A Class A2 flame-retardant aluminum composite panel core material and its preparation method

Abstract

This invention discloses an A2-grade flame-retardant aluminum composite panel core material and its preparation method. The flame-retardant aluminum composite panel core material comprises the following raw materials in parts by weight: 10-12 parts of matrix resin, 85-90 parts of flame retardant, 0.5-1.5 parts of flame retardant synergist, 0.01-0.03 parts of benzoyl peroxide, 1-2 parts of anionic surfactant, 2-4 parts of compatibilizer, 1-2 parts of antioxidant, and 0.5-1.5 parts of antibacterial agent. The aluminum composite panel core material contains a flame retardant, which decomposes upon heating during combustion, releasing water vapor, absorbing a large amount of heat, reducing the surface temperature of the material, and diluting the concentration of oxygen and combustible gases. At the same time, it forms a "worm-like" fluffy char layer that effectively insulates against heat and oxygen and prevents combustibles from escaping. The addition of the flame retardant synergist promotes further densification of the formed char layer, preventing the char layer from burning through or falling off, further improving the flame-retardant effect of the aluminum composite panel core material, achieving a flame-retardant grade of A2.

Description

Technical Field

[0001] This invention relates to the field of aluminum composite panel core materials, specifically to an A2 grade flame-retardant aluminum composite panel core material and its preparation method. Background Technology

[0002] Aluminum composite panels (ACPs), as a new type of composite decorative material, combine the advantages of both materials. Their core material is a low-density plastic sheet, significantly reducing the material's weight. Compared to aluminum of the same thickness, it weighs only 1 / 9 of an aluminum sheet and less than 1 / 4 of a steel sheet of the same thickness, meeting the requirements of modern high-rise buildings for reducing building load. It also possesses the advantages of aluminum, such as heat insulation, aesthetics, and a high-end appearance. ACPs are widely used in building curtain walls, interior and exterior decoration, advertising signs, vehicle and ship decoration, and furniture manufacturing due to their advanced composite material structure and characteristics, excellent cost-effectiveness and ease of processing, diverse decorative effects and durability, and significant resource conservation and environmental friendliness. While ACPs are frequently used in landmark buildings such as airports, large stadiums, and theaters, their plastic core material makes them flammable, thus reducing their safety. Summary of the Invention

[0003] The purpose of this invention is to provide an A2-grade flame-retardant aluminum composite panel core material and its preparation method, which solves the problem that the flame-retardant rating of aluminum composite panel core materials cannot reach the A-grade level at present.

[0004] The objective of this invention can be achieved through the following technical solutions:

[0005] A method for preparing A2-grade flame-retardant aluminum composite panel core material specifically includes the following steps:

[0006] Step a1: Mix diphenyl phosphate and toluene, purge with nitrogen, stir and add dimethylchlorosilane at 150-200 r / min and 0℃, and react for 6-8 h at 30-40℃ to obtain silicon-containing phosphate. Mix silicon-containing phosphate, allyl alcohol, chloroplatinic acid and DMF, purge with nitrogen, and react for 3-5 h at 120-150 r / min and 80-85℃ to obtain flame retardant additive.

[0007] Step a2: Mix cyanuric chloride and tetrahydrofuran, purge with nitrogen, stir at 200-300 r / min and 0-5℃, add flame retardant additive and triethylamine, react for 3-4 h, add synergistic monomer, heat to 50-60℃, react for 6-8 h, add 4-maleimide-phenol, heat to 90-100℃, react for 8-10 h to obtain flame retardant synergist;

[0008] Step a3: Weigh the following raw materials by weight: 10-12 parts of matrix resin, 85-90 parts of flame retardant, 0.5-1.5 parts of flame retardant synergist, 0.01-0.03 parts of benzoyl peroxide, 1-2 parts of anionic surfactant, 2-4 parts of compatibilizer, 1-2 parts of antioxidant and 0.5-1.5 parts of antibacterial agent. Mix the raw materials and melt-blend them under the conditions of 60-80 r / min and 190-200℃, then press them into molds to obtain the flame-retardant aluminum composite panel core material.

[0009] Furthermore, in step a1, the molar ratio of diphenyl phosphate and dimethylchlorosilane is 1:1, the molar ratio of silanized phosphate and allyl alcohol is 1:1, and the amount of chloroplatinic acid used is 0.01% of the mass of allyl alcohol.

[0010] Furthermore, the molar ratio of cyanuric chloride, flame retardant additive, triethylamine, synergist monomer and 4-maleimide-based phenol in step a2 is 2:2:6:1:2.

[0011] Furthermore, the matrix resin mentioned in step a3 is prepared by blending low-density polyethylene, polypropylene, ethylene-octene copolymer and ethylene-ethyl acrylate in a mass ratio of 6:2:1:1, and the flame retardant is prepared by blending magnesium hydroxide and expandable graphite in a mass ratio of 6:1. The flame retardant aluminum composite panel core material can be made into a flat plate or a honeycomb shape.

[0012] Furthermore, the synergistic monomer is prepared by the following steps:

[0013] Step b1: Mix DOPO, formaldehyde solution and anhydrous ethanol evenly, and react for 8-10 h at a speed of 150-200 r / min and a temperature of 80-85℃ to obtain intermediate 1. Mix intermediate 1 with acetonitrile, purge with nitrogen, and stir and add triethylamine at a speed of 120-150 r / min and a temperature of 0℃. After stirring for 1-1.5 h, add acryloyl chloride, raise the temperature to 20-25℃, and react for 10-15 h to obtain intermediate 2. Mix intermediate 2, bis(2-mercaptoethyl)amine, benzophenone and DMF, and react for 20-30 min at a speed of 120-150 r / min, a temperature of 20-25℃, and under ultraviolet irradiation to obtain the modifier.

[0014] Step b2: Mix phenyltrimethoxysilane, isopropanol, deionized water and sodium hydroxide evenly, purge with nitrogen, and react for 3-5 hours at a speed of 150-200 r / min and a temperature of 85-88℃. Cool down to 20-25℃ and continue the reaction for 10-15 hours to obtain sodium octaphenyltetrasiloxane tetrasilanolate. Mix sodium octaphenyltetrasiloxane tetrasilanolate, triethylamine and tetrahydrofuran, purge with nitrogen, and stir and add methyldichlorosilane at a speed of 120-150 r / min and a temperature of 0℃ to obtain dihydrocage-type silsesquioxane.

[0015] Step b3: Mix dihydro-cage-type silsesquioxane, allyl alcohol glycidyl ether, caster catalyst and toluene evenly, purge with nitrogen, and react for 10-15 h at a rotation speed of 150-200 r / min and a temperature of 80-85℃ to obtain pretreated cage-type silsesquioxane. Mix the pretreated cage-type silsesquioxane, modifier, triphenylphosphine and tetrahydrofuran, and react for 10-12 h at a rotation speed of 200-300 r / min and a temperature of 70-75℃ to obtain synergistic monomer.

[0016] Furthermore, in step b1, the ratio of DOPO to formaldehyde solution is 1 mol: 80 mL, the formaldehyde solution has a mass fraction of 37%, the molar ratio of intermediate 1, acryloyl chloride and triethylamine is 1:1.1:1.2, the molar ratio of intermediate 2 and bis(2-mercaptoethyl)amine is 2:1, and the amount of benzophenone used is 0.2% of the mass of bis(2-mercaptoethyl)amine.

[0017] Furthermore, in step b2, the ratio of phenyltrimethoxysilane, isopropanol, deionized water, and sodium hydroxide is 6 mmol:6 mmol:7 mL:4 mmol, and the mass ratio of octaphenyltetrasiloxane tetrasilanolate sodium, triethylamine, and methyldichlorosilane is 11:4.5:3.5.

[0018] Furthermore, in step b3, the molar ratio of dihydro-cage silsesquioxane to allyl alcohol glycidyl ether is 1:2, the amount of caster catalyst is 0.01% of the mass of allyl alcohol glycidyl ether, the molar ratio of pretreated cage silsesquioxane to modifier is 1:2, and the amount of triphenylphosphine is 3% of the mass of modifier.

[0019] The beneficial effects of this invention: This invention discloses an A2-grade flame-retardant aluminum composite panel core material, comprising a matrix resin, a flame retardant, a flame retardant synergist, benzoyl peroxide, an anionic surfactant, a compatibilizer, an antioxidant, and an antibacterial agent. The flame retardant synergist is made from diphenyl phosphate and dimethylchlorosilane, where the P-OH on diphenyl phosphate reacts with the Si-Cl on dimethylchlorosilane to obtain a silica-containing phosphate. The silica-containing phosphate is then reacted with allyl alcohol, where the Si-H bonds on the silica-containing phosphate react with the double bonds on the allyl alcohol to obtain a flame retardant additive. Cyanide chloride is then reacted with the flame retardant additive, where the chlorine atom sites on the cyanide chloride react with the hydroxyl groups on the flame retardant additive. A synergistic monomer is then added, where the hydroxyl groups on the synergistic monomer react with the chlorine atom sites. Finally, 4-maleimide-phenol is added, where the phenolic hydroxyl groups on the 4-maleimide-phenol react with the remaining chlorine atom sites to obtain the flame retardant synergist.

[0020] The synergistic monomer was prepared by nucleophilic addition reaction of DOPO and formaldehyde solution to obtain intermediate 1. Intermediate 1 was reacted with acryloyl chloride, causing the hydroxyl group on intermediate 1 to react with the acryl chloride on acryloyl chloride, to obtain intermediate 2. Intermediate 2 was reacted with bis(2-mercaptoethyl)amine under ultraviolet irradiation in the presence of benzophenone, causing the double bond on intermediate 2 to react with the mercapto group on bis(2-mercaptoethyl)amine, to obtain the modifier. Phenylacetyltrimethoxysilane was hydrolyzed and condensed to obtain sodium octaphenyltetrasiloxane tetrasilanolate. Sodium octaphenyltetrasiloxane tetrasilanolate and methyl... The dichlorosilane reaction causes the sodium silanolate on octaphenyltetrasiloxane tetrasilanolate to react with the Si-Cl bond on methyldichlorosilane, yielding a dihydrocage-type silsesquioxane. The dihydrocage-type silsesquioxane is then reacted with allyl glycidyl ether, causing the Si-H bond on the dihydrocage-type silsesquioxane to react with the double bond on the allyl glycidyl ether, yielding a pretreated cage-type silsesquioxane. Finally, the pretreated cage-type silsesquioxane is reacted with a modifier, causing the epoxy group on the pretreated cage-type silsesquioxane to react with the secondary amine on the modifier, forming a new hydroxyl group, thus yielding a synergistic monomer.

[0021] The core material of this aluminum composite panel contains flame retardants. When burned, it decomposes upon heating, releasing water vapor, absorbing a large amount of heat, and lowering the surface temperature of the material. The water vapor also dilutes the concentration of oxygen and combustible gases, while forming a loose, worm-like char layer that effectively insulates against heat and oxygen and prevents combustibles from escaping. The addition of flame retardant enhancers generates highly dehydrating substances such as phosphoric acid and polymetaphosphoric acid, promoting the dehydration and carbonization of the polymer surface. The cage-like silsesquioxane structure within the molecule further densifies the formed char layer, preventing it from burning through or peeling off, thus further enhancing the flame retardant effect of the aluminum composite panel core material. Detailed Implementation

[0022] The technical solutions in the embodiments of the present invention will be clearly and completely described below. Obviously, the described embodiments are only some embodiments of the present invention, and not all embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those skilled in the art without creative effort are within the scope of protection of the present invention.

[0023] Example 1: A method for preparing A2-grade flame-retardant aluminum composite panel core material, specifically including the following steps:

[0024] Step a1: Diphenyl phosphate and toluene are mixed, and nitrogen gas is introduced for protection. Under the conditions of 150 r / min and 0℃, dimethylchlorosilane is added and the mixture is heated to 30℃ for 6 h to obtain silicon-containing phosphate. Silicon-containing phosphate, allyl alcohol, chloroplatinic acid and DMF are mixed, and nitrogen gas is introduced for protection. Under the conditions of 120 r / min and 80℃, the mixture is reacted for 3 h to obtain flame retardant additive.

[0025] Step a2: Mix cyanuric chloride and tetrahydrofuran, purge with nitrogen, stir at 200 r / min and 0℃, add flame retardant additive and triethylamine, react for 3 h, add synergistic monomer, heat to 50℃ and react for 6 h, add 4-maleimide-based phenol, heat to 90℃ and react for 8 h to obtain flame retardant synergist;

[0026] Step a3: Weigh the following raw materials by weight: 10 parts of matrix resin, 85 parts of flame retardant, 0.5 parts of flame retardant synergist, 0.01 parts of benzoyl peroxide, 1 part of anionic surfactant, 2 parts of compatibilizer, 1 part of antioxidant and 0.5 parts of antibacterial agent. Mix the raw materials, melt-blend them at a speed of 60 r / min and a temperature of 190℃, and then press them into molds to obtain flame-retardant aluminum composite panel core material.

[0027] In step a1, the molar ratio of diphenyl phosphate and dimethylchlorosilane is 1:1, the molar ratio of silanized phosphate and allyl alcohol is 1:1, and the amount of chloroplatinic acid used is 0.01% of the mass of allyl alcohol.

[0028] The molar ratio of cyanuric chloride, flame retardant additive, triethylamine, synergist monomer and 4-maleimide-based phenol in step a2 is 2:2:6:1:2.

[0029] The matrix resin mentioned in step a3 is prepared by blending low-density polyethylene, polypropylene, ethylene-octene copolymer and ethylene-ethyl acrylate in a mass ratio of 6:2:1:1. The low-density polyethylene is model M2320, the polypropylene is model K8003, the ethylene-octene copolymer is model 871L, and the ethylene-ethyl acrylate is model 4720. The flame retardant is prepared by blending magnesium hydroxide and expandable graphite in a mass ratio of 6:1. The expandable graphite has a particle size of 270μm and an expansion ratio of 350mL / g. The compatibilizer is model PE-12H and PE-12L. The antioxidant is model 1010 and 1076. The antibacterial agent is model JL-1086 and LF-106.

[0030] The synergistic monomer is prepared by the following steps:

[0031] Step b1: Mix DOPO, formaldehyde solution and anhydrous ethanol evenly, and react for 8 hours at 150 r / min and 80℃ to obtain intermediate 1. Mix intermediate 1 with acetonitrile, purge with nitrogen, and stir and add triethylamine at 120 r / min and 0℃. After stirring for 1 hour, add acryloyl chloride, raise the temperature to 20℃ and react for 10 hours to obtain intermediate 2. Mix intermediate 2, bis(2-mercaptoethyl)amine, benzophenone and DMF, and react for 20 minutes at 120 r / min and 20℃ under ultraviolet irradiation to obtain the modifier.

[0032] Step b2: Mix phenyltrimethoxysilane, isopropanol, deionized water and sodium hydroxide evenly, purge with nitrogen, and react for 3 hours at 150 r / min and 85°C. Then cool to 20°C and continue the reaction for 10 hours to obtain sodium octaphenyltetrasiloxane tetrasilanolate. Mix sodium octaphenyltetrasiloxane tetrasilanolate, triethylamine and tetrahydrofuran, purge with nitrogen, and stir and add methyldichlorosilane at 120 r / min and 0°C for 3 hours to obtain dihydrocage-type silsesquioxane.

[0033] Step b3: Dihydrocage-type silsesquioxane, allyl alcohol glycidyl ether, caster catalyst and toluene are mixed evenly, and nitrogen gas is introduced for protection. The mixture is reacted for 10 h at a rotation speed of 150 r / min and a temperature of 80 °C to obtain pretreated cage-type silsesquioxane. The pretreated cage-type silsesquioxane, modifier, triphenylphosphine and tetrahydrofuran are mixed and reacted for 10 h at a rotation speed of 200 r / min and a temperature of 70 °C to obtain synergistic monomer.

[0034] In step b1, the ratio of DOPO to formaldehyde solution is 1 mol: 80 mL, the formaldehyde solution has a mass fraction of 37%, the molar ratio of intermediate 1, acryloyl chloride and triethylamine is 1:1.1:1.2, the molar ratio of intermediate 2 and bis(2-mercaptoethyl)amine is 2:1, and the amount of benzophenone used is 0.2% of the mass of bis(2-mercaptoethyl)amine.

[0035] The ratio of phenyltrimethoxysilane, isopropanol, deionized water and sodium hydroxide used in step b2 is 6 mmol:6 mmol:7 mL:4 mmol, and the mass ratio of octaphenyltetrasiloxane tetrasilanolate sodium, triethylamine and methyldichlorosilane is 11:4.5:3.5.

[0036] In step b3, the molar ratio of dihydro-cage silsesquioxane to allyl alcohol glycidyl ether is 1:2, the amount of caster catalyst is 0.01% of the mass of allyl alcohol glycidyl ether, the molar ratio of pretreated cage silsesquioxane to modifier is 1:2, and the amount of triphenylphosphine is 3% of the mass of modifier.

[0037] Example 2, a method for preparing A2-grade flame-retardant aluminum composite panel core material, specifically includes the following steps:

[0038] Step a1: Diphenyl phosphate and toluene are mixed, and nitrogen gas is introduced for protection. Under the conditions of 150 r / min and 0℃, dimethylchlorosilane is added and the mixture is heated to 35℃ for 7 h to obtain silicon-containing phosphate. Silicon-containing phosphate, allyl alcohol, chloroplatinic acid and DMF are mixed, and nitrogen gas is introduced for protection. Under the conditions of 120 r / min and 85℃, the mixture is reacted for 4 h to obtain flame retardant additive.

[0039] Step a2: Mix cyanuric chloride and tetrahydrofuran, purge with nitrogen, stir at 200 r / min and 5°C, add flame retardant additive and triethylamine, react for 3 h, add synergistic monomer, heat to 55°C and react for 7 h, add 4-maleimide-based phenol, heat to 95°C and react for 9 h to obtain flame retardant synergist;

[0040] Step a3: Weigh the following raw materials by weight: 11 parts of matrix resin, 88 parts of flame retardant, 1 part of flame retardant synergist, 0.02 parts of benzoyl peroxide, 1.5 parts of anionic surfactant, 3 parts of compatibilizer, 1.5 parts of antioxidant and 1 part of antibacterial agent. Mix the raw materials, melt-blend them at a speed of 60 r / min and a temperature of 195℃, and then press them into molds to obtain the flame-retardant aluminum composite panel core material.

[0041] In step a1, the molar ratio of diphenyl phosphate and dimethylchlorosilane is 1:1, the molar ratio of silanized phosphate and allyl alcohol is 1:1, and the amount of chloroplatinic acid used is 0.01% of the mass of allyl alcohol.

[0042] The molar ratio of cyanuric chloride, flame retardant additive, triethylamine, synergist monomer and 4-maleimide-based phenol in step a2 is 2:2:6:1:2.

[0043] The matrix resin mentioned in step a3 is prepared by blending low-density polyethylene, polypropylene, ethylene-octene copolymer and ethylene-ethyl acrylate in a mass ratio of 6:2:1:1. The low-density polyethylene is model M2320, the polypropylene is model K8003, the ethylene-octene copolymer is model 871L, and the ethylene-ethyl acrylate is model 4720. The flame retardant is prepared by blending magnesium hydroxide and expandable graphite in a mass ratio of 6:1. The expandable graphite has a particle size of 270μm and an expansion ratio of 350mL / g. The compatibilizer is model PE-12H and PE-12L. The antioxidant is model 1010 and 1076. The antibacterial agent is model JL-1086 and LF-106.

[0044] The synergistic monomer is prepared by the following steps:

[0045] Step b1: Mix DOPO, formaldehyde solution and anhydrous ethanol evenly, and react for 9 h at 150-200 r / min and 80℃ to obtain intermediate 1. Mix intermediate 1 with acetonitrile, purge with nitrogen, and stir at 150 r / min and 0℃ while adding triethylamine. After stirring for 1.3 h, add acryloyl chloride, raise the temperature to 25℃ and react for 13 h to obtain intermediate 2. Mix intermediate 2, bis(2-mercaptoethyl)amine, benzophenone and DMF, and react for 25 min at 150 r / min and 20℃ under ultraviolet irradiation to obtain the modifier.

[0046] Step b2: Mix phenyltrimethoxysilane, isopropanol, deionized water and sodium hydroxide evenly, purge with nitrogen, and react for 4 hours at 200 r / min and 85°C. Then cool to 20°C and continue the reaction for 15 hours to obtain sodium octaphenyltetrasiloxane tetrasilanolate. Mix sodium octaphenyltetrasiloxane tetrasilanolate, triethylamine and tetrahydrofuran, purge with nitrogen, and stir and add methyldichlorosilane at 120 r / min and 0°C for 4 hours to obtain dihydrocage-type silsesquioxane.

[0047] Step b3: Dihydrocage-type silsesquioxane, allyl alcohol glycidyl ether, caster catalyst and toluene are mixed evenly, and nitrogen gas is introduced for protection. The reaction is carried out for 13 hours at a speed of 200 r / min and a temperature of 80 °C to obtain pretreated cage-type silsesquioxane. The pretreated cage-type silsesquioxane, modifier, triphenylphosphine and tetrahydrofuran are mixed and reacted for 11 hours at a speed of 300 r / min and a temperature of 70 °C to obtain synergistic monomer.

[0048] In step b1, the ratio of DOPO to formaldehyde solution is 1 mol: 80 mL, the formaldehyde solution has a mass fraction of 37%, the molar ratio of intermediate 1, acryloyl chloride and triethylamine is 1:1.1:1.2, the molar ratio of intermediate 2 and bis(2-mercaptoethyl)amine is 2:1, and the amount of benzophenone used is 0.2% of the mass of bis(2-mercaptoethyl)amine.

[0049] The ratio of phenyltrimethoxysilane, isopropanol, deionized water and sodium hydroxide used in step b2 is 6 mmol:6 mmol:7 mL:4 mmol, and the mass ratio of octaphenyltetrasiloxane tetrasilanolate sodium, triethylamine and methyldichlorosilane is 11:4.5:3.5.

[0050] In step b3, the molar ratio of dihydro-cage silsesquioxane to allyl alcohol glycidyl ether is 1:2, the amount of caster catalyst is 0.01% of the mass of allyl alcohol glycidyl ether, the molar ratio of pretreated cage silsesquioxane to modifier is 1:2, and the amount of triphenylphosphine is 3% of the mass of modifier.

[0051] Example 3, a method for preparing A2-grade flame-retardant aluminum composite panel core material, specifically includes the following steps:

[0052] Step a1: Diphenyl phosphate and toluene are mixed, and nitrogen gas is introduced for protection. Under the conditions of 200 r / min and 0℃, dimethylchlorosilane is added while stirring. The mixture is then heated to 40℃ and reacted for 8 hours to obtain a silicon-containing phosphate. The silicon-containing phosphate, allyl alcohol, chloroplatinic acid and DMF are mixed, and nitrogen gas is introduced for protection. Under the conditions of 150 r / min and 85℃, the mixture is reacted for 5 hours to obtain a flame retardant additive.

[0053] Step a2: Mix cyanuric chloride and tetrahydrofuran, purge with nitrogen, stir at 300 r / min and 5°C, add flame retardant additive and triethylamine, react for 4 h, add synergistic monomer, heat to 60°C and react for 8 h, add 4-maleimide-based phenol, heat to 100°C and react for 10 h to obtain flame retardant synergist;

[0054] Step a3: Weigh the following raw materials by weight: 12 parts of matrix resin, 90 parts of flame retardant, 1.5 parts of flame retardant synergist, 0.03 parts of benzoyl peroxide, 2 parts of anionic surfactant, 4 parts of compatibilizer, 2 parts of antioxidant and 1.5 parts of antibacterial agent. Mix the raw materials, melt-blend them at a speed of 80 r / min and a temperature of 200℃, and then press them into molds to obtain the flame-retardant aluminum composite panel core material.

[0055] In step a1, the molar ratio of diphenyl phosphate and dimethylchlorosilane is 1:1, the molar ratio of silanized phosphate and allyl alcohol is 1:1, and the amount of chloroplatinic acid used is 0.01% of the mass of allyl alcohol.

[0056] The molar ratio of cyanuric chloride, flame retardant additive, triethylamine, synergist monomer and 4-maleimide-based phenol in step a2 is 2:2:6:1:2.

[0057] The matrix resin mentioned in step a3 is prepared by blending low-density polyethylene, polypropylene, ethylene-octene copolymer and ethylene-ethyl acrylate in a mass ratio of 6:2:1:1. The low-density polyethylene is model M2320, the polypropylene is model K8003, the ethylene-octene copolymer is model 871L, and the ethylene-ethyl acrylate is model 4720. The flame retardant is prepared by blending magnesium hydroxide and expandable graphite in a mass ratio of 6:1. The expandable graphite has a particle size of 270μm and an expansion ratio of 350mL / g. The compatibilizer is model PE-12H and PE-12L. The antioxidant is model 1010 and 1076. The antibacterial agent is model JL-1086 and LF-106.

[0058] The synergistic monomer is prepared by the following steps:

[0059] Step b1: Mix DOPO, formaldehyde solution and anhydrous ethanol evenly, and react for 10 h at 200 r / min and 85 °C to obtain intermediate 1. Mix intermediate 1 with acetonitrile, purge with nitrogen, and stir and add triethylamine at 150 r / min and 0 °C. After stirring for 1.5 h, add acryloyl chloride, raise the temperature to 25 °C and react for 15 h to obtain intermediate 2. Mix intermediate 2, bis(2-mercaptoethyl)amine, benzophenone and DMF, and react for 30 min at 150 r / min, 25 °C and ultraviolet irradiation to obtain the modifier.

[0060] Step b2: Mix phenyltrimethoxysilane, isopropanol, deionized water and sodium hydroxide evenly, purge with nitrogen, and react for 5 hours at 200 r / min and 88°C. Then cool to 25°C and continue the reaction for 15 hours to obtain sodium octaphenyltetrasiloxane tetrasilanolate. Mix sodium octaphenyltetrasiloxane tetrasilanolate, triethylamine and tetrahydrofuran, purge with nitrogen, and stir and add methyldichlorosilane at 150 r / min and 0°C for 5 hours to obtain dihydrocage-type silsesquioxane.

[0061] Step b3: Dihydrocage-type silsesquioxane, allyl alcohol glycidyl ether, caster catalyst and toluene are mixed evenly, and nitrogen gas is introduced for protection. The mixture is reacted for 15 h at a rotation speed of 200 r / min and a temperature of 85 °C to obtain pretreated cage-type silsesquioxane. The pretreated cage-type silsesquioxane, modifier, triphenylphosphine and tetrahydrofuran are mixed and reacted for 12 h at a rotation speed of 300 r / min and a temperature of 75 °C to obtain synergistic monomer.

[0062] In step b1, the ratio of DOPO to formaldehyde solution is 1 mol: 80 mL, the formaldehyde solution has a mass fraction of 37%, the molar ratio of intermediate 1, acryloyl chloride and triethylamine is 1:1.1:1.2, the molar ratio of intermediate 2 and bis(2-mercaptoethyl)amine is 2:1, and the amount of benzophenone used is 0.2% of the mass of bis(2-mercaptoethyl)amine.

[0063] The ratio of phenyltrimethoxysilane, isopropanol, deionized water and sodium hydroxide used in step b2 is 6 mmol:6 mmol:7 mL:4 mmol, and the mass ratio of octaphenyltetrasiloxane tetrasilanolate sodium, triethylamine and methyldichlorosilane is 11:4.5:3.5.

[0064] In step b3, the molar ratio of dihydro-cage silsesquioxane to allyl alcohol glycidyl ether is 1:2, the amount of caster catalyst is 0.01% of the mass of allyl alcohol glycidyl ether, the molar ratio of pretreated cage silsesquioxane to modifier is 1:2, and the amount of triphenylphosphine is 3% of the mass of modifier.

[0065] Example 4: The flame-retardant aluminum composite panel core material obtained in Example 1 was hot-pressed into a plate-shaped material.

[0066] Example 5: The flame-retardant aluminum composite panel core material obtained in Example 1 was hot-pressed to obtain a honeycomb material.

[0067] Comparative Example 1: This comparative example did not include a flame retardant synergist compared to Example 1, but the remaining steps were the same.

[0068] Comparative Example 2: This comparative example uses a synergistic monomer instead of a flame retardant synergist, but the other steps are the same as in Example 1.

[0069] Comparative Example 3: This comparative example uses butanol instead of flame retardant additives, but the other steps are the same as in Example 1.

[0070] The flame retardant performance level of the core materials prepared in Examples 1-3 and Comparative Examples 1-3 was determined according to the standard GB / T8624-2012, and the test results are shown in Table 1 below.

[0071] Table 1

[0072]

[0073] As shown in Table 1, this application has excellent flame retardant properties.

[0074] The above description is merely an example and illustration of the concept of the present invention. Those skilled in the art can make various modifications or additions to the specific embodiments described or use similar methods to replace them, as long as they do not deviate from the concept of the invention or exceed the scope defined in the claims, they should all fall within the protection scope of the present invention.

Claims

1. A method for preparing A2-grade flame-retardant aluminum composite panel core material, characterized in that: Specifically, the steps include the following: Step A1: Mix diphenyl phosphate and toluene, purge with nitrogen, stir and add dimethylchlorosilane, heat and react to obtain silicic phosphate. Mix silicic phosphate, allyl alcohol, chloroplatinic acid and DMF, purge with nitrogen and react to obtain flame retardant additive. Step A2: Mix cyanuric chloride and tetrahydrofuran, purge with nitrogen, stir and add flame retardant additive and triethylamine, react, add synergistic monomer, heat and react, add 4-maleimide-phenol, heat and react to obtain flame retardant synergist. Step A3: Weigh the following raw materials in parts by weight: 10-12 parts of matrix resin, 85-90 parts of flame retardant, 0.5-1.5 parts of flame retardant synergist, 0.01-0.03 parts of benzoyl peroxide, 1-2 parts of anionic surfactant, 2-4 parts of compatibilizer, 1-2 parts of antioxidant and 0.5-1.5 parts of antibacterial agent. Melt and blend the raw materials and then press them into molds to obtain the flame-retardant aluminum composite panel core material. The synergistic monomer is prepared by the following steps: Step B1: DOPO, formaldehyde solution and anhydrous ethanol are mixed and reacted to obtain intermediate 1. Intermediate 1 is mixed with acetonitrile, nitrogen gas is introduced for protection, and triethylamine is added while stirring. After stirring, acryloyl chloride is added and the mixture is heated to obtain intermediate 2. Intermediate 2, bis(2-mercaptoethyl)amine, benzophenone and DMF are mixed and reacted under ultraviolet light to obtain the modifier. Step B2: Mix phenyltrimethoxysilane, isopropanol, deionized water and sodium hydroxide evenly, purge with nitrogen gas, and react to obtain sodium octaphenyltetrasiloxane tetrasilanolate. Mix sodium octaphenyltetrasiloxane tetrasilanolate, triethylamine and tetrahydrofuran, purge with nitrogen gas, stir and add methyldichlorosilane to react to obtain dihydro-cage-type silsesquioxane. Step B3: Mix dihydro-cage silsesquioxane, allyl alcohol glycidyl ether, caster catalyst and toluene evenly, purge with nitrogen for protection, and react to obtain pretreated cage silsesquioxane. Mix the pretreated cage silsesquioxane, modifier, triphenylphosphine and tetrahydrofuran, and react to obtain synergistic monomer.

2. The preparation method of the A2-level flame-retardant aluminum plastic panel core material according to claim 1, characterized in that: The molar ratio of diphenyl phosphate and dimethylchlorosilane in step A1 is 1:1, and the molar ratio of silanized phosphate and allyl alcohol is 1:

1.

3. The preparation method of the A2-level flame-retardant aluminum plastic panel core material according to claim 1, characterized in that: The molar ratio of cyanuric chloride, flame retardant additive, triethylamine, synergist monomer and 4-maleimide-based phenol in step A2 is 2:2:6:1:

2.

4. The preparation method of the A2-level flame-retardant aluminum plastic panel core material according to claim 1, characterized in that: The matrix resin mentioned in step A3 is prepared by blending low-density polyethylene, polypropylene, ethylene-octene copolymer and ethylene-ethyl acrylate in a mass ratio of 6:2:1:1, and the flame retardant is prepared by blending magnesium hydroxide and expandable graphite in a mass ratio of 6:

1.

5. The method for preparing the A2 fire-retardant aluminum plastic panel core material according to claim 1, characterized in that: The ratio of DOPO to formaldehyde solution in step B1 is 1 mol: 80 mL, the molar ratio of intermediate 1, acryloyl chloride and triethylamine is 1:1.1:1.2, and the molar ratio of intermediate 2 and bis(2-mercaptoethyl)amine is 2:

1.

6. The method for preparing the A2 fire-retardant aluminum plastic panel core material according to claim 1, characterized in that: The ratio of phenyltrimethoxysilane, isopropanol, deionized water and sodium hydroxide used in step B2 is 6 mmol:6 mmol:7 mL:4 mmol, and the mass ratio of octaphenyltetrasiloxane tetrasilanolate sodium, triethylamine and methyldichlorosilane is 11:4.5:3.

5.

7. The method for preparing the A2 fire-retardant aluminum plastic panel core material according to claim 1, characterized in that: The molar ratio of dihydro-cage silsesquioxane and allyl alcohol glycidyl ether in step B3 is 1:2, and the molar ratio of pretreated cage silsesquioxane and modifier is 1:

2.

8. A flame retardant aluminum-plastic panel core material of grade A2, characterized in that: Prepared according to any one of the preparation methods described in claims 1-7.

9. The A2 fire-retardant aluminum plastic panel core material according to claim 8, characterized in that: The flame-retardant aluminum-plastic composite core material is made into a flat or honeycomb shape.

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