Preparation method of anti-corrosion coating as well as product and application of anti-corrosion coating

Abstract

The invention relates to the technical field of anti-corrosion coatings, in particular to a preparation method of an anti-corrosion coating as well as a product and application of the anti-corrosion coating. The preparation method of the anti-corrosion coating comprises the following steps: S1, dissolving a vitrification agent aqueous solution in DMF (Dimethyl Formamide) to obtain a vitrification agent / DMF solution; s2, a water absorbent is added into the vitrification agent / DMF solution to obtain a vitrification agent / DMF solution with the water content smaller than 0.1%, then a polysilazane solution is added for mixing, heating and stirring are conducted under protective gas, and a mixed solution is obtained; s3, mixing and grinding the mixed solution, an anti-rust pigment and an auxiliary agent to obtain an anti-corrosion coating; the vitrification agent aqueous solution is an IVB group element vitrification agent aqueous solution. The IVB group element vitrification agent aqueous solution and the polysilazane solution are mixed to obtain the mixed solution, under the condition that zinc powder does not need to be added, the anti-corrosion coating can achieve a neutral salt spray test for more than 2000 hours, and a thin coating is obtained.

Description

Technical Field

[0001] The present invention relates to the technical field of anti-corrosion coatings, and particularly to a preparation method, product and application of an anti-corrosion coating. Background Art

[0002] For anti-corrosion coatings applied to Q235 carbon steel, zinc powder is often added to the anti-corrosion coating. When the zinc powder and Q235 carbon steel form a primary battery in a corrosive environment, due to the potential difference, zinc, as the anode, will preferentially lose electrons and undergo an oxidation reaction, thereby protecting the carbon steel as the cathode and preventing the carbon steel from being corroded. Chinese invention patent CN116515371B (January 5, 2024) discloses an epoxy zinc-rich system coating obtained with phenolic epoxy resin and zinc powder as the main raw materials, improving the corrosion resistance and durability of the coating formed by the coating, and the coating thickness is 60 - 80 μm; however, in some application scenarios with extremely strict requirements for the coating thickness and requiring an ultra-thin coating, the epoxy zinc-rich system coating is difficult to achieve an ideal neutral salt spray test effect. Based on this situation, in the use of coatings in some application fields, the dacromet process is adopted; Chinese invention patent CN114456711B (March 10, 2023) discloses a chromium-free dacromet coating solution, which discloses that zinc-aluminum alloy powder is added to the chromium-free dacromet coating solution, and a method for implementing anti-corrosion by using the dacromet zinc-aluminum coating process on the surface of carbon steel. In the neutral salt spray test, the maximum salt spray corrosion resistance can reach 1500 hours.

[0003] When the thickness of the coating formed by the anti-corrosion coating is limited to 20 - 30 μm, and it is required to have excellent corrosion resistance without adding zinc powder to the anti-corrosion coating, the existing technical solutions are difficult to meet this requirement.

[0004] Therefore, providing an anti-corrosion coating without zinc powder and forming a thin coating is the main technical problem to be solved currently. Summary of the Invention

[0005] To solve the above technical problems, the first aspect of the present invention provides a preparation method of an anti-corrosion coating, including the following steps:

[0006] S1. Dissolve the phosphatizing agent aqueous solution in DMF to obtain a phosphatizing agent / DMF solution;

[0007] S2. Add a water absorbent to the phosphatizing agent / DMF solution to obtain a phosphatizing agent / DMF solution with a water content < 0.1%, then add a polysilazane solution for mixing, and perform heating and stirring under a protective gas to obtain a mixed solution;

[0008] S3. Mix and grind the mixed solution, rust-inhibiting pigment, resin, reinforcing agent, auxiliary agent, and solvent to obtain an anti-corrosion coating;

[0009] The conversion agent aqueous solution is a conversion agent aqueous solution of Group IVB elements.

[0010] During the experiment, the inventor found that by mixing a conversion agent aqueous solution of Group IVB elements with a polysilazane solution to obtain a mixed solution, without adding zinc powder, the anti-corrosion coating can reach more than 2000 hours of neutral salt spray test and obtain a thin coating in the case of thin coating; however, the technical resistance problem encountered by the inventor during the experiment is that local pitting corrosion will occur in the salt spray resistance when the anti-corrosion coating is spray-applied; the inventor found during the experiment that when the conversion agent / DMF solution is not dewatered and the conversion agent / DMF solution and polysilazane are not mixed to obtain a mixed solution for preparation, the anti-corrosion coating obtained has pitting corrosion defects earlier when performing the neutral salt spray test. When a conversion agent / DMF solution with a water content of <0.1% and a polysilazane solution are mixed and heated and stirred under a protective gas to obtain a mixed solution for preparation, the salt spray resistance of the anti-corrosion coating reaches 2000 hours and no irregular local pitting corrosion occurs; the possible reason is that when the water content in the conversion agent / DMF solution is high, the polysilazane hydrolyzes when encountering water, forming a trace amount of silicon oxide gel, resulting in local pitting corrosion in the salt spray resistance when the anti-corrosion coating is spray-applied.

[0011] In one embodiment, the conversion agent aqueous solution of Group IVB elements includes one or a combination of hafnium fluoride aqueous solution, titanium fluoride aqueous solution, and zirconium fluoride aqueous solution.

[0012] In one embodiment, the reaction process that may occur during the preparation of the anti-corrosion coating is as described in the following formula:

[0013]

[0014] X is any one of Ti, Zr, and Hf elements.

[0015] In one embodiment, the mass concentration of the conversion agent in the conversion agent / DMF solution is 2-10%.

[0016] In one embodiment, the conversion agent aqueous solution is hafnium fluoride aqueous solution.

[0017] In one embodiment, the conversion agent aqueous solution is titanium fluoride aqueous solution.

[0018] In one embodiment, the conversion agent aqueous solution is zirconium fluoride aqueous solution.

[0019] In one embodiment, in S2, a water absorbent is added to the conversion agent / DMF solution to obtain a conversion agent / DMF solution with a water content of <0.1%.

[0020] In one embodiment, in S2, a water absorbent of the same mass is added to the ceraming agent / DMF solution, and it is stored for 24 hours. Then, when the water content rate of the ceraming agent / DMF solution is <0.1%, a polysilazane solution is added for mixing.

[0021] The inventors found during the experiment that when a ceraming agent / DMF solution with a water content rate <0.1% and a polysilazane solution are used in combination, the salt spray test time of the anti-corrosion coating can be increased, and large-area corrosion can be avoided within 1700 h. When a ceraming agent / DMF solution with a water content rate greater than 0.1% and a polysilazane solution are used in combination, local pitting corrosion occurs during the salt spray resistance performance test of the anti-corrosion coating. The possible reason is that commercially available ceraming agents usually exist in the form of aqueous solutions, and the polysilazane used contains a large number of active Si-N bonds, which are extremely easy to react with water to form trace amounts of silicon oxide gels, resulting in local pitting corrosion in the salt spray resistance performance when the anti-corrosion coating is spray-applied.

[0022] In one embodiment, the water absorbent in S2 includes one or a combination of more of anhydrous calcium chloride, silica gel for water absorption, and molecular sieve.

[0023] In one embodiment, the water absorbent is anhydrous calcium chloride.

[0024] In one embodiment, the water absorbent is silica gel for water absorption.

[0025] In one embodiment, the water absorbent is molecular sieve.

[0026] In one embodiment, the polysilazane in S2 includes one or a combination of more of methyl polysilazane ammonolyzed with ammonia, perhydropolysilazane, vinyl polysilazane, or polysilazane ammonolyzed with long-chain primary amine.

[0027] In one embodiment, the methyl polysilazane ammonolyzed with ammonia in S2 is a commercially available methyl polysilazane.

[0028] In one embodiment, the commercially available methyl polysilazane includes methylsilylhydropolysilazane.

[0029] In one embodiment, the commercially available manufacturer model of the methyl polysilazane includes YCP05 of Hangzhou Yuci High-Tech Materials Technology Co., Ltd.

[0030] In one embodiment, the polysilazane in S2 is perhydropolysilazane.

[0031] In one embodiment, the polysilazane in S2 is vinyl polysilazane.

[0032] In one embodiment, the commercially available manufacturer models of the vinyl polysilazane include Durazane from Merck, Germany TM 1800.

[0033] The inventors found during the experiment that when a phosphatizing agent / DMF solution with a water content < 0.1% and a polysilazane solution were mixed, the obtained anti-corrosion coating could avoid corrosion when the salt spray resistance reached 2000 hours; however, the inventors also found during the experiment that when a phosphatizing agent / DMF solution with a water content < 0.1% and polysilazane were directly mixed, local pitting corrosion occurred when the salt spray resistance of the obtained anti-corrosion coating reached 2000 hours. The possible reason is that at room temperature, some acidic phosphatizing agents randomly combine with the amino groups in the polysilazane, resulting in local unevenness on the surface of the obtained anti-corrosion coating after spraying. After long-term neutral salt spray testing, although large-area corrosion did not occur, irregular local pitting corrosion occurred; to solve the problem of irregular local pitting corrosion, the inventors found during the experiment that by first mixing the phosphatizing agent / DMF solution and the polysilazane solution to obtain a mixed solution, and pre-reacting the acidic phosphatizing agent with the amino groups of the polysilazane to make the phosphatizing agent react with the polysilazane, and then cooperating with rust-inhibiting pigments and additives, the phosphatizing agent in the obtained anti-corrosion coating was evenly distributed after spraying. When sprayed on sandblasted Q235 carbon steel and then subjected to salt spray testing, the salt spray resistance of the obtained anti-corrosion coating reached 2000h, and no irregular pitting corrosion occurred.

[0034] In one embodiment, the polysilazane in S2 is a polysilazane ammonolyzed with a long-chain primary amine.

[0035] In one embodiment, the preparation method of the polysilazane ammonolyzed with a long-chain primary amine includes the following steps:

[0036] A1. Dissolve methylhydrodichlorosilane in a solvent to form solution a;

[0037] A2. Add a primary amine to solution a and stir to react to obtain a product;

[0038] A3. After filtering off the solids from the product, perform vacuum distillation to obtain a polysilazane oligomer, and heat it under nitrogen protection to obtain a polysilazane ammonolyzed with a long-chain primary amine;

[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 to the primary amine is 1:(3-3.2);

[0042] In one embodiment, the molar ratio of the methylsilane to the primary amine is 1:3.1;

[0043] In one embodiment, the primary amine includes undecylamine, dodecylamine, and octadecylamine.

[0044] In one embodiment, the method for preparing the polysilazane ammonolyzed with a long-chain primary amine includes the following steps:

[0045] A1. Dissolve methylhydrodichlorosilane in n-hexane to form solution a, and the mass concentration of methylhydrodichlorosilane in solution a is 10%;

[0046] A2. Slowly drop a 10% dodecylamine n-hexane solution into solution a and stir to react, and control the reaction temperature below 25 °C to obtain a product. The molar ratio of methylhydrodichlorosilane to dodecylamine is 1:3.1;

[0047] A3. After filtering off the solids from the product, perform vacuum distillation to obtain a polysilazane oligomer. Under nitrogen protection, heat the polysilazane oligomer to 150 °C to obtain a polysilazane ammonolyzed with a long-chain primary amine.

[0048] The inventors found during the experiment that although the coating prepared from the polysilazane prepared by the ammonia ammonolysis method has a zinc-free high-level anti-corrosion performance, the reactivity of its short-chain amino groups is very easy to react with H 2 XF 6 to form salt precipitation. By using a special polysilazane ammonolyzed with a long-chain primary amine, the salt spray resistance of the anti-corrosion coating can be improved.

[0049] In one embodiment, the mass ratio of the ceramicizing agent / DMF solution to the polysilazane solution in S2 is 1:(20 - 40).

[0050] In one embodiment, the polysilazane solution is composed of polysilazane and a solvent, and the mass ratio of the polysilazane to the solvent is 1:1.

[0051] In one embodiment, the solvent includes xylene.

[0052] In one embodiment, S2 is heated and stirred at 80 °C for 2 h under a protective gas.

[0053] In one embodiment, the protective gas in S2 includes argon and nitrogen.

[0054] In one embodiment, the protective gas in S2 is argon.

[0055] In one embodiment, the protective gas in S2 is nitrogen.

[0056] In one embodiment, the anti-rust pigment in S3 includes one or a combination of more than one of zinc phosphomolybdate, aluminum phosphate, zinc phosphate, and aluminum phosphomolybdate.

[0057] In one embodiment, the anti-rust pigment in S3 is zinc phosphomolybdate.

[0058] In one embodiment, the anti-rust pigment in S3 is aluminum phosphate.

[0059] In one embodiment, the anti-rust pigment in S3 is zinc phosphate.

[0060] In one embodiment, the anti-rust pigment in S3 is aluminum phosphomolybdate.

[0061] In one embodiment, the mass ratio of the mixed solution, anti-rust pigment, resin, reinforcing agent, auxiliary agent, and solvent in S3 is 100:(10 - 20):(8 - 12):(5 - 9):(2 - 5):(10 - 20).

[0062] In one embodiment, the mass ratio of the mixed solution, anti-rust pigment, resin, reinforcing agent, auxiliary agent, and solvent in S3 is 100:15:10:7:3.4:15.

[0063] In one embodiment, the resin in S3 includes a 30% by mass solution of chlorinated rubber in xylene.

[0064] In one embodiment, the reinforcing agent in S3 includes carbon black and mica.

[0065] In one embodiment, the reinforcing agent in S3 consists of carbon black and mica, and the mass ratio of carbon black to mica is 1:2.5.

[0066] In one embodiment, the auxiliary agent in S3 includes a anti-settling agent, a thixotropic agent, a dispersant, an anti-foaming agent, and a leveling agent.

[0067] In one embodiment, the auxiliary agent in S3 consists of an anti-settling agent, a thixotropic agent, a dispersant, an anti-foaming agent, and a leveling agent.

[0068] In one embodiment, the mass ratio of the anti-settling agent, thixotropic agent, dispersant, anti-foaming agent, and leveling agent is 1.5:1:0.3:0.3:0.3.

[0069] In one embodiment, the anti-settling agent is fumed nano-silica, and the purchasable manufacturers and models of the fumed nano-silica include Evonik Degussa fumed nano-silica R972.

[0070] In one embodiment, the purchasable manufacturer model of the thixotropic agent includes BYK410 from BYK Chemie GmbH.

[0071] In one embodiment, the commercially available manufacturer model of the dispersant includes BYK163 from BYK Chemie GmbH, Germany.

[0072] In one embodiment, the commercially available manufacturer model of the defoamer includes WSS980 from Wuseshi New Materials (Hangzhou) Co., Ltd.

[0073] In one embodiment, the commercially available manufacturer model of the leveling agent includes TEGO410 from Degussa, Germany.

[0074] In one embodiment, the solvent in S3 includes ethyl acetate.

[0075] The inventor found during the experiment that in order to extend the salt spray resistance performance of the anticorrosive coating, when a mixed solution is formed by a phosphating agent / DMF solution and a polysilazane solution and then combined with rust preventive pigments and additives, increasing the amount of the phosphating agent / DMF solution can improve the salt spray resistance of the anticorrosive coating to 2300h with a uniform surface and no corrosion.

[0076] The inventor found during the experiment that when a phosphating agent aqueous solution of Group IVB elements is combined with polysilazane in the anticorrosive coating, without adding zinc powder, the coating formed by the anticorrosive coating can achieve excellent performance of more than 2000 hours in the neutral salt spray test; however, the inventor found that although the salt spray test of the anticorrosive coating obtained by mixing the phosphating agent, polysilazane and other raw materials can be greatly improved, the inventor proposed a better solution; the reason is that the commonly available phosphating agents on the market are usually in the form of aqueous solutions, and polysilazane contains a large number of active Si-N bonds, and the Si-N bonds are prone to react with water; in view of this technical resistance problem, the inventor creatively found during the experiment that after the phosphating agent / DMF solution is dehydrated to reduce the moisture content and then mixed with the polysilazane solution, a mixed solution can be obtained, which can ensure that the Si-N bonds are not damaged at room temperature and gels are not easily generated; however, the inventor found during the experiment that even if the Si-N bonds are effectively protected, when the salt spray test results are further improved, new problems arise. At room temperature, some acidic phosphating agents will randomly combine with the amino groups in the polysilazane, causing the phosphating agent to react with the polysilazane. After being formulated into an anticorrosive coating and sprayed, there will be a locally uneven phenomenon, which may be the formation of ammonium salt precipitates; after a long-term neutral salt spray test, although there is no large-area corrosion on the coating, there are irregular local pitting corrosion problems. Based on the above problems, the inventor creatively found that the dehydrated acidic phosphating agent is pre-reacted with the amino groups of the polysilazane to promote the uniform reaction of the phosphating agent with the polysilazane, and then the anticorrosive coating formed by combining with rust preventive pigments and additives can evenly distribute the phosphating agent after spraying, solving the above problems.

[0077] The second aspect of the present invention provides an anti-corrosion coating, which is prepared by the preparation method of the anti-corrosion coating described above.

[0078] The third aspect of the present invention provides an application of the anti-corrosion coating, and the anti-corrosion coating is applied to the technical fields of petrochemical industry, traffic engineering, hardware tools, and power engineering.

[0079] Beneficial effects

[0080] 1. In this application, an aqueous solution of a IVB group element passivator and a polysilazane solution are mixed to obtain a mixed solution. Without adding zinc powder, the anti-corrosion coating can pass a neutral salt spray test for more than 2000 hours and obtain a thin coating.

[0081] 2. In this application, when an aqueous solution of a passivator / DMF solution with a water content < 0.1% and a polysilazane solution are mixed and heated and stirred under a protective gas to obtain a mixed solution for preparing the anti-corrosion coating, the salt spray resistance reaches 2000 hours.

[0082] 3. In this application, when an aqueous solution of a passivator / DMF solution with a water content < 0.1% and a polysilazane solution are used in combination, the salt spray test time of the anti-corrosion coating can be increased, and large-area corrosion can be avoided within 1700 h.

[0083] 4. In this application, when a mixed solution is formed by an aqueous solution of a passivator / DMF solution and a polysilazane solution and then combined with a rust-inhibiting pigment and an additive, increasing the amount of the aqueous solution of a passivator / DMF solution can improve the salt spray performance of the anti-corrosion coating.

[0084] 5. In this application, when an aqueous solution of a passivator / DMF solution, a polysilazane solution ammonolyzed with a long-chain primary amine, and a rust-inhibiting pigment are combined, the salt spray resistance of the anti-corrosion coating can reach 2300 h with a uniform surface and no corrosion. Description of the drawings

[0085] Figure 1 It is a state diagram when the evaluation in Table 2 of the performance test is A.

[0086] Figure 2 It is a state diagram when the evaluation in Table 2 of the performance test is B.

[0087] Figure 3 It is an enlarged view of the state when the evaluation in Table 2 of the performance test is B. Detailed implementation manners

[0088] Example 1

[0089] This example provides a preparation method of an anti-corrosion coating, including the following steps:

[0090] S1. Dissolve the aqueous solution of the ceramicizing agent in DMF to obtain a ceramicizing agent / DMF solution;

[0091] S2. Add a water absorbent to the ceramicizing agent / DMF solution, then add a polysilazane solution and mix them. Heat and stir under a protective gas to obtain a mixed solution;

[0092] S3. Mix and grind 100 g of the mixed solution, 15 g of a rust preventive 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.

[0093] The aqueous solution of the ceramicizing agent is an aqueous solution of zirconium fluoroaluminate. The mass concentration of zirconium fluoroaluminate in the aqueous solution of zirconium fluoroaluminate is 45%. Dissolve the aqueous solution of zirconium fluoroaluminate in DMF to obtain a zirconium fluoroaluminate / DMF solution.

[0094] The mass concentration of zirconium fluoroaluminate in the zirconium fluoroaluminate / DMF solution is 5%.

[0095] In S2, add anhydrous calcium chloride, which is a water absorbent of the same mass, to the zirconium fluoroaluminate / DMF solution and store it for 24 hours to obtain a zirconium fluoroaluminate / DMF solution with a water content of 0.05%. Add a polysilazane solution formed by uniformly mixing 100 g of polysilazane and 100 g of xylene to 5 g of the zirconium fluoroaluminate / DMF solution with a water content of 0.05%. Heat and stir at 80 °C for 2 h under a protective gas. The stirring speed is 500 r / min to obtain a mixed solution.

[0096] The polysilazane is vinyl polysilazane.

[0097] The commercially available manufacturer model of the vinyl polysilazane is Durazane 1800 from Merck, Germany. TM 1800.

[0098] The protective gas in S2 is nitrogen.

[0099] The rust preventive pigment in S3 is zinc phosphate.

[0100] The resin in S3 includes a 30% mass concentration solution of chlorinated rubber in xylene.

[0101] The reinforcing agent in S3 consists of 5 g of mica and 2 g of carbon black.

[0102] The auxiliary agent in S3 consists of 1.5 g of an anti-settling agent, 1 g of a thixotropic agent, 0.3 g of a dispersant, 0.3 g of an antifoaming agent, and 0.3 g of a leveling agent.

[0103] The solvent in S3 is ethyl acetate.

[0104] The source of the chlorinated rubber in the 30% chlorinated rubber xylene solution is Shenzhen Yitian Chemical Co., Ltd., and the model is E0301.

[0105] The mica is purchased from Chuzhou Baota Sericite Mining Co., Ltd. and the model is 2000-mesh wet-process sericite.

[0106] The carbon black is purchased from Mitsubishi Carbon Black MA100, Japan.

[0107] The CAS number of ethyl acetate is 141-78-6.

[0108] The anti-settling agent is fumed nano-silica, and the fumed nano-silica is purchased from Evonik Degussa fumed nano-silica R972.

[0109] The thixotropic agent is purchased from BYK410, Germany.

[0110] The CAS number of dicumyl peroxide is 80-43-3.

[0111] The dispersant is purchased from BYK163, Germany.

[0112] The defoamer is purchased from Wuseshi New Materials (Hangzhou) Co., Ltd. WSS980.

[0113] The leveling agent is purchased from Degussa TEGO410, Germany.

[0114] In the second aspect of this embodiment, an anti-corrosion coating is provided, which is prepared by the preparation method of the anti-corrosion coating described above.

[0115] In the third aspect of this embodiment, an application of the anti-corrosion coating is provided, and the anti-corrosion coating is applied to the fields of petrochemical industry, transportation engineering, hardware tools, and power engineering technology.

[0116] Example 2

[0117] This embodiment provides a preparation method of an anti-corrosion coating, which includes the following steps:

[0118] S1. Dissolve the phosphatizing agent aqueous solution in DMF to obtain a phosphatizing agent / DMF solution;

[0119] S2. Add a water absorbent to the phosphatizing agent / DMF solution, then add a polysilazane solution for mixing, and perform heating and stirring under a protective gas to obtain a mixed solution;

[0120] S3. Mix 100 g of the mixed solution, 15 g of the rust preventive 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, and obtain the anticorrosive coating after mixing and grinding.

[0121] The aqueous solution of the phosphatizing agent is an aqueous solution of fluotitanic acid. The mass concentration of fluotitanic acid in the aqueous solution of fluotitanic acid is 50%. The aqueous solution of fluotitanic acid is dissolved in DMF to obtain a fluotitanic acid / DMF solution.

[0122] The mass concentration of fluotitanic acid in the fluotitanic acid / DMF solution is 5%.

[0123] In S2, add the same mass of the water absorbent anhydrous calcium chloride to the fluotitanic acid / DMF solution, store it for 24 hours, and obtain a fluotitanic acid / DMF solution with a water content of 0.05%. Add a polysilazane solution formed by mixing 100 g of polysilazane and 100 g of xylene evenly to 5 g of the fluotitanic acid / DMF solution with a water content of 0.05%. Under a protective gas, carry out heating and stirring at 80 °C for 2 h, and the stirring speed is 500 r / min to obtain a mixed solution.

[0124] The polysilazane in S2 is methyl polysilazane.

[0125] The methyl polysilazane is methylsilyl hydrogen polysilazane, and the purchase manufacturer model of the methylsilyl hydrogen polysilazane is YCP05 of Hangzhou Yuci High-Tech Materials Technology Co., Ltd.

[0126] The protective gas in S2 is nitrogen.

[0127] The rust preventive pigment in S3 is zinc phosphate.

[0128] The resin is a 30% mass concentration dichlororubber xylene solution.

[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 the anti-settling agent, 1 g of the thixotropic agent, 0.3 g of the dispersant, 0.3 g of the defoaming agent, and 0.3 g of the leveling agent.

[0131] The solvent is ethyl acetate.

[0132] The purchase source of dichlororubber in the 30% mass concentration dichlororubber xylene solution is Shenzhen Yitian Chemical Co., Ltd., and the model is E0301.

[0133] The purchase manufacturer and model of the mica are 2000-mesh wet mica of Chuzhou Baota Sericite Mining Co., Ltd.

[0134] The purchase manufacturer and model of the carbon black are Mitsubishi Carbon Black MA100 of Japan.

[0135] The CAS number of the ethyl acetate is 141-78-6.

[0136] The anti-settling agent is fumed nano-silica, and the manufacturer and model of the fumed nano-silica are Evonik Degussa fumed nano-silica R972.

[0137] The manufacturer and model of the thixotropic agent are BYK410 of BYK Chemie GmbH.

[0138] The CAS number of the dicumyl peroxide is 80-43-3.

[0139] The manufacturer and model of the dispersant are BYK163 of BYK Chemie GmbH.

[0140] The manufacturer and model of the defoamer are WSS980 of Wuse Stone New Materials (Hangzhou) Co., Ltd.

[0141] The manufacturer and model of the leveling agent are TEGO410 of Degussa.

[0142] In the second aspect of this embodiment, an anti-corrosion coating is provided, which is prepared by the preparation method of the anti-corrosion coating described above.

[0143] In the third aspect of this embodiment, an application of the anti-corrosion coating is provided, and the anti-corrosion coating is applied to the fields of petrochemical industry, traffic engineering, hardware tools, and power engineering technology.

[0144] Example 3

[0145] This embodiment provides a preparation method of an anti-corrosion coating, which includes the following steps:

[0146] S1. Dissolve the phosphatizing agent aqueous solution in DMF to obtain a phosphatizing agent / DMF solution;

[0147] S2. Add a water absorbent to the phosphatizing agent / DMF solution, then add a polysilazane solution for mixing, and carry out heating and stirring under a protective gas to obtain a mixed solution;

[0148] S3. Mix and grind 100 g of the mixed solution, 15 g of the anti-rust pigment, 10 g of the resin, 7 g of the enhancer, 3.4 g of the auxiliary agent, and 15 g of the solvent to obtain the anti-corrosion coating.

[0149] The phosphatizing agent aqueous solution is an aqueous solution of zirconium fluoride, and the mass concentration of zirconium fluoride in the aqueous solution of zirconium fluoride is 45%. The aqueous solution of zirconium fluoride is dissolved in DMF to obtain a zirconium fluoride / DMF solution.

[0150] The mass concentration of zirconium fluoride in the zirconium fluoride / DMF solution is 5%.

[0151] In the S2, an equal mass of anhydrous calcium chloride, a water absorbent, is added to the fluorozirconic acid / DMF solution and stored for 24 hours to obtain a fluorozirconic acid / DMF solution with a water content of 0.05%. 100 g of polysilazane and 100 g of xylene are added to 10 g of the fluorozirconic acid / DMF solution and mixed evenly to form a polysilazane solution. The solution is heated and stirred at 80° C. for 2 hours under protective gas, and the stirring speed is 500 r / min to obtain a mixed solution.

[0152] The polysilazane is vinyl polysilazane.

[0153] The vinyl polysilazane can be purchased from Merck Durazane in Germany. TM 1800.

[0154] The protective gas in S2 is nitrogen.

[0155] The anti-rust pigment in S3 is zinc phosphate.

[0156] The resin is a chlorinated rubber xylene solution with a mass concentration of 30%.

[0157] The reinforcing agent consists of 5g of mica and 2g of carbon black.

[0158] The auxiliary agent consists of 1.5 g of anti-settling agent, 1 g of thixotropic agent, 0.3 g of dispersant, 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 30% mass concentration chlorinated rubber xylene solution is purchased from Shenzhen Jitian Chemical Co., Ltd., model number E0301.

[0161] The mica was purchased from a manufacturer and model of 2000 mesh wet-process sericite from Chuzhou Pagoda Sericite Mining Co., Ltd.

[0162] The carbon black was purchased from Mitsubishi Carbon Black MA100 of Japan.

[0163] The CAS number of the ethyl acetate is 141-78-6.

[0164] The anti-settling agent is fumed nano-silica, and the manufacturer and model of the fumed nano-silica is Evonik Degussa fumed nano-silica R972.

[0165] The thixotropic agent was purchased from BYK410 of Germany.

[0166] The CAS number of the dicumyl peroxide is 80-43-3.

[0167] The purchased manufacturer model of the dispersant is BYK163 from BYK Chemie GmbH, Germany.

[0168] The purchased manufacturer model of the defoamer is WSS980 from Wuseshi New Materials (Hangzhou) Co., Ltd.

[0169] The purchased manufacturer model of the leveling agent is TEGO410 from Degussa GmbH, Germany.

[0170] In the second aspect of this embodiment, an anti-corrosion coating is provided, which is prepared by the preparation method of the anti-corrosion coating described above.

[0171] In the third aspect of this embodiment, an application of the anti-corrosion coating is provided, and the anti-corrosion coating is applied to the fields of petrochemical industry, transportation engineering, hardware tools, and power engineering technology.

[0172] Example 4

[0173] This embodiment provides a preparation method of an anti-corrosion coating, which includes the following steps:

[0174] S1. Dissolve the metal phosphate conversion coating agent aqueous solution in DMF to obtain a metal phosphate conversion coating agent / DMF solution;

[0175] S2. Add a water absorbent to the metal phosphate conversion coating agent / DMF solution, then add the polysilazane solution for mixing, and carry out heating and stirring under a protective gas to obtain a mixed solution;

[0176] S3. Mix and grind 100 g of the mixed solution, 15 g of the rust preventive 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.

[0177] The metal phosphate conversion coating agent aqueous solution is an aqueous solution of zirconium fluoride, and the mass concentration of zirconium fluoride in the aqueous solution of zirconium fluoride is 45%. The aqueous solution of zirconium fluoride is dissolved in DMF to obtain a zirconium fluoride / DMF solution.

[0178] The mass concentration of zirconium fluoride in the zirconium fluoride / DMF solution is 5%.

[0179] In S2, add the same mass of the water absorbent anhydrous calcium chloride to the zirconium fluoride / DMF solution, store it for 24 hours to obtain a zirconium fluoride / DMF solution with a moisture content of 0.05%. Add the polysilazane solution formed by mixing 100 g of polysilazane and 100 g of xylene evenly to 5 g of the zirconium fluoride / DMF solution with a moisture content of 0.05%. Under the protective gas, carry out heating and stirring at 80 °C for 2 h, and the stirring speed is 500 r / min to obtain a mixed solution.

[0180] The polysilazane in the polysilazane solution in S2 is a polysilazane ammonolyzed with long-chain primary amine.

[0181] The method for preparing polysilazane by aminolysis with long-chain primary amine comprises the following steps:

[0182] A1. Dissolving methylhydrogendichlorosilane in n-hexane to form a solution a, wherein the mass concentration of methylhydrogendichlorosilane in the solution a is 10%;

[0183] A2. Slowly dripping a 10% dodecylamine n-hexane solution into solution a for stirring reaction, and controlling the reaction temperature below 25°C to obtain a product, wherein the molar ratio of methylhydrogendichlorosilane to dodecylamine is 1:3.1;

[0184] A3. After filtering out the solid from the product, the product was distilled under reduced pressure to obtain a polysilazane oligomer. Under nitrogen protection, the polysilazane oligomer was heated to 150° C. to obtain a polysilazane that was aminolyzed with a long-chain primary amine.

[0185] The protective gas in S2 is nitrogen.

[0186] The anti-rust 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 consists of 5g of mica and 2g of carbon black.

[0189] The auxiliary agent consists of 1.5 g of anti-settling agent, 1 g of thixotropic agent, 0.3 g of dispersant, 0.3 g of defoaming agent and 0.3 g of leveling agent.

[0190] The solvent is ethyl acetate.

[0191] The chlorinated rubber in the 30% mass concentration chlorinated rubber xylene solution is purchased from Shenzhen Jitian Chemical Co., Ltd., model number E0301.

[0192] The mica was purchased from a manufacturer and model of 2000 mesh wet-process sericite from Chuzhou Pagoda Sericite Mining Co., Ltd.

[0193] The carbon black was purchased from 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-silica, and the manufacturer and model of the fumed nano-silica is Evonik Degussa fumed nano-silica R972.

[0196] The thixotropic agent was purchased from BYK410 of Germany.

[0197] The CAS number of the dicumyl peroxide is 80-43-3.

[0198] The purchased manufacturer model of the dispersant is BYK163 from BYK in Germany.

[0199] The purchased manufacturer model of the defoamer is WSS980 from Wuseshi New Materials (Hangzhou) Co., Ltd.

[0200] The purchased manufacturer model of the leveling agent is TEGO410 from Degussa in Germany.

[0201] In the second aspect of this embodiment, an anti-corrosion coating is provided, which is prepared by the preparation method of the anti-corrosion coating described above.

[0202] In the third aspect of this embodiment, an application of the anti-corrosion coating is provided, and the anti-corrosion coating is applied to the fields of petrochemical industry, transportation engineering, hardware tools, and power engineering technology.

[0203] Comparative Example 1

[0204] This comparative example provides a preparation method of an anti-corrosion coating, including the following steps:

[0205] S1. Dissolve the metal conversion agent aqueous solution in DMF to obtain a metal conversion agent / DMF solution;

[0206] S2. Mix and grind 100 g of a 50% mass concentration vinyl polysilazane xylene solution, 2.5 g of the metal conversion agent / DMF solution, 15 g of rust-inhibiting pigment, 10 g of resin, 7 g of reinforcing agent, 3.4 g of auxiliary agent, and 15 g of solvent to obtain the anti-corrosion coating.

[0207] The vinyl polysilazane in the vinyl polysilazane xylene solution is vinyl polysilazane.

[0208] The purchased manufacturer model of the vinyl polysilazane is Durazane 1800 from Merck in Germany. TM 1800.

[0209] The rust-inhibiting pigment is zinc phosphate.

[0210] The metal conversion agent aqueous solution is an aqueous solution of zirconium fluoride, and the mass concentration of zirconium fluoride in the aqueous solution of zirconium fluoride is 45%. The aqueous solution of zirconium fluoride is dissolved in DMF to obtain a zirconium fluoride / DMF solution.

[0211] The mass concentration of zirconium fluoride in the zirconium fluoride / DMF solution is 5%.

[0212] The resin is a 30% mass concentration chlorinated rubber xylene solution.

[0213] The reinforcing agent is composed of 5 g of mica and 2 g of carbon black.

[0214] The auxiliary agent consists of 1.5 g of anti-settling agent, 1 g of thixotropic agent, 0.3 g of dispersant, 0.3 g of defoaming agent and 0.3 g of leveling agent.

[0215] The solvent is ethyl acetate.

[0216] The chlorinated rubber in the 30% mass concentration chlorinated rubber xylene solution is purchased from Shenzhen Jitian Chemical Co., Ltd., model number E0301.

[0217] The mica was purchased from a manufacturer and model of 2000 mesh wet-process sericite from Chuzhou Pagoda Sericite Mining Co., Ltd.

[0218] The carbon black was purchased from 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-silica, and the manufacturer and model of the fumed nano-silica is Evonik Degussa fumed nano-silica R972.

[0221] The thixotropic agent was purchased from BYK410 of Germany.

[0222] The CAS number of the dicumyl peroxide is 80-43-3.

[0223] The dispersant was purchased from BYK163 of Germany.

[0224] The defoamer was purchased from WSS980 of Wusheshi New Materials (Hangzhou) Co., Ltd.

[0225] The leveling agent was purchased from Germany's TEGO410.

[0226] The second aspect of this comparative example provides an anti-corrosion coating, which is prepared by the anti-corrosion coating preparation method.

[0227] Comparative Example 2

[0228] This comparative example provides a method for preparing an anti-corrosion coating, comprising the following steps:

[0229] S1. The pottery agent aqueous solution is dissolved in DMF to obtain a pottery agent / DMF solution;

[0230] S2. An equal amount of anhydrous calcium chloride was added to the ceramic / DMF solution and stored for 24 hours to obtain a ceramic / DMF solution having a water content of 0.05%;

[0231] S3. Mix 100 g of a polysiilazane xylene solution with a mass concentration of 50%, 2.5 g of a surface treatment agent / DMF solution with a moisture content of 0.05%, 15 g of a rust preventive pigment, 10 g of a resin, 7 g of a reinforcing agent, 3.4 g of an additive, and 15 g of a solvent, and then grind them to obtain an anti-corrosion coating.

[0232] The polysiilazane in the polysiilazane xylene solution is vinylpolysiilazane.

[0233] The purchased manufacturer model of the vinylpolysiilazane is Durazane 1800 from Merck, Germany. TM 1800.

[0234] The surface treatment agent aqueous solution is a zirconium fluoride aqueous solution. The mass concentration of zirconium fluoride in the zirconium fluoride aqueous solution is 45%. The zirconium fluoride aqueous solution is dissolved in DMF to obtain a zirconium fluoride / DMF solution.

[0235] The mass concentration of zirconium fluoride in the zirconium fluoride / DMF solution is 5%.

[0236] The rust preventive pigment is zinc phosphate.

[0237] The resin is a 30% mass concentration of chlorinated rubber xylene solution.

[0238] The reinforcing agent consists of 5 g of mica and 2 g of carbon black.

[0239] The additive consists of 1.5 g of an anti-settling agent, 1 g of a thixotropic agent, 0.3 g of a dispersant, 0.3 g of an anti-foaming agent, and 0.3 g of a leveling agent.

[0240] The solvent is ethyl acetate.

[0241] The purchased source of the chlorinated rubber in the 30% mass concentration of chlorinated rubber xylene solution is Shenzhen Yitian Chemical Co., Ltd., and the model is E0301.

[0242] The purchased manufacturer and model of the mica is 2000-mesh wet-process sericite mica from Chuzhou Baota Sericite Mica Mining Co., Ltd.

[0243] The purchased manufacturer and model of the carbon black is 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-silica. The purchased manufacturer and model of the fumed nano-silica is Evonik Degussa fumed nano-silica R972.

[0246] The purchased manufacturer model of the thixotropic agent is BYK410 from BYK.

[0247] The CAS number of the dicumyl peroxide is 80-43-3.

[0248] The purchased manufacturer model of the dispersant is BYK163 from BYK Chemie Germany.

[0249] The purchased manufacturer model of the defoamer is WSS980 from Wuseshi New Materials (Hangzhou) Co., Ltd.

[0250] The purchased manufacturer model of the leveling agent is TEGO410 from Degussa Germany.

[0251] In the second aspect of this comparative example, an anti-corrosion coating is provided, which is prepared by the preparation method of the anti-corrosion coating described above.

[0252] Comparative Example 3

[0253] This comparative example provides a preparation method of an anti-corrosion coating, including the following steps:

[0254] Mix and grind 100 g of a 50% polysiilazane xylene solution, 15 g of a rust-inhibiting pigment, 10 g of a resin, 7 g of a reinforcing agent, 3.4 g of an additive, and 15 g of a solvent to obtain an anti-corrosion coating.

[0255] The polysiilazane in the polysiilazane xylene solution is vinylpolysiilazane.

[0256] The purchased manufacturer model of the vinylpolysiilazane is Durazane TM1800 from Merck Germany.

[0257] The rust-inhibiting pigment is zinc phosphate.

[0258] The resin is a 30% chlorinated rubber xylene solution.

[0259] The reinforcing agent consists of 5 g of mica and 2 g of carbon black.

[0260] The additive consists of 1.5 g of an anti-settling agent, 1 g of a thixotropic agent, 0.3 g of a dispersant, 0.3 g of a defoamer, and 0.3 g of a leveling agent.

[0261] The solvent is ethyl acetate.

[0262] The source of the chlorinated rubber in the 30% chlorinated rubber xylene solution is Shenzhen Yitian Chemical Co., Ltd., and the model is E0301.

[0263] The purchased manufacturer and model of the mica is 2000-mesh wet-ground mica from Chuzhou Baota Sericite Mining Co., Ltd.

[0264] The purchased manufacturer and model of the carbon black is Mitsubishi Carbon Black MA100 from Japan.

[0265] The CAS number of the ethyl acetate is 141-78-6.

[0266] The anti-settling agent is fumed nano-silica, and the manufacturer and model of the fumed nano-silica are Evonik Degussa fumed nano-silica R972.

[0267] The manufacturer and model of the thixotropic agent purchased are BYK410 of BYK Chemie GmbH.

[0268] The CAS number of the dicumyl peroxide is 80-43-3.

[0269] The manufacturer and model of the dispersant purchased are BYK163 of BYK Chemie GmbH.

[0270] The manufacturer and model of the defoamer purchased are WSS980 of Wuseshi New Materials (Hangzhou) Co., Ltd.

[0271] The manufacturer and model of the leveling agent purchased are TEGO410 of Degussa.

[0272] The second aspect of this comparative example provides an anti-corrosion coating, which is prepared by the preparation method of the anti-corrosion coating described above.

[0273] Comparative Example 4

[0274] This comparative example provides a preparation method of an anti-corrosion coating, including the following steps:

[0275] S1. Dissolve the zirconate aqueous solution in DMF to obtain a zirconate / DMF solution;

[0276] S2. Add a water absorbent to the zirconate / DMF solution, then add a polysilazane solution for mixing, and carry out heating and stirring under a protective gas to obtain a mixed solution;

[0277] S3. Mix and grind 100 g of the mixed solution, 15 g of an anti-rust 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;

[0278] The zirconate aqueous solution is a zirconium fluoride aqueous solution, and the mass concentration of zirconium fluoride in the zirconium fluoride aqueous solution is 45%. The zirconium fluoride aqueous solution is dissolved in DMF to obtain a zirconium fluoride / DMF solution.

[0279] The mass concentration of zirconium fluoride in the zirconium fluoride / DMF solution is 5%.

[0280] In the S2, an equal mass of anhydrous calcium chloride as a water absorbent is added to the fluorozirconic acid / DMF solution to obtain a fluorozirconic acid / DMF solution with a water content of 2%. 100 g of polysilazane and 100 g of xylene are added to 5 g of the fluorozirconic acid / DMF solution and mixed evenly to form a polysilazane solution. The mixture is heated and stirred at 80° C. for 2 h under protective gas to obtain a mixed solution.

[0281] The polysilazane is vinyl polysilazane.

[0282] The vinyl polysilazane can be purchased from Merck Durazane in Germany. TM 1800.

[0283] The protective gas in S2 is nitrogen.

[0284] The anti-rust pigment in S3 is zinc phosphate.

[0285] The resin is a chlorinated rubber xylene solution with a mass concentration of 30%.

[0286] The reinforcing agent consists of 5g of mica and 2g of carbon black.

[0287] The auxiliary agent consists of 1.5 g of anti-settling agent, 1 g of thixotropic agent, 0.3 g of dispersant, 0.3 g of defoaming agent and 0.3 g of leveling agent.

[0288] The solvent is ethyl acetate.

[0289] The chlorinated rubber in the 30% mass concentration chlorinated rubber xylene solution is purchased from Shenzhen Jitian Chemical Co., Ltd., model number E0301.

[0290] The mica was purchased from a manufacturer and model of 2000 mesh wet-process sericite from Chuzhou Pagoda Sericite Mining Co., Ltd.

[0291] The carbon black was purchased from Mitsubishi Carbon Black MA100 of Japan.

[0292] The CAS number of the ethyl acetate is 141-78-6.

[0293] The anti-settling agent is fumed nano-silica, and the manufacturer and model of the fumed nano-silica is Evonik Degussa fumed nano-silica R972.

[0294] The thixotropic agent was purchased from BYK410 of Germany.

[0295] The CAS number of the dicumyl peroxide is 80-43-3.

[0296] The dispersant was purchased from BYK163 of Germany.

[0297] The defoamer was purchased from WSS980 of Wusheshi New Materials (Hangzhou) Co., Ltd.

[0298] The leveling agent was purchased from Germany's TEGO410.

[0299] The second aspect of this comparative example provides an anti-corrosion coating, which is prepared by the anti-corrosion coating preparation method.

[0300] Comparative Example 5

[0301] This comparative example provides a method for preparing an anti-corrosion coating, comprising the following steps:

[0302] S1. The pottery agent aqueous solution is dissolved in DMF to obtain a pottery agent / DMF solution;

[0303] S2. 100 g of a 50% polysilazane xylene solution, 2.5 g of a ceramic agent / DMF solution, 15 g of an anti-rust pigment, 10 g of a resin, 7 g of a reinforcing agent, 3.4 g of an additive, and 15 g of a solvent were mixed and ground to obtain an anti-corrosion coating;

[0304] The ceramic 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 methylsilyl hydrogen polysilazane, and the manufacturer model of the methylsilyl hydrogen polysilazane is YCP05 from Hangzhou Yuanci High-tech Materials Technology Co., Ltd.

[0307] The anti-rust pigment is zinc phosphate.

[0308] The resin is a chlorinated rubber xylene solution with a mass concentration of 30%.

[0309] The reinforcing agent consists of 5g of mica and 2g of carbon black.

[0310] The auxiliary agent consists of 1.5 g of anti-settling agent, 1 g of thixotropic agent, 0.3 g of dispersant, 0.3 g of defoaming agent and 0.3 g of leveling agent.

[0311] The solvent is ethyl acetate.

[0312] The chlorinated rubber in the 30% mass concentration chlorinated rubber xylene solution is purchased from Shenzhen Jitian Chemical Co., Ltd., model number E0301.

[0313] The mica was purchased from Chuzhou Baota Sericite Mining Co., Ltd. and is 2000-mesh wet sericite.

[0314] The carbon black was purchased from Mitsubishi Chemical Carbon Black MA100, Japan.

[0315] The CAS number of ethyl acetate is 141-78-6.

[0316] The anti-settling agent is fumed nano-silica, which was purchased from Evonik Degussa fumed nano-silica R972.

[0317] The thixotropic agent was purchased from BYK Chemie GmbH BYK410, Germany.

[0318] The CAS number of dicumyl peroxide is 80-43-3.

[0319] The dispersant was purchased from BYK Chemie GmbH BYK163, Germany.

[0320] The defoaming agent was purchased from Wuseshi New Materials (Hangzhou) Co., Ltd. WSS980.

[0321] The leveling agent was purchased from Degussa TEGO410, Germany.

[0322] In the second aspect of this comparative example, an anti-corrosion coating is provided, which is prepared by the preparation method of the anti-corrosion coating described above.

[0323] Comparative Example 6

[0324] This comparative example provides a preparation method of an anti-corrosion coating, including the following steps:

[0325] S1. Dissolve the phosphatizing agent aqueous solution in DMF to obtain a phosphatizing agent / DMF solution. Add a water absorbent to the phosphatizing agent / DMF solution and store it for 24 hours to obtain a phosphatizing agent / DMF solution with a water content of 0.05%.

[0326] S2. Mix and grind 100 g of a 50% mass concentration of polysilazane xylene solution, 2.5 g of a phosphatizing agent / DMF solution with a water content of 0.05%, 15 g of a rust preventive 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 phosphatizing agent aqueous solution is an aqueous solution of fluotitanic acid. The mass concentration of fluotitanic acid in the aqueous solution of fluotitanic acid is 50%. The aqueous solution of fluotitanic acid is dissolved in DMF to obtain a fluotitanic acid / DMF solution.

[0328] The mass concentration of fluotitanic acid in the fluotitanic acid / DMF solution is 5%.

[0329] In the polysiilazane xylene solution, the polysilazane is methylsilyl hydrogen polysilazane, and the purchased manufacturer model of the methylsilyl hydrogen polysilazane is YCP05 of Hangzhou Yuci High-Tech Materials Technology Co., Ltd.

[0330] The rust preventive pigment is zinc phosphate.

[0331] The resin is a 30% mass concentration dichlororubber xylene solution.

[0332] The reinforcing agent consists of 5 g of mica and 2 g of carbon black.

[0333] The auxiliary agent consists of 1.5 g of anti-settling agent, 1 g of thixotropic agent, 0.3 g of dispersant, 0.3 g of defoaming agent and 0.3 g of leveling agent.

[0334] The solvent is ethyl acetate.

[0335] The purchased source of dichlororubber in the 30% mass concentration dichlororubber xylene solution is Shenzhen Yitian Chemical Co., Ltd., and the model is E0301.

[0336] The purchased manufacturer and model of the mica is 2000-mesh wet-process sericite mica of Chuzhou Pagoda Sericite Mining Co., Ltd.

[0337] The purchased manufacturer and model of the carbon black is 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-silica, and the purchased manufacturer and model of the fumed nano-silica is Evonik Degussa fumed nano-silica R972.

[0340] The purchased manufacturer model of the thixotropic agent is BYK410 of BYK.

[0341] The CAS number of dicumyl peroxide is 80-43-3.

[0342] The purchased manufacturer model of the dispersant is BYK163 of BYK.

[0343] The purchased manufacturer model of the defoaming agent is WSS980 of Wuseshi New Materials (Hangzhou) Co., Ltd.

[0344] The purchased manufacturer model of the leveling agent is TEGO410 of Degussa.

[0345] In the second aspect of this comparative example, an anti-corrosion coating is provided, which is prepared by the preparation method of the anti-corrosion coating described above.

[0346] Comparative Example 7

[0347] This comparative example provides a method for preparing an anti-corrosion coating, comprising the following steps:

[0348] 100 g of a polysilazane xylene solution with a mass concentration of 50%, 15 g of an anti-rust 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 were mixed and ground to obtain an anti-corrosion coating.

[0349] The polysilazane in the polysilazane xylene solution is methylsilyl hydrogen polysilazane, and the methylsilyl hydrogen polysilazane is purchased from the YCP05 methyl polysilazane of Hangzhou Yuanci High-tech Materials Technology Co., Ltd.

[0350] The anti-rust pigment is zinc phosphate.

[0351] The resin is a chlorinated rubber xylene solution with a mass concentration of 30%.

[0352] The reinforcing agent consists of 5g of mica and 2g of carbon black.

[0353] The auxiliary agent consists of 1.5 g of anti-settling agent, 1 g of thixotropic agent, 0.3 g of dispersant, 0.3 g of defoaming agent and 0.3 g of leveling agent.

[0354] The solvent is ethyl acetate.

[0355] The chlorinated rubber in the 30% mass concentration chlorinated rubber xylene solution is purchased from Shenzhen Jitian Chemical Co., Ltd., model number E0301.

[0356] The mica was purchased from a manufacturer and model of 2000 mesh wet-process sericite from Chuzhou Pagoda Sericite Mining Co., Ltd.

[0357] The carbon black was purchased from Mitsubishi Carbon Black MA100 of Japan.

[0358] The CAS number of the ethyl acetate is 141-78-6.

[0359] The anti-settling agent is fumed nano-silica, and the manufacturer and model of the fumed nano-silica is Evonik Degussa fumed nano-silica R972.

[0360] The thixotropic agent was purchased from BYK410 of Germany.

[0361] The CAS number of the dicumyl peroxide is 80-43-3.

[0362] The dispersant was purchased from BYK163 of Germany.

[0363] The defoamer was purchased from WSS980 of Wusheshi New Materials (Hangzhou) Co., Ltd.

[0364] The purchased manufacturer model of the leveling agent is Degussa TEGO410 from Germany.

[0365] This comparative example provides an anti-corrosion coating in the second aspect, which is prepared by the preparation method of the anti-corrosion coating described above.

[0366] Comparative Example 8

[0367] This comparative example provides a preparation method of an anti-corrosion coating, including the following steps:

[0368] S1. Dissolve the phosphatizing agent aqueous solution in DMF to obtain a phosphatizing agent / DMF solution;

[0369] S2. Mix and grind 167 g of inorganic ceramic resin, 5 g of phosphatizing 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 defoamer, and 0.3 g of leveling agent to obtain an anti-corrosion coating;

[0370] The phosphatizing agent aqueous solution is a zirconium fluoride aqueous solution, and the mass concentration of zirconium fluoride in the zirconium fluoride aqueous solution is 45%. The zirconium fluoride aqueous solution is dissolved in DMF to obtain a zirconium fluoride / DMF solution.

[0371] The mass concentration of zirconium fluoride in the zirconium fluoride / DMF solution is 5%.

[0372] The purchased manufacturer model 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 purchased manufacturer and model of the mica are 2000-mesh wet-process sericite from Chuzhou Baota Sericite Mining Co., Ltd.

[0375] The purchased manufacturer and model of the carbon black are Mitsubishi Carbon Black MA100 from Japan.

[0376] The purchased manufacturer and model of the nano-silica anti-settling agent are Evonik Degussa Aerosil nano-silica A200.

[0377] The purchased manufacturer and model of the modified urea solution anti-settling agent are BYK410 modified urea solution anti-settling agent from BYK Chemie GmbH, Germany.

[0378] The purchased manufacturer model of the dispersant is BYK163 from BYK Chemie GmbH, Germany.

[0379] The purchased manufacturer model of the defoamer is WSS980 from Wuseshi New Materials (Hangzhou) Co., Ltd.

[0380] The purchased manufacturer model of the leveling agent is Degussa TEGO410 from Germany.

[0381] In the second aspect of this comparative example, an anti-corrosion coating is provided, which is prepared by the preparation method of the anti-corrosion coating described above.

[0382] In the above-mentioned examples and comparative examples, the moisture content was measured using a Shanghai Anting Electronics ZSD-2J Karl Fischer moisture analyzer.

[0383] Performance testing

[0384] Sample preparation: The anti-corrosion coatings provided in Examples 1-4 and Comparative Examples 1-8 were added to a double-layer dispersion tank, dispersed with supercooled water for 30 minutes at a dispersion speed of 1500 r / min. After the slurry was sieved through a 100-mesh sieve, it was sprayed on sandblasted Q235 carbon steel, and after baking, a coating with a thickness of 25 μm was obtained, and pencil hardness testing, adhesion testing, and salt spray performance testing were carried out respectively; the results of pencil hardness testing and adhesion testing are shown in Table 1, and the results of salt spray performance testing are shown in Table 2.

[0385] The Q235 carbon steel was surface-cleaned by sandblasting to Sa3 level.

[0386] The anti-corrosion coatings provided in Examples 1-4 and Comparative Examples 1-8 were baked under the conditions of baking at 200 °C for 40 minutes.

[0387] The pencil hardness test was carried out using the standard method of GB 6739—86 "Pencil Hardness Test for Film Hardness".

[0388] The adhesion test was carried out using the standard method of GB / T 9286-1998 "Cross-Cut Test for Paints and Varnishes - Film".

[0389] The salt spray performance test was carried out using the standard method of GB / T10125-2012 "Artificial Atmosphere Corrosion Test - Salt Spray Test". In the test results, when the surface is uniform and there is no corrosion, it is evaluated as A; when local pitting corrosion appears, it is evaluated as B; when large-area corrosion appears, it is evaluated as C.

[0390] The state when the coating surface is uniform and there is no corrosion during the salt spray performance test is shown in Figure 1 .

[0391] The state when local pitting corrosion appears on the coating 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 with a red frame for display.

[0392] Table 1

[0393] Example Pencil hardness Adhesion Example 1 4H Grade 0 Example 2 4H Grade 0 Example 3 4H Grade 0 Example 4 4H Grade 0 Comparative Example 1 4H Grade 0 Comparative Example 2 4H Grade 0 Comparative Example 3 4H Grade 0 Comparative Example 4 4H Grade 0 Comparative Example 5 4H Grade 0 Comparative Example 6 4H Grade 0 Comparative Example 7 4H Grade 0 Comparative Example 8 5H Grade 0

[0394] As can be seen from the test results in Table 1, the anti-corrosion coatings provided in Examples 1-4 and Comparative Examples 1-8 have good adhesion and pencil hardness.

[0395] Table 2

[0396]

[0397]

[0398] Note: " / " in Table 2 indicates not detected. When the surface is uniformly consistent without any corrosion, it is evaluated as A; when local pitting corrosion appears, it is evaluated as B; when large-area corrosion appears, it is evaluated as C.

[0399] As can be seen from the test results in Table 2, for the anti-corrosion coatings provided in Examples 1, 2, 3, and 4, after the treatment with the phosphatizing agent / DMF solution for water removal, pre-reaction with polysilazane, and then compounding with rust-inhibiting pigments, fillers, and additives, the salt spray resistance of the obtained anti-corrosion coatings can reach 1700 h, and no irregular pitting corrosion occurs. Pitting corrosion does not occur until 1700 hours. It can be seen from Example 2 that the salt spray performance of the anti-corrosion coating obtained in Example 2 is worse than that of the anti-corrosion coating obtained in Example 1. From the long-term practical experience of the inventor, this is due to different polysilazanes. Examples 1 and Comparative Examples 1-4 all use vinyl polysilazane, Examples 2 and Comparative Examples 5-7 all use methylsilylhydride polysilazane, Example 3 uses vinyl polysilazane, and Example 4 uses polysilazane ammonolyzed with long-chain primary amine. By using specific polysilazane in the preparation method of the anti-corrosion coating provided in this application, the salt spray performance of the anti-corrosion coating can be improved. It can be seen from Example 2 compared with Comparative Examples 5, 6, and 7 that when the phosphatizing agent / DMF solution, polysilazane solution, and rust-inhibiting pigment are combined in Example 2, by controlling the water content of the phosphatizing agent / DMF solution and mixing the phosphatizing agent / DMF solution and polysilazane solution to obtain a mixed solution, the salt spray performance of the formed anti-corrosion coating is good.

[0400] As can be seen from the test results in Table 2, for the anti-corrosion coating provided in Comparative Example 1, during the preparation process, the phosphatizing agent / DMF solution was not treated for water removal, and the phosphatizing agent / DMF solution and polysilazane were not reacted to obtain a reaction solution, but only a simple mixture was made. As can be seen from the test results in Table 1, when the anti-corrosion coating provided in Comparative Example 1 was sprayed on sandblasted Q235 carbon steel and then subjected to a salt spray test, irregularly distributed local pitting corrosion would occur at 2000 h.

[0401] As can be seen from the test results in Table 2, for the anti-corrosion coating provided in Comparative Example 2, although the water content in the phosphatizing agent / DMF solution was controlled during the preparation process, the phosphatizing agent / DMF solution and the polysilazane solution were not used to react to obtain a reaction solution, but only a simple mixture was made. In Comparative Example 2, the phosphatizing agent / DMF solution and polysilazane were directly mixed. As a result, when the obtained anti-corrosion coating was sprayed on sandblasted Q235 carbon steel and then subjected to a salt spray test, irregularly distributed local pitting corrosion occurred at 2000 h.

[0402] As can be seen from the test results in Table 2, when the anti-corrosion coating provided in Comparative Example 3 did not use the phosphatizing agent / DMF solution, the polysilazane solution and the rust-inhibiting pigment in combination, when the obtained anti-corrosion coating was sprayed on sandblasted Q235 carbon steel and then subjected to a salt spray test, large-area corrosion occurred at 400 h. This also shows the crucial role of IVB group element-modified polysilazane in improving the salt spray resistance of polysilazane on carbon steel.

[0403] As can be seen from the test results in Table 2, when the anti-corrosion coating provided in Comparative Example 4 used a phosphatizing agent / DMF solution with a water content greater than 0.1% and a polysilazane solution in combination, local pitting corrosion occurred during the salt spray performance test of the anti-corrosion coating. This also verifies the key influence of the water content on the hydrolysis of the silicon-nitrogen bond proposed by the inventor, thereby further affecting the salt spray test results.

[0404] As can be seen from the test results in Table 2, for the anti-corrosion coating provided in Comparative Example 8, an inorganic ceramic resin was used. Compared with the anti-corrosion coating obtained using polysilazane, the salt spray resistance of the anti-corrosion coating provided in Comparative Example 8 was poor.

Claims

1. A method for preparing an anti-corrosion coating, characterized in that: The following steps are involved: S1. The pottery agent aqueous solution is dissolved in DMF to obtain a pottery agent / DMF solution; S2. A water absorbent is added to the ceramic / DMF solution to obtain a ceramic / DMF solution having a water content of <0.1%, and then the polysilazane solution is added and mixed, and heated and stirred under a protective gas to obtain a mixed solution; S3. The mixed solution, anti-rust pigment, resin, reinforcing agent, additive, solvent are mixed and ground to obtain an anti-corrosion coating; The ceramic aqueous solution is an aqueous solution of a ceramic element of group IVB.

2. The method for preparing the anticorrosive coating according to claim 1, characterized in that: The aqueous solution of the Group IVB element ceramic agent includes a combination of one or more of an aqueous solution of hafnic acid fluoroacid, an aqueous solution of fluorotitanic acid, and an aqueous solution of fluorozirconic acid.

3. The method for preparing the anticorrosive coating according to claim 1, characterized in that: In the step S2, an equal amount of water absorbent is added to the ceramic agent / DMF solution to obtain a ceramic agent / DMF solution with a water content of less than 0.1%.

4. The method for preparing the anticorrosive coating according to claim 1, characterized in that: The water absorbent in S2 includes one or more combinations of anhydrous calcium chloride, water-absorbing silica gel, and molecular sieves.

5. The method for preparing the anticorrosive coating according to claim 1, characterized in that: The polysilazane in S2 includes one or more of methyl polysilazane, perhydro polysilazane, vinyl polysilazane, or polysilazane ammonolyzed with ammonia gas or ammonolyzed with long-chain primary amine.

6. The method for preparing the anticorrosive coating according to claim 5, characterized in that: The method for preparing polysilazane by aminolysis with long-chain primary amine comprises the following steps: A1. dissolving methylsilane in a solvent to form a solution a; A2. Add a primary amine to solution a and stir to react to obtain a product; A3. After filtering out the solid from the product, the product was distilled under reduced pressure to obtain a polysilazane oligomer, which was heated under nitrogen to obtain a polysilazane aminolyzed with a long-chain primary amine; The number of carbon atoms in the primary amine is greater than 10.

7. The method for preparing the anticorrosive coating according to claim 1, characterized in that: The protective gas in S2 includes argon and nitrogen.

8. The method for preparing the anticorrosive coating according to claim 1, characterized in that: The anti-rust pigment in S3 includes one or more combinations of zinc phosphomolybdate, aluminum phosphate, zinc phosphate, and aluminum phosphomolybdate.

9. An anti-corrosion coating, characterized in that: The anti-corrosion coating is prepared by the preparation method of the anti-corrosion coating according to any one of claims 1 to 8.

10. Use of the anti-corrosion coating according to claim 9, characterized in that: The anti-corrosion coating is applied to the fields of petrochemical industry, traffic engineering, hardware tools, and electric power engineering technology.

Images