CN108948946B - Composite fireproof coating and preparation method thereof - Google Patents
Composite fireproof coating and preparation method thereof Download PDFInfo
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- CN108948946B CN108948946B CN201810527361.XA CN201810527361A CN108948946B CN 108948946 B CN108948946 B CN 108948946B CN 201810527361 A CN201810527361 A CN 201810527361A CN 108948946 B CN108948946 B CN 108948946B
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D163/00—Coating compositions based on epoxy resins; Coating compositions based on derivatives of epoxy resins
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
- C09D5/18—Fireproof paints including high temperature resistant paints
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
- C09D7/40—Additives
- C09D7/60—Additives non-macromolecular
- C09D7/61—Additives non-macromolecular inorganic
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
- C09D7/40—Additives
- C09D7/60—Additives non-macromolecular
- C09D7/63—Additives non-macromolecular organic
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/32—Phosphorus-containing compounds
- C08K2003/321—Phosphates
- C08K2003/322—Ammonium phosphate
- C08K2003/323—Ammonium polyphosphate
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/02—Flame or fire retardant/resistant
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/08—Stabilised against heat, light or radiation or oxydation
Abstract
The invention discloses a composite fireproof coating and a preparation method thereof, wherein the composite fireproof coating comprises the following components in percentage by mass: 20-40% of epoxy resin, 8-18% of waterborne polyurethane, 8-15% of microencapsulated ammonium polyphosphate fire retardant, 0.5-3% of nano mesoporous silica, 4-6% of pentaerythritol, 0-7% of potassium silicate, 3-10% of bentonite, 0.8-2.5% of auxiliary agent and the balance of water. The composite fireproof coating has excellent high temperature resistance, bonding performance and water resistance, and the coating does not foam, crack or peel under the high temperature condition, so that the service life of a member can be effectively prolonged.
Description
Technical Field
The invention relates to the technical field of fireproof coatings, in particular to a composite fireproof coating and a preparation method thereof.
Background
The fireproof coating is used on the surface of a combustible substrate, can reduce the flammability of the surface of a coated material, retards the fire spread of a fire disaster and is used for improving the fire endurance of the coated material. When the fireproof coating is coated on the surface of a base material, the fireproof coating has a flame retardant effect and is required to have excellent performances such as rust prevention, water prevention, corrosion prevention, wear resistance, heat resistance and the like. However, most of the current fire-retardant coatings are insufficient in thermal barrier property and corrosion resistance, so that the development thereof is limited. On the other hand, in order to improve the flame retardant performance of the coating, inorganic or organic particles are generally introduced and compounded with the inorganic or organic particles, but the inorganic nanoparticles have poor dispersibility and poor compatibility with organic resins, so that stress cracking is easily generated at the particle aggregation part, and the actual using effect of the fireproof coating is affected. Therefore, it is necessary to develop a fire retardant coating with excellent comprehensive properties.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide the composite fireproof coating and the preparation method thereof, so that the flame retardance and the compatibility of the fireproof coating are improved.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows:
the composite fireproof coating comprises the following components in percentage by mass: 20 to 40 percent of epoxy resin, 8 to 18 percent of waterborne polyurethane, 8 to 15 percent of microencapsulated ammonium polyphosphate fire retardant, 0.5 to 3 percent of nano mesoporous silica, 4 to 6 percent of pentaerythritol, 4 to 7 percent of potassium silicate, 3 to 10 percent of bentonite, 0.8 to 2.5 percent of auxiliary agent and the balance of water.
In the technical scheme, the flame resistance and the water resistance of the coating are enhanced by preferably selecting the components and the proportion of the fireproof coating. After the ammonium polyphosphate flame retardant is subjected to microencapsulation treatment, on one hand, the ammonium polyphosphate flame retardant can effectively improve the thermal stability and ensure the flame retardant property of a fireproof material, and on the other hand, the ammonium polyphosphate flame retardant can improve the compatibility of paint components and improve the water resistance of a fireproof paint, so that the flame retardant effect and the service life of the paint are ensured; the nano mesoporous silica has larger specific surface area, can be uniformly dispersed in a coating base material, has good compatibility, can be transferred to the surface of a carbon layer to form a silica resistance layer with good sealing and certain strength, prolongs the diffusion channel of combustible gas and oxygen, reduces the transfer of heat and mass on the surface of a material, and improves the flame retardant effect of the fireproof coating. The bentonite has excellent dispersibility in water, and the particles of the bentonite can be mutually crosslinked to form a continuous network structure, so that the water resistance of the coating is improved. Meanwhile, the components such as pentaerythritol, potassium silicate, bentonite, an auxiliary agent and the like are compounded to synergistically improve the heat insulation and flame retardant properties of the fireproof coating.
As a preferred embodiment of the composite fireproof coating, the composite fireproof coating comprises the following components in percentage by mass: 25-40% of epoxy resin, 10-15% of waterborne polyurethane, 10-12% of microencapsulated ammonium polyphosphate flame retardant, 1.2-2.5% of nano mesoporous silica, 4-6% of pentaerythritol, 0-7% of potassium silicate, 5-10% of bentonite, 0.8-2.5% of auxiliary agent and the balance of water.
As a preferred embodiment of the composite fireproof coating, the mass ratio of the microencapsulated ammonium polyphosphate flame retardant to the nano mesoporous silica is 5-9: 1.
The composite fireproof coating provided by the invention comprises the following components in percentage by mass: 30% of epoxy resin, 12% of waterborne polyurethane, 12% of microencapsulated ammonium polyphosphate flame retardant, 1.5% of nano mesoporous silica, 5% of pentaerythritol, 5% of potassium silicate, 5% of bentonite, 2.5% of assistant and the balance of water.
The composite fireproof coating provided by the invention comprises the following components in percentage by mass: 34% of epoxy resin, 12% of waterborne polyurethane, 10% of microencapsulated ammonium polyphosphate flame retardant, 2.0% of nano mesoporous silica, 6% of pentaerythritol, 4% of potassium silicate, 7% of bentonite, 2% of auxiliary agent and the balance of water.
The composite fireproof coating provided by the invention comprises the following components in percentage by mass: 25% of epoxy resin, 10% of waterborne polyurethane, 15% of microencapsulated ammonium polyphosphate flame retardant, 2.5% of nano mesoporous silica, 5% of pentaerythritol, 5% of potassium silicate, 9% of bentonite, 1.0% of assistant and the balance of water.
The composite fireproof coating provided by the invention comprises the following components in percentage by mass: 28% of epoxy resin, 16% of waterborne polyurethane, 11% of microencapsulated ammonium polyphosphate fire retardant, 2.0% of nano mesoporous silica, 5% of pentaerythritol, 5% of potassium silicate, 10% of bentonite, 1.8% of assistant and the balance of water.
In the technical scheme, the inventor further optimizes the formula of the composite fireproof coating through a plurality of tests, so that the flame resistance and the compatibility of the coating are improved.
As a preferable embodiment of the composite fireproof coating, the auxiliary agent is at least one of a film forming agent, a dispersing agent, a thickening agent, a leveling agent and an antifoaming agent.
The thickening agent adopts colloidal silicon dioxide, cellulose, polyacrylic acid, polyvinyl alcohol, polyacrylamide and the like, and is used for adjusting the viscosity or rheological property of the fireproof paint to form uniform paint components. The dispersing agent adopts water-based non-ionic high molecular surfactant, such as higher fatty acid ethoxy compound, modified polyacrylate ethylene oxide copolymer, ethylene oxide propylene oxide copolymer and other polyoxyethylene compounds, so that the coating components are in a relatively stable state for a long time. The defoaming agent is a modified polydimethylsiloxane defoaming agent or a polymer defoaming agent, and is used for inhibiting foams in the preparation or use process and eliminating bubbles generated in the film forming process of the coating. The film forming agent is aromatic hydrocarbon, petroleum solvent or butoxyethyl acetate. The leveling agent adopts 1, 2-propylene glycol and the like and is used for ensuring good leveling property of the fireproof coating.
As a preferred embodiment of the composite fire-retardant coating, the preparation method of the microencapsulated ammonium polyphosphate flame retardant comprises the following steps: mixing melamine and formaldehyde solution according to a molar ratio of 1: 2.5-3.5, adding a pH regulator to regulate the pH to 8-9, heating to 70-85 ℃, and reacting for 1-2 hours to generate a melamine formaldehyde prepolymer aqueous solution; mixing urea and formaldehyde solution according to a molar ratio of 1: 2.5-3.5, adding a pH regulator to regulate the pH to 8-9, heating to 70-85 ℃, and reacting for 1-2 hours to generate a urea-formaldehyde resin prepolymer aqueous solution; dispersing ammonium polyphosphate in absolute ethyl alcohol, adding a melamine formaldehyde prepolymer aqueous solution, adjusting the pH value to 3.5-4, reacting for 2-3 h, adding a urea formaldehyde resin prepolymer aqueous solution, adjusting the pH value to 3.5-4, reacting for 2-3 h, performing suction filtration, washing and drying to obtain the microencapsulated ammonium polyphosphate flame retardant.
The microencapsulated ammonium polyphosphate fire retardant is a melamine-urea-formaldehyde resin-ammonium polyphosphate expansion type fire retardant, can effectively improve the fire resistance of the fire-retardant coating, takes melamine and urea-formaldehyde resin as capsule materials, takes ammonium polyphosphate as a capsule core, and can prevent the three from migrating and separating out in the coating, thereby further improving the water resistance of the coating.
The invention also provides a preparation method of the composite coating, which comprises the following steps:
(1) adding water, epoxy resin and waterborne polyurethane into a reaction container, and uniformly stirring and mixing;
(2) adding nano mesoporous silica, and performing ultrasonic dispersion;
(3) adding microencapsulated ammonium polyphosphate flame retardant, pentaerythritol, potassium silicate, bentonite and an auxiliary agent, uniformly stirring, sieving and discharging to obtain the composite fireproof coating.
Compared with the prior art, the invention has the beneficial effects that:
the composite fireproof coating disclosed by the invention is prepared by matching epoxy resin, waterborne polyurethane, a microencapsulated ammonium polyphosphate flame retardant, nano mesoporous silica, potassium silicate, pentaerythritol and the like, has the effects of synergistically improving the high-temperature resistance, the bonding property and the water resistance of the coating, and can effectively prolong the service life of a member, and a coating does not foam, crack or peel under a high-temperature condition. The invention adopts melamine-urea-formaldehyde resin-ammonium polyphosphate microencapsulated flame retardant, and effectively improves the water resistance and flame retardant property of the fireproof coating. The nano mesoporous silicon dioxide can be uniformly dispersed in the coating base material, and has good compatibility.
Detailed Description
To better illustrate the objects, aspects and advantages of the present invention, the present invention will be further described with reference to specific examples. It will be understood by those skilled in the art that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
In the examples, the experimental methods used were all conventional methods unless otherwise specified, and the materials, reagents and the like used were commercially available without otherwise specified.
Example 1
As an embodiment of the composite fireproof coating, the composite fireproof coating of this embodiment includes the following components by mass percent: 30% of epoxy resin, 12% of waterborne polyurethane, 12% of microencapsulated ammonium polyphosphate flame retardant, 1.5% of nano mesoporous silica, 5% of pentaerythritol, 5% of potassium silicate, 5% of bentonite, 2.5% of auxiliary agent and the balance of water.
The preparation method of the composite fireproof coating comprises the following steps:
(1) adding water, epoxy resin and waterborne polyurethane into a reaction container, and uniformly stirring and mixing;
(2) adding nano mesoporous silica, and performing ultrasonic dispersion;
(3) adding microencapsulated ammonium polyphosphate flame retardant, pentaerythritol, potassium silicate, bentonite and an auxiliary agent, uniformly stirring, sieving and discharging to obtain the composite fireproof coating.
The preparation method of the microencapsulated ammonium polyphosphate flame retardant comprises the following steps:
1) mixing melamine and formaldehyde solution according to a molar ratio of 1: 3, adding a pH regulator to regulate the pH to 8-9, heating to 80 ℃ and reacting for 2 hours to generate a melamine formaldehyde prepolymer aqueous solution;
2) mixing urea and formaldehyde solution according to a molar ratio of 1: 3, adding a pH regulator to regulate the pH to 8-9, heating to 80 ℃ and reacting for 2 hours to generate a urea-formaldehyde resin prepolymer aqueous solution;
3) dispersing ammonium polyphosphate in absolute ethyl alcohol, adding a melamine formaldehyde prepolymer aqueous solution, adjusting the pH value to 3.5-4, reacting for 3 hours, adding a urea formaldehyde resin prepolymer aqueous solution, adjusting the pH value to 3.5-4, reacting for 3 hours, carrying out suction filtration, washing and drying to obtain the microencapsulated ammonium polyphosphate flame retardant, wherein the mass ratio of the melamine formaldehyde prepolymer aqueous solution to the urea formaldehyde resin prepolymer aqueous solution is 0.5: 1.
Example 2
As an embodiment of the composite fireproof coating, the composite fireproof coating of this embodiment includes the following components by mass percent: 34% of epoxy resin, 12% of waterborne polyurethane, 10% of microencapsulated ammonium polyphosphate flame retardant, 2.0% of nano mesoporous silica, 6% of pentaerythritol, 4% of potassium silicate, 7% of bentonite, 2% of auxiliary agent and the balance of water.
The preparation method of the composite fireproof coating comprises the following steps:
(1) adding water, epoxy resin and waterborne polyurethane into a reaction container, and uniformly stirring and mixing;
(2) adding nano mesoporous silica, and performing ultrasonic dispersion;
(3) adding microencapsulated ammonium polyphosphate flame retardant, pentaerythritol, potassium silicate, bentonite and an auxiliary agent, uniformly stirring, sieving and discharging to obtain the composite fireproof coating.
The preparation method of the microencapsulated ammonium polyphosphate flame retardant comprises the following steps:
1) mixing melamine and formaldehyde solution according to a molar ratio of 1: 2.5, adding a pH regulator to regulate the pH to 8-9, heating to 85 ℃ and reacting for 1h to generate a melamine formaldehyde prepolymer aqueous solution;
2) mixing urea and formaldehyde solution according to a molar ratio of 1: 2.5, adding a pH regulator to regulate the pH to 8-9, heating to 85 ℃ and reacting for 1h to generate a urea-formaldehyde resin prepolymer aqueous solution;
3) dispersing ammonium polyphosphate in absolute ethyl alcohol, adding a melamine formaldehyde prepolymer aqueous solution, adjusting the pH value to 3.5-4, reacting for 2 hours, adding a urea formaldehyde resin prepolymer aqueous solution, adjusting the pH value to 3.5-4, reacting for 2 hours, carrying out suction filtration, washing and drying to obtain the microencapsulated ammonium polyphosphate flame retardant, wherein the mass ratio of the melamine formaldehyde prepolymer aqueous solution to the urea formaldehyde resin prepolymer aqueous solution is 1: 1.
Example 3
As an embodiment of the composite fireproof coating, the composite fireproof coating of this embodiment includes the following components by mass percent: 25% of epoxy resin, 10% of waterborne polyurethane, 15% of microencapsulated ammonium polyphosphate flame retardant, 2.5% of nano mesoporous silica, 5% of pentaerythritol, 5% of potassium silicate, 9% of bentonite, 1.0% of assistant and the balance of water.
The preparation method of the composite fireproof coating comprises the following steps:
(1) adding water, epoxy resin and waterborne polyurethane into a reaction container, and uniformly stirring and mixing;
(2) adding nano mesoporous silica, and performing ultrasonic dispersion;
(3) adding microencapsulated ammonium polyphosphate flame retardant, pentaerythritol, potassium silicate, bentonite and an auxiliary agent, uniformly stirring, sieving and discharging to obtain the composite fireproof coating.
The preparation method of the microencapsulated ammonium polyphosphate flame retardant comprises the following steps:
1) mixing melamine and formaldehyde solution according to a molar ratio of 1: 3.5, adding a pH regulator to regulate the pH to 8-9, heating to 70 ℃ and reacting for 2 hours to generate a melamine formaldehyde prepolymer aqueous solution;
2) mixing urea and formaldehyde solution according to a molar ratio of 1: 3.5, adding a pH regulator to regulate the pH to 8-9, heating to 70 ℃ and reacting for 2 hours to generate a urea-formaldehyde resin prepolymer aqueous solution;
3) dispersing ammonium polyphosphate in absolute ethyl alcohol, adding a melamine formaldehyde prepolymer aqueous solution, adjusting the pH value to 3.5-4, reacting for 2.5 hours, adding a urea formaldehyde prepolymer aqueous solution, adjusting the pH value to 3.5-4, reacting for 2.5 hours, carrying out suction filtration, washing and drying to obtain the microencapsulated ammonium polyphosphate flame retardant, wherein the mass ratio of the melamine formaldehyde prepolymer aqueous solution to the urea formaldehyde prepolymer aqueous solution is 1.5: 1.
Example 4
As an embodiment of the composite fireproof coating, the composite fireproof coating of this embodiment includes the following components by mass percent: 28% of epoxy resin, 16% of waterborne polyurethane, 11% of microencapsulated ammonium polyphosphate flame retardant, 2.0% of nano mesoporous silica, 5% of pentaerythritol, 5% of potassium silicate, 10% of bentonite, 1.8% of assistant and the balance of water.
The preparation method of the composite fireproof coating comprises the following steps:
(1) adding water, epoxy resin and waterborne polyurethane into a reaction container, and uniformly stirring and mixing;
(2) adding nano mesoporous silica, and performing ultrasonic dispersion;
(3) adding microencapsulated ammonium polyphosphate flame retardant, pentaerythritol, potassium silicate, bentonite and an auxiliary agent, uniformly stirring, sieving and discharging to obtain the composite fireproof coating.
The preparation method of the microencapsulated ammonium polyphosphate flame retardant comprises the following steps:
1) mixing melamine and formaldehyde solution according to a molar ratio of 1: 3, adding a pH regulator to regulate the pH to 8-9, heating to 80 ℃ and reacting for 2 hours to generate a melamine formaldehyde prepolymer aqueous solution;
2) mixing urea and formaldehyde solution according to a molar ratio of 1: 3, adding a pH regulator to regulate the pH to 8-9, heating to 80 ℃ and reacting for 2 hours to generate a urea-formaldehyde resin prepolymer aqueous solution;
3) dispersing ammonium polyphosphate in absolute ethyl alcohol, adding a melamine formaldehyde prepolymer aqueous solution, adjusting the pH value to 3.5-4, reacting for 3 hours, adding a urea formaldehyde resin prepolymer aqueous solution, adjusting the pH value to 3.5-4, reacting for 3 hours, carrying out suction filtration, washing and drying to obtain the microencapsulated ammonium polyphosphate flame retardant, wherein the mass ratio of the melamine formaldehyde prepolymer aqueous solution to the urea formaldehyde resin prepolymer aqueous solution is 0.5: 1.
Example 5
As an embodiment of the composite fireproof coating, the composite fireproof coating of this embodiment includes the following components by mass percent: 40% of epoxy resin, 15% of waterborne polyurethane, 8% of microencapsulated ammonium polyphosphate flame retardant, 2.5% of nano mesoporous silica, 4% of pentaerythritol, 4% of potassium silicate, 3% of bentonite, 0.8% of auxiliary agent and the balance of water.
The preparation method of the composite fireproof coating comprises the following steps:
(1) adding water, epoxy resin and waterborne polyurethane into a reaction container, and uniformly stirring and mixing;
(2) adding nano mesoporous silica, and performing ultrasonic dispersion;
(3) adding microencapsulated ammonium polyphosphate flame retardant, pentaerythritol, potassium silicate, bentonite and an auxiliary agent, uniformly stirring, sieving and discharging to obtain the composite fireproof coating.
The preparation method of the microencapsulated ammonium polyphosphate flame retardant comprises the following steps:
1) mixing melamine and formaldehyde solution according to a molar ratio of 1: 3, adding a pH regulator to regulate the pH to 8-9, heating to 80 ℃ and reacting for 2 hours to generate a melamine formaldehyde prepolymer aqueous solution;
2) mixing urea and formaldehyde solution according to a molar ratio of 1: 3, adding a pH regulator to regulate the pH to 8-9, heating to 80 ℃ and reacting for 2 hours to generate a urea-formaldehyde resin prepolymer aqueous solution;
3) dispersing ammonium polyphosphate in absolute ethyl alcohol, adding a melamine formaldehyde prepolymer aqueous solution, adjusting the pH value to 3.5-4, reacting for 3 hours, adding a urea formaldehyde resin prepolymer aqueous solution, adjusting the pH value to 3.5-4, reacting for 3 hours, carrying out suction filtration, washing and drying to obtain the microencapsulated ammonium polyphosphate flame retardant, wherein the mass ratio of the melamine formaldehyde prepolymer aqueous solution to the urea formaldehyde resin prepolymer aqueous solution is 0.5: 1.
Example 6
As an embodiment of the composite fireproof coating, the composite fireproof coating of this embodiment includes the following components by mass percent: 20% of epoxy resin, 18% of waterborne polyurethane, 10% of microencapsulated ammonium polyphosphate flame retardant, 0.5% of nano mesoporous silica, 4% of pentaerythritol, 7% of potassium silicate, 6% of bentonite, 0.8% of auxiliary agent and the balance of water.
The preparation method of the composite fireproof coating comprises the following steps:
(1) adding water, epoxy resin and waterborne polyurethane into a reaction container, and uniformly stirring and mixing;
(2) adding nano mesoporous silica, and performing ultrasonic dispersion;
(3) adding microencapsulated ammonium polyphosphate flame retardant, pentaerythritol, potassium silicate, bentonite and an auxiliary agent, uniformly stirring, sieving and discharging to obtain the composite fireproof coating.
The preparation method of the microencapsulated ammonium polyphosphate flame retardant comprises the following steps:
1) mixing melamine and formaldehyde solution according to a molar ratio of 1: 3, adding a pH regulator to regulate the pH to 8-9, heating to 80 ℃ and reacting for 2 hours to generate a melamine formaldehyde prepolymer aqueous solution;
2) mixing urea and formaldehyde solution according to a molar ratio of 1: 3, adding a pH regulator to regulate the pH to 8-9, heating to 80 ℃ and reacting for 2 hours to generate a urea-formaldehyde resin prepolymer aqueous solution;
3) dispersing ammonium polyphosphate in absolute ethyl alcohol, adding a melamine formaldehyde prepolymer aqueous solution, adjusting the pH value to 3.5-4, reacting for 3 hours, adding a urea formaldehyde resin prepolymer aqueous solution, adjusting the pH value to 3.5-4, reacting for 3 hours, carrying out suction filtration, washing and drying to obtain the microencapsulated ammonium polyphosphate flame retardant, wherein the mass ratio of the melamine formaldehyde prepolymer aqueous solution to the urea formaldehyde resin prepolymer aqueous solution is 0.5: 1.
Example 7
As an embodiment of the composite fireproof coating, the composite fireproof coating of this embodiment includes the following components by mass percent: 40% of epoxy resin, 8% of waterborne polyurethane, 12% of microencapsulated ammonium polyphosphate flame retardant, 3% of nano mesoporous silica, 5% of pentaerythritol, 10% of bentonite, 2.5% of assistant and the balance of water.
The preparation method of the composite fireproof coating comprises the following steps:
(1) adding water, epoxy resin and waterborne polyurethane into a reaction container, and uniformly stirring and mixing;
(2) adding nano mesoporous silica, and performing ultrasonic dispersion;
(3) adding microencapsulated ammonium polyphosphate flame retardant, pentaerythritol, bentonite and an auxiliary agent, uniformly stirring, sieving and discharging to obtain the composite fireproof coating.
The preparation method of the microencapsulated ammonium polyphosphate flame retardant comprises the following steps:
1) mixing melamine and formaldehyde solution according to a molar ratio of 1: 3, adding a pH regulator to regulate the pH to 8-9, heating to 80 ℃ and reacting for 2 hours to generate a melamine formaldehyde prepolymer aqueous solution;
2) mixing urea and formaldehyde solution according to a molar ratio of 1: 3, adding a pH regulator to regulate the pH to 8-9, heating to 80 ℃ and reacting for 2 hours to generate a urea-formaldehyde resin prepolymer aqueous solution;
3) dispersing ammonium polyphosphate in absolute ethyl alcohol, adding a melamine formaldehyde prepolymer aqueous solution, adjusting the pH value to 3.5-4, reacting for 3 hours, adding a urea formaldehyde resin prepolymer aqueous solution, adjusting the pH value to 3.5-4, reacting for 3 hours, carrying out suction filtration, washing and drying to obtain the microencapsulated ammonium polyphosphate flame retardant, wherein the mass ratio of the melamine formaldehyde prepolymer aqueous solution to the urea formaldehyde resin prepolymer aqueous solution is 0.5: 1.
Comparative example 1
The composite fireproof coating comprises the following components in percentage by mass: 30% of epoxy resin, 12% of waterborne polyurethane, 12% of ammonium polyphosphate, 1.5% of nano mesoporous silica, 5% of pentaerythritol, 5% of potassium silicate, 5% of bentonite, 2.5% of an auxiliary agent and the balance of water.
The preparation method of the composite fireproof coating comprises the following steps:
(1) adding water, epoxy resin and waterborne polyurethane into a reaction container, and uniformly stirring and mixing;
(2) adding nano mesoporous silica, and performing ultrasonic dispersion;
(3) adding ammonium polyphosphate, pentaerythritol, potassium silicate, bentonite and an auxiliary agent, uniformly stirring, sieving and discharging to obtain the composite fireproof coating.
Comparative example 2
The composite fireproof coating comprises the following components in percentage by mass: 30% of epoxy resin, 12% of waterborne polyurethane, 12% of microencapsulated ammonium polyphosphate flame retardant, 1.5% of silicon dioxide, 5% of pentaerythritol, 5% of potassium silicate, 5% of bentonite, 2.5% of assistant and the balance of water.
The preparation method of the composite fireproof coating comprises the following steps:
(1) adding water, epoxy resin and waterborne polyurethane into a reaction container, and uniformly stirring and mixing;
(2) adding silicon dioxide, and performing ultrasonic dispersion;
(3) adding microencapsulated ammonium polyphosphate flame retardant, pentaerythritol, potassium silicate, bentonite and an auxiliary agent, uniformly stirring, sieving and discharging to obtain the composite fireproof coating.
The preparation method of the microencapsulated ammonium polyphosphate flame retardant comprises the following steps:
1) mixing melamine and formaldehyde solution according to a molar ratio of 1: 3, adding a pH regulator to regulate the pH to 8-9, heating to 80 ℃ and reacting for 2 hours to generate a melamine formaldehyde prepolymer aqueous solution;
2) mixing urea and formaldehyde solution according to a molar ratio of 1: 3, adding a pH regulator to regulate the pH to 8-9, heating to 80 ℃ and reacting for 2 hours to generate a urea-formaldehyde resin prepolymer aqueous solution;
3) dispersing ammonium polyphosphate in absolute ethyl alcohol, adding a melamine formaldehyde prepolymer aqueous solution, adjusting the pH value to 3.5-4, reacting for 3 hours, adding a urea formaldehyde resin prepolymer aqueous solution, adjusting the pH value to 3.5-4, reacting for 3 hours, carrying out suction filtration, washing and drying to obtain the microencapsulated ammonium polyphosphate flame retardant, wherein the mass ratio of the melamine formaldehyde prepolymer aqueous solution to the urea formaldehyde resin prepolymer aqueous solution is 0.5: 1.
Testing of the Properties of fire-resistant coatings
(1) Test for flame retardancy
The fire retardant coating of the invention is subjected to oxygen index measurement and vertical combustion experimental test.
The composite fireproof paint is painted onto PTFE board homogeneously, high vacuum silicone grease is used as demolding agent, and gradient temperature stoving is adopted. In the experiment, an HC-2 type oxygen index tester is used, and the oxygen index of a material sample is measured according to the national standard GB/T2406-93; according to the invention, a CFZ-2 vertical combustion instrument is used for carrying out a vertical combustion test according to the national standard GB 2408-80; the rate of heat release was determined by cone calorimeter with a thermal radiation flux of 40kW/m2The results are shown in Table 1.
TABLE 1
As can be seen from the results in Table 1, the components have the function of synergistically improving the flame retardant property of the coating by adjusting the mixture ratio of the components. In addition, the microencapsulated ammonium polyphosphate flame retardant has higher thermal stability, and a carbon layer generated in the combustion process has the functions of heat insulation and oxygen isolation, and further prevents the thermal decomposition of materials and the condensation phase of combustion, thereby improving the flame retardant property. The nano mesoporous silica has lower surface energy, is easy to migrate to the surface of the carbon layer to form a silica resistance layer with good sealing and certain strength, prolongs the diffusion channel of combustible gas and oxygen, reduces the transfer of heat and mass on the surface of the material, improves the vertical combustion grade of the material, and plays a good role in flame retardance.
(2) Adhesion force
And testing the adhesive force of the coating according to a Baige test method, brushing the fireproof coating of the embodiment 1-7 on the surface of the steel plate to enable the thickness of a dry film to be 3mm, and testing the coating.
Experimental results show that the fire retardant coating of examples 1-7 has a coating adhesion grade of 0 grade and has good adhesion.
(3) Water resistance test
The fireproof coating of examples 1 to 7 was coated on the surface of a steel plate, and naturally dried to a dry film thickness of 3mm, followed by curing for 10 days. And (3) sealing edges by using a mixture of rosin and paraffin in a mass ratio of 1:1, maintaining for 24 hours, soaking the sample in tap water for 48 hours, taking out, observing whether the coating has the phenomena of color change, falling, bubbling and the like, and calculating the weight loss rate according to the mass before and after soaking after natural air drying, wherein the results are shown in table 2.
| Group of | Weight loss ratio (%) |
| Example 1 | 2.6％ |
| Example 2 | 3.5％ |
| Example 3 | 3.2％ |
| Example 4 | 2.7％ |
| Example 5 | 5.5％ |
| Example 6 | 6.4％ |
| Example 7 | 7.2％ |
| Comparative example 1 | 13.5％ |
| Comparative example 2 | 15.8％ |
The examples 1 to 7 have no phenomena of discoloration, falling off, bubbling and the like, the surface of the material is flat, and the comparative examples 1 to 2 have the bubbling phenomenon. The results in Table 2 show that the weight loss rate of the examples 1 to 7 is obviously lower than that of the comparative examples 1 to 2, and the addition of the microencapsulated ammonium polyphosphate flame retardant and the silicon dioxide is favorable for improving the water resistance of the fireproof coating.
Finally, it should be noted that the above embodiments are only used for illustrating the technical solutions of the present invention and not for limiting the protection scope of the present invention, and although the present invention is described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that modifications or equivalent substitutions can be made on the technical solutions of the present invention without departing from the spirit and scope of the technical solutions of the present invention.
Claims (8)
1. The composite fireproof coating is characterized by comprising the following components in percentage by mass: 20-40% of epoxy resin, 8-18% of waterborne polyurethane, 8-15% of microencapsulated ammonium polyphosphate flame retardant, 0.5-3% of nano mesoporous silica, 4-6% of pentaerythritol, 0-7% of potassium silicate, 3-10% of bentonite, 0.8-2.5% of auxiliary agent and the balance of water, wherein the auxiliary agent is at least one of a film forming agent, a dispersing agent, a thickening agent, a flatting agent and a defoaming agent; the microencapsulated ammonium polyphosphate fire retardant is melamine-urea-formaldehyde resin-ammonium polyphosphate intumescent fire retardant, and the preparation method of the microencapsulated ammonium polyphosphate fire retardant comprises the following steps: mixing melamine and formaldehyde solution according to a molar ratio of 1: 2.5-3.5, adding a pH regulator to regulate the pH to 8-9, heating to 70-85 ℃, and reacting for 1-2 hours to generate a melamine formaldehyde prepolymer aqueous solution; mixing urea and formaldehyde solution according to a molar ratio of 1: 2.5-3.5, adding a pH regulator to regulate the pH to 8-9, heating to 70-85 ℃, and reacting for 1-2 hours to generate a urea-formaldehyde resin prepolymer aqueous solution; dispersing ammonium polyphosphate in absolute ethyl alcohol, adding a melamine formaldehyde prepolymer aqueous solution, adjusting the pH value to 3.5-4, reacting for 2-3 h, adding a urea formaldehyde resin prepolymer aqueous solution, adjusting the pH value to 3.5-4, reacting for 2-3 h, performing suction filtration, washing and drying to obtain the microencapsulated ammonium polyphosphate flame retardant.
2. The composite fireproof coating of claim 1, comprising the following components in percentage by mass: 25 to 40 percent of epoxy resin, 10 to 15 percent of waterborne polyurethane, 10 to 12 percent of microencapsulated ammonium polyphosphate fire retardant, 1.2 to 2.5 percent of nano mesoporous silica, 4 to 6 percent of pentaerythritol, 4 to 7 percent of potassium silicate, 5 to 10 percent of bentonite, 0.8 to 2.5 percent of auxiliary agent and the balance of water.
3. The composite fireproof coating of claim 1, wherein the mass ratio of the microencapsulated ammonium polyphosphate flame retardant to the nano mesoporous silica is 5-9: 1.
4. The composite fireproof coating of claim 1, comprising the following components in percentage by mass: 30% of epoxy resin, 12% of waterborne polyurethane, 12% of microencapsulated ammonium polyphosphate flame retardant, 1.5% of nano mesoporous silica, 5% of pentaerythritol, 5% of potassium silicate, 5% of bentonite, 2.5% of auxiliary agent and the balance of water.
5. The composite fireproof coating of claim 1, comprising the following components in percentage by mass: 34% of epoxy resin, 12% of waterborne polyurethane, 10% of microencapsulated ammonium polyphosphate flame retardant, 2.0% of nano mesoporous silica, 6% of pentaerythritol, 4% of potassium silicate, 7% of bentonite, 2% of auxiliary agent and the balance of water.
6. The composite fireproof coating of claim 1, comprising the following components in percentage by mass: 25% of epoxy resin, 10% of waterborne polyurethane, 15% of microencapsulated ammonium polyphosphate flame retardant, 2.5% of nano mesoporous silica, 5% of pentaerythritol, 5% of potassium silicate, 9% of bentonite, 1.0% of assistant and the balance of water.
7. The composite fireproof coating of claim 1, comprising the following components in percentage by mass: 28% of epoxy resin, 16% of waterborne polyurethane, 11% of microencapsulated ammonium polyphosphate fire retardant, 2.0% of nano mesoporous silica, 5% of pentaerythritol, 5% of potassium silicate, 10% of bentonite, 1.8% of assistant and the balance of water.
8. The preparation method of the composite fireproof coating according to any one of claims 1 to 7, wherein the method comprises the following steps:
(1) adding water, epoxy resin and waterborne polyurethane into a reaction container, and uniformly stirring and mixing;
(2) adding nano mesoporous silica, and performing ultrasonic dispersion;
(3) adding microencapsulated ammonium polyphosphate flame retardant, pentaerythritol, potassium silicate, bentonite and an auxiliary agent, uniformly stirring, sieving and discharging to obtain the composite fireproof coating.
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| CN113429859A (en) * | 2021-05-21 | 2021-09-24 | 深圳市华必达科技有限公司 | Functional mesoporous silica modified epoxy resin coating and preparation method thereof |
| CN114634753B (en) * | 2022-03-02 | 2023-07-28 | 湖南大川新型建材有限公司 | Preparation method of composite fireproof coating |
| CN116694204A (en) * | 2023-04-12 | 2023-09-05 | 北京理工大学 | Flame-retardant impact-resistant polyurea coating based on modified ammonium polyphosphate/two-dimensional nano filler reinforcement and preparation method thereof |
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