Novel organic silicon coating and preparation method thereof

Abstract

The invention relates to the technical field of coatings, and particularly provides a novel organic silicon coating and a preparation method thereof, and the novel organic silicon coating comprises organic silicon, resin, hollow glass beads and the like. The novel organic silicon coating has a unique organic silicon resin-hollow glass bead system, the flexibility of the novel organic silicon coating is improved by modifying organic silicon through the hollow glass beads, the stability of the organic silicon resin is improved in combination with the water-based acrylic resin, and finally the temperature difference resistance of the novel organic silicon coating is improved; and the application range under different temperature conditions is greatly expanded.

Description

Technical Field

[0001] This invention relates to the field of coating technology, and in particular to a novel organosilicon coating and its preparation method. Background Technology

[0002] Silicone coatings have advantages such as rapid surface drying, good adhesion, good flexibility, and convenient application. They are generally resistant to temperatures between 200-800℃. However, traditional silicone coatings of this type will crack and peel under sudden temperature changes, especially when the temperature drops from above 600℃ to 0℃, the paint film will quickly crack and even fall off the substrate.

[0003] Therefore, a novel organosilicon coating and its preparation method are needed. Summary of the Invention

[0004] To address the aforementioned problems, the present invention aims to provide a novel organosilicon coating and its preparation method.

[0005] On one hand, the present invention provides a method for preparing a novel organosilicon coating, the method comprising the following steps: Step 1: Take 5-15% by mass of methyltrimethoxysilane, 5-15% by mass of phenyltrimethoxysilane, 10-20% by mass of dimethyldiethoxysilane, 10-20% by mass of diphenyldiethoxysilane, 0.3-0.5% by mass of hydrofluoric acid, and make up the remaining mass of pure water; The methyltrimethoxysilane, phenyltrimethoxysilane, dimethyldiethoxysilane and diphenyldiethoxysilane were sequentially added to a reaction vessel and stirred at 25°C and 60 rpm for 2 hours. Then, hydrofluoric acid was added, and the mixture was heated to 60°C and refluxed for 2 hours. The mixture was then heated at 0.5°C / min and evaporated and concentrated until the solid content of the material in the reaction vessel was 95%. The mixture was then cooled to 25°C to obtain a semi-finished organosilicon product. Step 2: Take 30-50% by mass of the aforementioned organosilicon semi-finished product, 15-30% by mass of water-soluble acrylic resin, 3-5% by mass of dimethyl ethanolamine, and make up the remaining mass of pure water; The organosilicon semi-finished product and the water-soluble acrylic resin were added to a reaction vessel and stirred at 25°C and 100 rpm for 1 hour. Then, the dimethyl ethanolamine was slowly added at 0.02 times the mass fraction of the dimethyl ethanolamine per second. After stirring at 25°C and 100 rpm for 30 minutes, deionized water was added, and the mixture was stirred at 25°C and 100 rpm for another hour to obtain the water-based organosilicon resin. Step 3: Take 40-50% by mass of the aforementioned water-based silicone resin, 5-10% by mass of water-based aluminum silver paste, 2-4% by mass of 220-mesh hollow glass microspheres, 0.5-1.5% by mass of fumed silica, 10-20% by mass of glass powder, 0.3-0.5% by mass of PE100 wetting agent, 0.2-0.4% by mass of B-313 defoamer, 0.3-0.5% by mass of ASE-60 thickener, and add the remaining pure water to make up the mass fraction. The water-based silicone resin, the water-based aluminum silver paste, the 220-mesh hollow glass microspheres, the fumed silica, the glass powder, the PE100 wetting agent, the B-313 defoamer, the ASE-60 thickener, and the pure water are sequentially added to a reaction vessel and stirred at 60 rpm for 30 minutes to obtain the novel silicone coating.

[0006] Furthermore, the mass fraction of the methyltrimethoxysilane is 10%.

[0007] Furthermore, the phenyltrimethoxysilane has a mass fraction of 9%.

[0008] Furthermore, the mass fraction of the dimethyldiethoxysilane is 15%.

[0009] Furthermore, the mass fraction of the diphenyldiethoxysilane is 16%.

[0010] Furthermore, the mass fraction of the organosilicon semi-finished product is 40%.

[0011] Furthermore, the water-soluble acrylic resin has a mass fraction of 22%.

[0012] Furthermore, the water-based silicone resin has a mass fraction of 45%.

[0013] Furthermore, the water-based aluminum silver paste has a mass fraction of 7%.

[0014] Furthermore, the mass fraction of the 220-mesh hollow glass microspheres is 3%.

[0015] Furthermore, the glass powder has a mass fraction of 14%.

[0016] Further, the hydrofluoric acid has a mass fraction of 0.4%, the dimethyl ethanolamine has a mass fraction of 4%, the fumed silica has a mass fraction of 1%, the PE100 wetting agent has a mass fraction of 0.4%, the B-313 defoamer has a mass fraction of 0.3%, and the ASE-60 thickener has a mass fraction of 0.4%.

[0017] On the other hand, the present invention provides a novel organosilicon coating prepared by the method described above.

[0018] The present invention can bring the following beneficial effects: This invention discloses a novel organosilicon coating with a unique organosilicon resin-hollow glass microsphere system. The invention improves the elasticity of organosilicon by modifying it with hollow glass microspheres, and enhances the stability of the organosilicon resin by combining it with water-based acrylic resin, ultimately improving the temperature difference resistance of the novel organosilicon coating and significantly expanding its applicability under different temperature conditions. The water-based organosilicon resin prepared with water-based acrylic resin exhibits good anti-cracking and anti-powdering properties at high temperatures. The addition of appropriately meshed hollow glass microspheres results in low density and high elasticity, effectively mitigating the problem of coating cracking under large temperature differences in environments with rapid heating and cooling. The components of this invention, prepared using a unique process and proportioning method, synergistically form the organosilicon resin-hollow glass microsphere system. It should be noted that the process parameters and drug proportions of this invention are not derived from simple experiments and involve a degree of chance and inventiveness. Detailed Implementation

[0019] To more clearly illustrate the overall concept of the present invention, the overall solution of the present invention will be described in detail below by way of embodiments; in the following description, numerous specific details are set forth in order to provide a more thorough understanding of the present invention; however, it will be apparent to those skilled in the art that the present invention may be practiced without one or more of these details; in other instances, some technical features known in the art have not been described in order to avoid confusion with the present invention.

[0020] In this invention, the reactor was purchased from Wenzhou Xinpai Machinery Co., Ltd., FYF type 50L, and 50L was fed each time; the hollow glass microspheres were purchased from Lingshou County Xucheng Mineral Products Processing Plant; PE100 was purchased from Wuxi Handerson Chemical Products Co., Ltd.; B-313 was purchased from Guangdong Zhongke Hongtai New Materials Co., Ltd.; ASE-60 was purchased from Wuxi Handerson Chemical Products Co., Ltd.; and the commercially available high-temperature resistant silicone paint was Linjiang Bridge brand 600℃ type.

[0021] Unless otherwise specified, all raw material components in the following examples are commercially available, all experimental instruments used are standard laboratory instruments, and the performance testing methods are those known in the art. The overall ambient temperature was 25°C, the air humidity was 40%, and ultraviolet light was avoided.

[0022] The preferred implementation method is as follows: Example 1: The preparation method of the novel organosilicon coating is as follows: Step 1: Take 10% methyltrimethoxysilane, 9% phenyltrimethoxysilane, 15% dimethyldiethoxysilane, 16% diphenyldiethoxysilane, 0.4% hydrofluoric acid, and make up the remaining mass fraction with pure water. The methyltrimethoxysilane, phenyltrimethoxysilane, dimethyldiethoxysilane and diphenyldiethoxysilane were sequentially added to a reaction vessel and stirred at 25°C and 60 rpm for 2 hours. Then, hydrofluoric acid was added, and the mixture was heated to 60°C and refluxed for 2 hours. The mixture was then heated at 0.5°C / min and evaporated and concentrated until the solid content of the material in the reaction vessel was 95%. The mixture was then cooled to 25°C to obtain a semi-finished organosilicon product. Step 2: Take 40% by mass of the aforementioned organosilicon semi-finished product, 22% by mass of water-soluble acrylic resin, 4% by mass of dimethyl ethanolamine, and make up the remaining mass of pure water; The organosilicon semi-finished product and the water-soluble acrylic resin were added to a reaction vessel and stirred at 25°C and 100 rpm for 1 hour. Then, the dimethyl ethanolamine was slowly added at 0.02 times the mass fraction of the dimethyl ethanolamine per second. After stirring at 25°C and 100 rpm for 30 minutes, deionized water was added, and the mixture was stirred at 25°C and 100 rpm for another hour to obtain the water-based organosilicon resin. Step 3: Take 45% by mass of the aforementioned water-based silicone resin, 7% by mass of water-based aluminum silver paste, 3% by mass of 220-mesh hollow glass microspheres, 1% by mass of fumed silica, 14% by mass of glass powder, 0.4% by mass of PE100 wetting agent, 0.3% by mass of B-313 defoamer, 0.4% by mass of ASE-60 thickener, and add the remaining pure water to make up the mass fraction. The water-based silicone resin, the water-based aluminum silver paste, the 220-mesh hollow glass microspheres, the fumed silica, the glass powder, the PE100 wetting agent, the B-313 defoamer, the ASE-60 thickener, and the pure water are sequentially added to a reaction vessel and stirred at 60 rpm for 30 minutes to obtain the novel silicone coating.

[0023] Example 2-21: The only difference between Example 2 and Example 1 is that the mass fraction of methyltrimethoxysilane is 5%; The only difference between Example 3 and Example 1 is that the mass fraction of methyltrimethoxysilane is 15%; The only difference between Example 4 and Example 1 is that the mass fraction of phenyltrimethoxysilane is 5%; The only difference between Example 5 and Example 1 is that the mass fraction of phenyltrimethoxysilane is 15%; The only difference between Example 6 and Example 1 is that the mass fraction of dimethyldiethoxysilane is 10%. The only difference between Example 7 and Example 1 is that the mass fraction of dimethyldiethoxysilane is 20%. The only difference between Example 8 and Example 1 is that the mass fraction of diphenyldiethoxysilane is 10%. The only difference between Example 9 and Example 1 is that the mass fraction of diphenyldiethoxysilane is 20%. The only difference between Example 10 and Example 1 is that the mass fraction of the organosilicon semi-finished product is 30%. The only difference between Example 11 and Example 1 is that the mass fraction of the organosilicon semi-finished product is 50%. The only difference between Example 12 and Example 1 is that the mass fraction of the water-soluble acrylic resin is 15%. The only difference between Example 13 and Example 1 is that the mass fraction of the water-soluble acrylic resin is 30%. The only difference between Example 14 and Example 1 is that the mass fraction of the water-based silicone resin is 40%. The only difference between Example 15 and Example 1 is that the water-based silicone resin has a mass fraction of 50%. The only difference between Example 16 and Example 1 is that the water-based aluminum silver paste has a mass fraction of 5%. The only difference between Example 17 and Example 1 is that the water-based aluminum silver paste has a mass fraction of 10%. The only difference between Example 18 and Example 1 is that the mass fraction of the 220-mesh hollow glass microspheres is 2%. The only difference between Example 19 and Example 1 is that the mass fraction of the 220-mesh hollow glass microspheres is 4%. The only difference between Example 20 and Example 1 is that the mass fraction of the glass powder is 10%. The only difference between Example 21 and Example 1 is that the mass fraction of glass powder is 20%.

[0024] Comparative Examples 1-37: The only difference between Comparative Example 1 and Example 1 is that the mass fraction of methyltrimethoxysilane is 2%; The only difference between Comparative Example 2 and Example 1 is that the mass fraction of methyltrimethoxysilane is 25%. The only difference between Comparative Example 3 and Example 1 is that the mass fraction of phenyltrimethoxysilane is 2%; The only difference between Comparative Example 4 and Example 1 is that the mass fraction of phenyltrimethoxysilane is 25%. The only difference between Comparative Example 5 and Example 1 is that the mass fraction of dimethyldiethoxysilane is 5%; The only difference between Comparative Example 6 and Example 1 is that the mass fraction of dimethyldiethoxysilane is 30%. The only difference between Comparative Example 7 and Example 1 is that the mass fraction of diphenyldiethoxysilane is 5%; The only difference between Comparative Example 8 and Example 1 is that the mass fraction of diphenyldiethoxysilane is 30%. The only difference between Comparative Example 9 and Example 1 is that the mass fraction of the organosilicon semi-finished product is 15%. The only difference between Comparative Example 10 and Example 1 is that the mass fraction of the organosilicon semi-finished product is 60%. The only difference between Comparative Example 11 and Example 1 is that the mass fraction of the water-soluble acrylic resin is 6%. The only difference between Comparative Example 12 and Example 1 is that the mass fraction of the water-soluble acrylic resin is 40%. The only difference between Comparative Example 13 and Example 1 is that the mass fraction of the waterborne silicone resin is 20%. The only difference between Comparative Example 14 and Example 1 is that the waterborne silicone resin has a mass fraction of 60%. The only difference between Comparative Example 15 and Example 1 is that the water-based aluminum silver paste has a mass fraction of 2%. The only difference between Comparative Example 16 and Example 1 is that the water-based aluminum silver paste has a mass fraction of 15%. The only difference between Comparative Example 17 and Example 1 is that the mass fraction of 220-mesh hollow glass microspheres is 1%. The only difference between Comparative Example 18 and Example 1 is that the mass fraction of 220-mesh hollow glass microspheres is 8%. The only difference between Comparative Example 19 and Example 1 is that the mass fraction of the glass powder is 5%. The only difference between Comparative Example 20 and Example 1 is that the mass fraction of glass powder is 25%. The only difference between Comparative Example 21 and Example 1 is that the mass fraction of hydrofluoric acid is 0.1%; The only difference between Comparative Example 22 and Example 1 is that the mass fraction of hydrofluoric acid is 1%; The only difference between Comparative Example 23 and Example 1 is that the mass fraction of dimethylethanolamine is 1%. The only difference between Comparative Example 24 and Example 1 is that the mass fraction of dimethylethanolamine is 10%. The only difference between Comparative Example 25 and Example 1 is that the mass fraction of fumed silica is 0.2%; The only difference between Comparative Example 26 and Example 1 is that the mass fraction of fumed silica is 3%; The only difference between Comparative Example 27 and Example 1 is that the mass fraction of the PE100 wetting agent is 0.1%. The only difference between Comparative Example 28 and Example 1 is that the mass fraction of the PE100 wetting agent is 2%. The only difference between Comparative Example 29 and Example 1 is that the mass fraction of defoamer B-313 is 0.1%. The only difference between Comparative Example 30 and Example 1 is that the mass fraction of defoamer B-313 is 2%; The only difference between Comparative Example 31 and Example 1 is that the mass fraction of ASE-60 thickener is 0.1%. The only difference between Comparative Example 32 and Example 1 is that the mass fraction of ASE-60 thickener is 2%. The only difference between Comparative Example 33 and Example 1 is that the dimethylethanolamine was added at a rate of 0.06 times the mass fraction of the dimethylethanolamine per second. The only difference between Comparative Example 34 and Example 1 is that the hollow glass microspheres have a mesh size of 40. The only difference between Comparative Example 35 and Example 1 is that the hollow glass microspheres have a mesh size of 400. The only difference between Comparative Example 36 and Example 1 is that the hollow glass microspheres were replaced with an equal mass of pure water. The only difference between Comparative Example 37 and Example 1 is that the novel silicone coating was replaced with an equal mass of commercially available high-temperature silicone paint.

[0025] Prepare three times the number of 0.5mm thick 20×20cm S30815 heat-resistant steel plates as examples. Coat each group of three plates with the corresponding example coating. Specifically, dilute each example coating with four times its mass of pure water, mix thoroughly, and brush onto the corresponding steel plate surface at a density of 0.2 kg / m². After two days, place the plates in a heating chamber and heat from 25℃ to 600℃ within 2 minutes. Then immerse them in a refrigerant bath and cool to 0℃ within 2 minutes. After drying with 25℃ cold air, observe the surface under 800 lux light using a 10x magnifying glass. After observation, return the plates to the heating chamber for the next hot-cold cycle until cracks ≥5mm long and ≥0.2mm wide appear on the coating surface. Record the number of cycles at this point. The experimental results are shown in Table 1, in units of cycles. The final result for each example is the median of three experiments.

[0026] Table 1: Test results of temperature cycling resistance of the coating surface for each example:

[0027] As can be seen from the data in Table 1, compared with other examples, the novel organosilicon coating prepared by the embodiment of the present invention, especially the novel organosilicon coating and its preparation method of embodiment 1 of the present invention, can withstand more temperature change cycles under the same usage amount and method; that is, the novel organosilicon coating obtained by the present invention, especially the method of embodiment 1 of the present invention, has better temperature difference resistance.

[0028] It should be noted that the above process parameters and effects have a non-linear correlation, and the compatibility with other components and processes of this invention should be considered. The above descriptions are merely embodiments of this invention and are not intended to limit the invention; various modifications and variations can be made to this invention by those skilled in the art; any modifications, equivalent substitutions, improvements, etc., made within the spirit and principle of this invention should be included within the scope of the claims of this invention.

Claims

1. A method for preparing a novel organosilicon coating, characterized in that, The preparation method of the novel organosilicon coating includes the following steps: Step 1: Take 5-15% by mass of methyltrimethoxysilane, 5-15% by mass of phenyltrimethoxysilane, 10-20% by mass of dimethyldiethoxysilane, 10-20% by mass of diphenyldiethoxysilane, 0.3-0.5% by mass of hydrofluoric acid, and make up the remaining mass of pure water; The methyltrimethoxysilane, phenyltrimethoxysilane, dimethyldiethoxysilane and diphenyldiethoxysilane were sequentially added to a reaction vessel and stirred at 25°C and 60 rpm for 2 hours. Then, hydrofluoric acid was added, and the mixture was heated to 60°C and refluxed for 2 hours. The mixture was then heated at 0.5°C / min and evaporated and concentrated until the solid content of the material in the reaction vessel was 95%. The mixture was then cooled to 25°C to obtain a semi-finished organosilicon product. Step 2: Take 30-50% by mass of the aforementioned organosilicon semi-finished product, 15-30% by mass of water-soluble acrylic resin, 3-5% by mass of dimethyl ethanolamine, and make up the remaining mass of pure water; The organosilicon semi-finished product and the water-soluble acrylic resin were added to a reaction vessel and stirred at 25°C and 100 rpm for 1 hour. Then, the dimethyl ethanolamine was slowly added at 0.02 times the mass fraction of the dimethyl ethanolamine per second. After stirring at 25°C and 100 rpm for 30 minutes, deionized water was added, and the mixture was stirred at 25°C and 100 rpm for another hour to obtain the water-based organosilicon resin. Step 3: Take 40-50% by mass of the aforementioned water-based silicone resin, 5-10% by mass of water-based aluminum silver paste, 2-4% by mass of 220-mesh hollow glass microspheres, 0.5-1.5% by mass of fumed silica, 10-20% by mass of glass powder, 0.3-0.5% by mass of PE100 wetting agent, 0.2-0.4% by mass of B-313 defoamer, 0.3-0.5% by mass of ASE-60 thickener, and add the remaining amount of pure water. The water-based silicone resin, the water-based aluminum silver paste, the 220-mesh hollow glass microspheres, the fumed silica, the glass powder, the PE100 wetting agent, the B-313 defoamer, the ASE-60 thickener, and the pure water are sequentially added to a reaction vessel and stirred at 60 rpm for 30 minutes to obtain the novel silicone coating.

2. The method for preparing the novel organosilicon coating according to claim 1, characterized in that, The mass fraction of the methyltrimethoxysilane is 10%.

3. The method for preparing the novel organosilicon coating according to claim 1, characterized in that, The mass fraction of the phenyltrimethoxysilane is 9%.

4. The method for preparing the novel organosilicon coating according to claim 1, characterized in that, The mass fraction of the dimethyldiethoxysilane is 15%.

5. The method for preparing the novel organosilicon coating according to claim 1, characterized in that, The mass fraction of the diphenyldiethoxysilane is 16%.

6. The method for preparing the novel organosilicon coating according to claim 1, characterized in that, The mass fraction of the organosilicon semi-finished product is 40%.

7. The method for preparing the novel organosilicon coating according to claim 1, characterized in that, The water-soluble acrylic resin has a mass fraction of 22%.

8. The method for preparing the novel organosilicon coating according to claim 1, characterized in that, The water-based silicone resin has a mass fraction of 45%.

9. The method for preparing the novel organosilicon coating according to claim 1, characterized in that, The water-based aluminum silver paste has a mass fraction of 7%.

10. The method for preparing the novel organosilicon coating according to claim 1, characterized in that, The mass fraction of the 220-mesh hollow glass microspheres is 3%.

11. The method for preparing the novel organosilicon coating according to claim 1, characterized in that, The glass powder has a mass fraction of 14%.

12. The method for preparing the novel organosilicon coating according to claim 1, characterized in that, The hydrofluoric acid has a mass fraction of 0.4%, the dimethyl ethanolamine has a mass fraction of 4%, the fumed silica has a mass fraction of 1%, the PE100 wetting agent has a mass fraction of 0.4%, the B-313 defoamer has a mass fraction of 0.3%, and the ASE-60 thickener has a mass fraction of 0.4%.

13. A novel organosilicon coating prepared by the method of preparing a novel organosilicon coating as described in any one of claims 1 to 12.

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