CN116589903A - Fireproof coating and preparation method thereof - Google Patents

Fireproof coating and preparation method thereof Download PDF

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Publication number
CN116589903A
CN116589903A CN202310508927.5A CN202310508927A CN116589903A CN 116589903 A CN116589903 A CN 116589903A CN 202310508927 A CN202310508927 A CN 202310508927A CN 116589903 A CN116589903 A CN 116589903A
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parts
self
stirring
agent
fireproof
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于颖
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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
    • 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
    • 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
    • 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
    • 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
    • C09D7/65—Additives macromolecular
    • 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
    • C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
    • C08K3/20—Oxides; Hydroxides
    • C08K3/22—Oxides; Hydroxides of metals
    • C08K2003/2217—Oxides; Hydroxides of metals of magnesium
    • C08K2003/2224—Magnesium hydroxide
    • 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
    • C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
    • C08K3/20—Oxides; Hydroxides
    • C08K3/22—Oxides; Hydroxides of metals
    • C08K2003/2227—Oxides; Hydroxides of metals of aluminium
    • 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
    • C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
    • C08K3/20—Oxides; Hydroxides
    • C08K3/22—Oxides; Hydroxides of metals
    • C08K2003/2237—Oxides; Hydroxides of metals of titanium
    • C08K2003/2241—Titanium dioxide
    • 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
    • C08K3/30—Sulfur-, selenium- or tellurium-containing compounds
    • C08K2003/3045—Sulfates
    • C08K2003/3063—Magnesium sulfate
    • 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
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
    • Y02W30/00—Technologies for solid waste management
    • Y02W30/50—Reuse, recycling or recovery technologies
    • Y02W30/91—Use of waste materials as fillers for mortars or concrete

Abstract

The invention discloses a fireproof coating and a preparation method thereof, and the fireproof coating comprises the following raw materials in parts by weight: 10-15 parts of epoxy resin, 8-12 parts of epoxy acrylic resin, 5-10 parts of self-made fire extinguishing agent microcapsules, 6-12 parts of self-made fireproof fibers, 4-7 parts of defoamer, 4-8 parts of flatting agent, 3-6 parts of coupling agent and 4-8 parts of inorganic filler. The preparation method comprises the following steps: s1: weighing epoxy resin, epoxy acrylic resin, self-made fire extinguishing agent microcapsules, self-made fireproof fibers, defoamer, flatting agent, coupling agent and inorganic filler according to the proportion; s2: adding epoxy resin and epoxy acrylic resin into a container, stirring, adding qualification fire-extinguishing microcapsules and self-made fireproof fibers, transferring into a reaction kettle, reacting at a certain temperature, and cooling for later use; s3: adding a defoaming agent, a leveling agent, a coupling agent and an inorganic filler into the product obtained in the step S2, stirring at a certain stirring rate, and standing for 0.5-1 h to obtain the fireproof coating.

Description

Fireproof coating and preparation method thereof
Technical Field
The invention belongs to the technical field of fireproof coatings, and particularly relates to a fireproof coating and a preparation method thereof.
Background
The fireproof paint is one kind of paint for fireproof steel structure, facing fireproof paint, fireproof cable paint, fireproof prestressed concrete floor, etc. The flame retardant is usually prepared by adding flame retardant, additive and the like into a coating base material, and the flame retardant has the fireproof protection function through incombustibility, low thermal conductivity or heat absorption. The flame retardant properties and weather resistance of fire-retardant coatings are achieved by adding flame retardants including ammonium polyphosphate, pentaerythritol, aluminum hydroxide, etc. to the coating substrate as disclosed in the literature. There has also been a related study of preparing fire-retardant coatings with a low molecular weight carbon source, a char-forming catalyst and a blowing agent to make up an intumescent flame retardant. However, the flame retardant can only prevent the spread of the fire area, but it is difficult to actively extinguish the fire in a short time, and the extinguishing agent having the extinguishing effect is generally difficult to stably exist in the coating.
Disclosure of Invention
Aiming at the problems in the prior art, the invention aims to provide a fireproof coating, which comprises the following raw materials in parts by weight: 10-15 parts of epoxy resin, 8-12 parts of epoxy acrylic resin, 5-10 parts of self-made fire extinguishing agent microcapsules, 6-12 parts of self-made fireproof fibers, 4-7 parts of defoamer, 4-8 parts of flatting agent, 3-6 parts of coupling agent and 4-8 parts of inorganic filler.
Further, the self-made fire extinguishing microcapsule is prepared by the following method:
1) Melamine, urea and butyraldehyde are mixed according to the mass ratio of 1: (1.5-2.5): (3-5) adding the mixture into deionized water, regulating the pH value of the mixture to 8.6-8.9, heating to 40-48 ℃, stirring for 4-8 hours, and cooling to room temperature to obtain the prepolymer.
2) And (3) dispersing the pre-mixed material in an aqueous solution of chitosan and sodium alginate, rapidly stirring and carrying out ultrasonic treatment, then adding perfluoro-hexanone, continuously adding perfluoro-hexyl ethyl triethoxysilane and acetic acid, continuously stirring and reacting for 2-6 h, and standing for 5-10 h to gel the mixture, thus obtaining the fire extinguishing microcapsule.
Further, the average molecular weight of the prepolymer was 1.2X10 4 ～1.8×10 4 And/or the weight average molecular weight of the prepolymer is 0.4X10 4 ～1×10 4 。
Further, the mass ratio of the chitosan to the sodium alginate in the aqueous solution of the chitosan and the sodium alginate is 1.2-1.8: 1, a step of; the mass ratio of the prepolymer to the perfluorinated hexanone to the perfluorinated hexyl ethyl triethoxysilane to the acetic acid is 1: (1.22-1.64): (0.36-0.68): (5-15).
Further, the self-made fireproof fiber is prepared by the following method:
(1) Crushing plant fibers, sieving with a 800-1000 mesh sieve, transferring to a high-pressure reaction kettle, adding phosphoric acid solution, and reacting at 60-80 ℃ for 3-6 hours to obtain acidified fiber slurry.
(2) Adding a magnesium sulfate preparation, diatomite and talcum powder into the acidified fiber slurry, stirring at 50-75 ℃ for 4-7 hours, adding a surfactant, and continuously stirring for 3-6 hours to obtain the self-made fireproof fiber.
Further, the mass-volume ratio of the magnesium sulfate preparation, the diatomite, the talcum powder and the acidified fiber slurry is (2.5-4) g: (3.2-4.8) g: (1.8-3.6) g: (30-50) mL.
Further, the surfactant is any one of sodium dodecyl benzene sulfonate, sodium dodecyl sulfate and octyl phenol polyoxyethylene ether.
Further, the defoamer is selected from melamine or dicyandiamide; the coupling agent is selected from the mass ratio of 1: (1.05-1.2) a titanate coupling agent and a silane coupling agent.
Further, the inorganic filler is selected from the group consisting of 1: (0.6-0.7): (0.4-0.5): (0.45-0.6) titanium dioxide, graphite, magnesium hydroxide and aluminum hydroxide.
The invention also provides a preparation method of the fireproof coating, which comprises the following steps:
s1: according to the proportion, the epoxy resin, the epoxy acrylic resin, the self-made fire extinguishing agent microcapsule, the self-made fireproof fiber, the defoaming agent, the leveling agent, the coupling agent and the inorganic filler are weighed.
S2: adding epoxy resin and epoxy acrylic resin into a container, stirring, adding qualification fire-extinguishing microcapsules and self-made fireproof fibers, transferring into a reaction kettle, reacting at a certain temperature, and cooling for later use.
S3: adding a defoaming agent, a leveling agent, a coupling agent and an inorganic filler into the product obtained in the step S2, stirring at a certain stirring rate, and standing for 0.5-1 h to obtain the fireproof coating.
Preferably, the reaction temperature in the reaction kettle in the step S2 is 60-80 ℃ and the reaction lasts for 4-10 hours.
Preferably, the stirring speed in the step S3 is 1500-2000 r/min, and the stirring time is 2-3 h.
The invention also has the following beneficial effects:
1. in the invention, the magnesium sulfate preparation adopted by the self-made fireproof fiber is prepared from MgSO with a certain concentration 4 MgO-MgSO composed of solution and light burned MgO 4 -H 2 The O ternary gel system is used for modifying plant fibers, wherein the self-made fibers modified by the magnesium sulfate preparation have the characteristics of moisture absorption and halogen return, and halogen elements are easily adsorbed and combined in the process of further preparing the protective coating, so that the protective coating has more excellent fireproof performance.
2. According to the invention, the self-made fire-extinguishing microcapsule adopts a prepolymer obtained by polymerizing melamine-urea-butyraldehyde as a core material, chitosan, sodium alginate and perfluoro-hexanone are coated on the surface of the core material to be used as a shell material, wherein the perfluoro-hexanone contained in the shell has a fire-extinguishing effect when heated, and then the melamine-urea-butyraldehyde in the core material also has a fire-extinguishing component, and the fire-extinguishing effect is performed after the shell material is consumed, so that the qualification fire-extinguishing microcapsule has long-acting and excellent fire-extinguishing and fireproof performances.
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Detailed Description
The following detailed description of the embodiments of the present invention is provided on the premise of the technical solution of the present invention, and the detailed implementation manner and specific operation process are provided, and it should be noted that, for those skilled in the art, several improvements and modifications can be made without departing from the principle of the present invention, and these improvements and modifications should also be considered as the protection scope of the present invention.
Example 1
The fireproof paint comprises the following raw materials in parts by weight: 10 parts of epoxy resin, 8 parts of epoxy acrylic resin, 5 parts of self-made fire extinguishing agent microcapsules, 6 parts of self-made fireproof fibers, 4 parts of defoamer, 4 parts of flatting agent, 3 parts of coupling agent and 4 parts of inorganic filler.
The self-made fire extinguishing microcapsule is prepared by the following method:
1) Melamine, urea and butyraldehyde are mixed according to the mass ratio of 1:1.5:3 adding the mixture into deionized water, adjusting the pH value of the mixture to 8.6, heating to 40 ℃, stirring for 4 hours, and cooling to room temperature to obtain the prepolymer.
2) And (3) dispersing the pre-mixed material in an aqueous solution of chitosan and sodium alginate, rapidly stirring and carrying out ultrasonic treatment, then adding perfluoro-hexanone, continuously adding perfluoro-hexyl ethyl triethoxysilane and acetic acid, continuously stirring and reacting for 2 hours, and standing for 5 hours to gel the mixture to obtain the fire extinguishing microcapsule.
Wherein the average molecular weight of the prepolymer is 1.2×104, and/or the weight average molecular weight of the prepolymer is 0.4×104. The mass ratio of the chitosan to the sodium alginate in the aqueous solution of the chitosan and the sodium alginate is 1.2:1, a step of; the mass ratio of the prepolymer to the perfluorinated hexanone to the perfluorinated hexyl ethyl triethoxysilane to the acetic acid is 1:1.22:0.36:5.
the self-made fireproof fiber is prepared by the following method:
(1) Crushing plant fibers, sieving with a 800-mesh sieve, transferring to a high-pressure reaction kettle, adding a phosphoric acid solution, and reacting at 60 ℃ for 3 hours to obtain acidified fiber slurry.
(2) Adding a magnesium sulfate preparation, diatomite and talcum powder into the acidified fiber slurry, then stirring at 50 ℃ for 4 hours, adding a surfactant, and continuing stirring for 3 hours to obtain the self-made fireproof fiber.
Wherein the mass volume ratio of the magnesium sulfate preparation to the diatomite to the talcum powder to the acidified fiber slurry is 2.5g:3.2g:1.8g:30mL. The surfactant is sodium dodecyl benzene sulfonate. The defoamer is selected from melamine; the coupling agent is selected from the mass ratio of 1:1.05 titanate coupling agent and silane coupling agent. The inorganic filler is selected from the following materials in mass ratio of 1:0.6:0.4: titanium dioxide, graphite, magnesium hydroxide and aluminum hydroxide of 0.45.
The preparation method of the fireproof paint comprises the following steps:
s1: according to the proportion, the epoxy resin, the epoxy acrylic resin, the self-made fire extinguishing agent microcapsule, the self-made fireproof fiber, the defoaming agent, the leveling agent, the coupling agent and the inorganic filler are weighed.
S2: adding epoxy resin and epoxy acrylic resin into a container, stirring, adding qualification fire-extinguishing microcapsules and self-made fireproof fibers, transferring into a reaction kettle, reacting at a certain temperature, and cooling for later use.
S3: and (2) adding a defoaming agent, a leveling agent, a coupling agent and an inorganic filler into the product obtained in the step (S2), stirring at a certain stirring rate, and standing for 0.5h to obtain the fireproof coating.
Wherein the temperature of the reaction kettle in the step S2 is 60 ℃, the reaction is carried out for 4 hours, the stirring speed in the step S3 is 1500r/min, and the stirring time is 2 hours.
Example 2
The fireproof paint comprises the following raw materials in parts by weight: 15 parts of epoxy resin, 12 parts of epoxy acrylic resin, 10 parts of self-made fire extinguishing agent microgel, 12 parts of self-made fireproof fiber, 7 parts of defoamer, 8 parts of flatting agent, 6 parts of coupling agent and 8 parts of inorganic filler.
The self-made fire extinguishing microcapsule is prepared by the following method:
1) Melamine, urea and butyraldehyde are mixed according to the mass ratio of 1:2.5:5, adding the mixture into deionized water, adjusting the pH value of the mixture to 8.9, heating to 48 ℃, stirring for 8 hours, and cooling to room temperature to obtain the prepolymer.
2) And (3) dispersing the pre-mixed material in an aqueous solution of chitosan and sodium alginate, rapidly stirring and carrying out ultrasonic treatment, then adding perfluoro-hexanone, continuously adding perfluoro-hexyl ethyl triethoxysilane and acetic acid, continuously stirring and reacting for 6 hours, and standing for 10 hours to gel the mixture to obtain the fire extinguishing microcapsule.
Wherein the average molecular weight of the prepolymer is 1.8X104, and/or the weight average molecular weight of the prepolymer is 1X 104. The mass ratio of the chitosan to the sodium alginate in the aqueous solution of the chitosan and the sodium alginate is 1.8:1, a step of; the mass ratio of the prepolymer to the perfluorinated hexanone to the perfluorinated hexyl ethyl triethoxysilane to the acetic acid is 1:1.64:0.68:15.
the self-made fireproof fiber is prepared by the following method:
(1) Crushing plant fibers, sieving with a 1000-mesh sieve, transferring to a high-pressure reaction kettle, adding a phosphoric acid solution, and reacting at 80 ℃ for 6 hours to obtain acidified fiber slurry.
(2) Adding the magnesium sulfate preparation, diatomite and talcum powder into the acidified fiber slurry, stirring at 75 ℃ for 7 hours, adding the surfactant, and continuing stirring for 6 hours to obtain the self-made fireproof fiber.
Wherein the mass volume ratio of the magnesium sulfate preparation to the diatomite to the talcum powder to the acidified fiber slurry is 4g:4.8g:3.6g:50mL. The surfactant is sodium dodecyl sulfonate. The defoamer is selected from dicyandiamide; the coupling agent is selected from the mass ratio of 1:1.2 titanate coupling agents and silane coupling agents. The inorganic filler is selected from the following materials in mass ratio of 1:0.7:0.5: titanium dioxide, graphite, magnesium hydroxide and aluminum hydroxide of 0.6.
The preparation method of the fireproof paint comprises the following steps:
s1: according to the proportion, the epoxy resin, the epoxy acrylic resin, the self-made fire extinguishing agent microcapsule, the self-made fireproof fiber, the defoaming agent, the leveling agent, the coupling agent and the inorganic filler are weighed.
S2: adding epoxy resin and epoxy acrylic resin into a container, stirring, adding qualification fire-extinguishing microcapsules and self-made fireproof fibers, transferring into a reaction kettle, reacting at a certain temperature, and cooling for later use.
S3: and (2) adding a defoaming agent, a leveling agent, a coupling agent and an inorganic filler into the product obtained in the step (S2), stirring at a certain stirring rate, and standing for 1h to obtain the fireproof coating.
Wherein the temperature of the reaction kettle in the step S2 is 80 ℃, the reaction is carried out for 10 hours, the stirring speed in the step S3 is 2000r/min, and the stirring time is 3 hours.
Example 3
The fireproof paint comprises the following raw materials in parts by weight: 12 parts of epoxy resin, 10 parts of epoxy acrylic resin, 7 parts of self-made fire extinguishing agent microcapsules, 8 parts of self-made fireproof fibers, 5 parts of defoamer, 5 parts of flatting agent, 4 parts of coupling agent and 5 parts of inorganic filler.
The self-made fire extinguishing microcapsule is prepared by the following method:
1) Melamine, urea and butyraldehyde are mixed according to the mass ratio of 1:1.7:3.8, adding the mixture into deionized water, adjusting the pH value of the mixture to 8.7, heating to 44 ℃, stirring for 6 hours, and cooling to room temperature to obtain the prepolymer.
2) And (3) dispersing the pre-mixed material in an aqueous solution of chitosan and sodium alginate, rapidly stirring and carrying out ultrasonic treatment, then adding perfluoro-hexanone, continuously adding perfluoro-hexyl ethyl triethoxysilane and acetic acid, continuously stirring and reacting for 4 hours, and standing for 7 hours to gel the mixture to obtain the fire extinguishing microcapsule.
Wherein the average molecular weight of the prepolymer is 1.4X10 4 And/or the weight average molecular weight of the prepolymer is 0.6X10 4 . The mass ratio of the chitosan to the sodium alginate in the aqueous solution of the chitosan and the sodium alginate is 1.4:1, a step of; the mass ratio of the prepolymer to the perfluorinated hexanone to the perfluorinated hexyl ethyl triethoxysilane to the acetic acid is 1:1.42:0.44:8.
the self-made fireproof fiber is prepared by the following method:
(1) Crushing plant fibers, sieving with a 900-mesh sieve, transferring to a high-pressure reaction kettle, adding a phosphoric acid solution, and reacting for 4 hours at 70 ℃ to obtain acidified fiber slurry.
(2) Adding a magnesium sulfate preparation, diatomite and talcum powder into the acidified fiber slurry, then stirring at 55 ℃ for 5 hours, adding a surfactant, and continuing stirring for 4 hours to obtain the self-made fireproof fiber.
Wherein the mass volume ratio of the magnesium sulfate preparation to the diatomite to the talcum powder to the acidified fiber slurry is 3g:3.8g:2.6g:40mL. The surfactant is sodium dodecyl sulfate. The defoamer is selected from melamine; the coupling agent is selected from the mass ratio of 1:1.1 titanate coupling agents and silane coupling agents. The inorganic filler is selected from the following materials in mass ratio of 1:0.65:0.44: titanium dioxide, graphite, magnesium hydroxide and aluminum hydroxide of 0.48.
The preparation method of the fireproof paint comprises the following steps:
s1: according to the proportion, the epoxy resin, the epoxy acrylic resin, the self-made fire extinguishing agent microcapsule, the self-made fireproof fiber, the defoaming agent, the leveling agent, the coupling agent and the inorganic filler are weighed.
S2: adding epoxy resin and epoxy acrylic resin into a container, stirring, adding qualification fire-extinguishing microcapsules and self-made fireproof fibers, transferring into a reaction kettle, reacting at a certain temperature, and cooling for later use.
S3: and (2) adding a defoaming agent, a leveling agent, a coupling agent and an inorganic filler into the product obtained in the step (S2), stirring at a certain stirring rate, and standing for 0.7h to obtain the fireproof coating.
Wherein, the temperature of the reaction kettle in the step S2 is 70 ℃, the reaction is carried out for 6 hours, the stirring speed in the step S3 is 1600r/min, and the stirring time is 3 hours.
Example 4
The fireproof paint comprises the following raw materials in parts by weight: 14 parts of epoxy resin, 11 parts of epoxy acrylic resin, 9 parts of self-made fire extinguishing agent microcapsules, 10 parts of self-made fireproof fibers, 6 parts of defoamer, 7 parts of flatting agent, 5 parts of coupling agent and 7 parts of inorganic filler.
The self-made fire extinguishing microcapsule is prepared by the following method:
1) Melamine, urea and butyraldehyde are mixed according to the mass ratio of 1:2.4:4.8, adding the mixture into deionized water, adjusting the pH value of the mixture to 8.8, heating to 46 ℃, stirring for 7 hours, and cooling to room temperature to obtain the prepolymer.
2) And (3) dispersing the pre-mixed material in an aqueous solution of chitosan and sodium alginate, rapidly stirring and carrying out ultrasonic treatment, then adding perfluoro-hexanone, continuously adding perfluoro-hexyl ethyl triethoxysilane and acetic acid, continuously stirring and reacting for 5 hours, and standing for 8 hours to gel the mixture to obtain the fire extinguishing microcapsule.
Wherein the average of the prepolymerMolecular weight of 1.7X10 4 And/or the weight average molecular weight of the prepolymer is 0.8X10 4 . The mass ratio of the chitosan to the sodium alginate in the aqueous solution of the chitosan and the sodium alginate is 1.6:1, a step of; the mass ratio of the prepolymer to the perfluorinated hexanone to the perfluorinated hexyl ethyl triethoxysilane to the acetic acid is 1:1.58:0.61:14.
the self-made fireproof fiber is prepared by the following method:
(1) Crushing plant fibers, sieving with a 900-mesh sieve, transferring to a high-pressure reaction kettle, adding a phosphoric acid solution, and reacting at 75 ℃ for 5 hours to obtain acidified fiber slurry.
(2) Adding a magnesium sulfate preparation, diatomite and talcum powder into the acidified fiber slurry, then stirring at 70 ℃ for 6 hours, adding a surfactant, and continuing stirring for 3-6 hours to obtain the self-made fireproof fiber.
Wherein the mass volume ratio of the magnesium sulfate preparation to the diatomite to the talcum powder to the acidified fiber slurry is 3.8g:4.6g:3.2g:45mL. The surfactant is octyl phenol polyoxyethylene ether. The defoamer is selected from dicyandiamide; the coupling agent is selected from the mass ratio of 1:1.18 titanate coupling agents and silane coupling agents. The inorganic filler is selected from the following materials in mass ratio of 1:0.68:0.48: titanium dioxide, graphite, magnesium hydroxide and aluminum hydroxide of 0.55.
The preparation method of the fireproof paint comprises the following steps:
s1: according to the proportion, the epoxy resin, the epoxy acrylic resin, the self-made fire extinguishing agent microcapsule, the self-made fireproof fiber, the defoaming agent, the leveling agent, the coupling agent and the inorganic filler are weighed.
S2: adding epoxy resin and epoxy acrylic resin into a container, stirring, adding qualification fire-extinguishing microcapsules and self-made fireproof fibers, transferring into a reaction kettle, reacting at a certain temperature, and cooling for later use.
S3: and (2) adding a defoaming agent, a leveling agent, a coupling agent and an inorganic filler into the product obtained in the step (S2), stirring at a certain stirring rate, and standing for 0.8h to obtain the fireproof coating.
Wherein the temperature of the reaction kettle in the step S2 is 75 ℃, the reaction is carried out for 8 hours, the stirring speed in the step S3 is 1900r/min, and the stirring time is 3 hours.
Performance test:
(1) The fireproof paint prepared in examples 1 to 4 was tested for performance indexes including water resistance, alkali resistance and fire resistance according to the technical requirements of the concrete construction fireproof paint in GA 98-2005.
(2) The fireproof paint prepared in the examples 1-4 is coated on a polished wood board with the thickness of 18cm multiplied by 0.5cm, wherein the coating is coated for 1 day at intervals of 1.2+/-0.02 mm each time, the coating thickness of the wood board is 1+/-0.06 mm by 5 times, and the wood board is dried in an oven at 35 ℃ in a blasting way; placing the test sample plate on the iron ring with the coating surface facing downwards, keeping the vertical distance between the iron ring and the alcohol burner at 7cm, moving the burner to the lower part of the test sample plate to burn the fireproof coating when the flame temperature is raised to 1000 ℃, fixing the temperature sensor head wrapped by the heat insulation material on the back fire surface of the wood board, recording the back surface temperature once every 5min, burning for 80min, and testing the result shown in table 1,
table 1. Test results:
as can be seen from the test results in Table 1, the fireproof paint prepared in the examples of the present invention has excellent comprehensive properties.

Claims (10)

1. The fireproof coating is characterized by comprising the following raw materials in parts by weight: 10-15 parts of epoxy resin, 8-12 parts of epoxy acrylic resin, 5-10 parts of self-made fire extinguishing agent microcapsules, 6-12 parts of self-made fireproof fibers, 4-7 parts of defoamer, 4-8 parts of flatting agent, 3-6 parts of coupling agent and 4-8 parts of inorganic filler;
the self-made fire extinguishing microcapsule is prepared by the following method:
1) Melamine, urea and butyraldehyde are mixed according to the mass ratio of 1: (1.5-2.5): (3-5) adding the mixture into deionized water, regulating the pH value of the mixture to 8.6-8.9, heating to 40-48 ℃, stirring for 4-8 hours, and cooling to room temperature to obtain a prepolymer;
2) And (3) dispersing the pre-mixed material in an aqueous solution of chitosan and sodium alginate, rapidly stirring and carrying out ultrasonic treatment, then adding perfluoro-hexanone, continuously adding perfluoro-hexyl ethyl triethoxysilane and acetic acid, continuously stirring and reacting for 2-6 h, and standing for 5-10 h to gel the mixture, thus obtaining the fire extinguishing microcapsule.
2. A fire retardant coating according to claim 1 wherein the average molecular weight of the prepolymer is 1.2 x 10 4 ～1.8×10 4 ；
And/or the number of the groups of groups,
the weight average molecular weight of the prepolymer is 0.4X10 4 ～1×10 4 。
3. The fire-retardant coating according to claim 1, wherein the mass ratio of chitosan to sodium alginate in the aqueous solution of chitosan and sodium alginate is 1.2-1.8: 1, a step of; the mass ratio of the prepolymer to the perfluorinated hexanone to the perfluorinated hexyl ethyl triethoxysilane to the acetic acid is 1: (1.22-1.64): (0.36-0.68): (5-15).
4. The fire retardant coating of claim 1, wherein the self-made fire retardant fiber is prepared by the following method:
the self-made fireproof fiber is prepared by the following method:
(1) Crushing plant fibers, sieving with a 800-1000 mesh sieve, then transferring to a high-pressure reaction kettle, adding phosphoric acid solution, and reacting for 3-6 hours at 60-80 ℃ to obtain acidified fiber slurry;
(2) Adding a magnesium sulfate preparation, diatomite and talcum powder into the acidified fiber slurry, stirring at 50-75 ℃ for 4-7 hours, adding a surfactant, and continuously stirring for 3-6 hours to obtain the self-made fireproof fiber.
5. The fire retardant coating according to claim 4, wherein the mass to volume ratio of the magnesium sulfate preparation, the diatomite, the talcum powder and the acidified fiber slurry is (2.5-4) g: (3.2-4.8) g: (1.8-3.6) g: (30-50) mL;
and/or the number of the groups of groups,
the surfactant is any one of sodium dodecyl benzene sulfonate, sodium dodecyl sulfate and octyl phenol polyoxyethylene ether.
6. A fire retardant coating according to claim 1, wherein the defoamer is selected from melamine or dicyandiamide; the coupling agent is selected from the mass ratio of 1: (1.05-1.2) a titanate coupling agent and a silane coupling agent.
7. A fire retardant coating according to claim 1, wherein the inorganic filler is selected from the group consisting of 1: (0.6-0.7): (0.4-0.5): (0.45-0.6) titanium dioxide, graphite, magnesium hydroxide and aluminum hydroxide.
8. A method of preparing a fire retardant coating according to any one of claims 1 to 7, comprising the steps of:
s1: weighing epoxy resin, epoxy acrylic resin, self-made fire extinguishing agent microcapsules, self-made fireproof fibers, defoamer, flatting agent, coupling agent and inorganic filler according to the proportion;
s2: adding epoxy resin and epoxy acrylic resin into a container, stirring, adding qualification fire-extinguishing microcapsules and self-made fireproof fibers, transferring into a reaction kettle, reacting at a certain temperature, and cooling for later use;
s3: adding a defoaming agent, a leveling agent, a coupling agent and an inorganic filler into the product obtained in the step S2, stirring at a certain stirring rate, and standing for 0.5-1 h to obtain the fireproof coating.
9. The method for preparing fire retardant coating according to claim 8, wherein the reaction temperature in the reaction kettle in the step S2 is 60-80 ℃ for 4-10 h.
10. The method for preparing a fire retardant coating according to claim 8, wherein the stirring rate in the step S3 is 1500-2000 r/min and the stirring time is 2-3 h.
CN202310508927.5A 2023-05-08 2023-05-08 Fireproof coating and preparation method thereof Pending CN116589903A (en)

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Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114736554A (en) * 2022-06-15 2022-07-12 浙江虹达特种橡胶制品有限公司杭州分公司 Environment-friendly fireproof coating and preparation method thereof

Patent Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114736554A (en) * 2022-06-15 2022-07-12 浙江虹达特种橡胶制品有限公司杭州分公司 Environment-friendly fireproof coating and preparation method thereof

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