A two-component fireproof and heat-insulating coating and its preparation method
Through the design of two-component fire-resistant thermal insulation coatings, a dense barrier layer is formed using specific components and modification treatments, which solves the problem of low carbon strength and easy fall off of existing coatings, and achieves a long-term fire-resistant and thermal insulation effect.
Patent Information
- Application Number
- CN202411541898.3
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- Filing Date
- 2024-10-31
- Publication Date
- 2025-07-04
- Estimated Expiration
- 2044-10-31
AI Technical Summary
The existing fire-resistant and heat-insulating coatings have low carbon strength and are easy to fall off, affecting the fire-resistant and heat-insulating effect and cannot protect buildings for a long time.
Two-component fire-retardant and heat-insulating coatings are used, including agent A and agent B. A is composed of bisphenol A-type epoxy resin, expanded flame retardant, glass fiber, needle wollastonite, vapor-phase silica and diluent. Agent B is composed of polyamide curing agent, diluent and amino cage polysilsesquioxane modified needle wollastonite. By limiting the proportion of each component and the modification treatment, a dense barrier layer is formed to enhance the strength and adhesion of carbon.
The prepared paint is not easy to fall off after being charcoal, it has a long burn-resistant time, and has good fire-proof and heat insulation effect, which improves the thermal stability and mechanical properties of the paint and provides long-term protection.
Abstract
Description
Technical Field
[0001] This application relates to the field of coatings, and more specifically, it relates to a two-component fireproof and heat-insulating coating and a preparation method thereof. Background Art
[0002] Fireproof and heat-insulating coatings generally consist of components such as binders, dispersants, flame retardants, fillers, and additives, and have the effects of fireproofing and heat insulation. They can be coated on the surface of buildings to improve the fireproof ability of buildings. They are a widely used special coating. Currently, the fireproof and heat-insulating coatings are mainly intumescent fireproof coatings. In case of a fire, the intumescent fireproof coating can foam to form a foam layer, isolate oxygen to retard the fire, and play a role in protecting the building. However, the charring strength of the intumescent fireproof coating is insufficient, and the char layer is easy to fall off, resulting in the failure of fireproof and heat insulation and affecting the safety of life and property. How to provide a fireproof and heat-insulating coating with a long burning resistance time and not easy to fall off, so that it can provide long-term protection for buildings, has high research and production value. Summary of the Invention
[0003] In order to solve the problem that the fireproof and heat-insulating coating has low charring strength and is easy to fall off, this application provides a two-component fireproof and heat-insulating coating and a preparation method thereof.
[0004] In the first aspect, this application provides a two-component fireproof and heat-insulating coating, including Agent A and Agent B. 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 acicular 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-based cage-like polyhedral oligomeric silsesquioxane 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, and 7-10 parts of amino cage-like polyhedral oligomeric silsesquioxane modified acicular wollastonite;
[0005] Preferably, the mass ratio of Agent A to Agent B is (2-3):1.
[0006] Using bisphenol A epoxy resin and polyamide curing agent as raw materials, after curing, it has good adhesion to the matrix, small volume shrinkage, can better exert the flame retardant and heat insulation effects of the flame retardant and filler, and form better protection for the matrix; adding a certain mass of intumescent flame retardant, which dehydrates after heating to form a fluffy, porous and closed carbon layer, weakens the heat conduction between the substrate and the heat source, and prevents the diffusion of combustible gases, achieving the effect of fire prevention and heat insulation; adding a certain mass of fumed silica as a thixotropic agent, effectively preventing the settlement of glass fibers and acicular wollastonite in the coating, making the carbonization more stable, reducing the adverse impact on the film adhesion, and making the prepared coating more uniform. The intumescent flame retardant can better protect the substrate as a whole after expansion. By adding a certain mass of epoxy-functionalized polyhedral oligomeric silsesquioxane (POSS) modified glass fibers to agent A and a certain mass of amino-functionalized POSS modified acicular wollastonite to agent B, the modified glass fibers and acicular wollastonite have better compatibility with the coating; the epoxy-functionalized POSS and amino-functionalized POSS migrate to the upper layer of the coating film and participate in the curing of bisphenol A epoxy resin and polyamide curing agent to form a flame retardant layer. The prepared fireproof and heat-insulating coating is more uniform and dense, has better fireproof and heat-insulating effects, forms a barrier layer with high thermal stability, and together with the intumescent flame retardant, forms a stronger and denser barrier layer with better fireproof and heat-insulating effects; during the migration of POSS to the upper layer of the coating film, it drives the better arrangement and interpenetration of glass fibers and acicular wollastonite in the upper layer of the coating film, further improving the heat insulation effect. Acicular wollastonite has a natural acicular structure, good heat insulation effect and stable performance, can better improve the mechanical and friction properties of the coating matrix, and enhance the thermal stability and dimensional stability of the coating. Glass fibers have good heat insulation effects and fibrous structures. By adding glass fibers and acicular wollastonite with different melting points and morphologies as fillers and interpenetrating them inside the coating, the prepared fireproof and heat-insulating coating is not easy to fall off after carbonization, improving the carbonization strength of the coating, making the carbon layer more difficult to fall off and having a longer burning resistance time. Through the combined action of the above components, the glass fibers and acicular wollastonite in the upper layer of the coating film are densely arranged, and the lower layer of the coating film also contains unmodified glass fibers and acicular wollastonite arranged in an interpenetrating manner, forming a multi-layer heat insulation and reinforcement structure of the coating with good performance.
[0007] In a specific feasible embodiment, the aspect ratio of the glass fibers in the glass fibers and the epoxy-functionalized POSS modified glass fibers is 300 - 600:1, and the aspect ratio of the wollastonite in the acicular wollastonite and the amino-functionalized POSS modified acicular wollastonite is 10 - 20:1.
[0008] By adopting the above technical solution, glass fibers with a relatively large aspect ratio are not easily separated from the coating, have good interfacial bonding, good heat insulation effect, the coating is flexible and not easily cracked, has good adhesion to the substrate, and acicular wollastonite with a relatively small aspect ratio is evenly interspersed and arranged among the glass fibers in the coating, filling the gaps, forming a good mechanical interlock with the glass fibers, having a good effect on enhancing the structure of the coating, and the obtained coating has good fire resistance performance and strong adhesion.
[0009] In a specific feasible embodiment, the mass ratio of epoxy cage polyhedral oligomeric silsesquioxane grafted glass fiber to amino cage polyhedral oligomeric silsesquioxane modified acicular wollastonite is 1.5:1.
[0010] The inventor found through experiments that the above ratio can achieve the optimal flame retardant effect. This may be because epoxy cage polyhedral oligomeric silsesquioxane grafted glass fiber and amino cage polyhedral oligomeric silsesquioxane modified acicular wollastonite can better participate in the crosslinking of the coating, form a barrier layer with an appropriate thickness on the coating surface, and the glass fibers and acicular wollastonite achieve the optimal arrangement.
[0011] In a specific feasible embodiment, the mass ratio of glass fiber to acicular wollastonite is 1:(0.9 - 1.1).
[0012] By adopting the above technical solution, the addition content of roughened glass fiber acicular wollastonite is appropriate, and it has a good effect on improving the strength and adhesion performance of char formation.
[0013] In a specific feasible embodiment, the preparation steps of epoxy cage polyhedral oligomeric silsesquioxane include: mixing water and acetone evenly, adding sodium hydroxide to dissolve, dropping phenyltrimethoxysilane and 3-glycidyletheroxypropyltrimethoxysilane, concentrating by rotary evaporation after reaction, drying, washing to neutrality with water, and drying to obtain epoxy cage polyhedral oligomeric silsesquioxane. Any conventional preparation process or commercially available brand of functional POSS can be used in the modification step of this application. Preferably, in this application, POSS containing epoxy groups and hydroxyl groups is prepared by conventional hydrolysis, and the defective corner POSS generated by controlling the reaction conditions contains hydroxyl groups and epoxy groups, which is beneficial to modifying the filler, has good compatibility in the coating, is evenly dispersed, can better participate in the curing of the coating, and the obtained coating is relatively uniform and dense, with good fireproof and heat insulation effects.
[0014] In a specific feasible embodiment, the preparation steps of epoxy cage polyhedral oligomeric silsesquioxane grafted glass fiber include: adding epoxy cage polyhedral oligomeric silsesquioxane and glass fiber to an ethanol aqueous solution, stirring evenly, performing ultrasonic treatment, heating for reaction, distilling under reduced pressure, filtering, washing, and drying in vacuum to obtain epoxy cage polyhedral oligomeric silsesquioxane grafted glass fiber.
[0015] By adopting the above technical solution, epoxy-based cage-shaped polyhedral oligomeric silsesquioxane is modified with glass fiber. During the migration process, the epoxy-based cage-shaped polyhedral oligomeric silsesquioxane drives the glass fiber to be arranged more uniformly and tightly in the upper layer of the coating film, fully isolating the heat intrusion of the heat source, and the modification steps are relatively simple.
[0016] In a specific feasible embodiment, the glass fiber is a roughened glass fiber.
[0017] By adopting the above technical solution, the surface of the roughened glass fiber has more minute depressions and active hydroxyl groups, and has a better modification effect with the epoxy-based cage-shaped silsesquioxane. The roughened glass fiber and acicular wollastonite interpenetrate each other in the coating system and are not easily detached after the coating is heated and carbonized and expanded, so that the carbonized coating still has high strength and is not easily peeled off, providing stable fireproof and heat-insulating protection for the substrate.
[0018] In a specific feasible embodiment, the preparation steps of the roughened glass fiber include: adding the glass fiber into an aqueous hydrofluoric acid solution, then adding sodium sulfate, magnesium fluoride, and water, stirring evenly, filtering, washing, and drying to obtain the roughened glass fiber.
[0019] By adopting the above technical solution, the roughening steps are relatively simple, the depressions formed on the surface of the glass fiber are relatively uniform, and the prepared roughened glass fiber does not excessively reduce the strength and is evenly interspersed in the coating and is not easily detached, preferably improving the structural stability of the coating after carbonization and having a longer burning resistance time.
[0020] In a specific feasible embodiment, the intumescent flame retardant includes ammonium polyphosphate, pentaerythritol, and melamine in a mass ratio of 1:2:(3 - 3.1).
[0021] By adopting the above technical solution, the selection and proportioning of the acid source, carbon source, and gas source can form carbon more stably, release a large amount of gas, and the formed carbon layer can better seal the surface of the substrate, effectively blocking the transfer of heat to the substrate, and having a good flame retardant effect.
[0022] In a second aspect, the present application provides a preparation method of a two-component fireproof and heat-insulating coating, which is characterized in that: the preparation method includes the following steps:
[0023] S1: Weigh each component of agent A according to mass parts, mix them, and stir at a speed of 300 - 500 revolutions per minute for 5 - 10 minutes to obtain agent A;
[0024] S2: Weigh each component of agent B according to mass parts, mix them, and stir at a speed of 400 - 900 revolutions per minute for 5 - 8 minutes to obtain agent B;
[0025] S3: When in use, mix agent A and agent B to obtain the fireproof and heat-insulating coating.
[0026] By adopting the above scheme, the preparation method is relatively simple, and each component is evenly mixed. The acicular wollastonite and glass fiber are better interpenetrated to increase the charring strength of the coating and block heat. The epoxy-based cage-shaped polyhedral oligomeric silsesquioxane has good compatibility in the coating and participates in crosslinking to improve the strength and adhesion of the coating. The prepared coating is relatively uniform and flat, and the filler is not easy to precipitate. The coating formed after curing has a good fireproof and heat-insulating protection effect on the substrate.
[0027] In summary, the present application has the following beneficial effects:
[0028] 1. The present application provides a flame retardant effect by using a relatively large mass of intumescent flame retardant, adding bisphenol A epoxy resin, polyamide curing agent and epoxy-based cage-shaped polyhedral oligomeric silsesquioxane and limiting the mass ratio. The epoxy-based cage-shaped polyhedral oligomeric silsesquioxane-modified glass fiber and amino-based cage-shaped polyhedral oligomeric silsesquioxane-modified acicular wollastonite participate in crosslinking to form a flame retardant and heat-insulating effect in turn on the upper layer of the coating film. The surface of the prepared coating after curing is denser, and the protection effect on the substrate is good; by adding a certain mass of glass fiber and acicular wollastonite and limiting the mass ratio, the two are interpenetrated to improve the strength of the carbon layer, and the carbon layer is not easy to fall off after carbonization, further prolonging the burning resistance time; the glass fiber is roughened glass fiber, so that its surface has more active groups and greater friction, and is more closely connected to the coating matrix, and has a better interpenetrating effect with acicular wollastonite, further improving the carbonization strength and longer burning resistance time.
[0029] 2. By limiting the aspect ratio of the glass fiber and acicular wollastonite, the mass ratio of the epoxy-based cage-shaped polyhedral oligomeric silsesquioxane grafted glass fiber and the amino-based cage-shaped polyhedral oligomeric silsesquioxane-modified acicular wollastonite, and the mass ratio of the glass fiber to the acicular wollastonite, the filling effect and strength are further improved, and the structural stability of the coating surface after carbonization is good, further improving the fire resistance performance. Specific Embodiments
[0030] The technical solutions of the present invention will be described more specifically in combination with several specific implementation examples below. The implementation examples are only part of the implementation examples of the present invention, rather than all; the following specific implementation examples can be combined with each other, and the same or similar concepts or processes may not be repeated in some implementation examples.
[0031] The experimental reagents in the preparation examples, implementation examples and comparative examples are all conventional commercially available brands or obtained by conventional preparation processes, unless otherwise specified.
[0032] The bisphenol A epoxy resin of this application was purchased from Yueyang Baling Jiayun Petrochemical Co., Ltd., BL-CYDE; the polyamide curing agent was polyamide 650; the ammonium polyphosphate was purchased from Haoyu International; the pentaerythritol was purchased from Hubei Yihua; the melamine was purchased from Aorong A012; the leveling agent was BYK-348; the fumed silica was purchased from Hubei Huifu Nano Materials HL380; the diluent was a mixture of xylene and n-butanol with a volume ratio of 1:1; the glass fiber was purchased from Chongjun Mineral Products Co., Ltd., with a diameter of 9-13 μm and a short cut length of 3 mm; the acicular wollastonite was purchased from Zhuanghua Mineral Products, with an aspect ratio of 2-3:1 and a mesh number of 325 mesh.
[0033] Preparation Example
[0034] Preparation Example 1: Epoxy-functionalized polyhedral oligomeric silsesquioxane:
[0035] Mix 10 ml of water and 140 ml of acetone evenly, add 2.3 g of sodium hydroxide to dissolve, dropwise add 12.8 g of phenyltrimethoxysilane and 3.4 g of 3-glycidoxypropyltrimethoxysilane, react at 20 °C for 36 h, then rotary evaporate and concentrate, dry, wash with water until neutral, and dry to obtain epoxy-functionalized polyhedral oligomeric silsesquioxane.
[0036] Preparation Example 2: Roughened glass fiber:
[0037] Add 100 g of glass fiber to 500 g of an aqueous hydrofluoric acid solution with a volume fraction of 30%, then add 1.2 g of sodium sulfate, 1 g of magnesium fluoride, and 500 ml of water, stir evenly, filter after 2 minutes, wash with deionized water, and dry to obtain roughened glass fiber.
[0038] Preparation Example 3: Epoxy-functionalized polyhedral oligomeric silsesquioxane-modified glass fiber:
[0039] Mix 50 g of glass fiber and 40 g of the epoxy-functionalized polyhedral oligomeric silsesquioxane prepared in Preparation Example 1 in 200 ml of a 25% wt aqueous ethanol solution, stir for 1 hour, perform ultrasonic treatment for 30 minutes, react at 80 °C for 20 hours, then perform vacuum distillation, suction filtration, washing, and vacuum drying for 7 hours to obtain epoxy-functionalized polyhedral oligomeric silsesquioxane-modified glass fiber.
[0040] Preparation Example 4: Amino-functionalized polyhedral oligomeric silsesquioxane-modified acicular wollastonite:
[0041] Mix 10 ml of water and 140 ml of acetone evenly, add 2.3 g of sodium hydroxide to dissolve, dropwise add 12.8 g of phenyltrimethoxysilane and 3.1 g of (3-aminopropyl)trimethoxysilane, react at 20 °C for 36 h, then rotary evaporate and concentrate, dry, wash with water until neutral, and dry to obtain amino-functionalized polyhedral oligomeric silsesquioxane.
[0042] 100 g of amino-caged polyhedral oligomeric silsesquioxane and 40 g of acicular wollastonite are 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 after 20 hours, distilled under reduced pressure, filtered, washed, and vacuum dried for 7 hours to obtain amino-caged polyhedral oligomeric silsesquioxane modified acicular wollastonite.
[0043] Example
[0044] Example 1
[0045] This example includes raw materials with the following weights: Agent A: 100 g of bisphenol A epoxy resin, 420 g of intumescent flame retardant, including 70 g of ammonium polyphosphate, 140 g of pentaerythritol, 210 g of melamine, 20 g of glass fiber, 20 g of acicular wollastonite, 70 g of fumed silica, 100 g of diluent, 5 g of leveling agent, 80 g of epoxy-caged polyhedral oligomeric silsesquioxane modified glass fiber prepared in Preparation Example 3; Agent B: 200 g of polyamide curing agent, 100 g of diluent, 100 g of amino-caged polyhedral oligomeric silsesquioxane modified acicular wollastonite prepared in Preparation Example 4.
[0046] The preparation method is as follows:
[0047] S1: Weigh each component of Agent A according to the mass parts, mix, and stir at a speed of 400 revolutions per minute for 8 minutes to obtain Agent A;
[0048] S2: Weigh each component of Agent B according to the mass parts, mix, and stir at a speed of 700 revolutions per minute for 8 minutes to obtain Agent B;
[0049] S3: Mix the amount of Agent A obtained in S1 and the amount of Agent B obtained in S2, and stir at a speed of 800 revolutions per minute for 15 minutes to obtain the fireproof and heat-insulating coating.
[0050] Example 2
[0051] This example includes raw materials with the following weights: Agent A: 200 g of bisphenol A epoxy resin, 420 g of intumescent flame retardant, including 70 g of ammonium polyphosphate, 140 g of pentaerythritol, 210 g of melamine, 40 g of glass fiber, 40 g of acicular wollastonite, 70 g of fumed silica, 100 g of diluent, 5 g of leveling agent, 100 g of epoxy-caged polyhedral oligomeric silsesquioxane modified glass fiber prepared in Preparation Example 3; Agent B: 100 g of polyamide curing agent, 150 g of diluent, 100 g of amino-caged polyhedral oligomeric silsesquioxane modified acicular wollastonite prepared in Preparation Example 4.
[0052] The preparation method is as follows:
[0053] S1: Weigh each component of Agent A according to the mass parts, mix, and stir at a speed of 400 revolutions per minute for 8 minutes to obtain Agent A;
[0054] S2: Weigh each component of Agent B according to the parts by mass, mix them, and stir for 8 minutes at a speed of 700 revolutions per minute to obtain Agent B.
[0055] S3: Mix the amount of Agent A prepared in S1 and the amount of Agent B prepared in S2, and stir for 15 minutes at a speed of 800 revolutions per minute to obtain the fireproof and heat-insulating coating.
[0056] Example 3
[0057] This example includes the following raw materials by weight: Agent A: 125 g of bisphenol A epoxy resin, 420 g of intumescent flame retardant, including 70 g of ammonium polyphosphate, 140 g of pentaerythritol, 210 g of melamine, 30 g of glass fiber, 30 g of acicular wollastonite, 50 g of fumed silica, 100 g of diluent, 4 g of leveling agent, 150 g of epoxy-based cage-shaped polyhedral oligomeric silsesquioxane-modified glass fiber prepared in Preparation Example 3; Agent B: 150 g of polyamide curing agent, 120 g of diluent, 70 g of amino cage-shaped polyhedral oligomeric silsesquioxane-modified acicular wollastonite prepared in Preparation Example 4.
[0058] The preparation method is as follows:
[0059] S1: Weigh each component of Agent A according to the parts by mass, mix them, and stir for 8 minutes at a speed of 400 revolutions per minute to obtain Agent A.
[0060] S2: Weigh each component of Agent B according to the parts by mass, mix them, and stir for 8 minutes at a speed of 700 revolutions per minute to obtain Agent B.
[0061] S3: Mix the amount of Agent A prepared in S1 and the amount of Agent B prepared in S2, and stir for 15 minutes at a speed of 800 revolutions per minute to obtain the fireproof and heat-insulating coating.
[0062] Example 4
[0063] This example includes the following raw materials by weight: Agent A: 125 g of bisphenol A epoxy resin, 420 g of intumescent flame retardant, including 70 g of ammonium polyphosphate, 140 g of pentaerythritol, 210 g of melamine, 30 g of glass fiber, 30 g of acicular wollastonite, 50 g of fumed silica, 100 g of diluent, 4 g of leveling agent, 132 g of epoxy-based cage-shaped polyhedral oligomeric silsesquioxane-modified glass fiber prepared in Preparation Example 3; Agent B: 150 g of polyamide curing agent, 120 g of diluent, 88 g of amino cage-shaped polyhedral oligomeric silsesquioxane-modified acicular wollastonite prepared in Preparation Example 4.
[0064] The preparation method is as follows:
[0065] S1: Weigh each component of Agent A according to the parts by mass, mix them, and stir for 8 minutes at a speed of 400 revolutions per minute to obtain Agent A.
[0066] S2: Weigh each component of Agent B according to the parts by mass, mix them, and stir for 8 minutes at a speed of 700 revolutions per minute to obtain Agent B.
[0067] S3: Mix the amount of Agent A prepared in S1 and the amount of Agent B prepared in S2, and stir for 15 minutes at a speed of 800 revolutions per minute to obtain the fireproof and heat-insulating coating.
[0068] Example 5
[0069] This example includes the following raw materials by weight: Agent A: 125 g of bisphenol A epoxy resin, 420 g of intumescent flame retardant, including 70 g of ammonium polyphosphate, 140 g of pentaerythritol, 210 g of melamine, 30 g of glass fiber, 30 g of acicular wollastonite, 50 g of fumed silica, 100 g of diluent, 4 g of leveling agent, 125 g of epoxy-functional cage-like polyhedral oligomeric silsesquioxane-modified glass fiber prepared in Preparation Example 3; Agent B: 150 g of polyamide curing agent, 120 g of diluent, 95 g of amino-functional cage-like polyhedral oligomeric silsesquioxane-modified acicular wollastonite prepared in Preparation Example 4.
[0070] The preparation method is as follows:
[0071] S1: Weigh each component of Agent A according to the parts by mass, mix them, and stir for 8 minutes at a speed of 400 revolutions per minute to obtain Agent A.
[0072] S2: Weigh each component of Agent B according to the parts by mass, mix them, and stir for 8 minutes at a speed of 700 revolutions per minute to obtain Agent B.
[0073] S3: Mix the amount of Agent A prepared in S1 and the amount of Agent B prepared in S2, and stir for 15 minutes at a speed of 800 revolutions per minute to obtain the fireproof and heat-insulating coating.
[0074] Example 6
[0075] This example includes the following raw materials by weight: Agent A: 125 g of bisphenol A epoxy resin, 420 g of intumescent flame retardant, including 70 g of ammonium polyphosphate, 140 g of pentaerythritol, 210 g of melamine, 30 g of glass fiber, 30 g of acicular wollastonite, 50 g of fumed silica, 100 g of diluent, 4 g of leveling agent, 140 g of epoxy-functional cage-like polyhedral oligomeric silsesquioxane-modified glass fiber prepared in Preparation Example 3; Agent B: 150 g of polyamide curing agent, 120 g of diluent, 80 g of amino-functional cage-like polyhedral oligomeric silsesquioxane-modified acicular wollastonite prepared in Preparation Example 4.
[0076] The preparation method is as follows:
[0077] S1: Weigh each component of Agent A according to the parts by mass, mix them, and stir for 8 minutes at a speed of 400 revolutions per minute to obtain Agent A.
[0078] S2: Weigh each component of Agent B according to parts by mass, mix them, and stir for 8 minutes at a speed of 700 revolutions per minute to obtain Agent B.
[0079] S3: Mix the amount of Agent A obtained in S1 and the amount of Agent B obtained in S2, and stir for 15 minutes at a speed of 800 revolutions per minute to obtain the fireproof and heat-insulating coating.
[0080] Example 7
[0081] This example includes the following raw materials by weight: Agent A: 125 g of bisphenol A epoxy resin, 420 g of intumescent flame retardant, including 70 g of ammonium polyphosphate, 140 g of pentaerythritol, 210 g of melamine, 30 g of roughened glass fiber prepared in Preparation Example 2, 30 g of acicular wollastonite, 50 g of fumed silica, 100 g of diluent, 4 g of leveling agent, 132 g of epoxy cage-type polyhedral oligomeric silsesquioxane modified glass fiber prepared in Preparation Example 3; Agent B: 150 g of polyamide curing agent, 120 g of diluent, 88 g of amino cage-type polyhedral oligomeric silsesquioxane modified acicular wollastonite prepared in Preparation Example 4.
[0082] The preparation method is as follows:
[0083] S1: Weigh each component of Agent A according to parts by mass, mix them, and stir for 8 minutes at a speed of 400 revolutions per minute to obtain Agent A.
[0084] S2: Weigh each component of Agent B according to parts by mass, mix them, and stir for 8 minutes at a speed of 700 revolutions per minute to obtain Agent B.
[0085] S3: Mix the amount of Agent A obtained in S1 and the amount of Agent B obtained in S2, and stir for 15 minutes at a speed of 800 revolutions per minute to obtain the fireproof and heat-insulating coating.
[0086] Comparative Example
[0087] Comparative Example 1
[0088] This comparative example includes the following raw materials by weight: Agent A: 125 g of bisphenol A epoxy resin, 420 g of intumescent flame retardant, including 70 g of ammonium polyphosphate, 140 g of pentaerythritol, 210 g of melamine, 30 g of glass fiber, 30 g of acicular wollastonite, 50 g of fumed silica, 100 g of diluent, 4 g of leveling agent; Agent B: 150 g of polyamide curing agent, 120 g of diluent.
[0089] The preparation method is as follows:
[0090] S1: Weigh each component of Agent A according to parts by mass, mix them, and stir for 8 minutes at a speed of 400 revolutions per minute to obtain Agent A.
[0091] S2: Weigh each component of Agent B according to parts by mass, mix them, and stir for 8 minutes at a speed of 700 revolutions per minute to obtain Agent B.
[0092] S3: The amount of Agent A obtained in S1 and the amount of Agent B obtained in S2 are mixed and stirred at a speed of 800 revolutions per minute for 15 minutes to obtain the fireproof and heat-insulating coating.
[0093] Comparative Example 2
[0094] This comparative example includes raw materials with the following weights: Agent A: 125 g of bisphenol A epoxy resin, 420 g of intumescent flame retardant, including 70 g of ammonium polyphosphate, 140 g of pentaerythritol, 210 g of melamine, 30 g of glass fiber, 30 g of acicular wollastonite, 50 g of fumed silica, 100 g of diluent, 4 g of leveling agent; Agent B: 150 g of polyamide curing agent, 120 g of diluent, 70 g of amino cage-shaped polyhedral oligomeric silsesquioxane-modified acicular wollastonite prepared in Preparation Example 4.
[0095] The preparation method is as follows:
[0096] S1: Weigh each component of Agent A according to the mass parts, mix them, and stir at a speed of 400 revolutions per minute for 8 minutes to obtain Agent A;
[0097] S2: Weigh each component of Agent B according to the mass parts, mix them, and stir at a speed of 700 revolutions per minute for 8 minutes to obtain Agent B;
[0098] S3: The amount of Agent A obtained in S1 and the amount of Agent B obtained in S2 are mixed and stirred at a speed of 800 revolutions per minute for 15 minutes to obtain the fireproof and heat-insulating coating.
[0099] Comparative Example 3
[0100] This comparative example includes raw materials with the following weights: Agent A: 125 g of bisphenol A epoxy resin, 420 g of intumescent flame retardant, including 70 g of ammonium polyphosphate, 140 g of pentaerythritol, 210 g of melamine, 30 g of glass fiber, 30 g of acicular wollastonite, 50 g of fumed silica, 100 g of diluent, 4 g of leveling agent, 150 g of epoxy cage-shaped polyhedral oligomeric silsesquioxane-modified glass fiber prepared in Preparation Example 3; Agent B: 150 g of polyamide curing agent, 120 g of diluent.
[0101] The preparation method is as follows:
[0102] S1: Weigh each component of Agent A according to the mass parts, mix them, and stir at a speed of 400 revolutions per minute for 8 minutes to obtain Agent A;
[0103] S2: Weigh each component of Agent B according to the mass parts, mix them, and stir at a speed of 700 revolutions per minute for 8 minutes to obtain Agent B;
[0104] S3: The amount of Agent A obtained in S1 and the amount of Agent B obtained in S2 are mixed and stirred at a speed of 800 revolutions per minute for 15 minutes to obtain the fireproof and heat-insulating coating.
[0105] Comparative Example 4
[0106] This comparative example includes raw materials with the following weights: Agent A: 125 g of bisphenol A epoxy resin, 420 g of intumescent flame retardant, including 70 g of ammonium polyphosphate, 140 g of pentaerythritol, 210 g of melamine, 90 g of glass fiber, 30 g of acicular wollastonite, 50 g of fumed silica, 100 g of diluent, 4 g of leveling agent, 90 g of epoxy cage-type polyhedral oligomeric silsesquioxane prepared in Preparation Example 1; Agent B: 150 g of polyamide curing agent, 120 g of diluent, 40 g of amino cage-type polyhedral oligomeric silsesquioxane, 30 g of acicular wollastonite.
[0107] The preparation method is as follows:
[0108] S1: Weigh each component of Agent A according to the mass parts, mix them, and stir at a speed of 400 revolutions per minute for 8 minutes to obtain Agent A;
[0109] S2: Weigh each component of Agent B according to the mass parts, mix them, and stir at a speed of 700 revolutions per minute for 8 minutes to obtain Agent B;
[0110] S3: Mix the amount of Agent A obtained in S1 and the amount of Agent B obtained in S2, and stir at a speed of 800 revolutions per minute for 15 minutes to obtain the fireproof and heat-insulating coating.
[0111] Comparative Example 5
[0112] This comparative example includes raw materials with the following weights: Agent A: 125 g of bisphenol A epoxy resin, 420 g of intumescent flame retardant, including 70 g of ammonium polyphosphate, 140 g of pentaerythritol, 210 g of melamine, 90 g of glass fiber, 30 g of acicular wollastonite, 50 g of fumed silica, 100 g of diluent, 4 g of leveling agent, 90 g of epoxy cage-type polyhedral oligomeric silsesquioxane prepared in Preparation Example 1; Agent B: 150 g of polyamide curing agent, 120 g of diluent, 70 g of amino cage-type polyhedral oligomeric silsesquioxane-modified acicular wollastonite prepared in Preparation Example 4.
[0113] The preparation method is as follows:
[0114] S1: Weigh each component of Agent A according to the mass parts, mix them, and stir at a speed of 400 revolutions per minute for 8 minutes to obtain Agent A;
[0115] S2: Weigh each component of Agent B according to the mass parts, mix them, and stir at a speed of 700 revolutions per minute for 8 minutes to obtain Agent B;
[0116] S3: Mix the amount of Agent A obtained in S1 and the amount of Agent B obtained in S2, and stir at a speed of 800 revolutions per minute for 15 minutes to obtain the fireproof and heat-insulating coating.
[0117] Comparative Example 6
[0118] This comparative example includes raw materials with the following weights: Agent A: 125 g of bisphenol A epoxy resin, 420 g of intumescent flame retardant, including 70 g of ammonium polyphosphate, 140 g of pentaerythritol, 210 g of melamine, 30 g of glass fiber, 30 g of acicular wollastonite, 50 g of fumed silica, 100 g of diluent, 4 g of leveling agent, and 150 g of epoxy cage-type polyhedral oligomeric silsesquioxane-modified glass fiber prepared in Preparation Example 3; Agent B: 150 g of polyamide curing agent, 120 g of diluent, 40 g of amino cage-type polyhedral oligomeric silsesquioxane, and 30 g of acicular wollastonite.
[0119] The preparation method is as follows:
[0120] S1: Weigh each component of Agent A according to the mass parts, mix them, and stir at a speed of 400 revolutions per minute for 8 minutes to obtain Agent A;
[0121] S2: Weigh each component of Agent B according to the mass parts, mix them, and stir at a speed of 700 revolutions per minute for 8 minutes to obtain Agent B;
[0122] S3: Mix the amount of Agent A obtained in S1 and the amount of Agent B obtained in S2, and stir at a speed of 800 revolutions per minute for 15 minutes to obtain the fireproof and heat-insulating coating.
[0123] Performance detection test Test 1: Coat the fireproof and heat-insulating coatings prepared in each example and comparative example on Q235 steel with a thickness of 1.5 mm, cure the coating, and then conduct a fire resistance limit test with reference to the standard "GB / T14907-2002". The test results are shown in Table 1.
[0124] Test 2: Coat the fireproof and heat-insulating coatings prepared in each example and comparative example on Q235 steel with a thickness of 1.5 mm, cure the coating, and test the adhesion of the coating to the steel (MPa) according to GB / T5210. The test results are shown in Table 1.
[0125] Table 1
[0126] 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
[0127] Combined with Examples 1-3, Comparative Examples 1-6 and Table 1, in this application, a large amount of intumescent flame retardant is added to bisphenol A epoxy resin, epoxy cage-type polyhedral oligomeric silsesquioxane-grafted glass fiber and amino cage-type polyhedral oligomeric silsesquioxane-grafted acicular wollastonite are added, and their sizes are limited to improve the flame retardant effect and participate in crosslinking. The mass ratio of acicular wollastonite and glass fiber is limited to strengthen the charring strength and reduce the char layer shedding. The fireproof and heat-insulating coatings prepared have better fire resistance limit performance and better adhesion after curing, and can provide stable fireproof and heat-insulating protection for buildings for a long time.
[0128] Combined with Examples 3-6 and Table 1, the present application further optimizes the cross-linked structure by limiting the mass ratio of epoxy-functionalized polyhedral oligomeric silsesquioxane grafted glass fiber and amino-functionalized polyhedral oligomeric silsesquioxane grafted acicular wollastonite, improving the flame retardant and heat insulation effects, and enhancing the fire resistance limit and adhesion performance.
[0129] Combined with Example 3, Example 7 and Table 1, the present application further defines the glass fiber as roughened glass fiber. The higher friction of the roughened glass fiber enables the coating to adhere stably and firmly after carbonization, providing better protection for the substrate.
[0130] This specific embodiment is only an interpretation of the present application and does not limit the present application. Those skilled in the art can make non-creative modifications to this embodiment as needed after reading this specification, but as long as it is within the scope of the claims of the present application, it is protected by the patent law.
Claims
1. A two-component fireproof and heat-insulating coating, characterized in that: The raw materials of the heat-insulating coating include Agent A and Agent B. 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 acicular wollastonite, 3-7 parts of fumed silica, 10-20 parts of diluent, 0.3-0.5 part of leveling agent, and 8-15 parts of epoxy cage-type polyhedral oligomeric silsesquioxane 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, and 7-10 parts of amino cage-type polyhedral oligomeric silsesquioxane modified acicular wollastonite; The aspect ratio of the glass fiber is 300-600:1, and the aspect ratio of the acicular wollastonite is 10-20:1; The mass ratio of the epoxy cage-type polyhedral oligomeric silsesquioxane modified glass fiber to the amino cage-type polyhedral oligomeric silsesquioxane modified acicular wollastonite is 1.5:
1. The preparation steps of the epoxy cage-type polyhedral oligomeric silsesquioxane include: mixing water and acetone evenly, adding sodium hydroxide to dissolve, dropping phenyltrimethoxysilane and 3-glycidyletheroxypropyltrimethoxysilane, spin-evaporating and concentrating after reaction, drying, washing to neutrality with water, and drying to obtain epoxy cage-type polyhedral oligomeric silsesquioxane. The preparation steps of the epoxy cage-type polyhedral oligomeric silsesquioxane modified glass fiber include: adding the epoxy cage-type polyhedral oligomeric silsesquioxane and glass fiber to an ethanol aqueous solution, stirring evenly, performing ultrasonic treatment, heating for reaction, distilling under reduced pressure, filtering, washing, and drying in vacuum to obtain epoxy cage-type polyhedral oligomeric silsesquioxane modified glass fiber.
2. The two-component fireproof and heat-insulating coating according to claim 1, characterized in that: The mass ratio of the glass fiber to the acicular wollastonite in Agent A is 1:(0.9-1.1).
3. The two-component fireproof and heat-insulating coating according to claim 1, characterized in that: The glass fiber is roughened glass fiber.
4. The two-component fireproof and heat-insulating coating according to claim 3, characterized in that: The preparation steps of the roughened glass fiber include: adding the glass fiber to an aqueous hydrofluoric acid solution, then adding sodium sulfate, magnesium fluoride, and water, stirring evenly, filtering, washing, and drying to obtain roughened glass fiber.
5. The two-component fireproof and heat-insulating coating according to claim 1, characterized in that: The intumescent flame retardant includes ammonium polyphosphate, pentaerythritol, and melamine in a mass ratio of 1:2:
3.
6. A method for preparing the two-component fireproof and heat-insulating coating according to any one of claims 1-5, characterized in that: The preparation method includes the following steps: S1: Weigh each component of Agent A according to parts by weight, mix them, and stir at a speed of 300-500 revolutions per minute for 5-10 minutes to obtain Agent A. S2: Weigh each component of Agent B according to parts by weight, mix them, and stir at a speed of 400-900 revolutions per minute for 5-8 minutes to obtain Agent B. S3: When in use, mix Agent A and Agent B to obtain a fireproof and heat-insulating coating.
Citation Information
Patent Citations
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