CN111662585A - Fireproof coating with heat insulation and preservation performance - Google Patents
Fireproof coating with heat insulation and preservation performance Download PDFInfo
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- C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
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- C08F220/18—Esters of monohydric alcohols or phenols of phenols or of alcohols containing two or more carbon atoms with acrylic or methacrylic acids
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- C09D133/00—Coating compositions based on homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Coating compositions based on derivatives of such polymers
- C09D133/04—Homopolymers or copolymers of esters
- C09D133/06—Homopolymers or copolymers of esters of esters containing only carbon, hydrogen and oxygen, the oxygen atom being present only as part of the carboxyl radical
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- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
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- C09D7/63—Additives non-macromolecular organic
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- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
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- C08L2207/53—Core-shell polymer
Abstract
The invention belongs to the technical field of coatings. A fireproof coating with heat insulation and preservation performance comprises the following components in percentage by mass: molybdenum disulfide and methacrylic acid modified acrylate core-shell emulsion, hyperbranched polyphosphate ammonium charring agent, melamine, pentaerythritol, nano titanium dioxide, nano titanium pyrophosphate, nano potassium hexatitanate, nano aluminum hydroxide, zinc borate, organic modified sepiolite, phosphate grafted bentonite, a dispersing agent, a defoaming agent, a film forming aid, a thickening agent and the balance of water. The fireproof coating has the advantages of fast curing, good film forming property, high coating hardness and strong adhesive force; the coating film has good fireproof and flame-retardant properties, and can form a uniform and compact expansion layer on the surface of the base material after being heated, thereby delaying the temperature rise speed of the base material, insulating heat, effectively isolating combustion heat, avoiding melting of the base material and obstructing flame transfer.
Description
Technical Field
The invention belongs to the technical field of coatings, and relates to a fireproof coating with heat insulation and preservation properties.
Background
For a long time, the fire disaster is a universal catastrophic problem in the world, seriously threatens the safety of human life and property, and the fire disaster caused by various reasons causes great loss to the life and property of people. Fire protection is an important field of fire-fighting science and technology, and the fire-proof coating is also an important component of a fire-proof material.
The fireproof coating is applied to the surface of a combustible base material, can reduce the flammability of the surface of the base material and retard the rapid spread of fire so as to improve the fire endurance of the coated material. There are two main types of fire-retardant coatings, non-intumescent fire-retardant coatings and intumescent fire-retardant coatings. The non-intumescent fire-retardant coating generally plays a role in fire prevention and heat insulation by adding inorganic fire-resistant materials to prevent fire, but is gradually eliminated due to the unsatisfactory fire-retardant effect. The expansion type fireproof coating is widely applied due to better fireproof performance, and can be divided into three types, namely a water type fireproof coating, an oil type fireproof coating and a powder type fireproof coating according to the coating forms, the dosage is gradually reduced because the solvent of the oil type fireproof coating volatilizes and easily pollutes the environment, and the most widely applied water-based thin-coating type fireproof coating reduces the pollution caused by solvent volatilization by taking water as the solvent. The existing thin-coating expansion type fireproof coating mainly adopts water-based polymer emulsion as a film forming substance, flame retardant components comprise ammonium polyphosphate, melamine, pentaerythritol, inorganic materials and the like, and the preparation method comprises the steps of high-speed dispersion, grinding and the like. The flame-retardant and fire-resistant performance of the existing water-based thin-coating type fireproof coating is easily influenced by the dispersibility of flame-retardant components in the coating, so that the fire-resistant performance of the coating is unstable, and the formed coating is easy to crack and fall off after high-temperature expansion and poor in heat insulation and fire resistance.
Disclosure of Invention
The technical problem to be solved by the invention is to provide a fireproof coating with heat insulation and preservation performances, which has the advantages of fast curing, good film forming property, high film hardness and strong adhesive force; the coating film has good fireproof and flame-retardant properties, and can form a uniform and compact expansion layer on the surface of the base material after being heated, thereby delaying the temperature rise speed of the base material, insulating heat, effectively isolating combustion heat, avoiding melting of the base material and obstructing flame transfer.
The technical scheme of the invention is as follows:
a fireproof coating with heat insulation and preservation performance comprises the following components in percentage by mass: 25-35% of molybdenum disulfide and methacrylic acid modified acrylate core-shell emulsion, 15-20% of hyperbranched poly-ammonium phosphate charring agent, 10-15% of melamine, 8-12% of pentaerythritol, 3-5% of nano titanium dioxide, 1-5% of nano titanium pyrophosphate, 2-3% of nano potassium hexatitanate, 5-10% of nano aluminum hydroxide, 2-5% of zinc borate, 1-3% of organic modified sepiolite, 1-3% of phosphate grafted bentonite, 0.5-1% of dispersing agent, 0.5-1% of defoaming agent, 0.5-1% of film forming additive, 0.5-1% of thickening agent and the balance of water.
Further, the molybdenum disulfide and methacrylic acid modified acrylate core-shell emulsion is prepared by polymerizing the core-shell emulsion by using an emulsifier, a core monomer mixture and a shell monomer mixture as main raw materials; the emulsifier is sodium dodecyl benzene sulfate, sodium dodecyl sulfate or polyethylene glycol octyl phenyl ether; the nuclear monomer mixture comprises n-butyl acrylate, methyl methacrylate and nano molybdenum disulfide; the shell monomer mixture comprises n-butyl acrylate, methyl methacrylate, methacrylic acid and nano molybdenum disulfide.
Further, the mass ratio of the core monomer mixture to the shell monomer mixture is 1-2: 2-3; the mass ratio of the total mass of the core monomer mixture and the shell monomer mixture to the emulsifier to the nano molybdenum disulfide to the methacrylic acid is 10: 0.1-1: 0.5-1: 0.1 to 1; the mass ratio of n-butyl acrylate to methyl methacrylate in the nuclear monomer mixture is 2-3: 1; the mass ratio of n-butyl acrylate to methyl methacrylate in the shell monomer mixture is 1-3: 1.
Further, the preparation method of the molybdenum disulfide and methacrylic acid modified acrylate core-shell emulsion comprises the following steps:
(1) dissolving an emulsifier in water to prepare an emulsifier aqueous solution, and averagely dividing the emulsifier aqueous solution into three parts for later use; respectively dripping the core monomer mixture and the shell monomer mixture into one part of the emulsifier aqueous solution, stirring and pre-emulsifying for 1-1.5h to respectively prepare a core monomer pre-emulsion and a shell monomer pre-emulsion; adding a buffer to the remaining portion of the aqueous emulsifier solution to produce an aqueous buffer solution; dissolving an initiator in water to prepare an initiator aqueous solution;
(2) mixing and stirring a buffer aqueous solution, an initiator aqueous solution accounting for 20-30% of the total mass of the initiator aqueous solution and a nuclear monomer pre-emulsion accounting for 40-50% of the total mass of the nuclear monomer pre-emulsion under the protection of inert gas, heating to 65-75 ℃, and preserving heat for 30-60min after blue light appears in the emulsion to prepare a seed emulsion;
(3) keeping the temperature at 65-75 ℃, dropwise adding the initiator aqueous solution accounting for 20-30% of the total mass of the initiator aqueous solution and the rest nuclear monomer pre-emulsion into the seed emulsion for 1.5-2.5h, heating to 75-85 ℃ after dropwise adding, and keeping the temperature for 1-1.5h to obtain a nuclear layer emulsion;
(4) and dropwise adding the rest initiator aqueous solution and the shell pre-emulsion into the core-shell emulsion for 1.5-2.5h, heating to 85-95 ℃ after dropwise adding, preserving heat for 1-1.5h, cooling, and adjusting the pH value to 8-9 to obtain the molybdenum disulfide and methacrylic acid modified acrylate core-shell emulsion.
Further, the buffer is sodium bicarbonate or sodium dihydrogen phosphate, and the dosage of the buffer is 0.1-0.5% of the sum of the mass of the n-butyl acrylate and the mass of the methyl methacrylate.
Further, the hyperbranched polyphosphoric acid amide charring agent is prepared from the following components in parts by weight: 5-15 parts of phosphoryl dichloride, 2-10 parts of melamine, 10-20 parts of triethylamine and 250 parts of acetonitrile.
Further, the organic modified sepiolite is sepiolite which is sequentially acidified by dilute hydrochloric acid and treated by a silane coupling agent.
Further, the preparation method of the organic modified sepiolite comprises the following steps: mixing sepiolite and 1% diluted hydrochloric acid uniformly, acidifying at constant temperature of 80-85 deg.C for 1-1.5h, drying, grinding, and sieving with 50 mesh sieve to obtain inorganic filler powder; mixing the inorganic filler powder with absolute ethyl alcohol, performing ultrasonic dispersion for 5-10min, and stirring at constant temperature of 50-60 ℃ for 30-45 min; adding a silane coupling agent, wherein the mass ratio of the silane coupling agent to the inorganic filler powder is 0.05-0.2:1, heating to 95-100 ℃, reacting for 2-3h, washing and drying to obtain the organic modified sepiolite.
Further, the preparation method of the phosphate grafted bentonite comprises the following steps: polyethylene glycol borate and pentaerythritol phosphate are mixed according to the mass ratio of 85: 10-15, stirring for 1-1.5h at 50-60 ℃, heating to 120-125 ℃ and reacting for 2-3h to obtain flexible phosphate; mixing bentonite and 50% ethanol water solution according to the mass ratio of 1-5:20, standing for 30-60min, and performing microwave radiation at the power of 2000-; mixing the treated bentonite and the flexible phosphate ester according to the mass ratio of 1-10:100, carrying out ultrasonic dispersion at 60-65 ℃ for 45-60min, and carrying out reaction at 120-125 ℃ for 5-6h to obtain the phosphate ester grafted bentonite.
Further, the dispersing agent is at least one of sodium tripolyphosphate, sodium hexametaphosphate and polyacrylamide.
Further, the defoaming agent is a dipropylene glycol monomethyl ether solution of polyether modified polysiloxane.
The film-forming additive is further characterized in that the film-forming additive is at least one of dodecyl alcohol ester, glycerol and ethylene glycol ethyl ether.
Further, the thickening agent is at least one of hydroxyethyl cellulose, methyl fiber, polyvinylpyrrolidone, polyethylene oxide and sodium polyacrylate.
The invention has the following beneficial effects:
according to the invention, the molybdenum disulfide and methacrylic acid modified acrylate core-shell emulsion are selected as film forming substances, and the molybdenum disulfide is introduced into the acrylic emulsion through core-shell polymerization, so that the molybdenum disulfide can be stably and uniformly dispersed in the coating, the film forming property and the adhesive force of the acrylic emulsion are not influenced, the water absorption of the coating is reduced, the water resistance of the coating is improved, and the cracking of the coating is effectively prevented. The molybdenum disulfide can play the separation and effect when being heated, restrain the combustion reaction and take the effect of forming charcoal when burning, delays the thermal decomposition of polymer, effectively reduces the combustible gas that produces because of polymer decomposition. The molybdenum disulfide and methacrylic acid modified acrylate core-shell emulsion and a carbon source in an expansion system are synergistic, so that the formed carbon is flame-retardant, the carbon content and the compactness of an expanded carbon layer are improved, and the thermal stability, the barrier property and the flame retardant property of the coating are improved.
The hyperbranched polyphosphazene charring agent provided by the invention has a flame retardant effect through the synergy of phosphorus and nitrogen elements, and has the advantages of good thermal stability, high charring rate and large high-temperature carbon residue; the selected organic modified sepiolite can be uniformly and stably dispersed in the coating, so that the strength and the water resistance of the expanded carbon layer are improved; the selected phosphate grafted bentonite can enable the bentonite to be uniformly dispersed in the coating to form a more compact and stable expanded carbon layer, and can effectively improve the thermal stability, flame retardance and smoke suppression performance of the fireproof coating; the selected nano aluminum hydroxide and the selected nano phosphorus borate can absorb a large amount of heat at the initial stage of combustion, reduce the generation of smoke during combustion, and simultaneously ensure that an expanded carbon layer is compact and uniform and is not easy to fall off; the selected nano titanium pyrophosphate and nano potassium hexatitanate are phase-change materials with temperature control performance, have low heat conductivity coefficient and high infrared refractive index, and endow the coating with good flame-retardant, heat-insulation, heat-preservation and temperature-control performances.
The fireproof coating takes phosphorus-containing substances as main flame retardants, at the initial stage of combustion, a solid coating is molten after being heated, an acid source is dehydrated, a carbon source is decomposed into carbon, a gas source is decomposed when a porous carbon layer is cured, gas is released to foam, a compact protective film with good adhesion is formed on the surface of a base material after an expanded carbon layer is cured, the volume of the cured protective film can be increased to 50-100 times that of the coating, pores are compact, and the fireproof coating has high strength and can absorb more non-combustible gas. The formation of the protective film can isolate heat to the maximum extent according to a heat absorption mechanism of phase change solid-liquid-gas-solid, cool and protect the base material, can effectively isolate combustion heat at a high temperature of 800 ℃, insulate heat and preserve heat, delay the temperature rise speed of the base material, avoid the melting of the base material, obstruct flame transfer and effectively reduce the generation of smoke during combustion. The minimum quasi-incombustible performance can be realized by the coating thickness of 200 mu m, namely, less than 8MJ heat release (including a base material) within 10min of combustion, and the experimental result of the mouse toxic gas is more than 9 min.
Detailed Description
The present invention will be described in detail with reference to examples, which are only preferred embodiments of the present invention and are not intended to limit the present invention.
Examples
The following table shows the formulation of 3 examples of the fireproof coating with thermal insulation and heat preservation properties of the present invention (unit:%), and the preparation method is conventional in the art.
Comparative example
The following table shows the formulation (unit:%) of 6 examples of the fireproof coating with thermal insulation and heat preservation properties of the present invention, which is prepared by stirring and grinding the materials conventionally used in the art.
The molybdenum disulfide and methacrylic acid modified acrylate core-shell emulsion is prepared by polymerizing a core monomer mixture and a shell monomer mixture which are used as main raw materials through the core-shell emulsion; the emulsifier is sodium dodecyl benzene sulfate; the nuclear monomer mixture comprises n-butyl acrylate, methyl methacrylate and nano molybdenum disulfide; the shell monomer mixture comprises n-butyl acrylate, methyl methacrylate, methacrylic acid and nano molybdenum disulfide.
Wherein the mass ratio of the core monomer mixture to the shell monomer mixture is 1: 3; the mass ratio of the total mass of the core monomer mixture and the shell monomer mixture to the emulsifier to the nano molybdenum disulfide to the methacrylic acid is 10: 0.5: 0.8: 0.8; the mass ratio of n-butyl acrylate to methyl methacrylate in the nuclear monomer mixture is 2.5: 1; the mass ratio of n-butyl acrylate to methyl methacrylate in the shell monomer mixture is 2.5: 1.
The preparation method of the molybdenum disulfide and methacrylic acid modified acrylate core-shell emulsion comprises the following steps:
(1) dissolving an emulsifier in water to prepare an emulsifier aqueous solution, and averagely dividing the emulsifier aqueous solution into three parts for later use; respectively dripping the core monomer mixture and the shell monomer mixture into one part of the emulsifier aqueous solution, stirring and pre-emulsifying for 1h to respectively prepare a core monomer pre-emulsion and a shell monomer pre-emulsion; adding sodium bicarbonate with the mass of 0.1-0.5% of the sum of the mass of the n-butyl acrylate and the mass of the methyl methacrylate into the rest part of the emulsifier aqueous solution to prepare a sodium bicarbonate aqueous solution; dissolving an initiator in water to prepare an initiator aqueous solution;
(2) mixing and stirring a sodium bicarbonate aqueous solution, an initiator aqueous solution accounting for 25% of the total mass of the initiator aqueous solution and a nuclear monomer pre-emulsion accounting for 45% of the total mass of the nuclear monomer pre-emulsion under the protection of inert gas, heating to 70 ℃, and preserving heat for 45min after blue light appears in the emulsion to prepare a seed emulsion;
(3) keeping the temperature at 70 ℃, dropwise adding an initiator aqueous solution accounting for 25% of the total mass of the initiator aqueous solution and the rest nuclear monomer pre-emulsion into the seed emulsion for 1h, heating to 80 ℃ after dropwise adding, and preserving the heat for 1h to obtain a nuclear layer emulsion;
(4) and (3) dropwise adding the rest initiator aqueous solution and the shell pre-emulsion into the core-shell emulsion for 2h, heating to 90 ℃ after dropwise adding, preserving heat for 1h, cooling, and adjusting the pH value to 8 to obtain the molybdenum disulfide and methacrylic acid modified acrylate core-shell emulsion.
The hyperbranched polyammonium phosphate char forming agent is prepared from the following components in parts by weight: 5-15 parts of phosphoryl dichloride, 2-10 parts of melamine, 10-20 parts of triethylamine and 250 parts of acetonitrile.
The preparation method of the organic modified sepiolite comprises the following steps: mixing sepiolite and 1% diluted hydrochloric acid uniformly, acidifying at constant temperature of 80-85 deg.C for 1-1.5h, drying, grinding, and sieving with 50 mesh sieve to obtain inorganic filler powder; mixing the inorganic filler powder with absolute ethyl alcohol, performing ultrasonic dispersion for 5-10min, and stirring at constant temperature of 50-60 ℃ for 30-45 min; adding a silane coupling agent, wherein the mass ratio of the silane coupling agent to the inorganic filler powder is 0.05-0.2:1, heating to 95-100 ℃, reacting for 2-3h, washing and drying to obtain the organic modified sepiolite.
The preparation method of the phosphate grafted bentonite comprises the following steps: polyethylene glycol borate and pentaerythritol phosphate are mixed according to the mass ratio of 85: 10-15, stirring for 1-1.5h at 50-60 ℃, heating to 120-125 ℃ and reacting for 2-3h to obtain flexible phosphate; mixing bentonite and 50% ethanol water solution according to the mass ratio of 1-5:20, standing for 30-60min, and performing microwave radiation at the power of 2000-; mixing the treated bentonite and the flexible phosphate ester according to the mass ratio of 1-10:100, carrying out ultrasonic dispersion at 60-65 ℃ for 45-60min, and carrying out reaction at 120-125 ℃ for 5-6h to obtain the phosphate ester grafted bentonite.
The fire-retardant coating with thermal insulation performance of the invention was tested according to the national standard GB12441-2005 for 3 examples and 6 comparative examples, and the test results are shown in tables 1-2.
Table 1:
table 2:
therefore, the fireproof coating has the advantages of good thermal stability, good flame retardant property, small smoke generation amount and good heat insulation performance.
The fireproof coating has the advantages of fast curing, good film forming property, high coating hardness and strong adhesive force; the coating has good fireproof and flame-retardant properties, and can form a uniform and compact expansion layer on the surface of the base material after being heated, thereby effectively isolating combustion heat, avoiding melting of the base material and blocking flame transfer.
Claims (10)
1. The fireproof coating with heat insulation and preservation performances is characterized by comprising the following components in percentage by mass: 25-35% of molybdenum disulfide and methacrylic acid modified acrylate core-shell emulsion, 15-20% of hyperbranched poly-ammonium phosphate charring agent, 10-15% of melamine, 8-12% of pentaerythritol, 3-5% of nano titanium dioxide, 1-5% of nano titanium pyrophosphate, 2-3% of nano potassium hexatitanate, 5-10% of nano aluminum hydroxide, 2-5% of zinc borate, 1-3% of organic modified sepiolite, 1-3% of phosphate grafted bentonite, 0.5-1% of dispersing agent, 0.5-1% of defoaming agent, 0.5-1% of film forming additive, 0.5-1% of thickening agent and the balance of water.
2. The fireproof coating with heat insulation and preservation performances according to claim 1, wherein the molybdenum disulfide and methacrylic acid modified acrylate core-shell emulsion is polymerized by using an emulsifier, a core monomer mixture and a shell monomer mixture as main raw materials; the emulsifier is sodium dodecyl benzene sulfate, sodium dodecyl sulfate or polyethylene glycol octyl phenyl ether; the nuclear monomer mixture comprises n-butyl acrylate, methyl methacrylate and nano molybdenum disulfide; the shell monomer mixture comprises n-butyl acrylate, methyl methacrylate, methacrylic acid and nano molybdenum disulfide.
3. The fireproof coating with heat insulation and preservation performances according to claim 2, wherein the mass ratio of the core monomer mixture to the shell monomer mixture is 1-2: 2-3; the mass ratio of the total mass of the core monomer mixture and the shell monomer mixture to the emulsifier to the nano molybdenum disulfide to the methacrylic acid is 10: 0.1-1: 0.5-1: 0.1 to 1; the mass ratio of n-butyl acrylate to methyl methacrylate in the nuclear monomer mixture is 2-3: 1; the mass ratio of n-butyl acrylate to methyl methacrylate in the shell monomer mixture is 1-3: 1.
4. The fireproof coating with heat insulation and preservation properties according to claim 1, wherein the hyperbranched polyphosphazene charring agent is prepared from the following components in parts by weight: 5-15 parts of phosphoryl dichloride, 2-10 parts of melamine, 10-20 parts of triethylamine and 250 parts of acetonitrile.
5. The fireproof coating with heat insulation and preservation properties according to claim 1, wherein the organic modified sepiolite is sepiolite treated by dilute hydrochloric acid acidification and silane coupling agent treatment in sequence.
6. The fireproof coating with heat insulation and preservation performance of claim 1, wherein the preparation method of the phosphate grafted bentonite comprises the following steps: polyethylene glycol borate and pentaerythritol phosphate are mixed according to the mass ratio of 85: 10-15, stirring for 1-1.5h at 50-60 ℃, heating to 120-125 ℃ and reacting for 2-3h to obtain flexible phosphate; mixing bentonite and 50% ethanol water solution according to the mass ratio of 1-5:20, standing for 30-60min, and performing microwave radiation at the power of 2000-; mixing the treated bentonite and the flexible phosphate ester according to the mass ratio of 1-10:100, carrying out ultrasonic dispersion at 60-65 ℃ for 45-60min, and carrying out reaction at 120-125 ℃ for 5-6h to obtain the phosphate ester grafted bentonite.
7. The fireproof coating with heat insulation and preservation properties according to claim 1, wherein the dispersant is at least one of sodium tripolyphosphate, sodium hexametaphosphate, and polyacrylamide.
8. The fireproof paint with heat insulation and preservation properties according to claim 1, wherein the defoaming agent is a dipropylene glycol monomethyl ether solution of polyether modified polysiloxane.
9. The fireproof coating with heat insulation and preservation properties according to claim 1, wherein the film forming aid is at least one of dodecyl alcohol ester, glycerol and ethylene glycol ethyl ether.
10. The fireproof paint with heat insulation and preservation properties according to claim 1, wherein the thickener is at least one of hydroxyethyl cellulose, methyl fiber, polyvinylpyrrolidone, polyethylene oxide, and sodium polyacrylate.
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