of the anti-corrosion coating can be improved by increasing the amount of the ceramifying agent / DMF solution.
[0084] 5. In the present application, when the ceramifying agent / DMF solution, the polysilazane solution, and the anti-rust pigment are used together, the salt spray of the anti-corrosion coating can reach 2300 hours, and the surface is uniform and consistent without any corrosion. BRIEF DESCRIPTION OF DRAWINGS
[0085] Figure 1 It is a state diagram when the performance test in Table 2 is evaluated as A.
[0086] Figure 2 It is a state diagram when the performance test in Table 2 is evaluated as B.
[0087] Figure 3 It is an enlarged view of the state when the performance test in Table 2 is evaluated as B. DETAILED DESCRIPTION
[0088] Example 1
[0089] The present embodiment provides a preparation method of an anti-corrosion coating, comprising the following steps:
[0090] S1. Dissolve the aqueous solution of ceramifying agent in DMF to obtain a ceramifying agent / DMF solution;
[0091] S2. Add the water absorbent to the ceramifying agent / DMF solution, then add the polysilazane solution for mixing, and perform heating and stirring under a protective gas to obtain a mixed solution;
[0092] S3. After mixing and grinding 100 g of the mixed solution, 15 g of anti-rust pigment, 10 g of resin, 7 g of reinforcing agent, 3.4 g of auxiliary agent, and 15 g of solvent, an anti-corrosion coating is obtained.
[0093] The aqueous solution of ceramifying agent is an aqueous solution of fluorozirconate, and the mass concentration of fluorozirconate in the aqueous solution of fluorozirconate is 45%. The aqueous solution of fluorozirconate is dissolved in DMF to obtain a fluorozirconate / DMF solution.
[0094] The mass concentration of fluorozirconate in the fluorozirconate / DMF solution is 5%.
[0095] In S2, the same mass of water-absorbing agent anhydrous calcium chloride is added to the fluorozirconate / DMF solution, and is stored for 24 hours to obtain a fluorozirconate / DMF solution with a water content of 0.05%. 5 g of the fluorozirconate / DMF solution with a water content of 0.05% is added to a polysilazane solution formed by uniformly mixing 100 g of polysilazane with 100 g of xylene, and heating and stirring are performed under a protective gas at 80°C for 2 hours, with a stirring speed of 500 r / min, to obtain a mixed solution.
[0096] The polysilazane is vinyl polysilazane.
[0097] The vinyl polysilazane is commercially available from Merck Durazane TM 1800.
[0098] The protective gas in S2 is nitrogen.
[0099] The anti-rust pigment in S3 is zinc phosphate.
[0100] The resin in S3 includes a chlorinated rubber xylene solution with a mass concentration of 30%.
[0101] The reinforcing agent in S3 is composed of 5 g of mica and 2 g of carbon black.
[0102] The auxiliary agent in S3 is composed of 1.5 g of anti-settling agent, 1 g of thixotropic agent, 0.3 g of dispersing agent, 0.3 g of defoaming agent, and 0.3 g of leveling agent.
[0103] The solvent in S3 is ethyl acetate.
[0104] The mass concentration is 30% chlorinated rubber xylene solution, and the purchase source of chlorinated rubber is Shenzhen Yutian Chemical Co., Ltd., and the model is E0301.
[0105] The purchase manufacturer and model of the mica are 2000 mesh wet method sericite mica of Chuzhou Baota Sericite Mica Mining Co., Ltd.
[0106] The purchase manufacturer and model of the carbon black are Mitsubishi carbon black MA100 of Japan.
[0107] The CAS number of the ethyl acetate is 141-78-6.
[0108] The anti-settling agent is fumed nano silicon dioxide, and the purchase manufacturer and model of the fumed nano silicon dioxide are Wanjing Degussa fumed nano silicon dioxide R972.
[0109] The purchase manufacturer and model of the thixotropic agent are BYK410 of Germany BYK.
[0110] The CAS number of the dicumyl peroxide is 80-43-3.
[0111] The purchase manufacturer and model of the dispersing agent are BYK163 of Germany BYK.
[0112] The purchase manufacturer and model of the defoaming agent are WSS980 of Wuseishi New Material (Hangzhou) Co., Ltd.
[0113] The purchase manufacturer and model of the leveling agent are TEGO410 of Germany Degussa.
[0114] The second aspect of the embodiment provides an anti-corrosion coating prepared by the preparation method of the anti-corrosion coating.
[0115] The third aspect of the embodiment provides an application of the anti-corrosion coating, and the anti-corrosion coating is applied to the fields of petrochemical industry, traffic engineering, hardware tools, and power engineering technology.
[0116] Embodiment 2
[0117] The embodiment provides a preparation method of an anti-corrosion coating, including the following steps:
[0118] S1. Dissolve the ceram agent aqueous solution in DMF to obtain a ceram agent / DMF solution;
[0119] S2. Add the water absorbent to the ceram agent / DMF solution, then add and mix the polysilazane solution, and heat and stir under a protective gas to obtain a mixed solution;
[0120] S3. 100 g of the mixed solution, 15 g of the anti-rust pigment, 10 g of the resin, 7 g of the reinforcing agent, 3.4 g of the auxiliary agent, and 15 g of the solvent are mixed and ground to obtain the anti-corrosion coating.
[0121] The ceramifying agent aqueous solution is a fluorotitanic acid aqueous solution, and the mass concentration of fluorotitanic acid in the fluorotitanic acid aqueous solution is 50%. The fluorotitanic acid aqueous solution is dissolved in DMF to obtain a fluorotitanic acid / DMF solution.
[0122] The mass concentration of fluorotitanic acid in the fluorotitanic acid / DMF solution is 5%.
[0123] In S2, the same mass of the water absorbent anhydrous calcium chloride is added to the fluorotitanic acid / DMF solution, and the mixture is stored for 24 hours to obtain a fluorotitanic acid / DMF solution with a water content of 0.05%. 5 g of the fluorotitanic acid / DMF solution with a water content of 0.05% is added to a polysilazane solution formed by uniformly mixing 100 g of polysilazane with 100 g of dimethylbenzene. The mixture is heated and stirred at 80°C under a protective gas for 2 hours at a stirring speed of 500 r / min to obtain a mixed solution.
[0124] The polysilazane in S2 is methyl polysilazane.
[0125] The methyl polysilazane is methyl silicon hydrogen polysilazane, and the model of the methyl silicon hydrogen polysilazane purchased from Hangzhou Yuanqi High-tech Materials Co., Ltd. is YCP05.
[0126] The protective gas in S2 is nitrogen.
[0127] The anti-rust pigment in S3 is zinc phosphate.
[0128] The resin is a chlorinated rubber dimethylbenzene solution with a mass concentration of 30%.
[0129] The reinforcing agent is composed of 5 g of mica and 2 g of carbon black.
[0130] The auxiliary agent is composed of 1.5 g of an anti-settling agent, 1 g of a thixotropic agent, 0.3 g of a dispersing agent, 0.3 g of an antifoaming agent, and 0.3 g of a leveling agent.
[0131] The solvent is ethyl acetate.
[0132] The chlorinated rubber in the chlorinated rubber dimethylbenzene solution with a mass concentration of 30% is purchased from Shenzhen Jiyida Chemical Co., Ltd., and the model is E0301.
[0133] The mica is purchased from Chuzhou Baota Sericite Mine Co., Ltd., and the model is 2000-mesh wet sericite.
[0134] The carbon black is purchased from Mitsubishi Carbon Black, Japan, and the model is MA100.
[0135] The CAS number of the ethyl acetate is 141-78-6.
[0136] The anti-settling agent is fumed nano-silica, and the purchase manufacturer and model of the fumed nano-silica is Wanjing Degosi fumed nano-silica R972.
[0137] The purchase manufacturer and model of the thixotropic agent is BYK410 of Germany BYK.
[0138] The CAS number of the dicumyl peroxide is 80-43-3.
[0139] The purchase manufacturer and model of the dispersing agent is BYK163 of Germany BYK.
[0140] The purchase manufacturer and model of the defoaming agent is WSS980 of Wuseishi New Material (Hangzhou) Co., Ltd.
[0141] The purchase manufacturer and model of the leveling agent is TEGO410 of Germany Degussa.
[0142] The second aspect of the embodiment provides an anti-corrosion coating prepared by the preparation method of the anti-corrosion coating.
[0143] The third aspect of the embodiment provides an application of the anti-corrosion coating, and the anti-corrosion coating is applied to the fields of petrochemical industry, traffic engineering, hardware tools, and power engineering technology.
[0144] Embodiment 3
[0145] The embodiment provides a preparation method of an anti-corrosion coating, including the following steps:
[0146] S1. Dissolving a ceram agent aqueous solution in DMF to obtain a ceram agent / DMF solution;
[0147] S2. Adding a water absorbent to the ceram agent / DMF solution, then adding a polysilazane solution for mixing, and heating and stirring under a protective gas to obtain a mixed solution;
[0148] S3. Mixing and grinding 100 g of the mixed solution, 15 g of a rust-proof pigment, 10 g of a resin, 7 g of a reinforcing agent, 3.4 g of an auxiliary agent, and 15 g of a solvent to obtain the anti-corrosion coating.
[0149] The ceram agent aqueous solution is a fluorozirconate aqueous solution, and the mass concentration of the fluorozirconate in the fluorozirconate aqueous solution is 45%.
[0150] The mass concentration of the fluorozirconate in the fluorozirconate / DMF solution is 5%.
[0151] The S2 is added with the same mass of water absorption agent, anhydrous calcium chloride, and stored for 24 hours to obtain a fluorozirconate / DMF solution with a water content of 0.05%. 10 g of the fluorozirconate / DMF solution is added with a polysilazane solution formed by uniformly mixing 100 g of polysilazane with 100 g of xylene. The mixture is heated and stirred at 80°C under a protective gas for 2 hours at a stirring speed of 500 r / min.
[0152] The polysilazane is a vinyl polysilazane.
[0153] The vinyl polysilazane is commercially available from Merck Durazane TM 1800.
[0154] The protective gas in the S2 is nitrogen.
[0155] The anti-rust pigment in the S3 is zinc phosphate.
[0156] The resin is a chlorinated rubber xylene solution with a mass concentration of 30%.
[0157] The reinforcing agent is composed of 5 g of mica and 2 g of carbon black.
[0158] The auxiliary agent is composed of 1.5 g of anti-settling agent, 1 g of thixotropic agent, 0.3 g of dispersing agent, 0.3 g of defoaming agent, and 0.3 g of leveling agent.
[0159] The solvent is ethyl acetate.
[0160] The chlorinated rubber in the chlorinated rubber xylene solution with a mass concentration of 30% is commercially available from Shenzhen Jitian Chemical Co., Ltd. with the model number E0301.
[0161] The mica is commercially available from Chuzhou Baota Sericite Mine Co., Ltd. with the model number 2000 mesh wet-process sericite.
[0162] The carbon black is commercially available from Mitsubishi Chemical Corporation, Japan with the model number MA100.
[0163] The CAS number of the ethyl acetate is 141-78-6.
[0164] The anti-settling agent is fumed nano-silica, which is commercially available from Wacker Chemie AG with the model number R972.
[0165] The thixotropic agent is commercially available from BYK-Chemie GmbH, Germany with the model number BYK 410.
[0166] The CAS number of the dicumyl peroxide is 80-43-3.
[0167] The dispersant is purchased from Germany BYK 163.
[0168] The antifoaming agent is purchased from WSS980 of Wusei New Material (Hangzhou) Co., Ltd.
[0169] The leveling agent is purchased from Germany Degussa TEGO 410.
[0170] The second aspect of the embodiment provides an anti-corrosion coating prepared by the preparation method of the anti-corrosion coating.
[0171] The third aspect of the embodiment provides an application of the anti-corrosion coating, which is applied to the fields of petrochemical industry, traffic engineering, hardware tools, and power engineering technology.
[0172] Embodiment 4
[0173] The embodiment provides a preparation method of an anti-corrosion coating, including the following steps.
[0174] S1. Dissolving a ceram agent aqueous solution in DMF to obtain a ceram agent / DMF solution;
[0175] S2. Adding a water absorbent to the ceram agent / DMF solution, and then adding a polysilazane solution to mix, and heating and stirring under a protective gas to obtain a mixed solution;
[0176] S3. Mixing and grinding 100 g of the mixed solution, 15 g of a rust-proof pigment, 10 g of a resin, 7 g of a reinforcing agent, 3.4 g of an auxiliary agent, and 15 g of a solvent to obtain the anti-corrosion coating.
[0177] The ceram agent aqueous solution is a fluorozirconate aqueous solution, the mass concentration of fluorozirconate in the fluorozirconate aqueous solution is 45%, and the fluorozirconate aqueous solution is dissolved in DMF to obtain a fluorozirconate / DMF solution.
[0178] The mass concentration of fluorozirconate in the fluorozirconate / DMF solution is 5%.
[0179] In S2, the same mass of the water absorbent anhydrous calcium chloride is added to the fluorozirconate / DMF solution, and is stored for 24 hours to obtain a fluorozirconate / DMF solution with a water content of 0.05%, 100 g of polysilazane is uniformly mixed with 100 g of dimethylbenzene to form a polysilazane solution, and heating and stirring are performed under a protective gas at 80 ℃ for 2 h, the stirring speed is 500 r / min, and a mixed solution is obtained.
[0180] The polysilazane in the polysilazane solution in S2 is a polysilazane ammonolyzed by a long-chain primary amine.
[0181] The preparation method of the long-chain primary amine ammonolysis polysilazane comprises the following steps:
[0182] A1. Dissolve methylhydrogen dichlorosilane in n-hexane to form a solution a, the mass concentration of methylhydrogen dichlorosilane in the solution a is 10%;
[0183] A2. Slowly drop a 10% mass concentration dodecylamine n-hexane solution into the solution a for stirring reaction, and control the reaction temperature below 25℃ to obtain a product, the molar ratio of methylhydrogen dichlorosilane and dodecylamine is 1:3.1;
[0184] A3. After filtering out the solid from the product, distill under reduced pressure to obtain a polysilazane oligomer, heat the polysilazane oligomer to 150℃ under nitrogen protection to obtain a long-chain primary amine ammonolysis polysilazane.
[0185] The protective gas in S2 is nitrogen.
[0186] The rust-proof pigment in S3 is zinc phosphate.
[0187] The resin is a chlorinated rubber xylene solution with a mass concentration of 30%.
[0188] The reinforcing agent is composed of mica 5g and carbon black 2g.
[0189] The auxiliary agent is composed of anti-settling agent 1.5g, thixotropic agent 1g, dispersing agent 0.3g, defoaming agent 0.3g and leveling agent 0.3g.
[0190] The solvent is ethyl acetate.
[0191] The purchase source of chlorinated rubber in the chlorinated rubber xylene solution with a mass concentration of 30% is Shenzhen Yitian Chemical Co., Ltd., and the model is E0301.
[0192] The purchase manufacturer and model of the mica are 2000 mesh wet-process sericite of Chuzhou Baota Sericite Mine Co., Ltd.
[0193] The purchase manufacturer and model of the carbon black are Mitsubishi carbon black MA100 of Japan.
[0194] The CAS number of the ethyl acetate is 141-78-6.
[0195] The anti-settling agent is fumed nano-silicon dioxide, and the purchase manufacturer and model of the fumed nano-silicon dioxide are Wanjing Degosai fumed nano-silicon dioxide R972.
[0196] The purchase manufacturer and model of the thixotropic agent are BYK410 of Germany BIK.
[0197] The CAS number of the dicumyl peroxide is 80-43-3.
[0198] The purchase manufacturer model of the dispersant is BYK163 of Germany BYK.
[0199] The purchase manufacturer model of the defoaming agent is WSS980 of Wusei New Material (Hangzhou) Co., Ltd.
[0200] The purchase manufacturer model of the leveling agent is TEGO410 of Germany Degussa.
[0201] The second aspect of the embodiment provides an anti-corrosion coating prepared by the preparation method of the anti-corrosion coating.
[0202] The third aspect of the embodiment provides an application of the anti-corrosion coating, and the anti-corrosion coating is applied to the fields of petrochemical industry, traffic engineering, hardware tools, and power engineering technology.
[0203] Comparative Example 1
[0204] The comparative example provides a preparation method of an anti-corrosion coating, including the following steps:
[0205] S1. Dissolving the aqueous solution of the ceramifying agent in DMF to obtain a ceramifying agent / DMF solution;
[0206] S2. After mixing and grinding 100g of a polysilazane xylene solution with a mass concentration of 50%, 2.5g of the ceramifying agent / DMF solution, 15g of a rust-proof pigment, 10g of a resin, 7g of a reinforcing agent, 3.4g of an auxiliary agent, and 15g of a solvent, an anti-corrosion coating is obtained.
[0207] The polysilazane in the polysilazane xylene solution is a vinyl polysilazane.
[0208] The purchase manufacturer model of the vinyl polysilazane is Durazane of Germany Merck. TM 1800.
[0209] The rust-proof pigment is zinc phosphate.
[0210] The aqueous solution of the ceramifying agent is an aqueous solution of fluorozirconate, the mass concentration of fluorozirconate in the aqueous solution of fluorozirconate is 45%, and the aqueous solution of fluorozirconate is dissolved in DMF to obtain a fluorozirconate / DMF solution.
[0211] The mass concentration of fluorozirconate in the fluorozirconate / DMF solution is 5%.
[0212] The resin is a chlorinated rubber xylene solution with a mass concentration of 30%.
[0213] The reinforcing agent is composed of 5g of mica and 2g of carbon black.
[0214] The auxiliary agent is composed of anti-settling agent 1.5g, thixotropic agent 1g, dispersing agent 0.3g, defoaming agent 0.3g and leveling agent 0.3g.
[0215] The solvent is ethyl acetate.
[0216] The mass concentration is 30% chlorinated rubber xylene solution, and the purchase source of chlorinated rubber is Shenzhen Yitian Chemical Co., Ltd., and the model is E0301.
[0217] The purchase manufacturer and model of the mica are 2000 mesh wet-process sericite of Chuzhou Baota Sericite Mine Co., Ltd.
[0218] The purchase manufacturer and model of the carbon black are Mitsubishi carbon black MA100 of Japan.
[0219] The CAS number of the ethyl acetate is 141-78-6.
[0220] The anti-settling agent is fumed nano-silicon dioxide, and the purchase manufacturer and model of the fumed nano-silicon dioxide are Wanjing Degosai fumed nano-silicon dioxide R972.
[0221] The purchase manufacturer and model of the thixotropic agent are BYK410 of Germany BIK.
[0222] The CAS number of the dicumyl peroxide is 80-43-3.
[0223] The purchase manufacturer and model of the dispersing agent are BYK163 of Germany BIK.
[0224] The purchase manufacturer and model of the defoaming agent are WSS980 of Wuseishi New Material (Hangzhou) Co., Ltd.
[0225] The purchase manufacturer and model of the leveling agent are TEGO410 of Germany Degao.
[0226] The second aspect of the present comparative example provides a kind of anticorrosive coating, which is prepared by the preparation method of the anticorrosive coating.
[0227] Comparative example 2
[0228] The present comparative example provides a kind of anticorrosive coating preparation method, including the following steps:
[0229] S1. Dissolve the ceram agent aqueous solution in DMF to obtain a ceram agent / DMF solution;
[0230] S2. Add the same mass of water-absorbing agent anhydrous calcium chloride to the ceram agent / DMF solution, store for 24 hours, and obtain a ceram agent / DMF solution with a moisture content of 0.05%;
[0231] S3. 100 g of a 50% mass concentration polysilazane xylene solution, 2.5 g of a 0.05% water content ceramifying agent / DMF solution, 15 g of a rust-proof pigment, 10 g of a resin, 7 g of a reinforcing agent, 3.4 g of an auxiliary agent, and 15 g of a solvent are mixed and ground to obtain an anti-corrosion coating.
[0232] The polysilazane in the polysilazane xylene solution is a vinyl polysilazane.
[0233] The manufacturer and model of the vinyl polysilazane are Durazane 1000 from Merck, Germany. TM 1800.
[0234] The ceramifying agent aqueous solution is a fluozirconic acid aqueous solution, the mass concentration of fluozirconic acid in the fluozirconic acid aqueous solution is 45%, and the fluozirconic acid aqueous solution is dissolved in DMF to obtain a fluozirconic acid / DMF solution.
[0235] The mass concentration of fluozirconic acid in the fluozirconic acid / DMF solution is 5%.
[0236] The rust-proof pigment is zinc phosphate.
[0237] The resin is a 30% mass concentration chlorinated rubber xylene solution.
[0238] The reinforcing agent is composed of 5 g of mica and 2 g of carbon black.
[0239] The auxiliary agent is composed of 1.5 g of an anti-settling agent, 1 g of a thixotropic agent, 0.3 g of a dispersing agent, 0.3 g of an antifoaming agent, and 0.3 g of a leveling agent.
[0240] The solvent is ethyl acetate.
[0241] The purchase source of the chlorinated rubber in the 30% mass concentration chlorinated rubber xylene solution is Shenzhen Jiyida Chemical Co., Ltd., and the model is E0301.
[0242] The purchase manufacturer and model of the mica are 2000-mesh wet-process sericite from Chuzhou Baota Sericite Mine Co., Ltd.
[0243] The purchase manufacturer and model of the carbon black are Mitsubishi Carbon Black MA100 from Japan.
[0244] The CAS number of the ethyl acetate is 141-78-6.
[0245] The anti-settling agent is fumed nano-silicon dioxide, and the purchase manufacturer and model of the fumed nano-silicon dioxide are WACKER Fumed Nano-Silicon Dioxide R972.
[0246] The purchase manufacturer and model of the thixotropic agent are BYK 410 from Germany.
[0247] The CAS number of the dicumyl peroxide is 80-43-3.
[0248] The purchase manufacturer model of the dispersant is BYK163 of Germany BYK.
[0249] The purchase manufacturer model of the defoaming agent is WSS980 of Wuse Stone New Material (Hangzhou) Co., Ltd.
[0250] The purchase manufacturer model of the leveling agent is TEGO410 of Germany Degussa.
[0251] The second aspect of the present comparative example provides an anti-corrosion coating prepared by the preparation method of the anti-corrosion coating.
[0252] Comparative Example 3
[0253] The present comparative example provides a preparation method of an anti-corrosion coating, comprising the following steps:
[0254] 100g of a polysilazane xylene solution with a mass concentration of 50%, 15g of anti-rust pigment, 10g of resin, 7g of reinforcing agent, 3.4g of auxiliary agent, and 15g of solvent are mixed and ground to obtain an anti-corrosion coating.
[0255] The polysilazane in the polysilazane xylene solution is a vinyl polysilazane.
[0256] The purchase manufacturer model of the vinyl polysilazane is Durazane TM1800 of Germany Merck.
[0257] The anti-rust pigment is zinc phosphate.
[0258] The resin is a chlorinated rubber xylene solution with a mass concentration of 30%.
[0259] The reinforcing agent is composed of 5g of mica and 2g of carbon black.
[0260] The auxiliary agent is composed of 1.5g of anti-settling agent, 1g of thixotropic agent, 0.3g of dispersant, 0.3g of defoaming agent, and 0.3g of leveling agent.
[0261] The solvent is ethyl acetate.
[0262] The purchase source of the chlorinated rubber in the chlorinated rubber xylene solution with a mass concentration of 30% is Shenzhen Jitian Chemical Co., Ltd., and the model is E0301.
[0263] The purchase manufacturer and model of the mica are 2000-mesh wet-process sericite of Chuzhou Baota Sericite Mica Mining Co., Ltd.
[0264] The purchase manufacturer and model of the carbon black are MA100 of Japan Mitsubishi Carbon Black.
[0265] The CAS number of the ethyl acetate is 141-78-6.
[0266] The anti-settling agent is fumed nano-silica, and the purchase manufacturer and model of the fumed nano-silica is Wanjing Degosi fumed nano-silica R972.
[0267] The purchase manufacturer and model of the thixotropic agent is BYK410 of Germany BYK.
[0268] The CAS number of the dicumyl peroxide is 80-43-3.
[0269] The purchase manufacturer and model of the dispersing agent is BYK163 of Germany BYK.
[0270] The purchase manufacturer and model of the defoaming agent is WSS980 of Wuseishixin Material (Hangzhou) Co., Ltd.
[0271] The purchase manufacturer and model of the leveling agent is TEGO410 of Germany Degao.
[0272] The second aspect of the present comparative example provides an anti-corrosion coating prepared by the preparation method of the anti-corrosion coating.
[0273] Comparative Example 4
[0274] The present comparative example provides a preparation method of an anti-corrosion coating, comprising the following steps:
[0275] S1. Dissolving the ceram agent aqueous solution in DMF to obtain a ceram agent / DMF solution;
[0276] S2. Adding the water absorbent to the ceram agent / DMF solution, then adding and mixing the polysilazane solution, and heating and stirring under a protective gas to obtain a mixed solution;
[0277] S3. Mixing and grinding 100 g of the mixed solution, 15 g of the anti-rust pigment, 10 g of the resin, 7 g of the reinforcing agent, 3.4 g of the auxiliary agent, and 15 g of the solvent to obtain the anti-corrosion coating;
[0278] The ceram agent aqueous solution is a fluozirconate aqueous solution, and the mass concentration of the fluozirconate in the fluozirconate aqueous solution is 45%. The fluozirconate aqueous solution is dissolved in DMF to obtain a fluozirconate / DMF solution.
[0279] The mass concentration of the fluozirconate in the fluozirconate / DMF solution is 5%.
[0280] The S2 is added with the same mass of water absorption agent anhydrous calcium chloride to obtain a fluorozirconate / DMF solution with a water content of 2%, 5g of fluorozirconate / DMF solution is added with a polysilazane solution formed by uniformly mixing 100g of polysilazane with 100g of xylene, and heated and stirred at 80°C for 2h under a protective gas to obtain a mixed solution.
[0281] The polysilazane is a vinyl polysilazane.
[0282] The vinyl polysilazane is commercially available from Germany Merck Durazane TM 1800.
[0283] The protective gas in the S2 is nitrogen.
[0284] The anti-rust pigment in the S3 is zinc phosphate.
[0285] The resin is a chlorinated rubber xylene solution with a mass concentration of 30%.
[0286] The reinforcing agent is composed of 5g of mica and 2g of carbon black.
[0287] The auxiliary agent is composed of 1.5g of anti-settling agent, 1g of thixotropic agent, 0.3g of dispersing agent, 0.3g of defoaming agent, and 0.3g of leveling agent.
[0288] The solvent is ethyl acetate.
[0289] The chlorinated rubber in the chlorinated rubber xylene solution with a mass concentration of 30% is commercially available from Shenzhen Jitian Chemical Co., Ltd., with a model number of E0301.
[0290] The mica is commercially available from Chuzhou Baota Sericite Mine Co., Ltd., with a model number of 2000-mesh wet-process sericite.
[0291] The carbon black is commercially available from Japan Mitsubishi Carbon Black MA100.
[0292] The CAS number of the ethyl acetate is 141-78-6.
[0293] The anti-settling agent is fumed nano-silicon dioxide, which is commercially available from Wanjing Degussa fumed nano-silicon dioxide R972.
[0294] The thixotropic agent is commercially available from Germany BYK, with a model number of BYK410.
[0295] The CAS number of the dicumyl peroxide is 80-43-3.
[0296] The dispersing agent is commercially available from Germany BYK, with a model number of BYK163.
[0297] The purchase manufacturer model of the defoaming agent is WSS980 of Wuse Stone New Material (Hangzhou) Co., Ltd.
[0298] The purchase manufacturer model of the leveling agent is TEGO410 of Germany Degussa.
[0299] The second aspect of the present comparative example provides a corrosion-resistant coating prepared by the preparation method of the corrosion-resistant coating.
[0300] Comparative Example 5
[0301] The present comparative example provides a preparation method of a corrosion-resistant coating, comprising the following steps:
[0302] S1. Dissolve the ceramifying agent aqueous solution in DMF to obtain a ceramifying agent / DMF solution;
[0303] S2. Mix and grind 100 g of a polysilazane xylene solution with a mass concentration of 50%, 2.5 g of the ceramifying agent / DMF solution, 15 g of a rust-proof pigment, 10 g of a resin, 7 g of a reinforcing agent, 3.4 g of an auxiliary agent, and 15 g of a solvent to obtain a corrosion-resistant coating;
[0304] The ceramifying agent aqueous solution is a fluorotitanic acid aqueous solution, the mass concentration of fluorotitanic acid in the fluorotitanic acid aqueous solution is 50%, and the fluorotitanic acid aqueous solution is dissolved in DMF to obtain a fluorotitanic acid / DMF solution.
[0305] The mass concentration of fluorotitanic acid in the fluorotitanic acid / DMF solution is 5%.
[0306] The polysilazane in the polysilazane xylene solution is methylsilazane, and the purchase manufacturer model of the methylsilazane is YCP05 of Hangzhou Yuanqi High-tech Materials Technology Co., Ltd.
[0307] The rust-proof pigment is zinc phosphate.
[0308] The resin is a chlorinated rubber xylene solution with a mass concentration of 30%.
[0309] The reinforcing agent is composed of 5 g of mica and 2 g of carbon black.
[0310] The auxiliary agent is composed of 1.5 g of an anti-settling agent, 1 g of a thixotropic agent, 0.3 g of a dispersing agent, 0.3 g of a defoaming agent, and 0.3 g of a leveling agent.
[0311] The solvent is ethyl acetate.
[0312] The purchase source of the chlorinated rubber in the chlorinated rubber xylene solution with a mass concentration of 30% is Shenzhen Jiyida Chemical Co., Ltd., and the model is E0301.
[0313] The purchase manufacturer and model of the mica are 2000 mesh wet method sericite mica of Chuzhou Baota Sericite Mica Mining Co., Ltd.
[0314] The purchase manufacturer and model of the carbon black are Mitsubishi carbon black MA100 of Japan.
[0315] The CAS number of the ethyl acetate is 141-78-6.
[0316] The anti-settling agent is fumed nano-silica, and the purchase manufacturer and model of the fumed nano-silica are Wanjian Degosi fumed nano-silica R972.
[0317] The purchase manufacturer and model of the thixotropic agent are BYK410 of Germany BYK.
[0318] The CAS number of the dicumyl peroxide is 80-43-3.
[0319] The purchase manufacturer and model of the dispersing agent are BYK163 of Germany BYK.
[0320] The purchase manufacturer and model of the defoaming agent are WSS980 of Wuseishi New Material (Hangzhou) Co., Ltd.
[0321] The purchase manufacturer and model of the leveling agent are TEGO410 of Germany Degussa.
[0322] The second aspect of the present comparative example provides an anti-corrosion coating prepared by the preparation method of the anti-corrosion coating.
[0323] Comparative Example 6
[0324] The present comparative example provides a preparation method of an anti-corrosion coating, comprising the following steps:
[0325] S1. Dissolve the ceramifying agent aqueous solution in DMF to obtain a ceramifying agent / DMF solution, add the water absorbing agent to the ceramifying agent / DMF solution, and store for 24 hours to obtain a ceramifying agent / DMF solution with a water content of 0.05%;
[0326] S2. Mix and grind 100 g of a 50% mass concentration polysilazane xylene solution, 2.5 grams of a ceramifying agent / DMF solution with a water content of 0.05%, 15 g of a rust-proof pigment, 10 g of a resin, 7 g of a reinforcing agent, 3.4 g of an auxiliary agent, and 15 g of a solvent to obtain an anti-corrosion coating;
[0327] The ceramifying agent aqueous solution is a fluorotitanic acid aqueous solution, and the mass concentration of fluorotitanic acid in the fluorotitanic acid aqueous solution is 50%. The fluorotitanic acid aqueous solution is dissolved in DMF to obtain a fluorotitanic acid / DMF solution.
[0328] The mass concentration of fluorotitanic acid in the fluorotitanic acid / DMF solution is 5%.
[0329] The polysilazane in the polysilazane xylene solution is methylsilazane, and the purchase manufacturer model thereof is YCP05 of Hangzhou Yuanqi High-tech Materials Co., Ltd.
[0330] The rust-proof pigment is zinc phosphate.
[0331] The resin is a chlorinated rubber xylene solution with a mass concentration of 30%.
[0332] The reinforcing agent is composed of mica 5g and carbon black 2g.
[0333] The auxiliary agent is composed of anti-settling agent 1.5g, thixotropic agent 1g, dispersant 0.3g, defoaming agent 0.3g and leveling agent 0.3g.
[0334] The solvent is ethyl acetate.
[0335] The purchase source of chlorinated rubber in the chlorinated rubber xylene solution with a mass concentration of 30% is Shenzhen Jitian Chemical Co., Ltd., and the model is E0301.
[0336] The purchase manufacturer and model of the mica are 2000-mesh wet-process sericite of Chuzhou Baota Sericite Mine Co., Ltd.
[0337] The purchase manufacturer and model of the carbon black are Mitsubishi carbon black MA100 of Japan.
[0338] The CAS number of the ethyl acetate is 141-78-6.
[0339] The anti-settling agent is fumed nano-silicon dioxide, and the purchase manufacturer and model thereof are WACKER fumed nano-silicon dioxide R972.
[0340] The purchase manufacturer and model of the thixotropic agent are BYK410 of Germany BYK.
[0341] The CAS number of the dicumyl peroxide is 80-43-3.
[0342] The purchase manufacturer and model of the dispersant are BYK163 of Germany BYK.
[0343] The purchase manufacturer and model of the defoaming agent are WSS980 of Wuseishi New Materials (Hangzhou) Co., Ltd.
[0344] The purchase manufacturer and model of the leveling agent are TEGO410 of Germany Degussa.
[0345] The second aspect of the present comparative example provides an anti-corrosion coating prepared by the preparation method of the anti-corrosion coating.
[0346] Comparative Example 7
[0347] The present comparative example provides a preparation method of an anti-corrosion coating, comprising the following steps:
[0348] After mixing and grinding 100 g of a polysilazane xylene solution with a mass concentration of 50%, 15 g of a rust-proof pigment, 10 g of a resin, 7 g of a reinforcing agent, 3.4 g of an additive, and 15 g of a solvent, an anti-corrosion coating is obtained.
[0349] The polysilazane in the polysilazane xylene solution is methylsilazane, and the manufacturer and model of the methylsilazane are YCP05 methylsilazane of Hangzhou Yuanqi High-tech Materials Co., Ltd.
[0350] The rust-proof pigment is zinc phosphate.
[0351] The resin is a chlorinated rubber xylene solution with a mass concentration of 30%.
[0352] The reinforcing agent is composed of 5 g of mica and 2 g of carbon black.
[0353] The additive is composed of 1.5 g of an anti-settling agent, 1 g of a thixotropic agent, 0.3 g of a dispersing agent, 0.3 g of a defoaming agent, and 0.3 g of a leveling agent.
[0354] The solvent is ethyl acetate.
[0355] The chlorinated rubber in the chlorinated rubber xylene solution with a mass concentration of 30% is purchased from Shenzhen Jiyida Chemical Co., Ltd., and the model is E0301.
[0356] The mica is purchased from Chuzhou Baota Sericite Mine Co., Ltd., and the model is 2000-mesh wet sericite.
[0357] The carbon black is purchased from Mitsubishi Carbon Black, Japan, and the model is MA100.
[0358] The CAS number of the ethyl acetate is 141-78-6.
[0359] The anti-settling agent is fumed nano-silicon dioxide, and the manufacturer and model of the fumed nano-silicon dioxide are WACKER Fumed Nano-Silicon Dioxide R972.
[0360] The manufacturer and model of the thixotropic agent are BYK 410 of BYK, Germany.
[0361] The CAS number of the dicumyl peroxide is 80-43-3.
[0362] The manufacturer and model of the dispersing agent are BYK 163 of BYK, Germany.
[0363] The manufacturer and model of the defoaming agent are WSS980 of Wuseishi New Materials (Hangzhou) Co., Ltd.
[0364] The purchasing manufacturer and model number of the flow agent is TEGO410 from Germany.
[0365] The second aspect of the present comparative example provides a corrosion-resistant coating prepared by the preparation method of the corrosion-resistant coating.
[0366] Comparative Example 8
[0367] The present comparative example provides a preparation method of a corrosion-resistant coating, comprising the following steps:
[0368] S1. Dissolve the aqueous solution of ceramifying agent in DMF to obtain a ceramifying agent / DMF solution;
[0369] S2. Mix and grind 167 g of inorganic ceramic resin, 5 g of the ceramifying agent / DMF solution, 15 g of anti-rust pigment, 5 g of mica, 2 g of carbon black, 1.5 g of nano-silica anti-settling agent, 1 g of modified urea solution anti-settling agent, 0.3 g of dispersant, 0.3 g of defoaming agent, and 0.3 g of flow agent to obtain a corrosion-resistant coating;
[0370] The aqueous solution of ceramifying agent is an aqueous solution of fluorozirconate, and the mass concentration of fluorozirconate in the aqueous solution of fluorozirconate is 45%. The aqueous solution of fluorozirconate is dissolved in DMF to obtain a fluorozirconate / DMF solution.
[0371] The mass concentration of fluorozirconate in the fluorozirconate / DMF solution is 5%.
[0372] The purchasing manufacturer and model number of the inorganic ceramic resin is 5200 inorganic ceramic resin from Shenzhen Haineng Chemical Co., Ltd.
[0373] The anti-rust pigment is zinc phosphate.
[0374] The purchasing manufacturer and model number of the mica are 2000-mesh wet-process sericite from Chuzhou Baota Sericite Mine Co., Ltd.
[0375] The purchasing manufacturer and model number of the carbon black are Mitsubishi carbon black MA100 from Japan.
[0376] The purchasing manufacturer and model number of the nano-silica anti-settling agent are WACKER fumed nano-silica A200.
[0377] The purchasing manufacturer and model number of the modified urea solution anti-settling agent are BYK410 modified urea solution anti-settling agent from Germany.
[0378] The purchasing manufacturer and model number of the dispersant are BYK163 from Germany.
[0379] The purchasing manufacturer and model number of the defoaming agent are WSS980 from Wuse Stone New Materials (Hangzhou) Co., Ltd.
[0380] The purchasing manufacturer model of the leveling agent is TEGO410 of Germany.
[0381] The second aspect of the present comparative example provides an anticorrosive coating prepared by the preparation method of the anticorrosive coating.
[0382] The water content in the above examples and comparative examples is measured by using a Shanghai Anting electronic ZSD-2J Karl Fischer water meter.
[0383] Performance test
[0384] Sample preparation: The anticorrosive coatings provided by examples 1-4 and comparative examples 1-8 are added into a double-layer dispersion tank, dispersed for 30 minutes by cooling water, the dispersion speed is 1500 r / min, the slurry is sieved through a 100-mesh sieve, sprayed on a sandblasted Q235 carbon steel, and a coating with a thickness of 25 μm is obtained after baking, and pencil hardness test, adhesion test, and salt spray performance test are carried out respectively. The results of pencil hardness test and adhesion test are shown in Table 1, and the results of salt spray performance test are shown in Table 2.
[0385] The Q235 carbon steel is subjected to Sa3 grade sandblasting surface cleaning.
[0386] The conditions for baking the anticorrosive coatings provided by examples 1-4 and comparative examples 1-8 are 200°C for 40 minutes.
[0387] The pencil hardness test is tested by using the standard method of GB 6739-86 “Pencil Hardness Method for Coating Film Hardness”.
[0388] The adhesion test is tested by using the standard method of GB / T 9286-1998 “Crosshatch Test for Paint and Varnish Film”.
[0389] The salt spray performance test is tested by using the standard method of GB / T 10125-2012 “Salt Spray Test for Artificial Atmosphere Corrosion Test”. In the test results, when the coating surface is uniform and there is no corrosion, it is evaluated as A, when there is local pitting corrosion, it is evaluated as B, and when there is large area corrosion, it is evaluated as C.
[0390] The state of the coating surface when it is uniform and there is no corrosion during the salt spray performance test is shown in Figure 1 .
[0391] The state of the coating when it appears local pitting corrosion during the salt spray performance test is shown in Figure 2 and Figure 3 , Figure 3 is Figure 2 an enlarged view, Figure 3 in which the local pitting corrosion is marked and displayed by a red frame.
[0392] Table 1
[0393] Example Pencil hardness Adhesion Example 1 4H 0 grade Example 2 4H 0 grade Example 3 4H 0 grade Example 4 4H 0 grade Comparative Example 1 4H 0 grade Comparative Example 2 4H 0 grade Comparative Example 3 4H 0 grade Comparative Example 4 4H 0 grade Comparative Example 5 4H 0 grade Comparative Example 6 4H 0 grade Comparative Example 7 4H 0 grade Comparative Example 8 5H 0 grade
[0394] As can be seen from the test results in Table 1, the anti-corrosion coatings provided by Examples 1-4 and Comparative Examples 1-8 have good adhesion and pencil hardness.
[0395] Table 2
[0396]
[0397]
[0398] Note: " / " in Table 2 means not detected, A is evaluated when the surface is uniform and consistent without any corrosion, B is evaluated when local pitting corrosion appears, and C is evaluated when large area corrosion appears.
[0399] As can be seen from the test results in Table 2, the anti-corrosion coatings provided by Examples 1, 2, 3, and 4 are prepared by using the devolatilized solution of the ceramifying agent / DMF solution, pre-reacting with the polysilazane, and compounding with the anti-rust pigment, pigment filler, and additive, and the salt spray of the obtained anti-corrosion coating can reach 1700h, and no irregular pitting corrosion appears until 1700 hours. As can be seen from Example 2, the salt spray performance of the anti-corrosion coating obtained in Example 2 is poorer than that of the anti-corrosion coating obtained in Example 1, which is due to different polysilazanes according to the long-term practical experience of the inventors. Examples 1 and Comparative Examples 1-4 all use vinyl polysilazane, Examples 2 and Comparative Examples 5-7 all use methylsilane polysilazane, Example 3 uses vinyl polysilazane, and Example 4 uses polysilazane ammonolyzed by long-chain primary amine. According to the preparation method of the anti-corrosion coating provided in the present application, using a specific polysilazane can improve the salt spray performance of the anti-corrosion coating. As can be seen from Examples 2, 5, 6, and 7, when the ceramifying agent / DMF solution, polysilazane solution, and anti-rust pigment are compounded in Example 2, the water content of the ceramifying agent / DMF solution is controlled, and the ceramifying agent / DMF solution and the polysilazane solution are mixed to obtain a mixed solution to form an anti-corrosion coating, and the salt spray performance of the anti-corrosion coating is good.
[0400] As can be seen from the test results in Table 2, the anti-corrosion coating provided by Comparative Example 1 is not subjected to water removal treatment of the ceramifying agent / DMF solution during preparation, and the ceramifying agent / DMF solution and the polysilazane are not reacted to obtain a reaction solution, but only a simple mixing is performed. As can be seen from the test results in Table 1, when the anti-corrosion coating provided by Comparative Example 1 is sprayed on the sandblasted Q235 carbon steel and subjected to salt spray test, irregularly distributed local pitting corrosion appears at 2000h.
[0401] As can be seen from the test results in Table 2, the anti-corrosion coating provided by Comparative Example 2, although the water content in the ceramifying agent / DMF solution was controlled during preparation, the ceramifying agent / DMF solution and the polysilazane solution were not reacted to obtain a reaction solution, but only a simple mixing was performed. In Comparative Example 2, the ceramifying agent / DMF solution and the polysilazane were directly mixed, so that when the obtained anti-corrosion coating was sprayed on the sandblasted Q235 carbon steel and then subjected to salt spray test, irregularly distributed local point corrosion occurred at 2000h.
[0402] As can be seen from the test results in Table 2, in the anti-corrosion coating provided by Comparative Example 3, the ceramifying agent / DMF solution, the polysilazane solution and the anti-rust pigment were not used for compounding, and when the obtained anti-corrosion coating was sprayed on the sandblasted Q235 carbon steel and then subjected to salt spray test, large-area corrosion occurred at 400h. This also illustrates the key role of the IVB group modified polysilazane in improving the salt spray resistance of the polysilazane on the carbon steel.
[0403] As can be seen from the test results in Table 2, in the anti-corrosion coating provided by Comparative Example 4, the ceramifying agent / DMF solution and the polysilazane solution with a water content greater than 0.1% were used for compounding, and when the anti-corrosion coating was subjected to salt spray test, local point corrosion occurred. This also verifies the key influence of the water content on the hydrolysis of the silicon-nitrogen bond, thereby further affecting the salt spray test results.
[0404] As can be seen from the test results in Table 2, in the anti-corrosion coating provided by Comparative Example 8, an inorganic ceramic resin was used, and the salt spray resistance of the anti-corrosion coating provided by Comparative Example 8 was poor compared with the anti-corrosion coating obtained by using polysilazane.
Claims
1. A method for preparing an anti-corrosion coating, characterized in that, Includes the following steps: S1. Dissolve the ceramic coating agent aqueous solution in DMF to obtain a ceramic coating agent / DMF solution; S2. Add a desiccant to the ceramic agent / DMF solution to obtain a ceramic agent / DMF solution with a water content of <0.1%, then add a polysilazane solution and mix. Heat and stir under a protective gas to obtain a mixed solution. S3. Mix and grind the mixed solution, anti-rust pigment, resin, reinforcing agent, additives, and solvent to obtain an anti-corrosion coating; The ceramic coating agent aqueous solution is an aqueous solution of a group IVB element ceramic coating agent; The polysilazane in S2 includes polysilazane that has been ammonolyzed with long-chain primary amines; The method for preparing polysilazane by ammonolysis of long-chain primary amines includes the following steps: A1. Dissolve methylsilane in a solvent to form solution a; A2. Add a primary amine to solution a and stir to react, obtaining the product; A3. After filtering out the solids from the product, the product was distilled under reduced pressure to obtain polysilazane oligomers, which were then heated under nitrogen protection to obtain polysilazane obtained by ammonolysis of long-chain primary amines. The primary amine has more than 10 carbon atoms.
2. The method for preparing the anti-corrosion coating as described in claim 1, characterized in that, The aqueous solution of the IVB group element ceramic agent includes one or more combinations of aqueous solutions of fluorohafnium acid, fluorotitanic acid, and fluorozirconic acid.
3. The method for preparing the anti-corrosion coating as described in claim 1, characterized in that, In step S2, an equal mass of water-absorbing agent is added to the ceramic agent / DMF solution to obtain a ceramic agent / DMF solution with a water content of <0.1%.
4. The method for preparing the anti-corrosion coating as described in claim 1, characterized in that, The water-absorbing agent in S2 includes one or more of anhydrous calcium chloride, water-absorbing silica gel, and molecular sieves.
5. The method for preparing the anti-corrosion coating as described in claim 1, characterized in that, The protective gas in S2 includes argon and nitrogen.
6. The method for preparing the anti-corrosion coating as described in claim 1, characterized in that, The anti-rust pigment in S3 includes one or more of zinc phosphomolybdate, aluminum phosphate, zinc phosphate, and aluminum phosphomolybdate.
7. An anti-corrosion coating, characterized in that, It is prepared by the method for preparing anti-corrosion coating as described in any one of claims 1-6.
8. The application of the anti-corrosion coating as described in claim 7, characterized in that, The anti-corrosion coating is applied in the fields of petrochemicals, transportation engineering, hardware tools, and power engineering.
Citation Information
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