A basalt flake-based high-temperature-resistant fireproof coating and a preparation method thereof

Abstract

The present application relates to the technical field of fireproof coating, and particularly discloses a basalt flake-based high-temperature-resistant fireproof coating, which comprises the following raw materials in parts by weight: 25-40 parts of basalt flake, 20-30 parts of borosilicon resin, 30-45 parts of organic silicon resin, and 0.5-2 parts of tetrabutyl titanate. The present application also discloses a preparation method of the basalt flake-based high-temperature-resistant fireproof coating. The prepared high-temperature-resistant fireproof coating can withstand long-time high temperature above 800 DEG C and short-time extreme high temperature of 2000 DEG C.

Description

Technical Field

[0001] This invention relates to the field of fire-retardant coating technology, specifically to a high-temperature resistant fire-retardant coating based on basalt flakes and its preparation method. Background Technology

[0002] Currently, most commercially available high-temperature fire-retardant coatings use organic silicone resins or inorganic ceramic materials as the matrix. For example, existing fire-retardant coating formulations generally include 50... wt %~70 wt % matrix resin (such as silicone resin or silica sol) and 30 wt %~50 wt Refractory fillers (such as mica and wollastonite) are used in some applications. For example, patent application CN115353756A discloses an inorganic high-temperature resistant non-stick ceramic coating, its preparation method, and its application. This inorganic high-temperature resistant non-stick ceramic coating includes the following raw materials: low-melting-point glass powder, curing agent, silicon nitride, titanium dioxide, alumina, titanium powder, silica sol, wetting and dispersing agent, thickener, and water. It can meet the requirements of a series of products that require long-lasting high-temperature resistance at 400~900℃. However, the high-temperature resistance of these fire-retardant coatings is limited. Prolonged exposure to temperatures above 800℃ can easily lead to decomposition or cracking, and it is difficult to maintain structural integrity at extreme temperatures (such as 2000℃).

[0003] Basalt flakes, as a type of flaky inorganic granular material, are an excellent additive in resin-based fire-retardant coatings. Due to their high specific surface area and flaky morphology, basalt flakes can significantly increase the high-temperature resistance of coatings. However, existing high-temperature fire-retardant coatings based on basalt flakes simply mix the flakes directly into the coating without surface modification. This results in poor dispersibility and insufficient interfacial bonding in the resin matrix, ultimately affecting the final high-temperature resistance. Summary of the Invention

[0004] The purpose of this invention is to provide a high-temperature resistant fireproof coating based on basalt flakes and its preparation method, which solves the problems of poor interfacial bonding and insufficient high-temperature resistance of existing high-temperature resistant fireproof coating systems. The preparation method is optimized to obtain a fireproof coating that can withstand long-term high temperatures above 800℃ and short-term extreme high temperatures of 2000℃.

[0005] To achieve the above objectives, the solution of the present invention is:

[0006] A high-temperature fire-retardant coating based on basalt flakes, comprising, by weight, the following raw materials: 25-40 parts basalt flakes, 20-30 parts borosilicate resin, 30-45 parts organosilicon resin, and 0.5-2 parts tetrabutyl titanate.

[0007] A method for preparing a high-temperature resistant fire-retardant coating based on basalt flakes includes the following steps:

[0008] Step 1: Basalt flake pretreatment:

[0009] First, according to the formula ratio, basalt flakes are immersed in 1~3 mol / L sodium hydroxide solution for etching for 1~2 hours to obtain pretreated basalt flakes, thereby enhancing the surface roughness of basalt flakes and the interfacial bonding force with the matrix resin.

[0010] Step 2, Preparation of borosilicate resin:

[0011] Then, according to the formula ratio, phenyltriethoxysilane and boric acid are mixed in a molar ratio of 1:1~2 and reacted at 60~100℃ for 3~5 hours to generate borosilicate resin.

[0012] Step 3: Preparation of the resin mixture system:

[0013] Then, according to the formula ratio, borosilicate resin and organosilicon resin are mixed at a mass ratio of 1:1~2 to form a composite resin matrix. Pretreated basalt flakes are then added to obtain the resin mixture system, with the pigment-to-binder ratio controlled at 30. wt % ~70 wt This ensures the density and fire resistance of subsequent coatings;

[0014] Step 4, Curing process:

[0015] Finally, add tetrabutyl titanate as a curing agent according to the ratio of total mass of resin mixture to mass of tetrabutyl titanate = 100: 0.5~2. Stir for 12~24 hours after mixing to obtain a uniformly mixed high-temperature fireproof coating.

[0016] In step 3, the silicone resin is a polymethylphenylsiloxane resin.

[0017] In step 1, the ratio of basalt flakes to sodium hydroxide solution is 10 g: 200~500 mL.

[0018] In step 1, the concentration of sodium hydroxide solution is 1~3 mol / L. If the concentration is too low, the etching effect will be poor, and if the concentration is too high, it will easily damage the structure of the basalt flakes.

[0019] In step 2, an excipient is added to the mixture of phenyltriethoxysilane and boric acid, wherein the molar ratio of the excipient to phenyltriethoxysilane is 0.5:1.

[0020] In step 2, the auxiliary material is xylene. The purpose of adding xylene is to dilute it, adjust the viscosity of the borosilicate resin, and facilitate the application of the coating.

[0021] In step 3, the ratio of borosilicate resin to organosilicon resin is 1:1~2. If the ratio is too low, the resin will not have sufficient heat resistance, and if the ratio is too high, the resin will have reduced flexibility.

[0022] In step 3, the pigment-to-matrix ratio (the ratio of basalt flakes to the composite resin matrix) in the resin mixture is controlled at 30. wt % ~ 70 wt This ensures a balance between the density and fire resistance time of subsequent coatings.

[0023] After adopting the above technical solution, the high-temperature resistant fireproof coating based on basalt flakes and its preparation method of the present invention have the following beneficial effects:

[0024] 1. By introducing a composite resin matrix of borosilicate resin and organosilicon resin, and adding basalt flakes, a fireproof coating that can withstand long-term high temperature above 800℃ and short-term extreme high temperature of 2000℃ is obtained.

[0025] 2. Etching treatment is applied to the basalt flakes to enhance their surface roughness, improve the resin anchoring effect, enhance the interfacial bonding force with the matrix resin, and reduce the risk of peeling.

[0026] 3. Tetrabutyl titanate is used as a curing agent, which is resistant to high temperatures and ensures the stability of the cured structure at high temperatures. Detailed Implementation

[0027] To further explain the technical solution of the present invention, the present invention will be described in detail below through specific embodiments.

[0028] Example 1

[0029] A method for preparing a high-temperature resistant fire-retardant coating based on basalt flakes includes the following steps:

[0030] Step 1: Basalt flake pretreatment:

[0031] Basalt flakes were first immersed in a 2 mol / L sodium hydroxide solution for etching. The ratio of basalt flakes to sodium hydroxide solution was 10 g: 200 mL, and the etching time was 1 h, resulting in pretreated basalt flakes.

[0032] Step 2, Preparation of borosilicate resin:

[0033] Then, phenyltriethoxysilane and boric acid were mixed in a molar ratio of 1:1.5, xylene was added, and the molar ratio of xylene to phenyltriethoxysilane was 0.5:1. The mixture was reacted at 80°C for 4 hours to produce borosilicate resin.

[0034] Step 3: Preparation of the resin mixture system:

[0035] Then, according to the formula ratio, 30 parts borosilicate resin and 45 parts organosilicon resin were mixed at a mass ratio of 1:1.5 to form a composite resin matrix. Next, 25 parts of pretreated basalt flakes were added to obtain the resin mixture system, with the pigment-to-binder ratio controlled at 33.3. wt %

[0036] Step 4, Curing process:

[0037] Finally, tetrabutyl titanate as a curing agent was added at a ratio of 100:1 (total mass of resin mixture: mass of tetrabutyl titanate). After mixing, the mixture was stirred for 12 hours to obtain a uniformly mixed high-temperature fireproof coating.

[0038] Example 2

[0039] A method for preparing a high-temperature resistant fire-retardant coating based on basalt flakes includes the following steps:

[0040] Step 1: Basalt flake pretreatment:

[0041] First, according to the formula ratio, basalt flakes were immersed in 1 mol / L sodium hydroxide solution for etching. The ratio of basalt flakes to sodium hydroxide solution was 10 g: 300 mL, and the etching time was 2 h to obtain pretreated basalt flakes.

[0042] Step 2, Preparation of borosilicate resin:

[0043] Then, according to the formula ratio, phenyltriethoxysilane and boric acid are mixed in a molar ratio of 1:1, xylene is added, and the molar ratio of xylene to phenyltriethoxysilane is 0.5:1. The mixture is reacted at 60°C for 3 hours to generate borosilicate resin.

[0044] Step 3: Preparation of the resin mixture system:

[0045] Then, according to the formula ratio, 30 parts borosilicate resin and 30 parts organosilicon resin were mixed in a 1:1 mass ratio to form a composite resin matrix. Next, 40 parts of pretreated basalt flakes were added to obtain the resin mixture system, with the pigment-to-binder ratio controlled at 66.7. wt %

[0046] Step 4, Curing process:

[0047] Finally, tetrabutyl titanate as a curing agent was added according to the ratio of total mass of resin mixture to mass of tetrabutyl titanate = 100:0.5. After mixing, the mixture was stirred for 18 hours to obtain a uniformly mixed high-temperature fireproof coating.

[0048] Example 3

[0049] A method for preparing a high-temperature resistant fire-retardant coating based on basalt flakes includes the following steps:

[0050] Step 1: Basalt flake pretreatment:

[0051] First, according to the formula ratio, basalt flakes were immersed in 3 mol / L sodium hydroxide solution for etching. The ratio of basalt flakes to sodium hydroxide solution was 10 g: 500 mL, and the etching time was 1.5 h to obtain pretreated basalt flakes.

[0052] Step 2, Preparation of borosilicate resin:

[0053] Then, according to the formula ratio, phenyltriethoxysilane and boric acid are mixed in a molar ratio of 1:2 and reacted at 100°C for 5 hours to generate borosilicate resin.

[0054] Step 3: Preparation of the resin mixture system:

[0055] Then, according to the formula ratio, 20 parts borosilicate resin and 40 parts organosilicon resin were mixed at a mass ratio of 1:2 to form a composite resin matrix. Next, 25 parts of pretreated basalt flakes were added to obtain the resin mixture system, with the pigment-to-binder ratio controlled at 41.6. wt %

[0056] Step 4, Curing process:

[0057] Finally, tetrabutyl titanate as a curing agent was added at a ratio of 100:2 (total mass of resin mixture: mass of tetrabutyl titanate). After mixing, the mixture was stirred for 24 hours to obtain a uniformly mixed high-temperature fireproof coating.

[0058] The sources of the raw materials involved in each embodiment are shown in Table 1.

[0059] Table 1. Sources of raw materials for high-temperature fire-retardant coatings in each embodiment.

[0060]

[0061] Comparative Example 1

[0062] Existing paint: 60 wt % silicone resin, 35 wt % mica filler, 1 wt % KH-550 curing agent and 4 wt % solvent (such as xylene).

[0063] The existing methods for preparing coatings are as follows:

[0064] Step 1: Pre-treatment of raw materials

[0065] Organosilicon resin: If it is in solid state, it needs to be heated to 60~80℃ to melt (liquid state can be used directly);

[0066] Mica filler: Dry at 100~120℃ for 1~2 hours to remove moisture;

[0067] KH-550 hardener: Use the undiluted solution directly to avoid moisture absorption;

[0068] Step 2: Mixing resin and filler

[0069] Then, stir 60% silicone resin at low speed (300~500 rpm), slowly add 35% mica filler, and avoid agglomeration. When the temperature rises to 50~60℃, disperse at high speed (1500~2000 rpm) for 20~30 minutes until uniform.

[0070] Step 3: Add curing agent and solvent

[0071] Then cool down to below 30-40℃, add 1 wt Add % KH-550 curing agent, stir at low speed for 10-30 minutes, and add 4% solvent (such as xylene) as needed to adjust the viscosity.

[0072] Application Example 1

[0073] The high-temperature fireproof coating prepared in Example 1 was applied to the surface of a substrate (steel, aluminum and other metal structural components) with a coating thickness of 10 μm and cured at room temperature for 24 hours to form a high-temperature fireproof coating on the substrate surface.

[0074] The high-temperature resistant fireproof coating worked continuously at 800℃ (inside a muffle furnace) for 52 hours without cracking, and maintained its structural integrity for 35 minutes under high-temperature impact at 2000℃ (butane gas flame); the adhesion was 5.8 MPa.

[0075] Application Example 2

[0076] The high-temperature fireproof coating prepared in Example 3 was applied to the surface of a substrate (steel, aluminum and other metal structural components) with a coating thickness of 10 μm and cured at room temperature for 24 hours to form a high-temperature fireproof coating on the substrate surface.

[0077] The high-temperature resistant fireproof coating can operate continuously at 800℃ (inside a muffle furnace) for 60 hours without cracking, and maintains structural integrity for 40 minutes under high-temperature impact at 2000℃ (butane gas flame); the adhesion is 6.2 MPa.

[0078] Application Example 3

[0079] The existing coating prepared in Comparative Example 1 was applied to a substrate (metal structural components such as steel and aluminum) with a coating thickness of 10 μm and cured at room temperature for 24 hours to form a high-temperature fireproof coating on the substrate surface.

[0080] The high-temperature fireproof coating cracked after 8 hours at 800°C (inside a muffle furnace) and peeled off after 5 minutes under high-temperature impact at 2000°C (butane gas flame); the adhesion was 3.0 MPa.

[0081] The above embodiments are not intended to limit the product form and style of the present invention. Any appropriate changes or modifications made by those skilled in the art should be considered as not departing from the patent scope of the present invention.

Claims

1. A high-temperature resistant fireproof coating based on basalt flakes, characterized in that: By weight, it includes the following raw materials in the following amounts: 25-40 parts basalt flakes, 20-30 parts borosilicate resin, 30-45 parts organosilicon resin and 0.5-2 parts tetrabutyl titanate; The preparation method of the high-temperature fire-retardant coating based on basalt flakes includes the following steps: Step 1: Basalt flake pretreatment: First, according to the formula ratio, basalt flakes are immersed in 1~3 mol / L sodium hydroxide solution for etching for 1~2 h to obtain pretreated basalt flakes; Step 2, Preparation of borosilicate resin: Then, according to the formula ratio, phenyltriethoxysilane and boric acid are mixed in a molar ratio of 1:1~2 and reacted at 60~100℃ for 3~5 hours to generate borosilicate resin. Step 3: Preparation of the resin mixture system: Then, according to the formula ratio, borosilicate resin and organosilicon resin are mixed at a mass ratio of 1:1~2 to form a composite resin matrix. Pretreated basalt flakes are then added to obtain the resin mixture system, wherein the ratio of basalt flakes to the composite resin matrix is ​​controlled at 30%. wt % ~ 70 wt % Step 4, Curing treatment: Finally, add tetrabutyl titanate as a curing agent according to the total mass of the resin mixture: the mass of tetrabutyl titanate = 100: 0.5~2, and stir for 12~24 hours after mixing to obtain a uniformly mixed high-temperature fireproof coating. In step 3, the silicone resin is a polymethylphenylsiloxane resin.

2. The high-temperature fire-retardant coating based on basalt flakes according to claim 1, characterized in that: In step 1, the ratio of basalt flakes to sodium hydroxide solution is 10g: 200~500mL.

3. The high-temperature fire-retardant coating based on basalt flakes according to claim 1, characterized in that: In step 2, an excipient is added to the mixture of phenyltriethoxysilane and boric acid, wherein the molar ratio of the excipient to phenyltriethoxysilane is 0.5:

1.

4. The high-temperature fire-retardant coating based on basalt flakes according to claim 3, characterized in that: In step 2, the excipient is xylene.

Images