A high-temperature resistant waterproof coating and its preparation method

Abstract

The present invention relates to a high temperature resistant waterproof coating and a preparation method thereof, and relates to the technical field of coatings. The high temperature resistant waterproof coating comprises the following components by weight: 45 to 55 parts of an organosilicon resin base material, 0.5 to 1.5 parts of a dispersant, 0.2 to 0.8 parts of a wetting agent, 10 to 20 parts of a modified filler, 0.1 to 0.5 parts of a drying agent, and 18 to 26 parts of a solvent; the organosilicon resin base material is obtained by subjecting a methylphenyl silicone resin and a methyl MQ silicone resin in a weight ratio of (79 to 86): (8 to 15) to oxygen-enriched microwave plasma composite treatment. The present invention forms an organosilicon resin-based system by subjecting a suitable proportion of methylphenyl silicone resin and methyl MQ silicone resin to oxygen-enriched microwave plasma composite treatment, and at the same time cooperates with a specific modified filler, which not only significantly improves the high temperature resistance of the coating, but also realizes the curing of the organosilicon coating under medium and low temperature conditions, making up for the shortcomings of the prior art.

Description

Technical Field

[0001] The present invention relates to the technical field of coatings, and in particular to a high temperature resistant waterproof coating and a preparation method thereof. Background Art

[0002] In today's rapidly developing technological era, especially in special fields such as aerospace and high-temperature industrial manufacturing, extremely stringent requirements are placed on the high-temperature resistance of materials. In these extreme environments, in order to withstand the test of high temperatures, equipment materials often need to be protected with high-temperature resistant coatings to ensure the safety and durability of the protected substrate.

[0003] Organosilicon coatings have always been a research hotspot in the field of high-temperature resistant coatings due to their unique molecular structure and chemical properties. Organosilicon resins have become an important raw material for the preparation of high-temperature resistant coatings due to their excellent heat resistance, weather resistance and chemical stability. However, the temperature resistance range of organosilicon high-temperature resistant coatings currently on the market is generally limited to 500-700°C, and it is difficult to maintain the integrity and stability of the coating under higher temperature conditions. At the same time, this type of coating often requires a baking temperature of up to 150-250°C during the curing process, which increases the difficulty and cost of construction. Therefore, the development of a high-temperature resistant coating that meets higher temperature protection requirements such as aerospace and has good low-temperature curing performance has important market value and significance. Summary of the invention

[0004] In order to solve the above problems, the present invention provides a high temperature resistant waterproof coating and a preparation method thereof.

[0005] In a first aspect, the present invention provides a high temperature resistant waterproof coating, which comprises the following components in parts by weight:

[0006] 45-55 parts of silicone resin base material, 0.5-1.5 parts of dispersant, 0.2-0.8 parts of wetting agent, 10-20 parts of modified filler, 0.1-0.5 parts of drying agent and 18-26 parts of solvent;

[0007] The organic silicone resin base material is obtained by subjecting methyl phenyl silicone resin and methyl MQ silicone resin in a weight ratio of (79-86):(8-15) to oxygen-enriched microwave plasma composite treatment;

[0008] The modified filler is obtained by modifying sericite powder, quartz powder, titanium dioxide and silicon dioxide aerogel powder with a silane coupling agent.

[0009] Furthermore, the high temperature resistant waterproof coating comprises the following components in parts by weight:

[0010] 48.5 parts of silicone resin base material, 1.0 part of dispersant, 0.5 part of wetting agent, 16 parts of modified filler, 0.3 part of dryer, and 22 parts of solvent.

[0011] Further, the preparation method of the silicone resin base material includes the following process:

[0012] Mix methylphenyl silicone resin and methyl MQ silicone resin to obtain a first mixture;

[0013] Add the first mixture into a microwave plasma treatment instrument for oxygen-rich microwave plasma composite treatment for 45 - 90 seconds, and then continue to introduce oxygen for 5 - 10 minutes to obtain the silicone resin base material;

[0014] Among them, the working condition parameters of the microwave plasma treatment instrument include: the discharge mode is glow discharge, the working medium is composed of oxygen and argon with a volume ratio of 10:1, the intake air volume is 55 - 75 mL / min, and the microwave power is 240 - 350 W.

[0015] Further, the weight ratio of the methylphenyl silicone resin to the methyl MQ silicone resin is 83:11.

[0016] Further, the preparation method of the modified filler includes the following process:

[0017] Add sericite powder, quartz powder, titanium dioxide powder, and silica aerogel powder into an aqueous solution of silane coupling agent with a mass fraction of 15 - 20% for heating and stirring to mix. After the water evaporates completely, perform vacuum drying and grinding and sieving to obtain the modified filler.

[0018] Further, the weight ratio of the sericite powder, the quartz powder, the titanium dioxide powder, the silica aerogel powder, and the aqueous solution of silane coupling agent is (7 - 11):(2 - 5):(1 - 3):(0.5 - 1.5):(10 - 15);

[0019] The working condition parameters of the heating and stirring to mix include: the temperature is 80 - 90 °C, and the stirring speed is 200 - 300 rpm.

[0020] Further, the weight ratio of the sericite powder, the quartz powder, the titanium dioxide powder, the silica aerogel powder, and the aqueous solution of silane coupling agent is 9:3:2:1:12.

[0021] Further, the dryer includes at least one of cobalt isooctanoate and manganese isooctanoate; the solvent includes water.

[0022] In a second aspect, the present invention provides a preparation method of the high-temperature resistant waterproof coating according to any one of the first aspect, and the preparation method includes the following steps:

[0023] Stir and mix silicone resin base material, dispersant, wetting agent and solvent to obtain a second mixture;

[0024] Add modified filler and dryer to the second mixture in sequence and stir and mix to obtain the high-temperature resistant waterproof coating.

[0025] The above technical solution provided by the embodiment of the present invention has at least the following advantages compared with the prior art:

[0026] The embodiment of the present invention provides a high-temperature resistant waterproof coating. In the present invention, an organosilicon resin base system is formed by subjecting a methylphenyl silicone resin and a methyl MQ silicone resin in an appropriate proportion to an oxygen-rich microwave plasma composite treatment. At the same time, in combination with specific modified fillers, not only the high-temperature resistance of the coating is significantly improved, but also the curing of the organosilicon-based coating under medium and low temperature conditions is realized, making up for the deficiencies of the prior art. Specifically:

[0027] 1) Composite treatment of organosilicon resin base material: In the present invention, a methylphenyl silicone resin and a methyl MQ silicone resin in an appropriate proportion are used as the base material for oxygen-rich microwave plasma composite treatment to promote the cross-linking and fusion between the two resin molecules, forming a denser and more stable network structure. It not only retains the high-temperature stability of the methylphenyl silicone resin, but also incorporates the easy processing characteristics of the methyl MQ silicone resin, realizing the complementarity of the two in terms of heat resistance, mechanical strength and chemical stability, thereby improving the high-temperature resistance and low-temperature curing performance of the organosilicon resin matrix.

[0028] 2) Synergistic strengthening effect of modified fillers: Sericite powder, quartz powder, titanium dioxide powder and silica aerogel powder itself have good heat resistance, hardness and chemical stability. After being modified by silane coupling agent, the interfacial defects between the filler and the organosilicon resin base material are reduced, the compatibility with the organosilicon resin base material is enhanced, and it can be more uniformly dispersed in the organosilicon resin base material, forming a denser coating structure, enabling the filler to more effectively play its promoting role in improving the heat resistance, hardness, etc. of the coating.

[0029] In summary, the high-temperature resistant waterproof coating provided by the present invention realizes the stability of the coating in a high-temperature environment and the curability under medium and low temperature conditions through the composite treatment of the organosilicon resin base material, the synergistic effect of the modified filler and the precise ratio of other components. This multi-level synergistic mechanism not only significantly improves the comprehensive performance of the coating, but also makes up for the deficiencies of the prior art in the curing conditions of high-temperature resistant coatings, broadening the application range of organosilicon-based high-temperature resistant coatings. Specific embodiments

[0030] To make the objectives, technical solutions, and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be described clearly and completely below. Apparently, the described embodiments are only a part rather than all of the embodiments of the present invention. All other embodiments obtained by those of ordinary skill in the art based on the embodiments of the present invention without creative efforts shall fall within the scope of protection of the present invention.

[0031] Unless otherwise specifically stated, all kinds of raw materials, reagents, instruments, equipment, etc. used in the present invention can be obtained through market purchases or can be prepared by existing methods.

[0032] In a first aspect, the present invention provides a high-temperature resistant waterproof coating. Calculated by weight parts, the high-temperature resistant waterproof coating comprises the following components:

[0033] 45 - 55 parts of organosilicon resin base material, 0.5 - 1.5 parts of dispersant, 0.2 - 0.8 parts of wetting agent, 10 - 20 parts of modified filler, 0.1 - 0.5 parts of dryer, and 18 - 26 parts of solvent;

[0034] The organosilicon resin base material is obtained by subjecting methylphenyl silicone resin and methyl MQ silicone resin with a weight ratio of (79 - 86):(8 - 15) to oxygen-enriched microwave plasma composite treatment;

[0035] The modified filler is obtained by modifying sericite powder, quartz powder, titanium dioxide powder, and silica aerogel powder with a silane coupling agent.

[0036] The embodiments of the present invention provide a high-temperature resistant waterproof coating. The present invention forms an organosilicon resin base system by subjecting methylphenyl silicone resin and methyl MQ silicone resin in an appropriate ratio to oxygen-enriched microwave plasma composite treatment, and at the same time, in combination with a specific modified filler, not only significantly improves the high-temperature resistance of the coating, but also realizes the curing of organosilicon coatings under medium and low temperature conditions, making up for the deficiencies of the prior art.

[0037] In the present invention, methylphenyl silicone resin is a type of organosilicon resin containing methyl and phenyl groups, and specifically, commercially available products such as Wacker's IC 900, Wacker's MP 50, etc. can be directly used, and preferably Wacker's MP 50.

[0038] In the present invention, methyl MQ silicone resin is a new type of organosilicon polymer material with a three-dimensional (non-linear) structure formed by a Si - O bond as the backbone of its molecules. Specifically, commercially available products such as YL - MQ102 from Laiyang Yulin Chemical Co., Ltd., SI - MQ102 from Laiyang Shengbang Organosilicon Technology Co., Ltd., etc. can be directly used, and preferably YL - MQ102 from Laiyang Yulin Chemical Co., Ltd.

[0039] In some specific embodiments, commercially available products such as BYK-103 and BYK-110 can be directly selected as the dispersant; commercially available products such as HY-352 can be directly used as the wetting agent.

[0040] In some specific embodiments, based on parts by weight, the high-temperature resistant waterproof coating comprises the following components:

[0041] 48.5 parts of silicone resin base material, 1.0 part of dispersant, 0.5 part of wetting agent, 16 parts of modified filler, 0.3 part of drier, and 22 parts of solvent.

[0042] In some specific embodiments, the preparation method of the silicone resin base material comprises the following process:

[0043] Mix methylphenyl silicone resin and methyl MQ silicone resin to obtain a first mixture.

[0044] Add the first mixture into a microwave plasma treatment instrument for oxygen-rich microwave plasma composite treatment for 45 - 90 seconds, and then continue to introduce oxygen for 5 - 10 minutes to obtain the silicone resin base material.

[0045] Among them, the working condition parameters of the microwave plasma treatment instrument include: the discharge mode is glow discharge, the working medium is composed of oxygen and argon with a volume ratio of 10:1, the intake air volume is 55 - 75 mL / min, and the microwave power is 240 - 350 W.

[0046] In some specific embodiments, the weight ratio of the methylphenyl silicone resin to the methyl MQ silicone resin is 83:11.

[0047] In some specific embodiments, the preparation method of the modified filler comprises the following process:

[0048] Add sericite powder, quartz powder, titanium dioxide powder, and silica aerogel powder into an aqueous solution of silane coupling agent with a mass fraction of 15 - 20% for heating and stirring and mixing. After the water has evaporated completely, perform vacuum drying and grinding and sieving to obtain the modified filler.

[0049] In some specific embodiments, commercially available silane coupling agents such as KH560 and KH570 can be directly selected.

[0050] In some specific embodiments, the weight ratio of the sericite powder, the quartz powder, the titanium dioxide powder, the silica aerogel powder, and the aqueous solution of silane coupling agent is (7 - 11):(2 - 5):(1 - 3):(0.5 - 1.5):(10 - 15);

[0051] The working condition parameters of the heating and stirring mixing include: the temperature is 80 - 90 °C, and the stirring speed is 200 - 300 rpm.

[0052] In some specific embodiments, the weight ratio of the sericite powder, the quartz powder, the titanium dioxide powder, the silica aerogel powder, and the silane coupling agent aqueous solution is 9:3:2:1:12.

[0053] In some specific embodiments, the drier includes at least one of cobalt isooctanoate and manganese isooctanoate; the solvent includes water.

[0054] In a second aspect, based on the same inventive concept, the present invention provides a preparation method of the high-temperature resistant waterproof coating according to any one of the first aspect, and the preparation method includes the following steps:

[0055] Stir and mix the silicone resin base material, the dispersant, the wetting agent, and the solvent to obtain a second mixture;

[0056] Add the modified filler and the drier to the second mixture in sequence and stir and mix to obtain the high-temperature resistant waterproof coating.

[0057] The preparation method of the high-temperature resistant waterproof coating provided by the present invention is realized based on the high-temperature resistant waterproof coating according to any one of the first aspect. Therefore, it has at least the beneficial effects of the high-temperature resistant waterproof coating according to any one of the first aspect, which will not be elaborated one by one here.

[0058] It should be noted that for the component raw materials involved in the high-temperature resistant waterproof coating and its preparation method provided in the embodiments of the present invention, without special limitations or specific descriptions, commercially available products can be directly used or prepared by existing public preparation methods. For example, the silica aerogel powder can directly use commercially available products such as the silica aerogel powder produced by Anhui Ke'ang Nano Technology Co., Ltd. or Qingguan Nano Technology (Jiangsu) Co., Ltd.; meanwhile, for the steps and parameters involved, without special limitations or specific descriptions, they can be carried out according to the processing technology of existing coatings or directly use existing equipment, which will not be elaborated one by one in this invention document.

[0059] The following will further elaborate the present invention with specific embodiments. It should be understood that these embodiments are only used to illustrate the present invention and not to limit the scope of the present invention. The experimental methods without specific conditions noted in the following embodiments are usually determined according to national standards. If there is no corresponding national standard, they are carried out according to general international standards, conventional conditions, or the conditions recommended by the manufacturer.

[0060] The information of some raw materials involved in the following examples and comparative examples is as follows:

[0061] Methylphenyl silicone resin: from Wacker MP 50.

[0062] Methyl MQ silicone resin: YL-MQ102 from Laiyang Yulin Chemical Co., Ltd.

[0063] Dispersant: BYK-103.

[0064] Wetting agent: HY-352.

[0065] Drying agent: cobalt isooctanoate.

[0066] Solvent: water.

[0067] Silane coupling agent: KH560.

[0068] Example 1

[0069] This example provides a high-temperature resistant waterproof coating. In parts by weight, the high-temperature resistant waterproof coating comprises the following components:

[0070] 48.5 parts of organosilicon resin base material, 1.0 part of dispersant, 0.5 part of wetting agent, 16 parts of modified filler, 0.3 part of drying agent and 22 parts of solvent;

[0071] The organosilicon resin base material is obtained by subjecting methylphenyl silicone resin and methyl MQ silicone resin with a weight ratio of 83:11 to oxygen-rich microwave plasma composite treatment;

[0072] The modified filler is obtained by modifying sericite powder, quartz powder, titanium dioxide powder and silica aerogel powder with a silane coupling agent.

[0073] The preparation method of the above high-temperature resistant waterproof coating comprises the following steps:

[0074] Step (1): Mix methylphenyl silicone resin and methyl MQ silicone resin to obtain a first mixture; add the first mixture into a microwave plasma treatment instrument for oxygen-rich microwave plasma composite treatment for 65 seconds, and then continue to introduce oxygen for 8 minutes to obtain the organosilicon resin base material; wherein, the working condition parameters of the microwave plasma treatment instrument include: the discharge mode is glow discharge, the working medium is composed of oxygen and argon with a volume ratio of 10:1, the intake air volume is 65 mL / min, and the microwave power is 290 W;

[0075] Step (2): Add sericite powder, quartz powder, titanium dioxide powder and silica aerogel powder into an aqueous solution of silane coupling agent with a mass fraction of 18%, heat and stir to mix. After the water has evaporated completely, conduct vacuum drying and grinding through a 200-mesh sieve to obtain the modified filler. Among them, the weight ratio of the sericite powder, the quartz powder, the titanium dioxide powder, the silica aerogel powder and the aqueous solution of silane coupling agent is 9:3:2:1:12. The working condition parameters of the heating and stirring mixture include: the temperature is 86°C and the stirring speed is 260 rpm.

[0076] Step (3): Stir and mix the organosilicon resin base material, dispersant, wetting agent and solvent obtained in step (1), with a stirring speed of 600 rpm and a stirring time of 15 minutes to obtain a second mixture.

[0077] Step (4): Sequentially add the modified filler and drier obtained in step (2) to the second mixture obtained in step (3), stir and mix with a stirring speed of 800 rpm and a stirring time of 20 minutes to obtain the high-temperature resistant waterproof coating.

[0078] Example 2

[0079] This example provides a high-temperature resistant waterproof coating. Calculated by weight parts, the high-temperature resistant waterproof coating comprises the following components:

[0080] 45 parts of organosilicon resin base material, 0.5 part of dispersant, 0.2 part of wetting agent, 10 parts of modified filler, 0.1 part of drier and 18 parts of solvent;

[0081] The organosilicon resin base material is obtained by subjecting methylphenyl silicone resin and methyl MQ silicone resin with a weight ratio of 79:8 to oxygen-rich microwave plasma composite treatment.

[0082] The modified filler is obtained by modifying sericite powder, quartz powder, titanium dioxide powder and silica aerogel powder with a silane coupling agent.

[0083] The preparation method of the above high-temperature resistant waterproof coating comprises the following steps:

[0084] Step (1): Mix methylphenyl silicone resin and methyl MQ silicone resin to obtain a first mixture. Add the first mixture into a microwave plasma treatment instrument for oxygen-rich microwave plasma composite treatment for 45 seconds, and then continue to introduce oxygen for 10 minutes to obtain the organosilicon resin base material. Among them, the working condition parameters of the microwave plasma treatment instrument include: the discharge mode is glow discharge, the working medium is composed of oxygen and argon with a volume ratio of 10:1, the intake air volume is 75 mL / min, and the microwave power is 350 W.

[0085] Step (2): Add sericite powder, quartz powder, titanium dioxide powder and silica aerogel powder into an aqueous solution of silane coupling agent with a mass fraction of 20%, heat and stir to mix. After the water has completely evaporated, perform vacuum drying and grinding through a 200-mesh sieve to obtain the modified filler. Among them, the weight ratio of the sericite powder, the quartz powder, the titanium dioxide powder, the silica aerogel powder and the aqueous solution of silane coupling agent is 7:2:1:0.5:10. The working condition parameters of the heating and stirring mixture include: the temperature is 86 °C and the stirring speed is 260 rpm.

[0086] Step (3): Stir and mix the organosilicon resin base material, dispersant, wetting agent and solvent obtained in step (1) at a stirring speed of 600 rpm for 15 minutes to obtain a second mixture.

[0087] Step (4): Sequentially add the modified filler and dryer obtained in step (2) to the second mixture obtained in step (3), stir and mix at a stirring speed of 800 rpm for 20 minutes to obtain the high-temperature resistant waterproof coating.

[0088] Example 3

[0089] This example provides a high-temperature resistant waterproof coating. By weight, the high-temperature resistant waterproof coating comprises the following components:

[0090] 55 parts of organosilicon resin base material, 1.5 parts of dispersant, 0.8 part of wetting agent, 20 parts of modified filler, 0.5 part of dryer and 26 parts of solvent;

[0091] The organosilicon resin base material is obtained by subjecting methylphenyl silicone resin and methyl MQ silicone resin with a weight ratio of 86:15 to oxygen-rich microwave plasma composite treatment.

[0092] The modified filler is obtained by modifying sericite powder, quartz powder, titanium dioxide powder and silica aerogel powder with a silane coupling agent.

[0093] The preparation method of the above high-temperature resistant waterproof coating comprises the following steps:

[0094] Step (1): Mix methylphenyl silicone resin and methyl MQ silicone resin to obtain a first mixture. Add the first mixture into a microwave plasma treatment instrument for oxygen-rich microwave plasma composite treatment for 90 seconds, and then continue to introduce oxygen for 5 minutes to obtain the organosilicon resin base material. Among them, the working condition parameters of the microwave plasma treatment instrument include: the discharge mode is glow discharge, the working medium is composed of oxygen and argon with a volume ratio of 10:1, the intake air volume is 55 mL / min, and the microwave power is 240 W.

[0095] Step (2): Add sericite powder, quartz powder, titanium dioxide powder and silica aerogel powder into an aqueous solution of silane coupling agent with a mass fraction of 15% for heating and stirring. After the water has completely evaporated, perform vacuum drying and grinding through a 200-mesh sieve to obtain the modified filler. Among them, the weight ratio of the sericite powder, the quartz powder, the titanium dioxide powder, the silica aerogel powder and the aqueous solution of silane coupling agent is 11:5:3:1.5:15. The working condition parameters of the heating and stirring include: the temperature is 86°C and the stirring speed is 260 rpm.

[0096] Step (3): Stir and mix the organosilicon resin base material, dispersant, wetting agent and solvent obtained in step (1) at a stirring speed of 600 rpm for 15 minutes to obtain a second mixture.

[0097] Step (4): Sequentially add the modified filler and dryer obtained in step (2) to the second mixture obtained in step (3) for stirring and mixing at a stirring speed of 800 rpm for 20 minutes to obtain the high-temperature resistant waterproof coating.

[0098] Comparative Example 1

[0099] This example provides a high-temperature resistant waterproof coating and its preparation method. The difference from Example 1 is only that: the organosilicon resin base material is directly compounded from methylphenyl silicone resin and methyl MQ silicone resin with a weight ratio of 83:11 (i.e., without oxygen-rich microwave plasma composite treatment); the modified filler is directly compounded from sericite powder, quartz powder, titanium dioxide powder and silica aerogel powder (i.e., without silane coupling agent modification treatment); the remaining steps and parameters are the same.

[0100] The preparation method of the above high-temperature resistant waterproof coating includes the following steps:

[0101] Step (1): Mix methylphenyl silicone resin and methyl MQ silicone resin to obtain the organosilicon resin base material.

[0102] Step (2): Directly mix and grind sericite powder, quartz powder, titanium dioxide powder and silica aerogel powder through a 200-mesh sieve to obtain the modified filler. Among them, the weight ratio of the sericite powder, the quartz powder, the titanium dioxide powder, the silica aerogel powder is 9:3:2:1.

[0103] Step (3): Stir and mix the organosilicon resin base material, dispersant, wetting agent and solvent obtained in step (1) at a stirring speed of 600 rpm for 15 minutes to obtain a second mixture.

[0104] Step (4): Add the modified filler obtained in step (2) and the dryer to the second mixture obtained in step (3) in sequence and stir and mix them. The stirring speed is 800 rpm and the stirring time is 20 minutes to obtain the high-temperature resistant waterproof coating.

[0105] Comparative Example 2

[0106] This example provides a high-temperature resistant waterproof coating and its preparation method. The difference from Example 1 is only that: the silicone resin base material is directly compounded from methylphenyl silicone resin and methyl MQ silicone resin with a weight ratio of 83:11 (i.e., without oxygen-rich microwave plasma composite treatment); the remaining steps and parameters are the same.

[0107] The preparation method of the above high-temperature resistant waterproof coating includes the following steps:

[0108] Step (1): Mix methylphenyl silicone resin and methyl MQ silicone resin to obtain the silicone resin base material;

[0109] Step (2): Add sericite powder, quartz powder, titanium dioxide powder and silica aerogel powder to an aqueous solution of silane coupling agent with a mass fraction of 18% and heat, stir and mix. After the water has completely evaporated, perform vacuum drying and grind through a 200-mesh sieve to obtain the modified filler; wherein, the weight ratio of the sericite powder, the quartz powder, the titanium dioxide powder, the silica aerogel powder and the aqueous solution of silane coupling agent is 9:3:2:1:12; the working condition parameters of the heating and stirring mixture include: the temperature is 86 °C and the stirring speed is 260 rpm;

[0110] Step (3): Stir and mix the silicone resin base material, dispersant, wetting agent and solvent obtained in step (1). The stirring speed is 600 rpm and the stirring time is 15 minutes to obtain a second mixture;

[0111] Step (4): Add the modified filler obtained in step (2) and the dryer to the second mixture obtained in step (3) in sequence and stir and mix them. The stirring speed is 800 rpm and the stirring time is 20 minutes to obtain the high-temperature resistant waterproof coating.

[0112] Comparative Example 3

[0113] This example provides a high-temperature resistant waterproof coating and its preparation method. The difference from Example 1 is only that: the modified filler is directly compounded from sericite powder, quartz powder, titanium dioxide powder and silica aerogel powder (i.e., without silane coupling agent modification treatment); the remaining steps and parameters are the same.

[0114] The preparation method of the above high-temperature resistant waterproof coating includes the following steps:

[0115] Step (1): Mix methyl phenyl silicone resin and methyl MQ silicone resin to obtain a first mixture; add the first mixture into a microwave plasma treatment instrument for oxygen-rich microwave plasma composite treatment for 65 seconds, and then continue to introduce oxygen for 8 minutes to obtain the silicone resin base material; wherein, the working condition parameters of the microwave plasma treatment instrument include: the discharge mode is glow discharge, the working medium is composed of oxygen and argon with a volume ratio of 10:1, the intake air volume is 65 mL / min, and the microwave power is 290 W;

[0116] Step (2): Directly mix sericite powder, quartz powder, titanium dioxide powder and silica aerogel powder and grind them through a 200-mesh sieve to obtain the modified filler; wherein, the weight ratio of the sericite powder, the quartz powder, the titanium dioxide powder and the silica aerogel powder is 9:3:2:1;

[0117] Step (3): Stir and mix the silicone resin base material, dispersant, wetting agent and solvent obtained in step (1) at a stirring speed of 600 rpm for 15 minutes to obtain a second mixture;

[0118] Step (4): Add the modified filler and dryer obtained in step (2) to the second mixture obtained in step (3) in sequence and stir and mix at a stirring speed of 800 rpm for 20 minutes to obtain the high-temperature resistant waterproof coating.

[0119] Comparative Example 4

[0120] This example provides a high-temperature resistant waterproof coating and its preparation method, which is only different from Example 1 in that: the silicone resin base material is obtained by oxygen-rich microwave plasma composite treatment of methyl phenyl silicone resin and methyl MQ silicone resin with a weight ratio of 11:86 (i.e., adjust the dosage ratio of methyl phenyl silicone resin and methyl MQ silicone resin); the remaining steps and parameters are the same.

[0121] Test Example

[0122] This example conducts high-temperature stability tests on the high-temperature resistant waterproof coatings obtained in the above Examples 1-3 and Comparative Examples 1-4.

[0123] Testing method: 1) Coat the high-temperature resistant waterproof coatings obtained from Examples 1 to 3 and Comparative Examples 1 to 4 respectively on the surface of a steel plate substrate that has been derusted and decontaminated. After coating, conduct surface drying (20 min) and bake at 65 °C for 2 hours to obtain a steel plate substrate sample with a coating to be tested; 2) Place the steel plate substrate sample with the coating to be tested in a muffle furnace, raise the temperature to 300 - 1200 °C at a rate of 50 °C / min, hold for 2 h, let it cool, and after it has cooled to room temperature (25 °C), observe whether there are phenomena such as delamination, peeling, bubbling, cracking, etc. on the coating, and record the heat resistance limit temperature of the coating (i.e., the limit temperature at which there are no phenomena such as delamination, peeling, bubbling, cracking, etc.).

[0124] The test results are shown in Table 1.

[0125] Table 1

[0126]

[0127]

[0128] As can be seen from Table 1, compared with Comparative Examples 1 to 4, the high-temperature resistant waterproof coatings provided by the examples of the present invention have better excellent high-temperature stability when baked at 70 °C for 2 hours to form a cured coating. For example, the heat resistance limit temperature of the high-temperature resistant waterproof coating provided by Example 1 can reach 1100 °C. At the same time, through the analysis and comparison of the test results of Comparative Example 1, Comparative Example 2, Comparative Example 3, and Example 1, it can be known that in Example 1 of the present invention, by using a specific silicone resin-based system and a specific modified filler in combination, the two have a significant positive synergistic effect, and the effect on improving the high-temperature stability of silicone-based coatings is more significant.

[0129] In addition, based on the results of the above high-temperature stability test, in this example, the water resistance of the high-temperature resistant waterproof coatings provided by Examples 1 to 3 was also tested according to the GB / T 1733 - 1993 test standard, and no phenomena such as bubbling, rusting, and peeling occurred.

[0130] In summary, the examples of the present invention provide a high-temperature resistant waterproof coating and its preparation method. Through the composite treatment of the silicone resin base material, the synergistic effect of the modified filler, and the precise ratio of other components, the stability of the coating in a high-temperature environment and the curability under medium and low-temperature conditions are achieved. This multi-level synergistic mechanism not only significantly improves the comprehensive performance of the coating but also makes up for the deficiencies in the curing conditions of existing high-temperature resistant coatings, broadening the application range of silicone-based high-temperature resistant coatings.

[0131] The various embodiments of the present invention may exist in the form of a range; it should be understood that the description in the form of a range is only for convenience and brevity and should not be construed as a rigid limitation on the scope of the present invention; therefore, it should be considered that the described range description has specifically disclosed all possible sub-ranges and single values within that range. For example, it should be considered that the range description from 1 to 6 has specifically disclosed sub-ranges such as from 1 to 3, from 1 to 4, from 1 to 5, from 2 to 4, from 2 to 6, from 3 to 6, etc., and single numbers within the range, such as 1, 2, 3, 4, 5, and 6, and this applies regardless of the range. Additionally, whenever a numerical range is indicated herein, it means including any cited number (fraction or integer) within the indicated range.

[0132] The above are only specific embodiments of the present invention, enabling those skilled in the art to understand or implement the present invention. Various modifications to these embodiments will be obvious to those skilled in the art, and the general principles defined herein can be implemented in other embodiments without departing from the spirit or scope of the present invention. Therefore, the present invention will not be limited to these embodiments shown herein, but rather to the broadest scope consistent with the principles and novel features claimed herein.

Claims

1. A high temperature resistant waterproof coating, characterized in that: The high temperature resistant waterproof coating comprises the following components in parts by weight: 45-55 parts of silicone resin base material, 0.5-1.5 parts of dispersant, 0.2-0.8 parts of wetting agent, 10-20 parts of modified filler, 0.1-0.5 parts of drying agent and 18-26 parts of solvent; The organic silicone resin base material is obtained by subjecting methyl phenyl silicone resin and methyl MQ silicone resin in a weight ratio of (79-86):(8-15) to oxygen-enriched microwave plasma composite treatment; The modified filler is obtained by modifying sericite powder, quartz powder, titanium dioxide and silicon dioxide aerogel powder with a silane coupling agent.

2. The high temperature resistant waterproof coating according to claim 1, characterized in that: The high temperature resistant waterproof coating comprises the following components in parts by weight: 48.5 parts of silicone resin base material, 1.0 parts of dispersant, 0.5 parts of wetting agent, 16 parts of modified filler, 0.3 parts of drying agent and 22 parts of solvent.

3. The high temperature resistant waterproof coating according to claim 1, characterized in that: Preparation method of the silicone resin base material The process includes: Mixing methyl phenyl silicone resin and methyl MQ silicone resin to obtain a first mixed material; The first mixed material is added into a microwave plasma treatment instrument to carry out oxygen-enriched microwave plasma composite treatment for 45 to 90 seconds, and then oxygen is continuously introduced for 5 to 10 minutes to obtain the silicone resin base material; The working condition parameters of the microwave plasma treatment instrument include: the discharge mode is glow discharge, the working medium is composed of oxygen and argon with a volume ratio of 10:1, the air intake volume is 55-75 mL / min, and the microwave power is 240-350 W.

4. The high temperature resistant waterproof coating according to claim 1, characterized in that: The weight ratio of the methyl phenyl silicone resin to the methyl MQ silicone resin is 83:

11.

5. The high temperature resistant waterproof coating according to claim 1, characterized in that: Preparation method of the modified filler The process includes: Sericite powder, quartz powder, titanium dioxide and silicon dioxide aerogel powder are added to a silane coupling agent aqueous solution with a mass fraction of 15-20%, heated, stirred and mixed, and vacuum dried and ground and sieved after the water is evaporated to obtain the modified filler.

6. The high temperature resistant waterproof coating according to claim 5, characterized in that: The weight ratio of the sericite powder, the quartz powder, the titanium dioxide, the silica aerogel powder and the silane coupling agent aqueous solution is (7-11):(2-5):(1-3):(0.5-1.5):(10-15); The working condition parameters of the heating, stirring and mixing include: a temperature of 80 to 90° C. and a stirring speed of 200 to 300 rpm.

7. The high temperature resistant waterproof coating according to claim 5, characterized in that: The weight ratio of the sericite powder, the quartz powder, the titanium dioxide, the silica aerogel powder and the silane coupling agent aqueous solution is 9:3:2:1:

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8. The high temperature resistant waterproof coating according to claim 1, characterized in that: The drying agent includes at least one of cobalt isooctanoate and manganese isooctanoate; and the solvent includes water.

9. A method for preparing a high temperature resistant waterproof coating according to any one of claims 1 to 8, characterized in that: The preparation method comprises the following steps: Stirring and mixing the silicone resin base material, the dispersant, the wetting agent and the solvent to obtain a second mixed material; The modified filler and the drying agent are sequentially added to the second mixed material, and stirred and mixed to obtain the high temperature resistant waterproof coating.

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