CN109266070B - Flame-retardant coating and preparation method thereof - Google Patents

Flame-retardant coating and preparation method thereof Download PDF

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CN109266070B
CN109266070B CN201810870555.XA CN201810870555A CN109266070B CN 109266070 B CN109266070 B CN 109266070B CN 201810870555 A CN201810870555 A CN 201810870555A CN 109266070 B CN109266070 B CN 109266070B
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flame retardant
retardant coating
flame
pentabromophenol
parts
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CN109266070A (en
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谭贺洵
汪洋
曾志伟
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Guangdong Xinhuangguan New Material Co ltd
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    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09DCOATING 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
    • C09D4/00Coating compositions, e.g. paints, varnishes or lacquers, based on organic non-macromolecular compounds having at least one polymerisable carbon-to-carbon unsaturated bond ; Coating compositions, based on monomers of macromolecular compounds of groups C09D183/00 - C09D183/16
    • C09D4/06Organic non-macromolecular compounds having at least one polymerisable carbon-to-carbon unsaturated bond in combination with a macromolecular compound other than an unsaturated polymer of groups C09D159/00 - C09D187/00
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09DCOATING 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
    • C09D5/00Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
    • C09D5/08Anti-corrosive paints
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09DCOATING 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
    • C09D5/00Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
    • C09D5/18Fireproof paints including high temperature resistant paints
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09DCOATING 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
    • C09D7/00Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
    • C09D7/40Additives
    • C09D7/60Additives non-macromolecular
    • C09D7/61Additives non-macromolecular inorganic
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09DCOATING 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
    • C09D7/00Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
    • C09D7/40Additives
    • C09D7/60Additives non-macromolecular
    • C09D7/63Additives non-macromolecular organic
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09DCOATING 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
    • C09D7/00Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
    • C09D7/40Additives
    • C09D7/66Additives characterised by particle size
    • C09D7/67Particle size smaller than 100 nm

Abstract

The invention discloses a flame-retardant coating and a preparation method thereof, wherein the coating comprises the following raw materials in percentage by weight: 25-45 parts of acrylic resin prepolymer, 20-35 parts of flame retardant, 0.5-1.5 parts of initiator, 4-9 parts of pigment, 1-3 parts of dispersant, 4-9 parts of inorganic filler, 2-4 parts of defoaming agent, 2-5 parts of film-forming assistant and 5-25 parts of solvent. According to the invention, the reactive flame retardant is added into the matrix resin, and the flame retardant and the acrylic resin prepolymer form a completely compatible whole, so that the prepared flame-retardant coating not only has an excellent and durable flame-retardant effect, but also has excellent physical and mechanical properties, water resistance, weather resistance and fatigue resistance.

Description

Flame-retardant coating and preparation method thereof
Technical Field
The invention belongs to the field of coatings, and particularly relates to a flame-retardant coating and a preparation method thereof.
Background
The flame-retardant coating is brushed on the surface of a flammable material, can play a certain decorative role at ordinary times, can slow down the spreading and propagation speed of flame once a fire breaks out, prevents combustion within a certain time, and achieves the purposes of protecting a base material, and enabling people to have enough time to leave a fire scene and organize for rescue. The fire-retardant principle of the fire-retardant coating can be roughly summarized into the following five points: (1) the fireproof coating has flame retardancy or incombustibility, so that the protected substrate is not directly contacted with air, the ignition of an object is delayed, and the combustion speed is slowed down; (2) the fireproof coating has low heat conductivity coefficient besides flame retardancy or incombustibility, and can delay the transmission of flame temperature to a protected substrate; (3) the fire-proof coating is heated to decompose non-combustible inert gas, and dilute combustible gas decomposed by the protected object when heated, so that the protected object is not easy to burn or the burning speed is reduced; (4) the nitrogen-containing fire-proof coating is heated to decompose NO and NH3The groups are combined with organic free radicals, the chain reaction is interrupted, and the temperature is reduced; (5) the expansion type fireproof coating expands and foams by heating to form a carbonaceous foam heat insulation layer to seal a protected object, so that the transfer of heat and a base material is delayed, and the object is prevented from catching fire and burning or the strength is prevented from being reduced due to the rise of temperature.
Acrylic resin is a very important matrix resin, has excellent physical and mechanical properties, water resistance, weather resistance and fatigue resistance, and is low in price, so that the acrylic resin is widely used in the fields of engineering materials, electronics, electric appliances, optical instruments, coatings, adhesives and the like. However, because of their low LOI, these polymers are easily ignited by gaseous substances in the air, and release a great deal of smoke during combustion, which not only causes serious property damage, but also endangers the life safety of people, thus limiting their application in some special fields. Therefore, how to make the coating prepared from the acrylic resin have good flame retardant effect is the research direction of many researchers.
Disclosure of Invention
Aiming at the technical problems in the prior art, the invention provides a flame-retardant coating which can overcome the defects in the prior art. The product series of the invention has obvious and durable flame retardant effect and good weather resistance.
The invention provides a flame-retardant coating which comprises the following raw materials in percentage by weight:
Figure GDA0002512815390000021
preferably, the acrylic resin prepolymer is a polymer of methyl acrylate, ethyl acrylate, butyl methacrylate, acrylic acid and t-butyl peroxybenzoate.
Preferably, the flame retardant comprises the following components: propiolic acid monomers, pentabromophenol and bromine water; reacting the propiolic acid monomer with the pentabromophenol under the catalysis of concentrated sulfuric acid to obtain the pentabromophenol propiolate, and reacting the pentabromophenol propiolate with bromine water to obtain the flame retardant.
Preferably, the initiator is one or more of tert-amyl peroxybenzoate, tert-butyl peroxy-3, 3, 5-trimethylhexanoate and tert-amyl peroxyacetate.
Preferably, the pigment comprises titanium dioxide, red lead powder and iron yellow; the dispersant is sodium hexametaphosphate.
Preferably, the inorganic filler comprises one or more of talc, nano zirconia, sepiolite and mica.
Preferably, the solvent includes toluene, methyl ethyl ketone and ethyl acetate.
Preferably, the coalescents include ethylene glycol, propylene glycol, and ethers.
Preferably, the defoaming agent is a silicone defoaming agent.
In addition, the preparation method of the flame retardant coating is also provided, wherein the acrylic resin prepolymer is dissolved in the solvent under the condition of stirring, the flame retardant is added after uniform stirring, the initiator is dropwise added, then the inorganic filler, the pigment, the dispersing agent, the defoaming agent and the film forming assistant are sequentially added, and the flame retardant coating is formed after uniform stirring and mixing and grinding to the fineness of 20-30 mu m.
Compared with the prior art, the invention has the following beneficial effects:
1. the novel reactive flame retardant is prepared by two-step synthesis, and is copolymerized with the acrylic resin prepolymer, and the flame retardant is introduced into a molecular chain of the acrylic resin, so that the prepared flame retardant coating has a good flame retardant effect, and also has excellent physical and mechanical properties, water resistance, weather resistance and fatigue resistance.
2. The reactive flame retardant and the acrylic resin prepolymer form a completely compatible whole, so that the flame retardance of the flame retardant coating prepared by the invention is not reduced along with the prolonging of time, the flame retardant coating has lasting flame retardance, and the production cost of enterprises is saved because the used matrix resin is the acrylic resin with low price.
Detailed Description
In order to further clarify and clarify the technical solution and effects of the present invention, the present invention is described in further detail below. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
Example 1
The invention provides a flame-retardant coating which comprises the following raw materials in percentage by weight:
Figure GDA0002512815390000031
Figure GDA0002512815390000041
the acrylic resin prepolymer is a polymer of methyl acrylate, ethyl acrylate, butyl methacrylate, acrylic acid and tert-butyl peroxybenzoate. The flame retardant comprises the following components: propiolic acid monomers, pentabromophenol and bromine water; the preparation steps are as follows: reacting the propiolic acid monomer with the pentabromophenol under the catalysis of concentrated sulfuric acid to obtain the pentabromophenol propiolate, adding a saturated sodium carbonate solution into a reaction mixture after the reaction is finished, and separating and purifying the pentabromophenol propiolate; reacting the purified pentabromophenol propiolate with bromine water to obtain a product, namely the flame retardant; wherein the propiolic acid monomer is propiolic acid and/or methyl propiolic acid. Preferably, the weight percentage of the propiolic acid monomer to the pentabromophenol is 1.5: 1; the molar ratio of the pentabromophenol propiolate to bromine in the bromine water is 1: 3.
The initiator is one or more of tert-amyl peroxybenzoate, tert-butyl peroxy-3, 3, 5-trimethylhexanoate and tert-amyl peroxyacetate.
The pigment comprises titanium dioxide, red lead powder and iron yellow, and the pigment plays a supporting role in the flame-retardant coating, so that the coating has certain physical and mechanical properties; the dispersing agent is sodium hexametaphosphate, and the pigment can be effectively and uniformly dispersed in the acrylic resin by adding the dispersing agent.
The inorganic filler comprises one or more of talcum powder, nano zirconium dioxide, sepiolite and mica, and the addition of the inorganic filler can improve the strength of the flame-retardant coating and increase the reaction area, so that the fireproof performance of the flame-retardant coating is effectively improved, and the addition of the inorganic filler also reduces the overall cost of the flame-retardant coating.
The solvent comprises toluene, methyl ethyl ketone and ethyl acetate, the solvent is formed by mixing the toluene, the methyl ethyl ketone and the ethyl acetate according to the volume ratio of 3:3:5, and the matrix resin and the flame retardant can be uniformly dispersed in the solvent according to the mixed solvent in the proportion.
The film-forming assistant comprises ethylene glycol, propylene glycol and ethers, and the addition of the film-forming assistant can promote the plastic flow and elastic deformation of a macromolecular compound, improve the coalescence performance and enable the flame-retardant coating to form a film within a wider construction temperature range.
The defoaming agent is a silicone defoaming agent, so that the dispersion speed of the pigment in the resin is improved, and the storage stability, the construction process and the coating smoothness are improved.
In addition, this embodiment also provides a preparation method of the flame retardant coating, in which the acrylic resin prepolymer is dissolved in the solvent according to a corresponding ratio under the condition of stirring, the flame retardant is added according to a corresponding ratio after uniformly stirring, the initiator according to a corresponding ratio is added dropwise, then the inorganic filler, the pigment, the dispersant, the defoamer and the film forming aid according to a corresponding ratio are sequentially added, and the mixture is ground to a fineness of 20 to 30 μm after uniformly stirring and mixing to form the flame retardant coating.
In this embodiment, a reactive flame retardant is introduced into a molecule of an acrylic resin prepolymer, so that the acrylic resin is modified in relevant physical and chemical properties, and a paint production technology that pigments and inorganic fillers are physically and chemically stable in a matrix resin is utilized, so that the prepared flame retardant paint not only has an excellent and durable flame retardant effect, but also has excellent physical and mechanical properties, water resistance, weather resistance and fatigue resistance.
Example 2
On the basis of the embodiment 1, the embodiment 2, as a preferred embodiment of the present invention, is a flame retardant coating, which comprises the following raw materials by weight:
Figure GDA0002512815390000051
the preparation method of the flame-retardant coating is the same as that of example 1.
Example 3
On the basis of the embodiment 1, the embodiment 3, as a preferred embodiment of the present invention, is a flame retardant coating, which comprises the following raw materials by weight:
Figure GDA0002512815390000061
the preparation method of the flame-retardant coating is the same as that of example 1.
Example 4
On the basis of the example 1, in this example 4, which is a preferred example of the present invention, a flame retardant coating comprises the following raw materials by weight:
Figure GDA0002512815390000062
the preparation method of the flame-retardant coating is the same as that of example 1.
The first table shows the results of the performance tests of the flame retardant coatings prepared in examples 2-4.
Watch 1
Figure GDA0002512815390000071
Resistance to detonation heat: the prepared pattern is vertically prevented from being placed in a constant-temperature oven (50 +/-2 ℃), taken out after a certain time, vertically placed in an environment which is not directly irradiated by sunlight, naturally dried, and observed whether the surface is uniform and compact or not and whether cracks and bubbles exist or not.
As shown in Table I, the flame retardant coatings prepared in examples 2-4 have low thermal conductivity, good thermal insulation, high oxygen index, good explosion and humidity resistance, good salt spray corrosion resistance, and excellent tensile strength, bonding strength and sanding property.
In conclusion, the flame-retardant coating prepared by the invention has excellent comprehensive fireproof effect, and also has the advantages of good weather resistance, water resistance, weather resistance, fatigue resistance, physical and mechanical properties, such as high tensile strength, high sanding resistance, high bonding strength and the like.
It will be clear to a person skilled in the art that the scope of the present invention is not limited to the examples discussed in the foregoing, but that several amendments and modifications thereof are possible without deviating from the scope of the present invention as defined in the attached claims. While the invention has been described in detail in the specification, such illustration and description are to be considered illustrative or exemplary and not restrictive. The invention is not limited to the disclosed embodiments.

Claims (8)

1. The flame-retardant coating is characterized by comprising the following raw materials in percentage by weight:
Figure FDA0002526559690000011
the acrylic resin prepolymer is a polymer of methyl acrylate, ethyl acrylate, butyl methacrylate, acrylic acid and tert-butyl peroxybenzoate;
the flame retardant comprises the following components: propiolic acid monomers, pentabromophenol and bromine water; the preparation steps of the flame retardant are as follows: reacting the propiolic acid monomer with the pentabromophenol under the catalysis of concentrated sulfuric acid to obtain the pentabromophenol propiolate, adding a saturated sodium carbonate solution into a reaction mixture after the reaction is finished, and separating and purifying the pentabromophenol propiolate; reacting the purified pentabromophenol propiolate with bromine water to obtain a product, namely the flame retardant; the propiolic acid monomer is propiolic acid and/or methyl propiolic acid, and the weight percentage of the propiolic acid monomer to the pentabromophenol is 1.5: 1; the molar ratio of the pentabromophenol propiolate to bromine in the bromine water is 1: 3.
2. A fire retardant coating according to claim 1, wherein said initiator is one or more of tert-amyl peroxybenzoate, tert-butyl peroxy-3, 3, 5-trimethylhexanoate and tert-amyl peroxyacetate.
3. The flame retardant coating of claim 1, wherein said pigments comprise titanium dioxide, red lead powder and iron yellow; the dispersant is sodium hexametaphosphate.
4. The flame retardant coating of claim 1, wherein said inorganic filler comprises one or more of talc, nano zirconia, sepiolite and mica.
5. The flame retardant coating according to claim 1, wherein the solvent comprises toluene, methyl ethyl ketone and ethyl acetate, and the toluene, the methyl ethyl ketone and the ethyl acetate are mixed according to a volume ratio of 3:3: 5.
6. The flame retardant coating of claim 1, wherein said coalescent comprises ethylene glycol, propylene glycol and ethers.
7. The flame retardant coating according to claim 1, wherein said defoaming agent is a silicone defoaming agent.
8. The preparation method of the flame retardant coating according to any one of claims 1 to 7, characterized by dissolving the acrylic resin prepolymer in the solvent according to the corresponding proportion under the condition of stirring, adding the flame retardant according to the corresponding proportion after uniformly stirring, dripping the initiator, then sequentially adding the inorganic filler, the pigment, the dispersant, the defoamer and the film forming aid according to the corresponding proportion, uniformly stirring and mixing, and then sanding to the fineness of 20-30 μm to form the flame retardant coating.
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CN110305489A (en) * 2019-06-26 2019-10-08 保定威尔达节能科技有限公司 A kind of fire prevention styrofoam fire prevention material and its preparation and application
CN111019572B (en) * 2019-11-15 2022-04-08 深圳昌茂粘胶新材料有限公司 Preparation method of flame-retardant acrylic pressure-sensitive adhesive
CN116197983B (en) * 2023-02-27 2024-02-06 江苏零界科技集团有限公司 Antibacterial mildew-proof wood and preparation method thereof

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