Two-component fireproof heat-insulating coating and preparation method thereof
By using a two-component system in fire-resistant thermal insulation coatings, combining bisphenol A-type epoxy resin, expanded flame retardant, modified fibers and wollastonite, a cross-linked flame retardant layer is formed, which solves the problem of insufficient carbonization strength of the existing coatings, significantly improves burning resistance and adhesion, and achieves long-term fire and heat insulation protection of the building.
Patent Information
- Application Number
- CN202411541898.3
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2024-10-31
- Publication Date
- 2025-02-25
- Estimated Expiration
- 2044-10-31
AI Technical Summary
The carbon-forming strength of existing fire-resistant and heat-insulating coatings is insufficient, and the carbon layer is prone to fall off, resulting in fire-proof and heat-insulating failure, affecting the fire-proof protection of buildings.
Two-component fire-retardant and heat-insulating coatings are used, including agent A and agent B. Bisphenol A-type epoxy resin, expanded flame retardant, glass fiber, needle-shaped wollastonite and vapor-phase silica are added to agent B. Polyamide curing agent, diluent and modified needle-shaped wollastonite are added to form a dense flame retardant layer through cross-linking reaction, which improves the strength and adhesion of the carbon layer.
It significantly improves the charcoal strength of the coating, extends the burn-resistant time, enhances the thermal stability and adhesion of the coating, and ensures long-term fire-proof and thermal insulation protection of the building.
Abstract
Description
Technical Field
[0001] The present application relates to the field of coatings, and more specifically, to a two-component fireproof and heat-insulating coating and a preparation method thereof. Background Art
[0002] Fireproof and heat-insulating coatings are generally composed of base materials, dispersants, flame retardants, fillers, additives and other components. They have fireproof and heat-insulating effects and can be applied on the surface of buildings to improve the fire resistance of buildings. They are a widely used special coating. At present, fireproof and heat-insulating coatings are mainly intumescent fire-retardant coatings. In the event of a fire, intumescent fire-retardant coatings can foam to form a foam layer, isolate oxygen to flame retardant and protect the building. However, the carbonization strength of intumescent fire-retardant coatings is insufficient, and the carbon layer is easy to fall off, causing the fireproof and heat-insulating failure, affecting the safety of life and property. How to provide a fireproof and heat-insulating coating with a long burning time and not easy to fall off, so that it can provide long-term protection for buildings, has high research and development and production value. Summary of the invention
[0003] In order to solve the problem that fire-proof and heat-insulating coatings have low charring strength and are easy to fall off, the present application provides a two-component fire-proof and heat-insulating coating and a preparation method thereof.
[0004] In the first aspect, the present application provides a two-component fireproof and heat-insulating coating, including agent A and agent B, wherein agent A includes the following raw materials in parts by weight: 10-20 parts of bisphenol A epoxy resin, 40-50 parts of intumescent flame retardant, 2-4 parts of glass fiber, 2-4 parts of needle-shaped wollastonite, 3-7 parts of fumed silica, 10-20 parts of diluent, 0.3-0.5 parts of leveling agent, 8-15 parts of epoxy cage-type polysilsesquioxane-modified glass fiber; agent B includes the following raw materials in parts by weight: 10-20 parts of polyamide curing agent, 10-15 parts of diluent, 7-10 parts of amino cage-type polysilsesquioxane-modified needle-shaped wollastonite; Preferably, the mass ratio of agent A to agent B is (2-3):1.
[0005] Bisphenol A epoxy resin and polyamide curing agent are used as raw materials. After curing, the coating has good adhesion to the substrate and small volume shrinkage, and can better exert the flame retardant and heat insulation effects of the flame retardant and filler, thus providing better protection for the substrate. A certain amount of intumescent flame retardant is added, which is dehydrated after heating to form a fluffy, porous, closed-structure carbon layer, which weakens the heat conduction between the substrate and the heat source and prevents the diffusion of combustible gas, thus achieving the effect of fireproofing and heat insulation. A certain amount of fumed silica is added as a thixotropic agent to effectively prevent the sedimentation of glass fiber and needle-shaped wollastonite in the coating, making the carbonization more stable, reducing the adverse effect on the adhesion of the coating film, and making the obtained coating more uniform. The intumescent flame retardant can better protect the substrate as a whole after expansion. By adding a certain amount of epoxy cage polysilsesquioxane-modified glass fiber to agent A and adding a certain amount of amino cage polysilsesquioxane-modified needle-shaped wollastonite to agent B, the modified glass fiber and needle-shaped wollastonite have better compatibility with the coating; the epoxy cage polysilsesquioxane and the amino cage polysilsesquioxane migrate to the upper layer of the coating and participate in the curing of bisphenol A epoxy resin and polyamide curing agent to form a flame retardant layer, so that the prepared fireproof and heat-insulating coating is more uniform and dense, and has better fireproof and heat-insulating effects, forming a barrier layer with higher thermal stability, and working together with the intumescent flame retardant, the barrier layer formed is stronger and denser, and has better fireproof and heat-insulating effects; in the process of migration of the cage polysilsesquioxane to the upper layer of the coating, the glass fiber and needle-shaped wollastonite are driven to be better arranged and interspersed in the upper layer of the coating, further improving the heat insulation effect. Needle-shaped wollastonite has a natural needle-shaped structure, good thermal insulation effect, stable performance, can improve the mechanical and friction properties of the coating matrix, enhance the thermal stability and dimensional stability of the coating, glass fiber has a good thermal insulation effect, and also has a fibrous structure. By adding glass fibers and needle-shaped wollastonite with different melting points and forms as fillers, interspersed inside the coating, the fireproof and heat-insulating coating obtained is not easy to fall off after carbonization, which improves the carbonization strength of the coating, making the carbon layer more difficult to fall off and longer burning time. Through the joint action of the above components, the glass fibers and needle-shaped wollastonite on the upper layer of the coating are densely arranged, and the lower layer of the coating also contains unmodified glass fibers and needle-shaped wollastonite interspersed and arranged, forming a multi-layer thermal insulation reinforcement structure of the coating with good performance.
[0006] In a specific embodiment, the aspect ratio of the glass fiber in the glass fiber and the epoxy cage polysilsesquioxane modified glass fiber is 300-600:1, and the aspect ratio of the acicular wollastonite and the amino cage polysilsesquioxane modified acicular wollastonite is 10-20:1.
[0007] By adopting the above technical scheme, glass fibers with relatively large lengths and diameters are not easy to fall out of the coating, have good interface bonding, and have good heat barrier effect. The coating is flexible and not easy to crack, and has good adhesion to the substrate. The needle-shaped wollastonite with relatively small lengths and diameters is evenly interspersed and arranged among the glass fibers in the coating to fill the gaps and form a good mechanical interlocking with the glass fibers, which has a good effect on reinforcing the structure of the coating. The resulting coating has good fire resistance and strong adhesion.
[0008] In a specific embodiment, the mass ratio of epoxy cage polysilsesquioxane grafted glass fiber to amino cage polysilsesquioxane modified needle-shaped wollastonite is 1.5:1.
[0009] The inventors found through experiments that the above ratio can achieve the optimal flame retardant effect. This may be because the epoxy cage polysilsesquioxane grafted glass fiber and the amino cage polysilsesquioxane modified needle-shaped wollastonite can better participate in the cross-linking of the coating, the barrier layer formed on the coating surface has an appropriate thickness, and the glass fiber and needle-shaped wollastonite achieve the optimal arrangement.
[0010] In a specific embodiment, the mass ratio of glass fiber to needle-shaped wollastonite is 1:(0.9-1.1).
[0011] By adopting the above technical solution, the addition content of roughened glass fiber needle-shaped wollastonite is appropriate, which has a good effect on improving the strength and adhesion performance of carbonization.
[0012] In a specific embodiment, the preparation steps of epoxy cage-type polysilsesquioxane include: mixing water and acetone evenly, adding sodium hydroxide to dissolve, adding phenyltrimethoxysilane and 3-glycidyloxypropyltrimethoxysilane dropwise, concentrating by rotary evaporation after the reaction, drying, washing with water to neutrality, and drying to obtain epoxy cage-type polysilsesquioxane. Any conventional preparation process or commercially available functional poss can be used for the modification step of the present application. Preferably, the present application prepares poss containing epoxy and hydroxyl groups by conventional hydrolysis. The corner-missing poss generated by controlling the reaction conditions contains hydroxyl and epoxy groups, which is beneficial to the modification of fillers, and has good compatibility in the coating, is evenly dispersed, and can better participate in the curing of the coating. The prepared coating is relatively uniform and dense, and has good fireproof and heat-insulating effects.
[0013] In a specific embodiment, the preparation steps of epoxy cage-type polysilsesquioxane grafted glass fiber include: adding epoxy cage-type polysilsesquioxane and glass fiber to ethanol aqueous solution, stirring evenly, ultrasonic treatment, heating reaction, reduced pressure distillation, suction filtration, washing, and vacuum drying to obtain epoxy cage-type polysilsesquioxane grafted glass fiber.
[0014] By adopting the above technical solution, the epoxy cage polysilsesquioxane and the glass fiber are modified. During the migration process, the epoxy cage polysilsesquioxane drives the glass fiber to arrange more evenly and tightly in the upper layer of the coating, fully isolating the heat intrusion from the heat source, and the modification steps are relatively simple.
[0015] In a specific embodiment, the glass fibers are roughened glass fibers.
[0016] By adopting the above technical scheme, the surface of the roughened glass fiber has more tiny depressions and active hydroxyl groups, and the modification effect with the epoxy cage-type semi-siloxane is better. The roughened glass fiber and the needle-shaped wollastonite are interspersed with each other in the coating system, and it is not easy to fall out after the coating is carbonized and expanded by heat, so that the carbonized coating still has high strength and is not easy to fall off, providing stable fireproof and heat-insulating protection for the substrate.
[0017] In a specific embodiment, the preparation steps of the roughened glass fiber include: adding the glass fiber to a hydrogen fluoride aqueous solution, then adding sodium sulfate, magnesium fluoride, and water, stirring evenly, filtering, washing, and drying to obtain the roughened glass fiber.
[0018] By adopting the above technical scheme, the roughening step is relatively simple, and the depressions formed on the surface of the glass fiber are relatively uniform. The roughened glass fiber obtained does not reduce the strength too much, and is evenly interspersed in the coating and is not easy to fall out. The structural stability of the coating after carbonization is greatly improved, and the burning time is longer.
[0019] In a specific embodiment, the intumescent flame retardant includes ammonium polyphosphate, pentaerythritol and melamine in a mass ratio of 1:2:(3-3.1).
[0020] By adopting the above technical scheme, the selection and proportion of acid source, carbon source and gas source can form carbon more stably and release a large amount of gas. The formed carbon layer can better seal the surface of the substrate, effectively block the transfer of heat to the substrate, and have a good flame retardant effect.
[0021] In a second aspect, the present application provides a method for preparing a two-component fire retardant and heat insulating coating, characterized in that the preparation method comprises the following steps: S1: Weigh the components of Agent A according to their weight, mix them, and stir them at a speed of 300-500 rpm for 5-10 minutes to obtain Agent A; S2: Weigh the components of Agent B according to their mass, mix them, and stir them at a speed of 400-900 rpm for 5-8 minutes to obtain Agent B; S3: When in use, agent A is mixed with agent B to obtain a fireproof and heat-insulating coating.
[0022] By adopting the above scheme, the preparation method is relatively simple, the components are mixed evenly, the needle-shaped wollastonite and glass fiber are well interspersed to increase the charring strength of the coating and block the heat, the epoxy cage-type polysilsesquioxane has good compatibility in the coating, participates in cross-linking to improve the strength and adhesion of the coating, the prepared coating is relatively uniform and smooth, the filler is not easy to precipitate, and the coating formed after curing has a good fireproof and heat-insulating protection effect on the substrate.
[0023] In summary, this application has the following beneficial effects: 1. The present application provides a flame retardant effect by adopting a large amount of intumescent flame retardant, adding bisphenol A epoxy resin, polyamide curing agent and epoxy cage polysilsesquioxane and limiting the mass ratio, epoxy cage polysilsesquioxane modified glass fiber and amino cage polysilsesquioxane modified needle-shaped wollastonite participate in cross-linking to form a flame retardant and heat-insulating effect in the upper layer of the coating film, and the surface of the obtained coating is denser after curing, and the protective effect on the substrate is good; by adding a certain mass of glass fiber and needle-shaped wollastonite and limiting the mass ratio, the interlacing of the two improves the strength of the carbon layer, and it is not easy to fall off after carbonization, further extending the burning time; the glass fiber is a coarsened glass fiber, so that its surface has more active groups and greater friction, and is more closely connected to the coating substrate, and the interlacing effect with the needle-shaped wollastonite is better, further improving the carbonization strength and the burning time.
[0024] 2. The present application further improves the filling effect and strength by limiting the aspect ratio of glass fiber and needle-shaped wollastonite, the mass ratio of epoxy cage polysilsesquioxane grafted glass fiber and amino cage polysilsesquioxane modified needle-shaped wollastonite, and the mass ratio of glass fiber to needle-shaped wollastonite. The coating surface has good structural stability after carbonization, which further improves the fire resistance performance. DETAILED DESCRIPTION
[0025] The following is a more specific description of the technical solution of the present invention in combination with several specific implementation examples. The embodiments are only partial embodiments of the present invention, not all of them. The following specific embodiments can be combined with each other, and the same or similar concepts or processes therein may not be repeated in some embodiments.
[0026] Unless otherwise specified, the experimental reagents in the preparation examples, embodiments and comparative examples are all conventional commercial brands or obtained through conventional preparation processes.
[0027] The bisphenol A epoxy resin of the present application was purchased from BL-CYDE of Yueyang Baling Jiayun Petrochemical Co., Ltd.; the polyamide curing agent is polyamide 650; ammonium polyphosphate is purchased from Haoyu International; pentaerythritol is purchased from Hubei Yihua; melamine is purchased from Aorong A012; the leveling agent is BYK-348; fumed silica is purchased from Hubei Huifu Nanomaterials HL380; the diluent is a mixture of xylene and n-butanol in a volume ratio of 1:1; the glass fiber is purchased from Chongjun Mineral Products Co., Ltd., with a diameter of 9-13μm and a short chopped length of 3mm; the needle-shaped wollastonite is purchased from Zhuanghua Mineral Products, with an aspect ratio of 2-3:1 and a mesh size of 325.
[0028] Preparation Example Preparation Example 1: Epoxy cage-type polysilsesquioxane: 10 ml of water and 140 ml of acetone were mixed evenly, 2.3 g of sodium hydroxide was added to dissolve, 12.8 g of phenyltrimethoxysilane and 3.4 g of 3-glycidyloxypropyltrimethoxysilane were added dropwise, and the mixture was reacted at 20° C. for 36 h, then concentrated by rotary evaporation, dried, washed with water until neutral, and dried to obtain epoxy cage-type polysilsesquioxane.
[0029] Preparation Example 2: Roughened glass fiber: 100g of glass fiber was added to 500g of 30% by volume hydrogen fluoride aqueous solution, and then 1.2g of sodium sulfate, 1g of magnesium fluoride, and 500ml of water were added, and stirred evenly. After 2 minutes, the mixture was filtered, washed with deionized water, and dried to obtain roughened glass fiber.
[0030] Preparation Example 3: Epoxy cage-type polysilsesquioxane modified glass fiber: 50 g of glass fiber and 40 g of the epoxy cage-type polysilsesquioxane prepared in Preparation Example 1 were added to 200 ml of a 25% wt ethanol aqueous solution, mixed, stirred for 1 hour, ultrasonically treated for 30 minutes, reacted at 80° C. for 20 hours, and then distilled under reduced pressure, filtered, washed, and vacuum dried for 7 hours to obtain epoxy cage-type polysilsesquioxane-modified glass fiber.
[0031] Preparation Example 4: Amino cage polysilsesquioxane modified needle-shaped wollastonite: Mix 10 ml of water and 140 ml of acetone evenly, add 2.3 g of sodium hydroxide to dissolve, add dropwise 12.8 g of phenyltrimethoxysilane and 3.1 g of (3-aminopropyl)trimethoxysilane, react at 20° C. for 36 h, then concentrate by rotary evaporation, dry, wash with water until neutral, and dry to obtain amino cage polysilsesquioxane.
[0032] 100 g of amino cage polysilsesquioxane and 40 g of needle-shaped wollastonite were added to 200 ml of 25% wt ethanol aqueous solution, mixed, stirred for 1 hour, ultrasonically treated for 30 minutes, heated to 80° C., reacted, and subjected to reduced pressure distillation after 20 hours, filtered, washed, and vacuum dried for 7 hours to obtain amino cage polysilsesquioxane-modified needle-shaped wollastonite. Example
[0033] Example 1 This embodiment includes the following raw materials by weight: Agent A: 100g of bisphenol A epoxy resin, 420g of intumescent flame retardant, including 70g of ammonium polyphosphate, 140g of pentaerythritol, 210g of melamine, 20g of glass fiber, 20g of needle-shaped wollastonite, 70g of fumed silica, 100g of diluent, 5g of leveling agent, 80g of epoxy cage-type polysilsesquioxane-modified glass fiber obtained in Preparation Example 3; Agent B: 200g of polyamide curing agent, 100g of diluent, 100g of amino cage-type polysilsesquioxane-modified needle-shaped wollastonite obtained in Preparation Example 4.
[0034] The preparation method is as follows: S1: Weigh the components of Agent A according to their mass, mix them, and stir them at a speed of 400 rpm for 8 minutes to obtain Agent A; S2: Weigh the components of Agent B according to their mass, mix them, and stir them at a speed of 700 rpm for 8 minutes to obtain Agent B; S3: The amount of Agent A prepared in S1 and the amount of Agent B prepared in S2 are mixed, and stirred at a speed of 800 rpm for 15 minutes to obtain a fire retardant and heat insulating coating.
[0035] Example 2 This embodiment includes the following raw materials by weight: Agent A: 200g of bisphenol A epoxy resin, 420g of intumescent flame retardant, including 70g of ammonium polyphosphate, 140g of pentaerythritol, 210g of melamine, 40g of glass fiber, 40g of needle-shaped wollastonite, 70g of fumed silica, 100g of diluent, 5g of leveling agent, 100g of epoxy cage-type polysilsesquioxane-modified glass fiber prepared in Preparation Example 3; Agent B: 100g of polyamide curing agent, 150g of diluent, 100g of amino cage-type polysilsesquioxane-modified needle-shaped wollastonite prepared in Preparation Example 4.
[0036] The preparation method is as follows: S1: Weigh the components of Agent A according to their mass, mix them, and stir them at a speed of 400 rpm for 8 minutes to obtain Agent A; S2: Weigh the components of Agent B according to their mass, mix them, and stir them at a speed of 700 rpm for 8 minutes to obtain Agent B; S3: The amount of Agent A prepared in S1 and the amount of Agent B prepared in S2 are mixed, and stirred at a speed of 800 rpm for 15 minutes to obtain a fire retardant and heat insulating coating.
[0037] Example 3 This embodiment includes the following raw materials by weight: Agent A: 125g of bisphenol A epoxy resin, 420g of intumescent flame retardant, including 70g of ammonium polyphosphate, 140g of pentaerythritol, 210g of melamine, 30g of glass fiber, 30g of needle-shaped wollastonite, 50g of fumed silica, 100g of diluent, 4g of leveling agent, 150g of epoxy cage-type polysilsesquioxane-modified glass fiber obtained in Preparation Example 3; Agent B: 150g of polyamide curing agent, 120g of diluent, 70g of amino cage-type polysilsesquioxane-modified needle-shaped wollastonite obtained in Preparation Example 4.
[0038] The preparation method is as follows: S1: Weigh the components of Agent A according to their mass, mix them, and stir them at a speed of 400 rpm for 8 minutes to obtain Agent A; S2: Weigh the components of Agent B according to their mass, mix them, and stir them at a speed of 700 rpm for 8 minutes to obtain Agent B; S3: The amount of Agent A prepared in S1 and the amount of Agent B prepared in S2 are mixed, and stirred at a speed of 800 rpm for 15 minutes to obtain a fire retardant and heat insulating coating.
[0039] Example 4 This embodiment includes the following raw materials by weight: Agent A: 125g of bisphenol A epoxy resin, 420g of intumescent flame retardant, including 70g of ammonium polyphosphate, 140g of pentaerythritol, 210g of melamine, 30g of glass fiber, 30g of needle-shaped wollastonite, 50g of fumed silica, 100g of diluent, 4g of leveling agent, 132g of epoxy cage-type polysilsesquioxane-modified glass fiber obtained in Preparation Example 3; Agent B: 150g of polyamide curing agent, 120g of diluent, 88g of amino cage-type polysilsesquioxane-modified needle-shaped wollastonite obtained in Preparation Example 4.
[0040] The preparation method is as follows: S1: Weigh the components of Agent A according to their mass, mix them, and stir them at a speed of 400 rpm for 8 minutes to obtain Agent A; S2: Weigh the components of Agent B according to their mass, mix them, and stir them at a speed of 700 rpm for 8 minutes to obtain Agent B; S3: The amount of Agent A prepared in S1 and the amount of Agent B prepared in S2 are mixed, and stirred at a speed of 800 rpm for 15 minutes to obtain a fire retardant and heat insulating coating.
[0041] Example 5 This embodiment includes the following raw materials by weight: Agent A: 125g of bisphenol A epoxy resin, 420g of intumescent flame retardant, including 70g of ammonium polyphosphate, 140g of pentaerythritol, 210g of melamine, 30g of glass fiber, 30g of needle-shaped wollastonite, 50g of fumed silica, 100g of diluent, 4g of leveling agent, 125g of epoxy cage-type polysilsesquioxane-modified glass fiber obtained in Preparation Example 3; Agent B: 150g of polyamide curing agent, 120g of diluent, 95g of amino cage-type polysilsesquioxane-modified needle-shaped wollastonite obtained in Preparation Example 4.
[0042] The preparation method is as follows: S1: Weigh the components of Agent A according to their mass, mix them, and stir them at a speed of 400 rpm for 8 minutes to obtain Agent A; S2: Weigh the components of Agent B according to their mass, mix them, and stir them at a speed of 700 rpm for 8 minutes to obtain Agent B; S3: The amount of Agent A prepared in S1 and the amount of Agent B prepared in S2 are mixed, and stirred at a speed of 800 rpm for 15 minutes to obtain a fire retardant and heat insulating coating.
[0043] Example 6 This embodiment includes the following raw materials by weight: Agent A: 125g of bisphenol A epoxy resin, 420g of intumescent flame retardant, including 70g of ammonium polyphosphate, 140g of pentaerythritol, 210g of melamine, 30g of glass fiber, 30g of needle-shaped wollastonite, 50g of fumed silica, 100g of diluent, 4g of leveling agent, 140g of epoxy cage-type polysilsesquioxane-modified glass fiber obtained in Preparation Example 3; Agent B: 150g of polyamide curing agent, 120g of diluent, 80g of amino cage-type polysilsesquioxane-modified needle-shaped wollastonite obtained in Preparation Example 4.
[0044] The preparation method is as follows: S1: Weigh the components of Agent A according to their mass, mix them, and stir them at a speed of 400 rpm for 8 minutes to obtain Agent A; S2: Weigh the components of Agent B according to their mass, mix them, and stir them at a speed of 700 rpm for 8 minutes to obtain Agent B; S3: The amount of Agent A prepared in S1 and the amount of Agent B prepared in S2 are mixed, and stirred at a speed of 800 rpm for 15 minutes to obtain a fire retardant and heat insulating coating.
[0045] Example 7 This embodiment includes the following raw materials by weight: Agent A: 125g of bisphenol A epoxy resin, 420g of intumescent flame retardant, including 70g of ammonium polyphosphate, 140g of pentaerythritol, 210g of melamine, 30g of roughened glass fiber prepared in Preparation Example 2, 30g of needle-shaped wollastonite, 50g of fumed silica, 100g of diluent, 4g of leveling agent, 132g of epoxy cage-type polysilsesquioxane-modified glass fiber prepared in Preparation Example 3; Agent B: 150g of polyamide curing agent, 120g of diluent, 88g of amino cage-type polysilsesquioxane-modified needle-shaped wollastonite prepared in Preparation Example 4.
[0046] The preparation method is as follows: S1: Weigh the components of Agent A according to their mass, mix them, and stir them at a speed of 400 rpm for 8 minutes to obtain Agent A; S2: Weigh the components of Agent B according to their mass, mix them, and stir them at a speed of 700 rpm for 8 minutes to obtain Agent B; S3: The amount of Agent A prepared in S1 and the amount of Agent B prepared in S2 are mixed, and stirred at a speed of 800 rpm for 15 minutes to obtain a fire retardant and heat insulating coating.
[0047] Comparative Example Comparative Example 1 This comparative example includes the following raw materials by weight: Agent A: 125g of bisphenol A epoxy resin, 420g of intumescent flame retardant, including 70g of ammonium polyphosphate, 140g of pentaerythritol, 210g of melamine, 30g of glass fiber, 30g of needle-shaped wollastonite, 50g of fumed silica, 100g of diluent, and 4g of leveling agent; Agent B: 150g of polyamide curing agent and 120g of diluent.
[0048] The preparation method is as follows: S1: Weigh the components of Agent A according to their mass, mix them, and stir them at a speed of 400 rpm for 8 minutes to obtain Agent A; S2: Weigh the components of Agent B according to their mass, mix them, and stir them at a speed of 700 rpm for 8 minutes to obtain Agent B; S3: The amount of Agent A prepared in S1 and the amount of Agent B prepared in S2 are mixed, and stirred at a speed of 800 rpm for 15 minutes to obtain a fire retardant and heat insulating coating.
[0049] Comparative Example 2 This comparative example includes the following raw materials by weight: Agent A: 125g of bisphenol A epoxy resin, 420g of intumescent flame retardant, including 70g of ammonium polyphosphate, 140g of pentaerythritol, 210g of melamine, 30g of glass fiber, 30g of needle-shaped wollastonite, 50g of fumed silica, 100g of diluent, and 4g of leveling agent; Agent B: 150g of polyamide curing agent, 120g of diluent, and 70g of amino cage-type polysilsesquioxane modified needle-shaped wollastonite obtained in Preparation Example 4.
[0050] The preparation method is as follows: S1: Weigh the components of Agent A according to their mass, mix them, and stir them at a speed of 400 rpm for 8 minutes to obtain Agent A; S2: Weigh the components of Agent B according to their mass, mix them, and stir them at a speed of 700 rpm for 8 minutes to obtain Agent B; S3: The amount of Agent A prepared in S1 and the amount of Agent B prepared in S2 are mixed, and stirred at a speed of 800 rpm for 15 minutes to obtain a fire retardant and heat insulating coating.
[0051] Comparative Example 3 This comparative example includes the following raw materials by weight: Agent A: 125g of bisphenol A epoxy resin, 420g of intumescent flame retardant, including 70g of ammonium polyphosphate, 140g of pentaerythritol, 210g of melamine, 30g of glass fiber, 30g of needle-shaped wollastonite, 50g of fumed silica, 100g of diluent, 4g of leveling agent, 150g of epoxy cage-type polysilsesquioxane modified glass fiber obtained in Preparation Example 3; Agent B: 150g of polyamide curing agent and 120g of diluent.
[0052] The preparation method is as follows: S1: Weigh the components of Agent A according to their mass, mix them, and stir them at a speed of 400 rpm for 8 minutes to obtain Agent A; S2: Weigh the components of Agent B according to their mass, mix them, and stir them at a speed of 700 rpm for 8 minutes to obtain Agent B; S3: The amount of Agent A prepared in S1 and the amount of Agent B prepared in S2 are mixed, and stirred at a speed of 800 rpm for 15 minutes to obtain a fire retardant and heat insulating coating.
[0053] Comparative Example 4 This comparative example includes the following raw materials by weight: Agent A: 125g of bisphenol A epoxy resin, 420g of intumescent flame retardant, including 70g of ammonium polyphosphate, 140g of pentaerythritol, 210g of melamine, 90g of glass fiber, 30g of needle-shaped wollastonite, 50g of fumed silica, 100g of diluent, 4g of leveling agent, 90g of epoxy cage-type polysilsesquioxane obtained in Preparation Example 1; Agent B: 150g of polyamide curing agent, 120g of diluent, 40g of amino cage-type polysilsesquioxane, and 30g of needle-shaped wollastonite.
[0054] The preparation method is as follows: S1: Weigh the components of Agent A according to their mass, mix them, and stir them at a speed of 400 rpm for 8 minutes to obtain Agent A; S2: Weigh the components of Agent B according to their mass, mix them, and stir them at a speed of 700 rpm for 8 minutes to obtain Agent B; S3: The amount of Agent A prepared in S1 and the amount of Agent B prepared in S2 are mixed, and stirred at a speed of 800 rpm for 15 minutes to obtain a fire retardant and heat insulating coating.
[0055] Comparative Example 5 This comparative example includes the following raw materials by weight: Agent A: 125g of bisphenol A epoxy resin, 420g of intumescent flame retardant, including 70g of ammonium polyphosphate, 140g of pentaerythritol, 210g of melamine, 90g of glass fiber, 30g of needle-shaped wollastonite, 50g of fumed silica, 100g of diluent, 4g of leveling agent, 90g of epoxy cage-type polysilsesquioxane prepared in Preparation Example 1; Agent B: 150g of polyamide curing agent, 120g of diluent, 70g of amino cage-type polysilsesquioxane-modified needle-shaped wollastonite prepared in Preparation Example 4.
[0056] The preparation method is as follows: S1: Weigh the components of Agent A according to their mass, mix them, and stir them at a speed of 400 rpm for 8 minutes to obtain Agent A; S2: Weigh the components of Agent B according to their mass, mix them, and stir them at a speed of 700 rpm for 8 minutes to obtain Agent B; S3: The amount of Agent A prepared in S1 and the amount of Agent B prepared in S2 are mixed, and stirred at a speed of 800 rpm for 15 minutes to obtain a fire retardant and heat insulating coating.
[0057] Comparative Example 6 This comparative example includes the following raw materials by weight: Agent A: 125g of bisphenol A epoxy resin, 420g of intumescent flame retardant, including 70g of ammonium polyphosphate, 140g of pentaerythritol, 210g of melamine, 30g of glass fiber, 30g of needle-shaped wollastonite, 50g of fumed silica, 100g of diluent, 4g of leveling agent, 150g of epoxy cage-type polysilsesquioxane modified glass fiber obtained in Preparation Example 3; Agent B: 150g of polyamide curing agent, 120g of diluent, 40g of amino cage-type polysilsesquioxane, and 30g of needle-shaped wollastonite.
[0058] The preparation method is as follows: S1: Weigh the components of Agent A according to their mass, mix them, and stir them at a speed of 400 rpm for 8 minutes to obtain Agent A; S2: Weigh the components of Agent B according to their mass, mix them, and stir them at a speed of 700 rpm for 8 minutes to obtain Agent B; S3: The amount of Agent A prepared in S1 and the amount of Agent B prepared in S2 are mixed, and stirred at a speed of 800 rpm for 15 minutes to obtain a fire retardant and heat insulating coating.
[0059] Performance test test 1: The fire retardant and heat-insulating coatings prepared in each embodiment and comparative example were coated on Q235 steel with a thickness of 1.5 mm, and the coating was cured. Then, the fire resistance limit test was carried out in accordance with the standard "GB / T14907-2002". The test results are shown in Table 1.
[0060] Test 2: The fire retardant and heat-insulating coatings prepared in each embodiment and comparative example were coated on Q235 steel with a thickness of 1.5 mm. The coating was cured and the adhesion of the coating to the steel was tested according to GB / T5210 (MPa). The test results are shown in Table 1.
[0061] Table 1 Fire resistance limit / h Adhesion / MPa Example 1 6.6 21.4 Example 2 6.9 23.5 Example 3 7.0 22.3 Example 4 7.7 22.0 Example 5 7.5 21.9 Example 6 7.4 22.1 Example 7 7.9 22.6 Comparative Example 1 4.8 18.6 Comparative Example 2 5.4 19.5 Comparative Example 3 5.3 19.9 Comparative Example 4 5.1 20.7 Comparative Example 5 5.8 21.4 Comparative Example 6 5.7 21.2 In combination with Examples 1-3, Comparative Examples 1-6 and Table 1, the present application adds a large amount of intumescent flame retardant to bisphenol A epoxy resin, adds epoxy cage polysilsesquioxane grafted glass fiber, amino cage polysilsesquioxane grafted needle-shaped wollastonite, and limits their size to enhance the flame retardant effect and participate in cross-linking, limits the mass ratio of needle-shaped wollastonite and glass fiber to enhance the carbonization strength and reduce the shedding of the carbon layer. The obtained coating has better fire resistance and adhesion after curing, and can provide stable fireproof and heat-insulating protection for buildings for a long time.
[0062] In combination with Examples 3-6 and Table 1, the present application further optimizes the cross-linking structure by limiting the mass ratio of epoxy cage polysilsesquioxane grafted glass fiber and amino cage polysilsesquioxane grafted needle-shaped wollastonite, thereby improving the flame retardant and heat insulation effects, and improving the fire resistance limit and adhesion performance.
[0063] In combination with Example 3, Example 7 and Table 1, the present application further limits the glass fiber to a roughened glass fiber. The higher friction of the roughened glass fiber allows the coating to adhere stably and firmly after carbonization, thereby providing better protection for the substrate.
[0064] This specific embodiment is merely an explanation of the present application and is not a limitation of the present application. After reading this specification, those skilled in the art may make modifications to the present embodiment without any creative contribution as needed, but such modifications are protected by the patent law as long as they are within the scope of the claims of the present application.
Claims
1. A two-component fireproof and heat-insulating coating, characterized in that: The raw materials of the thermal insulation coating include agent A and agent B. The agent A includes the following raw materials in parts by weight: 10-20 parts of bisphenol A epoxy resin, 40-50 parts of intumescent flame retardant, 2-4 parts of glass fiber, 2-4 parts of needle-shaped wollastonite, 3-7 parts of fumed silica, 10-20 parts of diluent, 0.3-0.5 parts of leveling agent, and 8-15 parts of epoxy cage-type polysilsesquioxane-modified glass fiber; the agent B includes the following raw materials in parts by weight: 10-20 parts of polyamide curing agent, 10-15 parts of diluent, and 7-10 parts of amino cage-type polysilsesquioxane-modified needle-shaped wollastonite.
2. The two-component fireproof and heat-insulating coating according to claim 1, characterized in that: The aspect ratio of the glass fiber is 300-600:1, and the aspect ratio of the needle-shaped wollastonite is 10-20:
1.
3. The two-component fireproof and heat-insulating coating according to claim 1, characterized in that: The mass ratio of the epoxy cage type polysilsesquioxane modified glass fiber to the amino cage type polysilsesquioxane modified needle-shaped wollastonite is 1.5:
1.
4. The two-component fireproof and heat-insulating coating according to claim 1, characterized in that: The mass ratio of glass fiber to needle-shaped wollastonite in the agent A is 1:(0.9-1.1).
5. The two-component fireproof and heat-insulating coating according to claim 1, characterized in that: The preparation steps of the epoxy cage type polysilsesquioxane include: mixing water and acetone evenly, adding sodium hydroxide to dissolve, dropping phenyltrimethoxysilane and 3-glycidyloxypropyltrimethoxysilane, concentrating by rotary evaporation after reaction, drying, washing with water until neutral, and drying to obtain the epoxy cage type polysilsesquioxane.
6. The two-component fireproof and heat-insulating coating according to claim 1, characterized in that: The preparation steps of the epoxy cage type polysilsesquioxane modified glass fiber include: adding epoxy cage type polysilsesquioxane and glass fiber into ethanol aqueous solution, stirring evenly, ultrasonic treatment, heating reaction, reduced pressure distillation, suction filtration, washing, vacuum drying to obtain epoxy cage type polysilsesquioxane modified glass fiber.
7. The two-component fireproof and heat-insulating coating according to claim 1, characterized in that: The glass fiber is a roughened glass fiber.
8. The two-component fireproof and heat-insulating coating according to claim 7, characterized in that: The preparation steps of the roughened glass fiber include: adding glass fiber into a hydrogen fluoride aqueous solution, then adding sodium sulfate, magnesium fluoride and water, stirring evenly, filtering, washing and drying to obtain the roughened glass fiber.
9. The two-component fireproof and heat-insulating coating according to claim 1, characterized in that: The intumescent flame retardant comprises ammonium polyphosphate, pentaerythritol and melamine in a mass ratio of 1:2:
3.
10. A method for preparing the two-component fireproof and heat-insulating coating according to any one of claims 1 to 9, characterized in that: The preparation method comprises the following steps: S1: Weigh the components of Agent A according to their weight, mix them, and stir them at a speed of 300-500 rpm for 5-10 minutes to obtain Agent A; S2: Weigh the components of Agent B according to their mass, mix them, and stir them at a speed of 400-900 rpm for 5-8 minutes to obtain Agent B; S3: When in use, agent A is mixed with agent B to obtain a fireproof and heat-insulating coating.
Citation Information
Patent Citations
High-performance epoxy resin and preparation method thereof
CN111205597A
Solvent-based ultrathin intumescent fire-retardant coating for steel structure and preparation method thereof
CN111961384A
Post-treatment enhancing method of TPU (Thermoplastic Polyurethane) workpiece
CN116023694A
Preparation and application of intumescent flame-retardant powder coating
CN118126603A
Flame retardant fillers prepared from bridged polysilsesquioxanes
US20140041908A1
Cited By
Outdoor intumescent fire retardant coating for steel structure and preparation method of outdoor intumescent fire retardant coating
CN122104005A