CN116622283A - Fireproof flame-retardant shell substrate coating and preparation method thereof - Google Patents
Fireproof flame-retardant shell substrate coating and preparation method thereof Download PDFInfo
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- CN116622283A CN116622283A CN202310906398.4A CN202310906398A CN116622283A CN 116622283 A CN116622283 A CN 116622283A CN 202310906398 A CN202310906398 A CN 202310906398A CN 116622283 A CN116622283 A CN 116622283A
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Classifications
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- 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
- C09D175/00—Coating compositions based on polyureas or polyurethanes; Coating compositions based on derivatives of such polymers
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- C09D5/18—Fireproof paints including high temperature resistant paints
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- 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
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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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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
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- C08K2003/382—Boron-containing compounds and nitrogen
- C08K2003/385—Binary compounds of nitrogen with boron
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- C—CHEMISTRY; METALLURGY
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Abstract
The invention discloses a fireproof flame-retardant shell substrate coating and a preparation method thereof, wherein the fireproof flame-retardant shell substrate coating comprises the following components: shell powder, a diluent, an auxiliary agent, a filler, a modified flame retardant and a base resin. Compared with the prior art, the shell-based coating is obtained by adopting scientific raw materials and proportions, and the components are mutually synergistic and promoted to show good heat insulation and flame retardance effects and also have good coating adhesive force.
Description
Technical Field
The invention relates to the technical field of fireproof materials, in particular to a fireproof flame-retardant shell substrate coating and a preparation method thereof.
Background
The fireproof flame-retardant shell base material coating is a coating with fireproof flame-retardant function, and the base material of the coating is made of natural materials such as shells and the like, so that the risk of fire can be effectively reduced. Such coatings are typically made of inorganic materials that remain stable at high temperatures and are not flammable. In addition, the fireproof flame-retardant shell substrate coating also has good weather resistance and corrosion resistance, is widely applied to the fields of building, transportation, electric power and the like, and has the characteristics of environmental protection, safety and high efficiency.
However, fire-retardant shell substrate coatings also have some problems and drawbacks, and the fire-retardant properties of the coatings are limited, and although fire-retardant shell substrate coatings can improve the fire-retardant properties of buildings, they are still limited. In extreme cases, the coating may not prevent the spread of the fire. The fireproof flame-retardant shell substrate coating has insufficient durability and adhesion, and can be subjected to the problems of falling, cracking and the like after long-term use, so that the fireproof performance of the fireproof flame-retardant shell substrate coating is affected. Thereby affecting the application range. Accordingly, there is a need for improved fire-retardant shell substrate coatings that address the problems and deficiencies thereof.
The invention patent application CN114149699A discloses a shell base material coating capable of preventing fire and retarding flame, which is characterized in that: the material is prepared from the following raw materials: shell powder, kaolin, light calcium carbonate, nano silicon dioxide and TiO 2 -bismuth alum-graphene ternary nanocomposite and binder powder; the grain size of the shell powder is 300-1500 meshes. The preparation method of the paint comprises the following steps: (S1) slurry preparation: mixing hydroxyethyl cellulose, water-based silicone oil, sodium alginate, polyethylene glycol, a dispersing agent, a defoaming agent with the formula amount of 40-60% and water, and stirring at a medium speed to prepare slurry; (S2) base material preparation: adding modified shell powder, zeolite powder, titanium pigment and diatomite into the slurry, and stirring at a high speed to obtain a base material; (S3) adding photocatalytic raw materials: adding silicone-acrylate emulsion, film forming additive and defoaming agent with the formula amount of 40-60% into the base material obtained in the step (S2), uniformly stirring at low speed, adding the photocatalytic composite colloid, and stirring at low speed. The invention has good flame resistance. However, the shell substrate coating prepared by the method has poor flame-retardant and heat-insulating effects, low adhesive force performance and easy falling of the coating after long-term use.
Disclosure of Invention
In view of the defects of poor flame-retardant and heat-insulating effects and low adhesive force performance of the shell substrate coating in the prior art, the invention aims to provide the fireproof flame-retardant shell substrate coating and the preparation method thereof.
In order to achieve the above object, the present invention adopts the following technical scheme:
a fireproof flame-retardant shell substrate coating comprises the following components: shell powder, a diluent, an auxiliary agent, a filler, a modified flame retardant and a base resin.
Preferably, the fireproof flame-retardant shell substrate coating comprises the following components in parts by weight: 30-50 parts of shell powder, 15-25 parts of diluent, 3-8 parts of auxiliary agent, 10-20 parts of filler, 20-30 parts of modified flame retardant and 20-40 parts of base resin.
Further preferably, the fireproof flame-retardant shell substrate coating comprises the following components in parts by weight: 40 parts of shell powder, 20 parts of diluent, 5 parts of auxiliary agent, 15 parts of filler, 25 parts of modified flame retardant and 30 parts of base resin.
Preferably, the diluent is at least one of water, isopropanol, butanol, ethanol, acetone, ketone, propylene glycol and ethylene glycol.
Preferably, the auxiliary agent is at least one of a thickening agent, a toughening agent and a defoaming agent.
More preferably, the auxiliary agent is a thickening agent and an antifoaming agent according to the mass ratio of 1-3: 2-4.
Preferably, the thickener is at least one of montmorillonite, magnesium silicate, talcum powder, hydroxypropyl methylcellulose, hydroxypropyl cellulose, methylcellulose, polyacrylamide, polyvinyl alcohol and sodium silicate.
Preferably, the defoaming agent is at least one of ethoxymethyl silicone oil, methyl silicone oil, polysiloxane, polyether silicone oil, fatty alcohol polyoxyethylene ether, polyoxyethylene stearate, alkylphenol fatty alcohol polyoxyethylene ether and stearic acid.
Preferably, the filler is at least one of mica powder, calcium silicate, calcium carbonate and silicon dioxide.
Preferably, the base resin is at least one of methyl acrylate, ethyl acrylate, bisphenol a type epoxy resin, aliphatic epoxy resin, phenolic alkyd resin, phenolic aldehyde acid resin, aqueous polyurethane resin and polyether polyurethane resin.
The preparation method of the modified flame retardant comprises the following steps:
s1, adding pentaerythritol and n-butyl acrylate into a phosphoric acid aqueous solution, stirring, and performing reduced pressure distillation to obtain a compound;
s2, adding boric acid into the polyethylene glycol 200, and stirring to obtain a reactant;
s3, adding the compound prepared in the step S1 into the reactant prepared in the step S2, stirring, and then heating and refluxing to obtain a liquid mixture;
s4, adding sepiolite into water, performing ultrasonic dispersion at room temperature, filtering, drying, collecting solids, adding the solids and the functional agent into the liquid mixture prepared in the step S3, stirring, and heating and stirring to obtain the modified flame retardant.
The preparation method of the modified flame retardant comprises the following steps of:
s1, adding 40-50 parts of pentaerythritol and 10-20 parts of n-butyl acrylate into 130-150 parts of 85-90 wt% phosphoric acid aqueous solution, stirring at 100-110 ℃ for 3-5 hours at 500-1000 rpm, and carrying out reduced pressure distillation for 1-3 hours at a reduced pressure of 1-10 kPa and a distillation temperature of 90-100 ℃ to obtain a compound;
s2, adding 10-20 parts of boric acid into 50-70 parts of polyethylene glycol 200, and stirring at 120-140 ℃ and 100-300 rpm for 1-5 hours to obtain a reactant;
s3, adding 80-90 parts of the compound prepared in the step S1 into 10-20 parts of the reactant prepared in the step S2, stirring at 40-60 ℃ and 100-300 rpm for 0.5-2 h, and then heating to 110-120 ℃ and refluxing for 2-6 h to obtain a liquid mixture;
s4, adding 30-50 parts of sepiolite into 900-1100 parts of water, performing ultrasonic dispersion for 0.5-2 hours at room temperature, wherein the ultrasonic power is 200-500W, the ultrasonic frequency is 40-60 kHz, then filtering and drying for 20-30 hours at 50-70 ℃ through a 100-300 mesh screen, collecting solids, adding the solids and 10-20 parts of functional agents into the liquid mixture prepared in the step S3, stirring for 0.5-2 hours at 40-60 ℃ at 100-500 rpm, and then heating to 110-130 ℃ and stirring for 2-6 hours at 100-300 rpm to obtain the modified flame retardant.
The functional agent is hexagonal boron nitride/carbon nano tube composite material.
The preparation method of the hexagonal boron nitride/carbon nano tube composite material comprises the following steps of:
z1, adding 0.5-2 parts of hexagonal boron nitride into 150-170 parts of 20-30wt% ethanol aqueous solution, performing ultrasonic dispersion for 20-40 min, wherein the ultrasonic power is 200-500W, the ultrasonic frequency is 40-60 kHz, then adding 0.1-0.5 part of Tris buffer solution, then adjusting the pH to 8.0-9.0 by using 0.05-0.2 mol/L sodium hydroxide aqueous solution, then adding 0.2-0.6 part of dopamine hydrochloride, and reacting for 2-10 h at 20-30 ℃ to obtain suspension; then adding 0.5-2 parts of a silane coupling agent KH550 into the suspension, stirring for 3-7 hours at 50-70 ℃ and 100-300 rpm, centrifugally separating for 2-10 minutes at 10000-20000 rpm, collecting solids, washing with absolute ethyl alcohol, and drying for 1-5 hours at 50-70 ℃ to obtain a hybrid;
z2, adding 0.5-2 parts of acidified carbon nano tubes into 80-120 parts of 70-85 wt% ethanol aqueous solution, performing ultrasonic dispersion for 20-40 min, wherein the ultrasonic power is 200-500W, the ultrasonic frequency is 40-60 kHz, adding 0.1-0.5 part of the hybrid prepared in the step Z1 under the protection of nitrogen, adjusting the pH value to 8.5-9.5 by using 0.5-2 mol/L sodium hydroxide aqueous solution, stirring at 50-60 ℃ at 100-300 rpm for 24-72 h, centrifuging at 10000-20000 rpm for 2-10 min, collecting solids, washing by using absolute ethanol, and drying in a vacuum oven at 30-50 ℃ for 2-6 h to obtain the functional agent.
The preparation method of the acidified carbon nano tube comprises the following steps of:
88-98 wt% of concentrated sulfuric acid and 60-69 wt% of concentrated nitric acid are prepared into a mixed solution according to the mass ratio of 2-4:1, 80-120 parts of the mixed solution and 0.5-2 parts of carbon nano tubes are mixed for 100-500 rpm and stirred for 0.5-2 hours, then 500-1500 parts of water is added for dilution, the solid is collected by filtration, and the acidified carbon nano tubes are obtained by flushing with water.
A fireproof flame-retardant shell substrate coating is prepared by the following steps:
step 1, adding a diluent and an auxiliary agent into base resin, and stirring at 100-500 rpm for 1-3 hours to prepare slurry;
step 2, adding shell powder into the slurry prepared in the step 1, and stirring at 800-1500 rpm for 0.5-2 h to prepare a base material;
and step 3, adding the filler and the modified flame retardant into the base material obtained in the step 2, and stirring for 1-10 hours at 50-300 rpm to obtain the shell substrate coating.
According to the invention, water, hydroxypropyl methyl cellulose and fatty alcohol polyoxyethylene ether AEO-9 are added into aqueous polyurethane resin for stirring, shell powder is added for stirring, then calcium silicate and a modified flame retardant are added, and stirring is carried out to obtain the shell substrate coating. The modified flame retardant is prepared by adding pentaerythritol and n-butyl acrylate into a phosphoric acid aqueous solution, heating, stirring, and distilling under reduced pressure to obtain a compound; adding boric acid into polyethylene glycol 200, heating and stirring to obtain a reactant; adding the compound into a reactant, heating, stirring and refluxing to obtain a liquid mixture; adding sepiolite into water for ultrasonic cleaning, then adding the cleaned sepiolite and the functional agent into the liquid mixture, heating and stirring to obtain the modified flame retardant. The functional agent is a hexagonal boron nitride/carbon nano tube composite material, hexagonal boron nitride is dispersed in ethanol water solution in an ultrasonic way, then Tris buffer solution is added, pH is regulated by sodium hydroxide water solution, dopamine hydrochloride is added, and the mixture reacts at normal temperature to obtain suspension; then adding a silane coupling agent KH550 into the suspension, stirring and centrifugally separating to obtain a hybrid; adding the acidified carbon nano tube into ethanol water solution for ultrasonic dispersion, adding the hybrid under the protection of nitrogen, adjusting the pH value by using sodium hydroxide water solution, stirring and centrifuging, and drying to obtain the functional agent.
The introduction of sepiolite facilitates the formation of more crosslinked and aromatic structures in the condensed phase, producing a more thermally stable and dense char, resisting heat transfer, and thus enhancing the barrier effect and thermal stability of the char. During combustion, the coating begins to decompose and release non-combustible gases (NH 3 And H 2 O). The main decomposition products of the coating are triazines, polyphosphates and derivatives thereof. As the temperature increases, the triazine compound and the phosphorus-containing compound form an expansion precursor through aromatization, cyclization and crosslinking reactions. With the release of non-combustible gases, these gases may dilute the combustible gases and cause further expansion of the precursor. Then, an expanded carbon layer is formed to cover the surface of the base material, and the generated carbon can effectively isolate heat, oxygen and combustible gas between the combustion zone and the base material, so that the heat insulation, flame retardance and smoke suppression effects are super strong. Sepiolite and liquid mixtures have excellent synergistic effects in coatings, mainly due to the formation of more crosslinked and aromatic structures in the condensed phase, resulting in combustion processesA denser and expanded carbon layer, thereby resisting penetration of heat and volatile products.
The silane coupling agent KH550 is grafted to the hexagonal boron nitride surface through reaction with dopamine hydrochloride. The hexagonal boron nitride and the carbon nano tube are uniformly and tightly combined, and the structure is complete, so that the hexagonal boron nitride and the carbon nano tube can form a synergistic effect, and the mechanical strength and the fire resistance of the coating are improved. The acidified carbon nano tube is well dispersed in a coating system, and the strength of a carbon layer is effectively enhanced by adding hexagonal boron nitride, and the carbon nano tube has good heat resistance. Due to the anisotropic heat transfer and physical barrier of hexagonal boron nitride and the supporting connection of carbon nanotubes, the density of the carbon layer can be increased, thereby limiting the transfer of radiant heat. The carbon nanotubes serve as supports for the connection between cracks and cover the carbon cavities, thereby increasing the density of the carbon in the combustion process and delaying the generation of the carbon.
The shell substrate coating after combustion presents a compact and uniform carbon skeleton network structure. The carbon skeleton structure plays a good role in supporting the carbon layer, increases the flame impact resistance, and enhances the strength of the carbon layer. The increase of the carbon content and strength is favorable for reducing heat transfer, thereby obtaining good heat insulation and flame retardant effects, the surface of the carbon skeleton obtained by combining grafted sepiolite is compact and complete, a plurality of honeycomb bubble structures are arranged in the carbon skeleton, the carbon nano tube tends to form a continuous reticular structure in the combustion process, and the carbon skeleton plays a role of supporting the carbon in the formation process of a carbon layer and fills carbon gaps. In addition, the formation of the silicon network also strengthens the carbon layer. In the combustion process, hexagonal boron nitride is bonded on the surface of the network structure, so that the support of a carbon network is enhanced, carbonization of a coating matrix is promoted, and the entry of combustible gas in the combustion process is prevented. In addition, the anisotropic heat transfer of hexagonal boron nitride planar heat dissipation and vertical surface heat preservation increases the diffusion of heat, so that the coating is heated more uniformly. In conclusion, the shell substrate coating disclosed by the invention is favorable for forming a continuous and stable carbon layer, and effectively inhibits and blocks heat transfer generated by released inflammable products and flame.
Coating hexagonal boron nitride with dopamine hydrochloride can improve reactivity and also improve dispersibility in water. The silane coupling agent KH550 is used as bridging agent, and the acidified carbon nano-tube is connected with the hybrid to prepare the functional agent. Due to the synergistic effect of the hexagonal boron nitride and the carbon nano tube, the functional agent can improve the thermal stability and oxidation resistance of the carbon layer, thereby enhancing the thermal barrier effect and the barrier effect, and the addition of the functional agent enables the carbon layer to present a compact and uniform carbon skeleton network structure, and simultaneously maintains part of silicon network, thereby presenting better heat insulation and flame retardance effects and also having good coating adhesive force.
Compared with the prior art, the invention has the beneficial effects that:
1) The shell substrate coating is prepared from scientific raw materials and proportions, has good fireproof and flame-retardant functions, and can effectively reduce the risk of fire disaster by using natural materials such as shells as the substrate, keep stable at high temperature and not easily burn; in addition, the fireproof flame-retardant shell substrate coating also has good weather resistance and corrosion resistance, and can be used in different environments.
2) According to the invention, through the preparation of the modified flame retardant, the components are mutually cooperated to promote, so that the prepared fireproof flame-retardant shell substrate coating generates a denser and porous carbon layer structure in the combustion process, thereby having better heat insulation and flame retardance effects and good coating adhesive force.
Detailed Description
The main material sources are as follows:
shell powder, particle size: 800 mesh.
Aqueous polyurethane resin: hefeihua new material science and technology limited company, goods number: 03.
tris buffer: jiangsu rhyme Tong New Material science and technology Co., ltd., model: SD01853.
Calcium silicate, particle size: 800 mesh.
Sepiolite: lingshu county, xuancheng mineral processing factory, goods number: XCHPSF35.
Hexagonal boron nitride, particle size: 100 mesh.
Carbon nanotubes: zhejiang Zhi Tina micro new material Co., ltd., fineness: 1-3 nm.
Example 1
A fireproof flame-retardant shell substrate coating is prepared by the following steps:
step 1, adding 20kg of water, 2kg of hydroxypropyl methylcellulose and 3kg of fatty alcohol polyoxyethylene ether AEO-9 into 30kg of aqueous polyurethane resin, and stirring at 300rpm for 2 hours to prepare slurry;
step 2, adding 40kg of shell powder into the slurry prepared in the step 1, and stirring at 1200rpm for 1h to prepare a base material;
and step 3, adding 15kg of calcium silicate and 25kg of modified flame retardant into the base material obtained in the step 2, and stirring at 100rpm for 5 hours to obtain the shell substrate coating.
The preparation method of the modified flame retardant comprises the following steps:
s1, adding 45g of pentaerythritol and 15g of n-butyl acrylate into 140g of 85wt% phosphoric acid aqueous solution, stirring at 800rpm at 105 ℃ for 4 hours, and carrying out reduced pressure distillation for 2 hours, wherein the reduced pressure is 5kPa, and the distillation temperature is 100 ℃ to obtain a compound;
s2, adding 15g of boric acid into 60g of polyethylene glycol 200, and stirring at 130 ℃ and 200rpm for 3 hours to obtain a reactant;
s3, adding 85g of the compound prepared in the step S1 into 15g of the reactant prepared in the step S2, stirring at 50 ℃ and 200rpm for 1h, and then heating to 115 ℃ and refluxing for 4h to obtain a liquid mixture;
s4, adding 40g of sepiolite into 1000g of water, performing ultrasonic dispersion for 1h at room temperature, wherein the ultrasonic power is 300W, the ultrasonic frequency is 50kHz, then filtering and drying for 24h at 60 ℃ through a 200-mesh screen, collecting solids, adding the solids and 15g of functional agent into the liquid mixture prepared in the step S3, stirring for 1h at 50 ℃ at 300rpm, and then heating to 120 ℃ and stirring for 4h at 200rpm to obtain the modified flame retardant.
The functional agent is hexagonal boron nitride/carbon nano tube composite material.
The preparation method of the hexagonal boron nitride/carbon nano tube composite material comprises the following steps:
z1, adding 1kg of hexagonal boron nitride into 160kg of 25wt% ethanol water solution, performing ultrasonic dispersion for 30min, wherein the ultrasonic power is 300W, the ultrasonic frequency is 50kHz, then adding 0.3kg of Tris buffer solution, then adjusting the pH to 8.5 by using 0.1mol/L sodium hydroxide water solution, then adding 0.4kg of dopamine hydrochloride, and reacting for 6h at 25 ℃ to obtain suspension; then adding 1kg of silane coupling agent KH550 into the suspension, stirring at 60 ℃ and 200rpm for 5h, centrifuging at 15000rpm for 5min, collecting solid, washing with absolute ethyl alcohol, and drying at 60 ℃ for 3h to obtain a hybrid;
z2, adding 1kg of acidified carbon nano tube into 100kg of 75wt% ethanol water solution, performing ultrasonic dispersion for 30min, wherein the ultrasonic power is 300W, the ultrasonic frequency is 50kHz, adding 0.3kg of the hybrid prepared in the step Z1 under the protection of nitrogen, adjusting the pH to 9 by using 1mol/L sodium hydroxide water solution, stirring at 55 ℃ and 200rpm for 48h, performing centrifugal separation at 15000rpm for 5min, collecting solid, washing by using absolute ethanol, and then drying in a vacuum oven at 40 ℃ for 4h to obtain the functional agent.
The preparation method of the acidified carbon nano tube comprises the following steps:
preparing a mixed solution by 90 weight percent of concentrated sulfuric acid and 65 weight percent of concentrated nitric acid according to the mass ratio of 3:1, mixing 100kg of the mixed solution with 1kg of carbon nano tubes at 200rpm, stirring for 1h, then adding 1000kg of water for dilution, filtering and collecting solids, and flushing with water to obtain the acidified carbon nano tubes.
Example 2
The preparation method of the fireproof flame-retardant shell substrate coating is basically the same as that of the example 1, and the only difference is that: the preparation method of the modified flame retardant is inconsistent.
The preparation method of the modified flame retardant comprises the following steps:
s1, adding 45g of pentaerythritol and 15g of n-butyl acrylate into 140g of 85wt% phosphoric acid aqueous solution, stirring at 800rpm at 105 ℃ for 4 hours, and carrying out reduced pressure distillation for 2 hours, wherein the reduced pressure is 5kPa, and the distillation temperature is 100 ℃ to obtain a compound;
s2, adding 15g of boric acid into 60g of polyethylene glycol 200, and stirring at 130 ℃ and 200rpm for 3 hours to obtain a reactant;
s3, adding 85g of the compound prepared in the step S1 into 15g of the reactant prepared in the step S2, stirring at 50 ℃ and 200rpm for 1h, and then heating to 115 ℃ and refluxing for 4h to obtain a liquid mixture;
and S4, adding 15g of the functional agent into the liquid mixture prepared in the step S3, stirring for 1h at 50 ℃ and 300rpm, then heating to 120 ℃ and stirring for 4h at 200rpm to obtain the modified flame retardant.
The functional agent was the same as in example 1.
The preparation method of the acidified carbon nanotubes is the same as in example 1.
Example 3
The preparation method of the fireproof flame-retardant shell substrate coating is basically the same as that of the example 1, and the only difference is that: the preparation method of the functional agent is inconsistent.
The preparation method of the functional agent comprises the following steps:
adding 1kg of acidified carbon nano tube into 100kg of 75wt% ethanol water solution, performing ultrasonic dispersion for 30min, adjusting the pH to 9 with 1mol/L sodium hydroxide water solution at the ultrasonic power of 300W and the ultrasonic frequency of 50kHz, stirring at 200rpm for 48h, performing centrifugal separation at 15000rpm for 5min, collecting solid, washing with absolute ethanol, and drying in a vacuum oven at 40 ℃ for 4h to obtain the functional agent.
The preparation method of the modified flame retardant is the same as that of example 1.
The preparation method of the acidified carbon nanotubes is the same as in example 1.
Example 4
The preparation method of the fireproof flame-retardant shell substrate coating is basically the same as that of the example 1, and the only difference is that: the functional agent is replaced by an equivalent amount of hybrid.
The preparation method of the hybrid comprises the following steps:
adding 1kg of hexagonal boron nitride into 160kg of 25wt% ethanol water solution, performing ultrasonic dispersion for 30min, wherein the ultrasonic power is 300W, the ultrasonic frequency is 50kHz, then adding 0.3kg of Tris buffer solution, then adjusting the pH to 8.5 by using 0.1mol/L sodium hydroxide water solution, then adding 0.4kg of dopamine hydrochloride, and reacting for 6h at 25 ℃ to obtain a suspension; then, 1kg of a silane coupling agent KH550 was added to the suspension, stirred at 200rpm at 60℃for 5 hours, centrifuged at 15000rpm for 5 minutes, and the solid was collected, washed with absolute ethanol and dried at 60℃for 3 hours to obtain a hybrid.
Comparative example 1
The preparation method of the fireproof flame-retardant shell substrate coating is basically the same as that of the example 1, and the only difference is that: the preparation method of the fireproof flame-retardant shell substrate coating is free from adding a modified flame retardant.
Test example 1
Fire-proof and flame-retardant performance test
Thermal insulation performance test: placing the steel plate coated with the shell substrate coating on an iron stand with the coating surface facing downwards, wherein the thickness of the coating is 0.5mm, placing an alcohol lamp in the center of the shell substrate coating, and recording the back surface temperatures of the steel plate for 2min, 5min and 10 min;
determination of Limiting Oxygen Index (LOI): the shell substrate coating is uniformly coated on wood strips with the size of 80mm multiplied by 10mm multiplied by 3mm according to the test of GB/T2406.2-2009 "Plastic Combustion Performance-oxygen index method", the coating thickness is 0.5mm, and each group of experiments are repeated 5 times;
UL94 vertical burn test: the vertical combustion tester is adopted to carry out experiments according to GB/T2408-2021 horizontal and vertical determination of plastic combustion performance, the wood strip size is 125mm multiplied by 13mm multiplied by 3mm, the shell substrate coating is uniformly coated on the wood strip, the coating thickness is 0.5mm, and each group of experiments are repeated for 5 times;
the results of the above tests are shown in Table 1.
Table 1: fire-proof and flame-retardant performance test results
( V0 assessment method: the sample rapidly self extinguishes to a non-flaming melt drip within 10 seconds after the flame is removed from ignition. The V1 assessment method is similar to V0 except that it requires a longer self-extinguishing time. This test allowed the melt to drip onto the cotton pad but not ignite the cotton. V2 is the same as V1 except that it allows the burning droplets to ignite cotton one foot below. V0 has best fireproof effect )
Test example 2
Adhesion Performance test
The adhesive force of the shell substrate coating is an important index for reacting the good performance of the coating film, and the coating film has better adhesive force and can be well adhered to the surface of the coated substrate, so that the decorative and fireproof effects of the fireproof coating can be better exerted.
The coated substrate selected for this test was a single ply plywood, size: 70mm multiplied by 50mm multiplied by 1mm, the surface of the test piece plate is flat and smooth, and no scar and obvious defect exists. Coating amount was 500g/m 2 And (5) drying at normal temperature for 24 hours after coating.
The method comprises the steps of fixing a sample piece on an operation platform of an adhesive force tester, rotating an instrument handle, enabling a stylus to make clockwise circular motion to scratch a paint film while the platform moves, enabling the paint film to be subjected to vertical external pressure and torsion generated by the rotating motion of a steel needle, enabling the stylus to scratch lines in the shape of overlapped circular rolling lines on a coating, loosening a bolt for fixing the sample piece after testing, sweeping paint film fragments on the sample piece by a brush, observing scratches on the paint film, and evaluating the adhesive force grade of the scratches. And (5) adhesive force grade assessment: according to the specification of GB/T1720-2020 paint film circle drawing test, the detection of the adhesion level aims at scoring on the upper side of a sample piece, 1-7 parts are marked on a round rolling line in sequence, the corresponding 7 levels are obtained, and then the integrity degree of each part is detected.
Each sample was tested 3 times. The most frequent grade was taken out and the test results are shown in Table 2.
Table 2: adhesion Performance test results
( If the paint film at the part 1 is intact, the paint film is rated as grade 1; the paint film at part 1 was damaged and part 2 was intact, rated as 2. And so on, stage 7 is the worst result. )
From the test results of test examples 1 and 2, it can be seen that the fireproof and flame retardant properties and the adhesive force properties of example 1 are best, probably because the sepiolite of the present invention is introduced to facilitate the generation of more crosslinked structures and aromatic structures in the condensed phase, to generate more thermally stable and dense char, and to resist heat transfer, thereby enhancing the barrier effect and thermal stability of the char. During combustion, the coating begins to separateTo decompose and release non-combustible gas (NH) 3 And H 2 O). The main decomposition products of the coating are triazines, polyphosphates and derivatives thereof. As the temperature increases, the triazine compound and the phosphorus-containing compound form an expansion precursor through aromatization, cyclization and crosslinking reactions. With the release of non-combustible gases, these gases may dilute the combustible gases and cause further expansion of the precursor. Then, an expanded carbon layer is formed to cover the surface of the base material, and the generated carbon can effectively isolate heat, oxygen and combustible gas between the combustion zone and the base material, so that the heat insulation, flame retardance and smoke suppression effects are super strong. Sepiolite and liquid mixtures have excellent synergistic effects in coatings, mainly due to the formation of more crosslinked and aromatic structures in the condensed phase, resulting in a denser and expanded char layer during combustion, which resists penetration of heat and volatile products.
Coating hexagonal boron nitride with dopamine hydrochloride can improve reactivity and also improve dispersibility in water. The silane coupling agent KH550 is used as bridging agent, and the acidified carbon nano-tube is connected with the hybrid to prepare the functional agent. The shell substrate coating after combustion presents a compact and uniform carbon skeleton network structure. The carbon skeleton structure plays a good role in supporting the carbon layer, increases the flame impact resistance, and enhances the strength of the carbon layer. The increase of the carbon content and strength is beneficial to reducing heat transfer, thereby obtaining good heat insulation and flame retardant effects, combining grafted sepiolite to obtain a compact and complete surface structure with a plurality of honeycomb bubbles inside, carbon nano tubes tend to form a continuous reticular structure in the combustion process, and play a role of supporting a framework frame of carbon in the carbon layer forming process so as to fill carbon gaps. In addition, the formation of the silicon network also strengthens the carbon layer. In the combustion process, hexagonal boron nitride is bonded on the surface of the network structure, so that the support of a carbon network is enhanced, carbonization of a coating matrix is promoted, and the entry of combustible gas in the combustion process is prevented. In addition, the anisotropic heat transfer of hexagonal boron nitride planar heat dissipation and vertical surface heat preservation increases the diffusion of heat, so that the coating is heated more uniformly. In conclusion, the shell substrate coating disclosed by the invention is favorable for forming a continuous and stable carbon layer, effectively inhibits and blocks heat transfer generated by released inflammable products and flame, and has good coating adhesive force.
Claims (9)
1. The fireproof flame-retardant shell substrate coating is characterized by comprising the following components: shell powder, a diluent, an auxiliary agent, a filler, a modified flame retardant and a base resin;
the preparation method of the modified flame retardant comprises the following steps:
s1, adding pentaerythritol and n-butyl acrylate into a phosphoric acid aqueous solution, stirring, and performing reduced pressure distillation to obtain a compound;
s2, adding boric acid into the polyethylene glycol 200, and stirring to obtain a reactant;
s3, adding the compound prepared in the step S1 into the reactant prepared in the step S2, stirring, and then heating and refluxing to obtain a liquid mixture;
s4, adding sepiolite into water, performing ultrasonic dispersion at room temperature, filtering, drying, collecting solids, adding the solids and the functional agent into the liquid mixture prepared in the step S3, stirring, and heating and stirring to obtain the modified flame retardant;
the functional agent is a hexagonal boron nitride/carbon nano tube composite material;
the preparation method of the hexagonal boron nitride/carbon nano tube composite material comprises the following steps of:
z1, adding 0.5-2 parts of hexagonal boron nitride into 150-170 parts of 20-30wt% ethanol aqueous solution, performing ultrasonic dispersion for 20-40 min, wherein the ultrasonic power is 200-500W, the ultrasonic frequency is 40-60 kHz, then adding 0.1-0.5 part of Tris buffer solution, then adjusting the pH to 8.0-9.0 by using 0.05-0.2 mol/L sodium hydroxide aqueous solution, then adding 0.2-0.6 part of dopamine hydrochloride, and reacting for 2-10 h at 20-30 ℃ to obtain suspension; then adding 0.5-2 parts of a silane coupling agent KH550 into the suspension, stirring for 3-7 hours at 50-70 ℃ and 100-300 rpm, centrifugally separating for 2-10 minutes at 10000-20000 rpm, collecting solids, washing with absolute ethyl alcohol, and drying for 1-5 hours at 50-70 ℃ to obtain a hybrid;
z2, adding 0.5-2 parts of acidified carbon nano tubes into 80-120 parts of 70-85 wt% ethanol water solution, performing ultrasonic dispersion for 20-40 min, wherein the ultrasonic power is 200-500W, the ultrasonic frequency is 40-60 kHz, adding 0.1-0.5 part of the hybrid prepared in the step Z1 under the protection of nitrogen, adjusting the pH value to 8.5-9.5 by using 0.5-2 mol/L sodium hydroxide water solution, stirring at 50-60 ℃ at 100-300 rpm for 24-72 h, centrifuging at 10000-20000 rpm for 2-10 min, collecting solids, washing with absolute ethanol, and drying in a vacuum oven at 30-50 ℃ for 2-6 h to obtain a functional agent;
the preparation method of the acidified carbon nano tube comprises the following steps of:
88-98 wt% of concentrated sulfuric acid and 60-69 wt% of concentrated nitric acid are prepared into a mixed solution according to the mass ratio of 2-4:1, 80-120 parts of the mixed solution and 0.5-2 parts of carbon nano tubes are mixed for 100-500 rpm and stirred for 0.5-2 hours, then 500-1500 parts of water is added for dilution, the solid is collected by filtration, and the acidified carbon nano tubes are obtained by flushing with water.
2. The fire-resistant and flame-retardant shell-based coating as claimed in claim 1, comprising the following components in parts by weight: 30-50 parts of shell powder, 15-25 parts of diluent, 3-8 parts of auxiliary agent, 10-20 parts of filler, 20-30 parts of modified flame retardant and 20-40 parts of base resin.
3. A fire-retardant shell substrate coating according to claim 1 or 2, wherein the diluent is at least one of water, isopropanol, butanol, ethanol, acetone, ketone, propylene glycol, ethylene glycol.
4. A fire-retardant shell substrate coating as claimed in claim 1 or claim 2, wherein the auxiliary agent is at least one of a thickener, a toughening agent and a defoamer.
5. The fireproof flame-retardant shell substrate coating according to claim 4, wherein the auxiliary agent is a thickener and an antifoaming agent according to a mass ratio of 1-3: 2-4, mixing;
the thickener is at least one of montmorillonite, magnesium silicate, talcum powder, hydroxypropyl methyl cellulose, hydroxypropyl cellulose, methyl cellulose, polyacrylamide, polyvinyl alcohol and sodium silicate;
the defoaming agent is at least one of ethoxymethyl silicone oil, methyl silicone oil, polysiloxane, polyether silicone oil, fatty alcohol polyoxyethylene ether, polyoxyethylene stearate, alkylphenol fatty alcohol polyoxyethylene ether and stearic acid.
6. A fire-retardant shell substrate coating according to claim 1 or 2, wherein the filler is at least one of mica powder, calcium silicate, calcium carbonate, silica.
7. A fire-retardant shell substrate coating as claimed in claim 1 or 2, wherein the modified flame retardant is prepared by the following steps in parts by weight:
s1, adding 40-50 parts of pentaerythritol and 10-20 parts of n-butyl acrylate into 130-150 parts of 85-90 wt% phosphoric acid aqueous solution, stirring at 100-110 ℃ for 3-5 hours at 500-1000 rpm, and carrying out reduced pressure distillation for 1-3 hours at a reduced pressure of 1-10 kPa and a distillation temperature of 90-100 ℃ to obtain a compound;
s2, adding 10-20 parts of boric acid into 50-70 parts of polyethylene glycol 200, and stirring at 120-140 ℃ and 100-300 rpm for 1-5 hours to obtain a reactant;
s3, adding 80-90 parts of the compound prepared in the step S1 into 10-20 parts of the reactant prepared in the step S2, stirring at 40-60 ℃ and 100-300 rpm for 0.5-2 h, and then heating to 110-120 ℃ and refluxing for 2-6 h to obtain a liquid mixture;
s4, adding 30-50 parts of sepiolite into 900-1100 parts of water, performing ultrasonic dispersion for 0.5-2 hours at room temperature, wherein the ultrasonic power is 200-500W, the ultrasonic frequency is 40-60 kHz, then filtering and drying for 20-30 hours at 50-70 ℃ through a 100-300 mesh screen, collecting solids, adding the solids and 10-20 parts of functional agents into the liquid mixture prepared in the step S3, stirring for 0.5-2 hours at 40-60 ℃ at 100-500 rpm, and then heating to 110-130 ℃ and stirring for 2-6 hours at 100-300 rpm to obtain a modified flame retardant; the functional agent is hexagonal boron nitride/carbon nano tube composite material.
8. The fire-retardant shell substrate coating according to claim 1 or 2, wherein the base resin is at least one of methyl acrylate, ethyl acrylate, bisphenol a epoxy resin, aliphatic epoxy resin, phenolic alkyd resin, phenolic aldehyde acid resin, aqueous polyurethane resin, polyether polyurethane resin.
9. A method for preparing the fireproof flame-retardant shell substrate coating according to any one of claims 1-8, which is characterized by comprising the following steps:
step 1, adding a diluent and an auxiliary agent into base resin, and stirring at 100-500 rpm for 1-3 hours to prepare slurry;
step 2, adding shell powder into the slurry prepared in the step 1, and stirring at 800-1500 rpm for 0.5-2 h to prepare a base material;
and step 3, adding the filler and the modified flame retardant into the base material obtained in the step 2, and stirring for 1-10 hours at 50-300 rpm to obtain the shell substrate coating.
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