High-temperature-resistant waterproof coating and preparation method thereof

Abstract

The invention relates to a high-temperature-resistant waterproof coating and a preparation method thereof, and relates to the technical field of coatings, and the high-temperature-resistant waterproof coating comprises the following components in parts by weight: 45-55 parts of an organic silicon resin base material, 0.5-1.5 parts of a dispersant, 0.2-0.8 part of a wetting agent, 10-20 parts of a modified filler, 0.1-0.5 part of a drier and 18-26 parts of a solvent; the organic silicon resin base material is obtained by performing oxygen-enriched microwave plasma composite treatment on methyl phenyl silicon resin and methyl MQ silicon resin in a weight ratio of (79-86): (8-15). Methyl phenyl silicone resin and methyl MQ silicone resin in a proper proportion are subjected to oxygen-enriched microwave plasma composite treatment to form an organic silicon resin-based system, and meanwhile, the organic silicon resin-based system is matched with the specific modified filler, so that the high-temperature resistance of the coating is remarkably improved, and the organic silicon coating is cured under medium and low temperature conditions; and the defects in the prior art are overcome.

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 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.

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

[0012] Mixing methyl phenyl silicone resin and methyl MQ silicone resin to obtain a first mixed material;

[0013] 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;

[0014] 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.

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

[0016] Furthermore, the preparation method of the modified filler comprises the following process:

[0017] 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.

[0018] Furthermore, 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);

[0019] 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.

[0020] Furthermore, 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 9:3:2:1:12.

[0021] Furthermore, the drying agent includes at least one of cobalt isooctanoate and manganese isooctanoate; and the solvent includes water.

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

[0023] Stirring and mixing the silicone resin base material, the dispersant, the wetting agent and the solvent to obtain a second mixed material;

[0024] 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.

[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. The present invention forms an organosilicon resin-based system by subjecting methylphenyl silicone resin and methyl MQ silicone resin to oxygen-enriched microwave plasma composite treatment in an appropriate proportion, and at the same time, combines with specific modified fillers, which not only significantly improves the high temperature resistance of the coating, but also enables the organosilicon coating to be cured under medium and low temperature conditions, thus making up for the deficiencies of the prior art. Specifically:

[0027] 1) Composite treatment of silicone resin base material: The present invention uses methyl phenyl silicone resin and methyl MQ silicone resin in an appropriate proportion as the base material for oxygen-enriched microwave plasma composite treatment to promote crosslinking and fusion between the two resin molecules to form a denser and more stable network structure, which not only retains the high temperature stability of the methyl phenyl silicone resin, but also incorporates the easy processing characteristics of the methyl MQ silicone resin, thereby achieving complementarity between the two in heat resistance, mechanical strength and chemical stability, thereby improving the high temperature resistance and low temperature curing performance of the silicone resin matrix.

[0028] 2) Synergistic enhancement of modified fillers: Sericite powder, quartz powder, titanium dioxide and silica aerogel powder themselves have good heat resistance, hardness and chemical stability. After being modified by silane coupling agent, the interface defects between the filler and the silicone resin base material are reduced, and the compatibility with the silicone resin base material is enhanced. It can be more evenly dispersed in the silicone resin base material to form a denser coating structure, so that the filler can more effectively play its role in promoting the heat resistance and hardness 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 silicone resin base material, the synergistic effect of the modified filler and the precise proportion of other components. This multi-level synergistic mechanism not only significantly improves the comprehensive performance of the coating, but also makes up for the shortcomings of the prior art in the curing conditions of high temperature resistant coatings, and broadens the application scope of silicone-based high temperature resistant coatings. DETAILED DESCRIPTION

[0030] In order to make the purpose, technical solution and advantages of the embodiments of the present invention clearer, the technical solution in the embodiments of the present invention will be clearly and completely described below. Obviously, the described embodiments are part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the present invention.

[0031] Unless otherwise specified, various raw materials, reagents, instruments and equipment used in the present invention can be purchased from the market or prepared by existing methods.

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

[0033] 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;

[0034] 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;

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

[0036] An embodiment of the present invention provides a high-temperature resistant waterproof coating. The present invention forms a silicone resin-based system by subjecting methylphenyl silicone resin and methyl MQ silicone resin to oxygen-enriched microwave plasma composite treatment with an appropriate proportion, and at the same time uses specific modified fillers to significantly improve the high-temperature resistance of the coating, and realizes the curing of the silicone coating under medium and low temperature conditions, thereby making up for the shortcomings of the prior art.

[0037] In the present invention, methylphenyl silicone resin is a type of organic silicone resin containing methyl and phenyl groups, and specifically, it can be directly used, for example, IC 900, Wacker MP 50 and other commercially available products, preferably Wacker MP 50.

[0038] In the present invention, methyl MQ silicone resin is a new type of organosilicon polymer material whose molecules have a three-dimensional (non-linear) structure composed of Si-O bonds as the skeleton. Specifically, commercially available products such as YL-MQ102 of Laiyang Yulin Chemical Co., Ltd. and SI-MQ102 of Laiyang Shengbang Organosilicon Technology Co., Ltd. can be directly used, and YL-MQ102 of Laiyang Yulin Chemical Co., Ltd. is preferred.

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

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

[0041] 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.

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

[0043] Mixing methyl phenyl silicone resin and methyl MQ silicone resin to obtain a first mixed material;

[0044] 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;

[0045] 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.

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

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

[0048] 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.

[0049] In some specific embodiments, the silane coupling agent can be directly selected from commercially available ones such as KH560, KH570, etc.

[0050] In some specific embodiments, 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);

[0051] 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.

[0052] In some specific embodiments, 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 9:3:2:1:12.

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

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

[0055] Stirring and mixing the silicone resin base material, the dispersant, the wetting agent and the solvent to obtain a second mixed material;

[0056] 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.

[0057] The method for preparing a high temperature resistant waterproof coating provided by the present invention is realized based on the high temperature resistant waterproof coating described in any one of the first aspects, and therefore has at least the beneficial effects of the high temperature resistant waterproof coating described in any one of the first aspects, which will not be described one by one here.

[0058] It should be noted that the components and raw materials involved in the high-temperature resistant waterproof coating and the preparation method thereof provided in the embodiments of the present invention, unless otherwise specified or specifically described, can be directly commercially available products or homemade using existing public preparation methods. For example, silica aerogel powder can be directly commercially available products such as silica aerogel powder produced by Anhui Keang Nano Technology Co., Ltd. or Qingguan Nano Technology (Jiangsu) Co., Ltd.; at the same time, the steps and parameters involved, unless otherwise specified or specifically described, can be carried out according to the processing technology of existing coatings or directly using existing equipment, and the present invention document will not repeat them one by one.

[0059] The present invention will be further described below in conjunction with specific examples. It should be understood that these examples are intended only to illustrate the present invention and are not intended to limit the scope of the present invention. The experimental methods in the following examples that do not specify specific conditions are usually measured according to national standards. If there is no corresponding national standard, then the conditions recommended by the manufacturer are followed.

[0060] Some of the raw material information involved in the following examples and comparative examples are as follows:

[0061] Methylphenyl silicone resin: 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] Drier: cobalt octanoate.

[0066] Solvent: Water.

[0067] Silane coupling agent: KH560.

[0068] Example 1

[0069] This example provides a high temperature resistant waterproof coating, which includes the following components in parts by weight:

[0070] 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;

[0071] The organic silicone resin base material is obtained by subjecting methyl phenyl silicone resin and methyl MQ silicone resin in a weight ratio of 83:11 to oxygen-enriched microwave plasma composite treatment;

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

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

[0074] Step (1): mixing methyl phenyl silicone resin and methyl MQ silicone resin to obtain a first mixture; adding the first mixture into a microwave plasma treatment instrument for oxygen-enriched microwave plasma composite treatment for 65 seconds, and then continuing 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 in a volume ratio of 10:1, the air intake is 65 mL / min, and the microwave power is 290 W;

[0075] Step (2): adding sericite powder, quartz powder, titanium dioxide and silica aerogel powder to a silane coupling agent aqueous solution with a mass fraction of 18%, heating, stirring and mixing, vacuum drying and grinding through a 200-mesh sieve after the water is evaporated, to obtain the modified filler; wherein 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 9:3:2:1:12; the working condition parameters of the heating, stirring and mixing include: a temperature of 86° C. and a stirring speed of 260 rpm;

[0076] Step (3): stirring and mixing 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;

[0077] Step (4): Add the modified filler and the drying agent obtained in step (2) to the second mixture obtained in step (3) in sequence and stir and mix them at a stirring speed of 800 rpm for 20 minutes to obtain the high temperature resistant waterproof coating.

[0078] Example 2

[0079] This example provides a high temperature resistant waterproof coating, which includes the following components in parts by weight:

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

[0081] The organic silicone resin base material is obtained by subjecting methyl phenyl silicone resin and methyl MQ silicone resin in a weight ratio of 79:8 to oxygen-enriched microwave plasma composite treatment;

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

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

[0084] Step (1): mixing methyl phenyl silicone resin and methyl MQ silicone resin to obtain a first mixture; adding the first mixture into a microwave plasma treatment instrument for oxygen-enriched microwave plasma composite treatment for 45 seconds, and then continuing to introduce oxygen for 10 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 in a volume ratio of 10:1, the air intake is 75 mL / min, and the microwave power is 350 W;

[0085] Step (2): adding sericite powder, quartz powder, titanium dioxide and silica aerogel powder to a 20% by mass silane coupling agent aqueous solution, heating and stirring to mix, and after the water evaporates, vacuum drying and grinding through a 200-mesh sieve to obtain the modified filler; wherein 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 7:2:1:0.5:10; the working condition parameters of the heating and stirring mixing include: a temperature of 86°C and a stirring speed of 260 rpm;

[0086] Step (3): stirring and mixing 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;

[0087] Step (4): Add the modified filler and the drying agent obtained in step (2) to the second mixture obtained in step (3) in sequence and stir and mix them 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, which includes the following components in parts by weight:

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

[0091] The organic silicone resin base material is obtained by subjecting methyl phenyl silicone resin and methyl MQ silicone resin in a weight ratio of 86:15 to oxygen-enriched microwave plasma composite treatment;

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

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

[0094] Step (1): mixing methyl phenyl silicone resin and methyl MQ silicone resin to obtain a first mixture; adding the first mixture into a microwave plasma treatment instrument for oxygen-enriched microwave plasma composite treatment for 90 seconds, and then continuing to introduce oxygen for 5 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 in a volume ratio of 10:1, the air intake is 55 mL / min, and the microwave power is 240 W;

[0095] Step (2): adding sericite powder, quartz powder, titanium dioxide and silica aerogel powder to a 15% by mass silane coupling agent aqueous solution, heating and stirring to mix, and after the water evaporates, vacuum drying and grinding through a 200-mesh sieve to obtain the modified filler; wherein 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 11:5:3:1.5:15; the working condition parameters of the heating and stirring mixing include: a temperature of 86°C and a stirring speed of 260 rpm;

[0096] Step (3): stirring and mixing 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;

[0097] Step (4): Add the modified filler and the drying agent obtained in step (2) to the second mixture obtained in step (3) in sequence and stir and mix them 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 a preparation method thereof, which differs from Example 1 only in that: the silicone resin base material is obtained by directly compounding methyl phenyl silicone resin and methyl MQ silicone resin in a weight ratio of 83:11 (i.e., no oxygen-enriched microwave plasma composite treatment is performed); the modified filler is obtained by directly compounding sericite powder, quartz powder, titanium dioxide and silica aerogel powder (i.e., no silane coupling agent modification treatment is performed); the remaining steps and parameters are the same.

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

[0101] Step (1): mixing methyl phenyl silicone resin and methyl MQ silicone resin to obtain the silicone resin base material;

[0102] Step (2): directly mixing and grinding sericite powder, quartz powder, titanium dioxide and silica aerogel powder, and passing through a 200-mesh sieve to obtain the modified filler; wherein the weight ratio of the sericite powder, the quartz powder, the titanium dioxide and the silica aerogel powder is 9:3:2:1;

[0103] Step (3): stirring and mixing 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;

[0104] Step (4): Add the modified filler and the drying agent obtained in step (2) to the second mixture obtained in step (3) in sequence and stir and mix them at a stirring speed of 800 rpm for 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 a preparation method thereof. The only difference from Example 1 is that the silicone resin base material is obtained by directly compounding methyl phenyl silicone resin and methyl MQ silicone resin in a weight ratio of 83:11 (i.e., no oxygen-enriched microwave plasma composite treatment is performed); the remaining steps and parameters are the same.

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

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

[0109] Step (2): adding sericite powder, quartz powder, titanium dioxide and silica aerogel powder to a silane coupling agent aqueous solution with a mass fraction of 18%, heating, stirring and mixing, vacuum drying and grinding through a 200-mesh sieve after the water is evaporated, to obtain the modified filler; wherein 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 9:3:2:1:12; the working condition parameters of the heating, stirring and mixing include: a temperature of 86° C. and a stirring speed of 260 rpm;

[0110] Step (3): stirring and mixing 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;

[0111] Step (4): Add the modified filler and the drying agent obtained in step (2) to the second mixture obtained in step (3) in sequence and stir and mix them at a stirring speed of 800 rpm for 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 a preparation method thereof. The only difference from Example 1 is that the modified filler is obtained by directly compounding sericite powder, quartz powder, titanium dioxide and silica aerogel powder (i.e., no silane coupling agent modification treatment is performed); the remaining steps and parameters are the same.

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

[0115] Step (1): mixing methyl phenyl silicone resin and methyl MQ silicone resin to obtain a first mixture; adding the first mixture into a microwave plasma treatment instrument for oxygen-enriched microwave plasma composite treatment for 65 seconds, and then continuing 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 in a volume ratio of 10:1, the air intake is 65 mL / min, and the microwave power is 290 W;

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

[0117] Step (3): stirring and mixing 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 the drying agent obtained in step (2) to the second mixture obtained in step (3) in sequence and stir and mix them 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 a preparation method thereof. The only difference from Example 1 is that the silicone resin base material is obtained by subjecting methylphenyl silicone resin and methyl MQ silicone resin in a weight ratio of 11:86 to oxygen-enriched microwave plasma composite treatment (i.e., adjusting the dosage ratio of methylphenyl silicone resin and methyl MQ silicone resin); the remaining steps and parameters are the same.

[0121] Test Case

[0122] In this example, the high temperature stability test was performed on the high temperature resistant waterproof coatings obtained in the above-mentioned Examples 1 to 3 and Comparative Examples 1 to 4.

[0123] Test method: 1) The high temperature resistant waterproof coatings obtained in Examples 1 to 3 and Comparative Examples 1 to 4 are respectively applied to the surface of the steel plate substrate that has been derusted and decontaminated, and after coating, the surface is dried (20 minutes) and baked at 65°C for 2 hours to obtain a steel plate substrate sample containing the coating to be tested; 2) The steel plate substrate sample containing the coating to be tested is placed in a muffle furnace, raised to 300-1200°C at 50°C / min and kept in the range of 2h, allowed to cool, and after cooling to room temperature (25°C), observe whether the coating has delamination, peeling, bubbling, cracking, etc., and record the heat resistance limit temperature of the coating (i.e., the limit temperature at which no delamination, peeling, bubbling, cracking, etc. occurs).

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

[0125] Table 1

[0126]

[0127]

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

[0129] In addition, based on the results of the above high temperature stability test, this example also conducted a water resistance test on the high temperature resistant waterproof coatings provided in Examples 1 to 3 according to the GB / T 1733-1993 test standard, and no blistering, rusting, or shedding occurred.

[0130] In summary, the embodiments of the present invention provide a high temperature resistant waterproof coating and a preparation method thereof, which achieves 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 silicone resin base material, the synergistic effect of the modified filler and the precise proportion of other components. This multi-level synergistic mechanism not only significantly improves the comprehensive performance of the coating, but also makes up for the shortcomings of the prior art in the curing conditions of high temperature resistant coatings, and broadens the application scope of silicone-based high temperature resistant coatings.

[0131] Various embodiments of the present invention may be presented 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 understood as a rigid limitation on the scope of the present invention; therefore, the range description should be considered to have specifically disclosed all possible sub-ranges and single numerical values ​​within the range. For example, the range description from 1 to 6 should be considered to have 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., as well as single numbers within the range, such as 1, 2, 3, 4, 5 and 6, which apply regardless of the range. In addition, whenever a numerical range is indicated herein, it is meant to include any cited number (fractional or integer) within the indicated range.

[0132] The foregoing is merely a specific embodiment of the present invention, which enables those skilled in the art to understand or implement the present invention. Various modifications to these embodiments will be apparent to those skilled in the art, and the general principles defined herein may 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 the embodiments shown herein, but rather to the widest 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:

12.

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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