CN112574632A - Environment-friendly fireproof coating and preparation method thereof - Google Patents
Environment-friendly fireproof coating and preparation method thereof Download PDFInfo
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- CN112574632A CN112574632A CN202011359207.XA CN202011359207A CN112574632A CN 112574632 A CN112574632 A CN 112574632A CN 202011359207 A CN202011359207 A CN 202011359207A CN 112574632 A CN112574632 A CN 112574632A
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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
- 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
- C09D133/18—Homopolymers or copolymers of nitriles
- C09D133/20—Homopolymers or copolymers of acrylonitrile
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- 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
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- 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
- C09D7/62—Additives non-macromolecular inorganic modified by treatment with other compounds
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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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- C09D7/65—Additives macromolecular
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- 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
- C08K3/02—Elements
- C08K2003/026—Phosphorus
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
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- C08L2201/02—Flame or fire retardant/resistant
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- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
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- C08L2205/00—Polymer mixtures characterised by other features
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Abstract
The invention discloses an environment-friendly fireproof coating which is characterized by being prepared from the following components in parts by weight: based on 30-60 parts of crown ether flame-retardant film-forming substance, 10-20 parts of hyperbranched polyurethane containing epoxy groups, 5-8 parts of diethyl phosphoryl ethyl triethoxysilane modified black phosphorus/rare earth oxide nanoparticle compound, 2-4 parts of polyacrylic acid, 15-25 parts of filler, 0.5-1.5 parts of flatting agent and 1-3 parts of dispersing agent; the crown ether-based flame-retardant film-forming substance is prepared by free radical polymerization of 4-acyl-18-crown ether, (2Z) -4-oxo-4- [3- (trifluoromethyl) -5, 6-dihydro- [1,2,4] triazolo [4,3-a ] pyrazin-7 (8H) -yl ] -1- (2,4, 5-trifluorophenyl) but-2-ene-2-amine, allyl triphenyl phosphonium bromide, N-trihydroxymethyl acrylamide, phenyl vinyl sulfone and acrylonitrile. The invention also discloses a preparation method of the environment-friendly fireproof coating. The environment-friendly fireproof coating disclosed by the invention is good in comprehensive performance, good in environment-friendly performance, fireproof and flame-retardant performance, excellent in water resistance and performance stability and strong in adhesive force with a base material.
Description
Technical Field
The invention relates to the technical field of building materials, in particular to an environment-friendly fireproof coating and a preparation method thereof.
Background
In recent years, with the rapid development of economy and the continuous improvement of living standard of substances, people have increasingly deep understanding on the importance of mental civilization construction, and the desires of improving the home environment, improving the comfort and the visual aesthetic feeling are more and more urgent, and the performance requirements on home decoration materials are also higher and higher. Under the situation, the coating is taken as a functional coating of common home decoration materials, becomes a new favorite of the current coating market, and has a very large market demand.
The fireproof coating is a functional coating for buildings, which has the advantages of widest application, strongest adaptability and most convenient construction in modern engineering, has a decorative function, more importantly, has a fireproof and flame-retardant function, and plays a great role in ensuring the safety of buildings. The fire-retardant coating in the prior art is usually prepared by adding a large amount of flame retardants containing halogen, nitrogen, phosphorus and the like into a formula of a common coating to realize a fire-retardant effect, the fire-retardant coating inevitably reduces the comprehensive performance of the coating along with the addition of a large amount of flame retardants, and the added flame retardants have unsatisfactory flame-retardant effect or generate toxic irritant gases during combustion and are easy to generate secondary pollution as wastes to hinder fire fighting and personnel evacuation and corrode instruments and equipment. In addition, the fireproof coating on the market at present has the defects of poor water resistance, poor storage stability, short fire-resistant time, long drying time, poor decoration and the like.
The Chinese patent with the application number of 201510555268.6 discloses a fireproof coating, which comprises the following components in parts by weight: 30-50 parts of anhydrous calcium chloride, 450 parts of flame retardant 400-containing materials, 50-70 parts of chlorinated paraffin, 30-50 parts of stone powder, 8-12 parts of magnesium powder, 15-30 parts of composite zinc phosphate, 8-10 parts of titanium dioxide, 10-20 parts of mica powder, 15-25 parts of thickening agent, 200 parts of film-forming agent 150-containing materials and 250 parts of deionized water 150-containing materials. The coating has the characteristics of long fire-resistant time, good decorative performance, good cohesiveness, excellent water resistance and the like, and an independent raw material selection method is adopted, so that the coating does not contain APEO, does not contain metal compounds such as lead or chromium and the like, and does not cause harm to the environment and human health. However, the chlorinated paraffin added in the paint contains halogen, toxic irritant gas is generated during combustion, the environment friendliness is poor, the paint contains a plurality of components, and the compatibility and the performance stability among the components need to be further improved; deionized water is used as a dispersion system, and the drying time is long.
Therefore, the environment-friendly fireproof coating which has the advantages of good comprehensive performance, good environment-friendly performance, good fireproof flame-retardant performance, excellent weather resistance, water resistance, decoration performance and performance stability, short drying time and strong adhesive force with the base material is developed, meets the market demand, has wide market value and application prospect, and has very important significance for promoting the development of the functional coating industry.
Disclosure of Invention
In order to overcome the defects in the prior art, the invention provides an environment-friendly fireproof coating which is characterized by being prepared from the following components in parts by weight: based on 30-60 parts of crown ether flame-retardant film-forming substance, 10-20 parts of hyperbranched polyurethane containing epoxy groups, 5-8 parts of diethyl phosphoryl ethyl triethoxysilane modified black phosphorus/rare earth oxide nanoparticle compound, 2-4 parts of polyacrylic acid, 15-25 parts of filler, 0.5-1.5 parts of flatting agent and 1-3 parts of dispersing agent; the crown ether-based flame-retardant film-forming substance is prepared by free radical polymerization of 4-acyl-18-crown ether, (2Z) -4-oxo-4- [3- (trifluoromethyl) -5, 6-dihydro- [1,2,4] triazolo [4,3-a ] pyrazin-7 (8H) -yl ] -1- (2,4, 5-trifluorophenyl) but-2-ene-2-amine, allyl triphenyl phosphonium bromide, N-trihydroxymethyl acrylamide, phenyl vinyl sulfone and acrylonitrile.
Preferably, the preparation method of the crown ether flame-retardant-based film-forming substance comprises the following steps: adding 4-acyl-18-crown ether, (2Z) -4-oxo-4- [3- (trifluoromethyl) -5, 6-dihydro- [1,2,4] triazolo [4,3-a ] pyrazin-7 (8H) -yl ] -1- (2,4, 5-trifluorophenyl) but-2-ene-2-amine, allyl triphenyl phosphine bromide, N-trimethylol methacrylamide, phenyl vinyl sulfone, acrylonitrile and an initiator into a high boiling point solvent, stirring for reaction for 3-5 hours at 65-75 ℃ under an inert gas atmosphere, cooling to room temperature after the reaction is finished, precipitating in water, washing the precipitated polymer for 3-7 times by using ethanol, finally drying at 85-95 ℃ in a vacuum drying oven to constant weight, obtaining the crown ether flame-retardant film-forming substance.
Preferably, the mass ratio of the 4-acyl-18-crown ether, (2Z) -4-oxo-4- [3- (trifluoromethyl) -5, 6-dihydro- [1,2,4] triazolo [4,3-a ] pyrazin-7 (8H) -yl ] -1- (2,4, 5-trifluorophenyl) but-2-en-2-amine, allyl triphenyl phosphine bromide, N-trimethylol methacrylamide, phenyl vinyl sulfone, acrylonitrile, initiator and high boiling point solvent is 0.3:0.6:1 (2-3):0.3 (1-2): 0.05-0.07: 20-30.
Preferably, the initiator is at least one of azobisisobutyronitrile and azobisisoheptonitrile.
Preferably, the high boiling point solvent is at least one of dimethyl sulfoxide, N-dimethylformamide, N-dimethylacetamide and N-methylpyrrolidone.
Preferably, the inert gas is any one of nitrogen, helium, neon and argon.
Preferably, the preparation method of the hyperbranched polyurethane containing epoxy groups is described in the first embodiment of the chinese patent with application No. 201510556363.8.
Preferably, the preparation method of the diethylphosphorylethyltriethoxysilane-modified black phosphorus/rare earth oxide nanoparticle composite comprises the following steps: dispersing the black phosphorus and rare earth oxide nanoparticles in ethanol, adding diethylphosphorylethyltriethoxysilane, stirring at 50-70 ℃ for reaction for 4-6 hours, and then performing rotary evaporation to remove ethanol to obtain the diethylphosphorylethyltriethoxysilane modified black phosphorus/rare earth oxide nanoparticle composite.
Preferably, the mass ratio of the black phosphorus to the rare earth oxide nanoparticles to the ethanol to the diethylphosphorylethyltriethoxysilane is 3 (1-2) to (15-25) to (0.3-0.5).
Preferably, the particle size of the black phosphorus is 800-1200 meshes.
Preferably, the preparation method of the rare earth oxide nanoparticles is described in Chinese patent application No. 201610381018.X, example 1.
Preferably, the polyacrylic acid has a weight average molecular weight of 2 to 5 ten thousand.
Preferably, the filler is at least one of titanium dioxide, calcium hydrogen phosphate and talcum powder.
Preferably, the particle size of the filler is 1000-1300 meshes.
Preferably, the leveling agent is one or more of a polyacrylate leveling agent, a cellulose acetate butyrate leveling agent and a polyvinyl butyral leveling agent.
Preferably, the dispersant is sodium hexametaphosphate and/or sodium polycarboxylate.
The invention also aims to provide a preparation method of the environment-friendly fireproof coating, which is characterized by comprising the following steps of: uniformly mixing the components in parts by weight, performing melt extrusion through a screw extruder, tabletting the molten material through a tabletting machine, controlling the thickness to be 2-5mm, cooling, crushing, feeding into a grinding machine, crushing and grading, separating fine powder, impurities and the like through a cyclone separator, separating a product through a powder sieve, wherein the powder sieve is 200 meshes and 300 meshes, and curing for 1-3 days to obtain the finished product of the environment-friendly fireproof coating.
Preferably, the melt extrusion temperature is 110-.
Adopt the produced beneficial effect of above-mentioned technical scheme to lie in:
(1) the preparation method of the environment-friendly fireproof coating provided by the invention is simple and easy to implement, wide in raw material source, low in requirements on equipment and reaction conditions, convenient to construct, high in production efficiency and finished product qualification rate, suitable for continuous large-scale production, and high in economic value, social value and ecological value.
(2) The environment-friendly fireproof coating provided by the invention overcomes the defects that the fireproof coating in the prior art inevitably reduces the comprehensive performance of the coating along with the addition of a large amount of flame retardant, and the added flame retardants have unsatisfactory flame retardant effect, or generate toxic irritant gases during combustion and are easy to generate secondary pollution as wastes, thus preventing fire fighting and personnel evacuation, simultaneously corrodes instruments and equipment, also overcomes the technical problems of poor water resistance, poor storage stability, short fire-resistant time, long drying time, poor decoration and the like of the fireproof coating in the current market, through the synergistic effect of the components, the prepared environment-friendly fireproof coating has the advantages of good comprehensive performance, good environment-friendly performance, good fireproof flame-retardant performance, excellent weather resistance, water resistance, decoration performance and performance stability, short drying time and strong adhesive force with a base material.
(3) The environment-friendly fireproof coating provided by the invention adopts a crown ether flame-retardant film-forming substance, and is prepared by free radical polymerization of 4-acyl-18-crown ether, (2Z) -4-oxo-4- [3- (trifluoromethyl) -5, 6-dihydro- [1,2,4] triazolo [4,3-a ] pyrazine-7 (8H) -yl ] -1- (2,4, 5-trifluorophenyl) butyl-2-ene-2-amine, allyl triphenyl phosphonium bromide, N-trihydroxymethyl acrylamide, phenyl vinyl sulfone and acrylonitrile; under the multiple actions of electronic effect, steric effect, conjugate effect and the like among all the comonomers, the prepared coating has good comprehensive performance, excellent weather resistance, good water resistance and performance stability and strong film forming capability, and a crown ether structure is introduced into a molecular chain of the coating, so that the flame-retardant and fireproof performance is effectively improved due to the synergistic effect of the unique hole structure and the phenylamide structure.
(4) According to the environment-friendly fireproof coating provided by the invention, the addition of the diethylphosphorylethyltriethoxysilane modified black phosphorus/rare earth oxide nanoparticle compound combines the excellent performances of the black phosphorus and the rare earth oxide nanoparticles, so that the prepared compound has better flame retardant and fireproof performances, and the diethylphosphorylethyltriethoxysilane is modified to improve the compatibility between the compound and a film-forming substance and improve the dispersion uniformity of the compound. The diethylphosphoryl on the diethylphosphorylethyltriethoxysilane introduced on the surface of the film-forming material and hydroxyl on the molecular chain of the film-forming material are subjected to ester exchange reaction under the catalytic action of amino on the film-forming material and triphenylphosphine bromide, so that the film-forming material and the film-forming material form an organic whole, and the comprehensive performance is improved.
(5) According to the environment-friendly fireproof coating provided by the invention, the phosphine bromide cationic group on the molecular chain of the film-forming substance is easily connected with the polyacrylic acid anionic group through ion exchange in an ionic bond manner, and the epoxy group on the epoxy group-containing hyperbranched polyurethane and the amino group on the molecular chain of the film-forming substance are connected through an open-loop reaction to form a three-dimensional network structure, so that the comprehensive performance of a coating film is effectively improved. The introduction of structures such as hyperbranched polyurethane, polyacrylic acid and the like can improve the compatibility among all components, so that the components form a uniform system and the performance stability is improved. The coating takes air as a dispersion medium, does not add water or organic solvent, and has better environmental protection property and faster drying speed.
Detailed Description
In order to make the technical solutions of the present invention better understood and make the above features, objects, and advantages of the present invention more comprehensible, the present invention is further described with reference to the following examples. The examples are intended to illustrate the invention only and are not intended to limit the scope of the invention; the preparation method of the hyperbranched polyurethane containing epoxy groups in the embodiment of the invention is disclosed in the first embodiment of Chinese patent application No. 201510556363.8; the preparation method of the rare earth oxide nanoparticles is disclosed in Chinese patent application example 1 with the application number of 201610381018. X; other raw materials were all purchased commercially.
Example 1
The environment-friendly fireproof coating is characterized by being prepared from the following components in parts by weight: based on 30 parts of crown ether flame-retardant film-forming substance, 10 parts of hyperbranched polyurethane containing epoxy groups, 5 parts of diethyl phosphoryl ethyl triethoxysilane modified black phosphorus/rare earth oxide nanoparticle compound, 2 parts of polyacrylic acid, 15 parts of filler, 0.5 part of flatting agent and 1 part of dispersing agent; the crown ether-based flame-retardant film-forming substance is prepared by free radical polymerization of 4-acyl-18-crown ether, (2Z) -4-oxo-4- [3- (trifluoromethyl) -5, 6-dihydro- [1,2,4] triazolo [4,3-a ] pyrazin-7 (8H) -yl ] -1- (2,4, 5-trifluorophenyl) but-2-ene-2-amine, allyl triphenyl phosphonium bromide, N-trihydroxymethyl acrylamide, phenyl vinyl sulfone and acrylonitrile.
The preparation method of the crown ether-based flame-retardant film-forming substance comprises the following steps: adding 4-acyl-18-crown ether, (2Z) -4-oxo-4- [3- (trifluoromethyl) -5, 6-dihydro- [1,2,4] triazolo [4,3-a ] pyrazin-7 (8H) -yl ] -1- (2,4, 5-trifluorophenyl) but-2-ene-2-amine, allyl triphenyl phosphine bromide, N-trihydroxymethyl acrylamide, phenyl vinyl sulfone, acrylonitrile and an initiator into a high boiling point solvent, stirring and reacting for 3 hours at 65 ℃ in an inert gas atmosphere, cooling to room temperature after the reaction is finished, precipitating in water, washing the precipitated polymer with ethanol for 3 times, and drying in a vacuum drying oven at 85 deg.C to constant weight to obtain crown ether-based flame-retardant film-forming substance.
The mass ratio of the 4-acyl-18-crown ether, (2Z) -4-oxo-4- [3- (trifluoromethyl) -5, 6-dihydro- [1,2,4] triazolo [4,3-a ] pyrazin-7 (8H) -yl ] -1- (2,4, 5-trifluorophenyl) but-2-ene-2-amine, allyl triphenyl phosphine bromide, N-trimethylol methacrylamide, phenyl vinyl sulfone, acrylonitrile, an initiator and a high boiling point solvent is 0.3:0.6:1:2:0.3:1:0.05: 20; the initiator is azobisisobutyronitrile; the high boiling point solvent is dimethyl sulfoxide; the inert gas is nitrogen.
The preparation method of the diethyl phosphoryl ethyl triethoxysilane modified black phosphorus/rare earth oxide nanoparticle compound comprises the following steps: dispersing black phosphorus and rare earth oxide nanoparticles into ethanol, adding diethylphosphorylethyltriethoxysilane into the ethanol, stirring the mixture at 50 ℃ for reaction for 4 hours, and then performing rotary evaporation to remove ethanol to obtain the diethylphosphorylethyltriethoxysilane modified black phosphorus/rare earth oxide nanoparticle composite.
The mass ratio of the black phosphorus to the rare earth oxide nanoparticles to the ethyl alcohol to the diethyl phosphoryl ethyl triethoxysilane is 3:1:15: 0.3; the particle size of the black phosphorus is 800 meshes.
The weight average molecular weight of the polyacrylic acid is 2 ten thousand; the filler is titanium dioxide; the particle size of the filler is 1000 meshes; the flatting agent is a polyacrylate flatting agent; the dispersant is sodium hexametaphosphate.
The preparation method of the environment-friendly fireproof coating is characterized by comprising the following steps: uniformly mixing the components in parts by weight, performing melt extrusion through a screw extruder, tabletting the molten material through a tabletting machine, controlling the thickness to be 2mm, cooling, crushing, feeding into a grinding machine, crushing and grading, separating fine powder, impurities and the like through a cyclone separator, separating a product through a powder sieve, sieving the powder with a 200-mesh sieve, and curing for 1 day to obtain a finished product of the environment-friendly fireproof coating; the melt extrusion temperature was 110 ℃.
Example 2
The environment-friendly fireproof coating is characterized by being prepared from the following components in parts by weight: based on 40 parts of crown ether flame-retardant film-forming substance, 13 parts of hyperbranched polyurethane containing epoxy groups, 6 parts of diethyl phosphoryl ethyl triethoxysilane modified black phosphorus/rare earth oxide nanoparticle compound, 2.5 parts of polyacrylic acid, 17 parts of filler, 0.7 part of flatting agent and 1.5 parts of dispersing agent; the crown ether-based flame-retardant film-forming substance is prepared by free radical polymerization of 4-acyl-18-crown ether, (2Z) -4-oxo-4- [3- (trifluoromethyl) -5, 6-dihydro- [1,2,4] triazolo [4,3-a ] pyrazin-7 (8H) -yl ] -1- (2,4, 5-trifluorophenyl) but-2-ene-2-amine, allyl triphenyl phosphonium bromide, N-trihydroxymethyl acrylamide, phenyl vinyl sulfone and acrylonitrile.
The preparation method of the crown ether-based flame-retardant film-forming substance comprises the following steps: adding 4-acyl-18-crown ether, (2Z) -4-oxo-4- [3- (trifluoromethyl) -5, 6-dihydro- [1,2,4] triazolo [4,3-a ] pyrazin-7 (8H) -yl ] -1- (2,4, 5-trifluorophenyl) but-2-ene-2-amine, allyl triphenyl phosphine bromide, N-trihydroxymethyl acrylamide, phenyl vinyl sulfone, acrylonitrile and an initiator into a high boiling point solvent, stirring and reacting for 3.5 hours at 67 ℃ in an inert gas atmosphere, cooling to room temperature after the reaction is finished, precipitating in water, washing the precipitated polymer with ethanol for 4 times, and finally drying in a vacuum drying oven at 87 ℃ to constant weight to obtain the crown ether flame-retardant-based film-forming substance.
The mass ratio of the 4-acyl-18-crown ether, (2Z) -4-oxo-4- [3- (trifluoromethyl) -5, 6-dihydro- [1,2,4] triazolo [4,3-a ] pyrazin-7 (8H) -yl ] -1- (2,4, 5-trifluorophenyl) but-2-ene-2-amine, allyl triphenyl phosphine bromide, N-trimethylol methacrylamide, phenyl vinyl sulfone, acrylonitrile, an initiator and a high boiling point solvent is 0.3:0.6:1:2.3:0.3:1.2:0.055: 23.
The initiator is azobisisoheptonitrile; the high boiling point solvent is N, N-dimethylformamide; the inert gas is helium.
The preparation method of the diethyl phosphoryl ethyl triethoxysilane modified black phosphorus/rare earth oxide nanoparticle compound comprises the following steps: dispersing black phosphorus and rare earth oxide nanoparticles into ethanol, adding diethylphosphorylethyltriethoxysilane into the ethanol, stirring the mixture at 55 ℃ for reaction for 4.5 hours, and then performing rotary evaporation to remove ethanol to obtain a diethylphosphorylethyltriethoxysilane modified black phosphorus/rare earth oxide nanoparticle compound; the mass ratio of the black phosphorus to the rare earth oxide nanoparticles to the ethyl alcohol to the diethyl phosphoryl ethyl triethoxysilane is 3:1.3:18: 0.35; the particle size of the black phosphorus is 900 meshes.
The weight average molecular weight of the polyacrylic acid is 3 ten thousand; the filler is double flying powder; the particle size of the filler is 1100 meshes; the leveling agent is cellulose acetate butyrate leveling agent; the dispersant is a sodium polycarboxylate salt.
The preparation method of the environment-friendly fireproof coating is characterized by comprising the following steps: uniformly mixing the components in parts by weight, performing melt extrusion through a screw extruder, tabletting the molten material through a tabletting machine, controlling the thickness to be 3mm, cooling, crushing, feeding into a grinding machine, crushing and grading, separating fine powder, impurities and the like through a cyclone separator, separating a product through a powder sieve, wherein the powder sieve is 220 meshes, and curing for 1.5 days to obtain a finished product of the environment-friendly fireproof coating; the melt extrusion temperature was 115 ℃.
Example 3
The environment-friendly fireproof coating is characterized by being prepared from the following components in parts by weight: based on 45 parts of crown ether flame-retardant film-forming substance, 15 parts of hyperbranched polyurethane containing epoxy groups, 6.5 parts of diethyl phosphoryl ethyl triethoxysilane modified black phosphorus/rare earth oxide nanoparticle compound, 3 parts of polyacrylic acid, 20 parts of filler, 1 part of leveling agent and 2 parts of dispersing agent; the crown ether-based flame-retardant film-forming substance is prepared by free radical polymerization of 4-acyl-18-crown ether, (2Z) -4-oxo-4- [3- (trifluoromethyl) -5, 6-dihydro- [1,2,4] triazolo [4,3-a ] pyrazin-7 (8H) -yl ] -1- (2,4, 5-trifluorophenyl) but-2-ene-2-amine, allyl triphenyl phosphonium bromide, N-trihydroxymethyl acrylamide, phenyl vinyl sulfone and acrylonitrile.
The preparation method of the crown ether-based flame-retardant film-forming substance comprises the following steps: adding 4-acyl-18-crown ether, (2Z) -4-oxo-4- [3- (trifluoromethyl) -5, 6-dihydro- [1,2,4] triazolo [4,3-a ] pyrazin-7 (8H) -yl ] -1- (2,4, 5-trifluorophenyl) but-2-ene-2-amine, allyl triphenyl phosphine bromide, N-trihydroxymethyl acrylamide, phenyl vinyl sulfone, acrylonitrile and an initiator into a high boiling point solvent, stirring and reacting for 4 hours at 70 ℃ in an inert gas atmosphere, cooling to room temperature after the reaction is finished, precipitating in water, washing the precipitated polymer with ethanol for 5 times, and drying in a vacuum drying oven at 90 deg.C to constant weight to obtain crown ether-based flame-retardant film-forming substance.
The mass ratio of the 4-acyl-18-crown ether, (2Z) -4-oxo-4- [3- (trifluoromethyl) -5, 6-dihydro- [1,2,4] triazolo [4,3-a ] pyrazin-7 (8H) -yl ] -1- (2,4, 5-trifluorophenyl) but-2-ene-2-amine, allyl triphenyl phosphine bromide, N-trimethylol methacrylamide, phenyl vinyl sulfone, acrylonitrile, an initiator and a high boiling point solvent is 0.3:0.6:1:2.5:0.3:1.5:0.06: 25; the initiator is azobisisobutyronitrile; the high boiling point solvent is N, N-dimethylacetamide; the inert gas is neon.
The preparation method of the diethyl phosphoryl ethyl triethoxysilane modified black phosphorus/rare earth oxide nanoparticle compound comprises the following steps: dispersing black phosphorus and rare earth oxide nanoparticles into ethanol, adding diethylphosphorylethyltriethoxysilane, stirring at 60 ℃ for 5 hours, and then performing rotary evaporation to remove ethanol to obtain the diethylphosphorylethyltriethoxysilane modified black phosphorus/rare earth oxide nanoparticle composite.
The mass ratio of the black phosphorus to the rare earth oxide nanoparticles to the ethyl alcohol to the diethyl phosphoryl ethyl triethoxysilane is 3:1.5:20: 0.4; the particle size of the black phosphorus is 1000 meshes; the weight average molecular weight of the polyacrylic acid was 3.5 ten thousand.
The filler is talcum powder; the particle size of the filler is 1150 meshes; the flatting agent is a polyvinyl butyral flatting agent; the dispersant is sodium hexametaphosphate.
The preparation method of the environment-friendly fireproof coating is characterized by comprising the following steps: uniformly mixing the components in parts by weight, performing melt extrusion through a screw extruder, tabletting the molten material through a tabletting machine, controlling the thickness to be 3.5mm, cooling, crushing, feeding into a grinding machine, crushing and grading, separating fine powder, impurities and the like through a cyclone separator, screening out a product through a powder screen, wherein the powder screen is 250 meshes, and curing for 2 days to obtain a finished product of the environment-friendly fireproof coating; the melt extrusion temperature was 120 ℃.
Example 4
The environment-friendly fireproof coating is characterized by being prepared from the following components in parts by weight: 55 parts of crown ether flame-retardant film-forming substance, 18 parts of hyperbranched polyurethane containing epoxy groups, 7 parts of diethyl phosphoryl ethyl triethoxysilane modified black phosphorus/rare earth oxide nanoparticle compound, 3.5 parts of polyacrylic acid, 23 parts of filler, 1.3 parts of flatting agent and 2.5 parts of dispersing agent; the crown ether-based flame-retardant film-forming substance is prepared by free radical polymerization of 4-acyl-18-crown ether, (2Z) -4-oxo-4- [3- (trifluoromethyl) -5, 6-dihydro- [1,2,4] triazolo [4,3-a ] pyrazin-7 (8H) -yl ] -1- (2,4, 5-trifluorophenyl) but-2-ene-2-amine, allyl triphenyl phosphonium bromide, N-trihydroxymethyl acrylamide, phenyl vinyl sulfone and acrylonitrile.
The preparation method of the crown ether-based flame-retardant film-forming substance comprises the following steps: adding 4-acyl-18-crown ether, (2Z) -4-oxo-4- [3- (trifluoromethyl) -5, 6-dihydro- [1,2,4] triazolo [4,3-a ] pyrazin-7 (8H) -yl ] -1- (2,4, 5-trifluorophenyl) but-2-ene-2-amine, allyl triphenyl phosphine bromide, N-trihydroxymethyl acrylamide, phenyl vinyl sulfone, acrylonitrile and an initiator into a high boiling point solvent, stirring and reacting for 4.5 hours at 73 ℃ in an inert gas atmosphere, cooling to room temperature after the reaction is finished, precipitating in water, washing the precipitated polymer with ethanol for 6 times, and finally drying in a vacuum drying oven at 93 ℃ to constant weight to obtain the crown ether flame-retardant-based film-forming substance.
The mass ratio of the 4-acyl-18-crown ether, (2Z) -4-oxo-4- [3- (trifluoromethyl) -5, 6-dihydro- [1,2,4] triazolo [4,3-a ] pyrazin-7 (8H) -yl ] -1- (2,4, 5-trifluorophenyl) but-2-ene-2-amine, allyl triphenyl phosphine bromide, N-trimethylol methacrylamide, phenyl vinyl sulfone, acrylonitrile, an initiator and a high boiling point solvent is 0.3:0.6:1:2.8:0.3:1.8:0.065: 28; the initiator is formed by mixing azodiisobutyronitrile and azodiisoheptonitrile according to the mass ratio of 3: 5; the high-boiling-point solvent is formed by mixing dimethyl sulfoxide, N-dimethylformamide, N-dimethylacetamide and N-methylpyrrolidone according to a mass ratio of 1:2:3: 2; the inert gas is argon.
The preparation method of the diethyl phosphoryl ethyl triethoxysilane modified black phosphorus/rare earth oxide nanoparticle compound comprises the following steps: dispersing black phosphorus and rare earth oxide nanoparticles into ethanol, adding diethylphosphorylethyltriethoxysilane into the ethanol, stirring the mixture at 68 ℃ for reaction for 5.8 hours, and then performing rotary evaporation to remove ethanol to obtain a diethylphosphorylethyltriethoxysilane modified black phosphorus/rare earth oxide nanoparticle compound; the mass ratio of the black phosphorus to the rare earth oxide nanoparticles to the ethyl alcohol to the diethyl phosphoryl ethyl triethoxysilane is 3:1.8:23: 0.45.
The particle size of the black phosphorus is 1150 meshes; the weight average molecular weight of the polyacrylic acid is 4.5 ten thousand; the filler is formed by mixing titanium dioxide, calcium carbonate and talcum powder according to the mass ratio of 1:3: 2; the grain size of the filler is 1250 meshes; the flatting agent is formed by mixing a polyacrylate flatting agent, a cellulose acetate butyrate flatting agent and a polyvinyl butyral flatting agent according to a mass ratio of 1:3: 2; the dispersing agent is formed by mixing sodium hexametaphosphate and sodium polycarboxylate according to the mass ratio of 3: 5.
The preparation method of the environment-friendly fireproof coating is characterized by comprising the following steps: uniformly mixing the components in parts by weight, performing melt extrusion through a screw extruder, tabletting the molten material through a tabletting machine, controlling the thickness to be 4.5mm, cooling, crushing, feeding into a grinding machine, crushing and grading, separating fine powder, impurities and the like through a cyclone separator, screening out a product through a powder screen, wherein the powder screen is 280 meshes, and curing for 2.5 days to obtain a finished product of the environment-friendly fireproof coating; the melt extrusion temperature was 125 ℃.
Example 5
The environment-friendly fireproof coating is characterized by being prepared from the following components in parts by weight: 60 parts of crown ether flame-retardant film-forming substance, 20 parts of hyperbranched polyurethane containing epoxy groups, 8 parts of diethyl phosphoryl ethyl triethoxysilane modified black phosphorus/rare earth oxide nanoparticle compound, 4 parts of polyacrylic acid, 25 parts of filler, 1.5 parts of flatting agent and 3 parts of dispersing agent; the crown ether-based flame-retardant film-forming substance is prepared by free radical polymerization of 4-acyl-18-crown ether, (2Z) -4-oxo-4- [3- (trifluoromethyl) -5, 6-dihydro- [1,2,4] triazolo [4,3-a ] pyrazin-7 (8H) -yl ] -1- (2,4, 5-trifluorophenyl) but-2-ene-2-amine, allyl triphenyl phosphonium bromide, N-trihydroxymethyl acrylamide, phenyl vinyl sulfone and acrylonitrile.
The preparation method of the crown ether-based flame-retardant film-forming substance comprises the following steps: adding 4-acyl-18-crown ether, (2Z) -4-oxo-4- [3- (trifluoromethyl) -5, 6-dihydro- [1,2,4] triazolo [4,3-a ] pyrazin-7 (8H) -yl ] -1- (2,4, 5-trifluorophenyl) but-2-ene-2-amine, allyl triphenyl phosphine bromide, N-trihydroxymethyl acrylamide, phenyl vinyl sulfone, acrylonitrile and an initiator into a high boiling point solvent, stirring and reacting for 5 hours at 75 ℃ in an inert gas atmosphere, cooling to room temperature after the reaction is finished, precipitating in water, washing the precipitated polymer with ethanol for 7 times, and finally drying in a vacuum drying oven at 95 ℃ to constant weight to obtain the crown ether flame-retardant-based film-forming substance.
The mass ratio of the 4-acyl-18-crown ether, (2Z) -4-oxo-4- [3- (trifluoromethyl) -5, 6-dihydro- [1,2,4] triazolo [4,3-a ] pyrazin-7 (8H) -yl ] -1- (2,4, 5-trifluorophenyl) but-2-ene-2-amine, allyl triphenyl phosphine bromide, N-trimethylol methacrylamide, phenyl vinyl sulfone, acrylonitrile, an initiator and a high boiling point solvent is 0.3:0.6:1:3:0.3:2:0.07: 30; the initiator is azobisisobutyronitrile; the high boiling point solvent is N-methyl pyrrolidone; the inert gas is nitrogen.
The preparation method of the diethyl phosphoryl ethyl triethoxysilane modified black phosphorus/rare earth oxide nanoparticle compound comprises the following steps: dispersing black phosphorus and rare earth oxide nanoparticles into ethanol, adding diethylphosphorylethyltriethoxysilane into the ethanol, stirring the mixture at 70 ℃ for reaction for 6 hours, and then performing rotary evaporation to remove ethanol to obtain a diethylphosphorylethyltriethoxysilane modified black phosphorus/rare earth oxide nanoparticle compound; the mass ratio of the black phosphorus to the rare earth oxide nanoparticles to the ethyl alcohol to the diethyl phosphoryl ethyl triethoxysilane is 3:2:25: 0.5.
The particle size of the black phosphorus is 1200 meshes.
The weight average molecular weight of the polyacrylic acid is 5 ten thousand; the filler is double flying powder; the particle size of the filler is 1300 meshes; the flatting agent is a polyacrylate flatting agent; the dispersant is sodium hexametaphosphate.
The preparation method of the environment-friendly fireproof coating is characterized by comprising the following steps: uniformly mixing the components in parts by weight, performing melt extrusion through a screw extruder, tabletting the molten material through a tabletting machine, controlling the thickness to be 5mm, cooling, crushing, feeding into a grinding machine, crushing and grading, separating fine powder, impurities and the like through a cyclone separator, separating a product through a powder sieve, and curing for 3 days to obtain a finished product of the environment-friendly fireproof coating; the melt extrusion temperature was 130 ℃.
Comparative example 1
This example provides an environmentally friendly fire retardant coating, which is formulated and prepared in substantially the same manner as in example 1, except that no hyperbranched polyurethane containing epoxy groups is added.
Comparative example 2
This example provides an environmentally friendly fire retardant coating having substantially the same formulation and preparation as in example 1, except that no 4-acyl-18-crown ether is added to the crown ether based flame retardant film forming material.
Comparative example 3
This example provides an environmentally friendly fire retardant coating having substantially the same formulation and preparation method as in example 1, except that the crown ether based flame retardant film forming material was prepared without the addition of (2Z) -4-oxo-4- [3- (trifluoromethyl) -5, 6-dihydro- [1,2,4] triazolo [4,3-a ] pyrazin-7 (8H) -yl ] -1- (2,4, 5-trifluorophenyl) but-2-en-2-amine.
Comparative example 4
The present example provides an environmentally friendly fire retardant coating, which has a formulation and a preparation method substantially the same as those of example 1, except that allyl triphenyl phosphonium bromide is not added in the preparation process of the crown ether based flame retardant film forming material.
Comparative example 5
This example provides an environmentally friendly fire retardant coating having substantially the same formulation and preparation method as example 1, except that the diethylphosphorylethyltriethoxysilane-modified black phosphorus/rare earth oxide nanoparticle composite is prepared without the addition of rare earth oxide nanoparticles.
Comparative example 6
This example provides an environmentally friendly fire retardant coating having substantially the same formulation and preparation method as example 1, except that no black phosphorus was added during the preparation of the diethylphosphorylethyltriethoxysilane modified black phosphorus/rare earth oxide nanoparticle composite.
The environmental protection fire-retardant coatings obtained in the above examples 1 to 5 and comparative examples 1 to 6 were subjected to the relevant performance tests, and the test results and the test methods are shown in Table 1.
As can be seen from Table 1, the environment-friendly fireproof coating disclosed by the embodiment of the invention has better fire-resistant, water-resistant and scrubbing-resistant performances and stronger adhesive force compared with a comparative product, which is the result of synergistic effect of the components.
TABLE 1 environmental protection fire-proof paint performance of examples and comparative examples
The foregoing shows and describes the general principles and broad features of the present invention and advantages thereof. It will be understood by those skilled in the art that the present invention is not limited to the embodiments described above, which are described in the specification and illustrated only to illustrate the principle of the present invention, but that various changes and modifications may be made therein without departing from the spirit and scope of the present invention, which fall within the scope of the invention as claimed. The scope of the invention is defined by the appended claims and equivalents thereof.
Claims (10)
1. The environment-friendly fireproof coating is characterized by being prepared from the following components in parts by weight: based on 30-60 parts of crown ether flame-retardant film-forming substance, 10-20 parts of hyperbranched polyurethane containing epoxy groups, 5-8 parts of diethyl phosphoryl ethyl triethoxysilane modified black phosphorus/rare earth oxide nanoparticle compound, 2-4 parts of polyacrylic acid, 15-25 parts of filler, 0.5-1.5 parts of flatting agent and 1-3 parts of dispersing agent; the crown ether-based flame-retardant film-forming substance is prepared by free radical polymerization of 4-acyl-18-crown ether, (2Z) -4-oxo-4- [3- (trifluoromethyl) -5, 6-dihydro- [1,2,4] triazolo [4,3-a ] pyrazin-7 (8H) -yl ] -1- (2,4, 5-trifluorophenyl) but-2-ene-2-amine, allyl triphenyl phosphonium bromide, N-trihydroxymethyl acrylamide, phenyl vinyl sulfone and acrylonitrile.
2. The environment-friendly fireproof coating according to claim 1, wherein the preparation method of the crown ether flame-retardant film-forming substance comprises the following steps: adding 4-acyl-18-crown ether, (2Z) -4-oxo-4- [3- (trifluoromethyl) -5, 6-dihydro- [1,2,4] triazolo [4,3-a ] pyrazin-7 (8H) -yl ] -1- (2,4, 5-trifluorophenyl) but-2-ene-2-amine, allyl triphenyl phosphine bromide, N-trimethylol methacrylamide, phenyl vinyl sulfone, acrylonitrile and an initiator into a high boiling point solvent, stirring for reaction for 3-5 hours at 65-75 ℃ under an inert gas atmosphere, cooling to room temperature after the reaction is finished, precipitating in water, washing the precipitated polymer for 3-7 times by using ethanol, finally drying at 85-95 ℃ in a vacuum drying oven to constant weight, obtaining the crown ether flame-retardant film-forming substance.
3. The environment-friendly fireproof coating of claim 2, wherein the mass ratio of the 4-acyl-18-crown ether, (2Z) -4-oxo-4- [3- (trifluoromethyl) -5, 6-dihydro- [1,2,4] triazolo [4,3-a ] pyrazin-7 (8H) -yl ] -1- (2,4, 5-trifluorophenyl) but-2-en-2-amine, allyl triphenyl phosphonium bromide, N-trimethylol methacrylamide, phenyl vinyl sulfone, acrylonitrile, initiator and high boiling point solvent is 0.3:0.6:1 (2-3):0.3 (1-2): 0.05-0.07: 20-30.
4. The environment-friendly fireproof coating of claim 1, wherein the initiator is at least one of azobisisobutyronitrile and azobisisoheptonitrile; the high boiling point solvent is at least one of dimethyl sulfoxide, N-dimethylformamide, N-dimethylacetamide and N-methylpyrrolidone; the inert gas is any one of nitrogen, helium, neon and argon.
5. The environment-friendly fireproof paint of claim 1, wherein the preparation method of the diethylphosphorylethyltriethoxysilane-modified black phosphorus/rare earth oxide nanoparticle composite comprises the following steps: dispersing the black phosphorus and rare earth oxide nanoparticles in ethanol, adding diethylphosphorylethyltriethoxysilane, stirring at 50-70 ℃ for reaction for 4-6 hours, and then performing rotary evaporation to remove ethanol to obtain the diethylphosphorylethyltriethoxysilane modified black phosphorus/rare earth oxide nanoparticle composite.
6. The environment-friendly fireproof coating of claim 5, wherein the mass ratio of the black phosphorus to the rare earth oxide nanoparticles to the ethanol to the diethylphosphorylethyltriethoxysilane is 3 (1-2) to (15-25) to (0.3-0.5).
7. The environment-friendly fireproof coating as claimed in claim 5, wherein the particle size of the black phosphorus is 800-1200 mesh.
8. The environment-friendly fireproof coating according to claim 1, wherein the polyacrylic acid has a weight average molecular weight of 2-5 ten thousand; the filler is at least one of titanium dioxide, calcium hydrogen phosphate and talcum powder; the particle size of the filler is 1000-1300 meshes.
9. The environment-friendly fireproof coating as claimed in claim 1, wherein the leveling agent is one or more of a polyacrylate leveling agent, a cellulose acetate butyrate leveling agent and a polyvinyl butyral leveling agent; the dispersing agent is sodium hexametaphosphate and/or sodium polycarboxylate.
10. A method for preparing the environment-friendly fireproof coating according to any one of claims 1 to 9, wherein the method comprises the following steps: uniformly mixing the components in parts by weight, performing melt extrusion through a screw extruder, tabletting the molten material through a tabletting machine, controlling the thickness to be 2-5mm, cooling, crushing, feeding into a grinding machine, crushing and grading, separating fine powder, impurities and the like through a cyclone separator, separating a product through a powder sieve, wherein the powder sieve is 200 meshes and 300 meshes, and curing for 1-3 days to obtain the finished product of the environment-friendly fireproof coating.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113717629A (en) * | 2021-09-15 | 2021-11-30 | 广东和润新材料股份有限公司 | Waterborne polyurethane flame-retardant coating based on aminated phospholene and preparation method thereof |
| CN114806156A (en) * | 2022-04-25 | 2022-07-29 | 青岛科技大学 | Nylon composite material with flame retardance, smoke suppression and reinforcement functions and preparation method thereof |
| CN114806332A (en) * | 2022-04-25 | 2022-07-29 | 东莞市瑞盟涂料有限公司 | Wear-resistant environment-friendly coating for vehicles and preparation process thereof |
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| CN102807817A (en) * | 2012-08-27 | 2012-12-05 | 安徽世林照明股份有限公司 | Method for preparing radiating coating of light-emitting diode (LED) lamp |
| CN104774547A (en) * | 2015-04-30 | 2015-07-15 | 马健 | Coating and preparing method thereof |
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- 2020-11-27 CN CN202011359207.XA patent/CN112574632A/en not_active Withdrawn
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102807817A (en) * | 2012-08-27 | 2012-12-05 | 安徽世林照明股份有限公司 | Method for preparing radiating coating of light-emitting diode (LED) lamp |
| CN104774547A (en) * | 2015-04-30 | 2015-07-15 | 马健 | Coating and preparing method thereof |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113717629A (en) * | 2021-09-15 | 2021-11-30 | 广东和润新材料股份有限公司 | Waterborne polyurethane flame-retardant coating based on aminated phospholene and preparation method thereof |
| CN114806156A (en) * | 2022-04-25 | 2022-07-29 | 青岛科技大学 | Nylon composite material with flame retardance, smoke suppression and reinforcement functions and preparation method thereof |
| CN114806332A (en) * | 2022-04-25 | 2022-07-29 | 东莞市瑞盟涂料有限公司 | Wear-resistant environment-friendly coating for vehicles and preparation process thereof |
| CN114806332B (en) * | 2022-04-25 | 2023-03-10 | 东莞市瑞盟涂料有限公司 | Wear-resistant environment-friendly coating for vehicles and preparation process thereof |
| CN114806156B (en) * | 2022-04-25 | 2023-10-27 | 青岛科技大学 | Flame-retardant smoke-inhibiting reinforced nylon composite material and preparation method thereof |
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