CN117964313A - Multifunctional fireproof and antiriot plate and preparation method thereof - Google Patents

Multifunctional fireproof and antiriot plate and preparation method thereof Download PDF

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CN117964313A
CN117964313A CN202410167918.9A CN202410167918A CN117964313A CN 117964313 A CN117964313 A CN 117964313A CN 202410167918 A CN202410167918 A CN 202410167918A CN 117964313 A CN117964313 A CN 117964313A
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reacting
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CN117964313B (en
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郑祯勋
李终云
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Jiangsu Meibiao Home Technology Co ltd
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Jiangsu Meibiao Home Technology Co ltd
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    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B28/00—Compositions of mortars, concrete or artificial stone, containing inorganic binders or the reaction product of an inorganic and an organic binder, e.g. polycarboxylate cements
    • C04B28/02—Compositions of mortars, concrete or artificial stone, containing inorganic binders or the reaction product of an inorganic and an organic binder, e.g. polycarboxylate cements containing hydraulic cements other than calcium sulfates
    • C04B28/04—Portland cements
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B20/00—Use of materials as fillers for mortars, concrete or artificial stone according to more than one of groups C04B14/00 - C04B18/00 and characterised by shape or grain distribution; Treatment of materials according to more than one of the groups C04B14/00 - C04B18/00 specially adapted to enhance their filling properties in mortars, concrete or artificial stone; Expanding or defibrillating materials
    • C04B20/10—Coating or impregnating
    • C04B20/1018—Coating or impregnating with organic materials
    • C04B20/1029—Macromolecular compounds
    • C04B20/1037—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2111/00—Mortars, concrete or artificial stone or mixtures to prepare them, characterised by specific function, property or use
    • C04B2111/20—Resistance against chemical, physical or biological attack
    • C04B2111/28—Fire resistance, i.e. materials resistant to accidental fires or high temperatures
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2201/00—Mortars, concrete or artificial stone characterised by specific physical values
    • C04B2201/50—Mortars, concrete or artificial stone characterised by specific physical values for the mechanical strength

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Ceramic Engineering (AREA)
  • Materials Engineering (AREA)
  • Structural Engineering (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Inorganic Chemistry (AREA)
  • Polyurethanes Or Polyureas (AREA)

Abstract

The invention discloses a multifunctional fireproof anti-riot board and a preparation method thereof, wherein the board comprises the following raw materials in parts by weight: 15-20 parts of cement, 5-10 parts of modified filler, 8-10 parts of silicon carbide, 3-5 parts of quartz sand, 2-3 parts of silica micropowder and 12-15 parts of water, wherein the modified filler is of a core-shell structure of polyurethane coated mesoporous silica, and the surface of the modified filler contains a metal organic framework, so that the mechanical property of the fireproof and anti-riot plate can be improved, further, the plate is prevented from bursting under the high temperature condition, the polyurethane coating on the surface contains elements such as phosphorus, boron, nitrogen and silicon, a compact carbon layer can be generated to be attached to the surface of a substrate during combustion, the effect of heat insulation and oxygen isolation is achieved, the possibility of bursting of the plate can be reduced due to the coating on the surface of the substrate, and a large amount of water vapor can be released when aluminum hydroxide is heated, so that the fireproof and flame-retardant effects are achieved.

Description

Multifunctional fireproof and antiriot plate and preparation method thereof
Technical Field
The invention relates to the technical field of composite board preparation, in particular to a multifunctional fireproof anti-riot board and a preparation method thereof.
Background
With the development of society, people have a stronger fire-proof consciousness, and various fire-proof and riot panels are applied to various places in life. The fire-proof and explosion-proof fire-proof plate is light, firm, impact-resistant and explosion-proof, has special fire-proof performance, ensures that fire fighters can avoid fire sources, ensures social life and property safety, is widely applied to the fields of interior decoration, furniture, cabinets, laboratory tables, outer walls and the like, and the fire-proof plate on the current market mainly has the following major categories: 1. mineral wool board, glass wool board; 2. a cement board; 3. perlite plates, floating bead plates and vermiculite plates; 4. fireproof gypsum board; 5. a calcium silicate fiberboard; 6. magnesium oxychloride fireproof plate. The advantages and disadvantages of each plate are that mineral wool plates and glass wool plates are light and incombustible, but short fibers are harmful to human bodies, have poor barrier property to fire smoke spreading and large workload of installation and construction, and cement plates have high strength and wide sources, so that the use frequency is increased, but the plates are easy to crack and perforate in a fire scene and lose protection, so that the application of the plates is limited to a certain extent.
Disclosure of Invention
The invention aims to provide a multifunctional fireproof and antiriot plate and a preparation method thereof, which solve the problem that the fireproof and antiriot effect of the plate in the prior art is poor.
The aim of the invention can be achieved by the following technical scheme:
the preparation method of the multifunctional fireproof antiriot plate comprises the following steps:
Weighing the following powder raw materials by weight: 15-20 parts of cement, 5-10 parts of modified filler, 8-10 parts of silicon carbide, 3-5 parts of quartz sand, 2-3 parts of silicon micropowder and 12-15 parts of water, uniformly mixing the raw materials, pouring the raw materials into a mold, and performing compression molding to obtain the multifunctional fireproof anti-riot board.
Further, the modified filler is prepared by the following steps:
Step A1: uniformly mixing 4-formylphenylboric acid, pentaerythritol and benzene, carrying out reflux reaction for 6-8 hours at the rotation speed of 120-150r/min and the temperature of 81-83 ℃ to obtain an intermediate 1, uniformly mixing p-hydroxyaniline and absolute ethyl alcohol, stirring and adding the intermediate 1 at the rotation speed of 150-200r/min and the temperature of 65-70 ℃ to react for 10-12 hours, adding DOPO, and continuing to react for 10-15 hours to obtain a modified monomer;
Step A2: uniformly mixing a modified monomer, polytetrahydrofuran ether glycol, dibutyl tin dilaurate and DMF (dimethyl formamide), stirring and adding diphenylmethane diisocyanate at the rotation speed of 150-200r/min and the temperature of 70-75 ℃, reacting for 1-2h, adding KH550, and continuously reacting for 1-1.5h to obtain modified polyurethane;
Step A3: dispersing pretreated filler in DMF, adding KH560 and modified polyurethane, reacting at the rotation speed of 120-150r/min and the temperature of 60-65 ℃ for 10-15h, cooling to room temperature, adding ammonium fluoride, continuing to react for 20-25h, filtering to remove filtrate, dispersing substrate in DMF, adding 2-aminobenzimidazole, stirring at the rotation speed of 60-80r/min and the temperature of 30-40 ℃ and the pH value of 11-12 for 6-8h, adjusting the pH value to be neutral, adding molybdenum trioxide at the temperature of 110-120 ℃ for reacting for 10-15h, and obtaining modified filler.
Further, the molar ratio of 4-formylphenylboronic acid to pentaerythritol in step A1 is 2:1, and the molar ratio of para-hydroxyaniline, intermediate 1 and DOPO is 2:1:2.
Further, the dosage ratio of the modified monomer, the polytetrahydrofuran ether glycol, the diphenyl diisocyanate and the KH550 in the step A2 is 1:2:4:2, the molecular weight of the polytetrahydrofuran ether glycol is 2000, and the dosage of the dibutyl tin dilaurate is 1-1.5% of the mass of the modified monomer.
Further, the dosage ratio of the pretreatment filler, KH560, modified polyurethane and ammonium fluoride in the step A3 is 2g to 3mL to 6g to 0.3g, and the molar ratio of epoxy groups, 2-aminobenzimidazole and molybdenum trioxide on the substrate is 2 to 1.
Further, the pretreatment filler is prepared by the following steps:
Step B1: uniformly mixing cetyl trimethyl ammonium bromide, ammonia water, ethanol and deionized water, stirring at the rotation speed of 1200-1500r/min and the temperature of 55-60 ℃, adding tetraethyl orthosilicate and 3-mercaptopropyl trimethoxy silane, reacting for 20-25h, filtering to remove filtrate, adding into hydrochloric acid solution, soaking for 3-5min, centrifuging to remove supernatant, and washing with deionized water to neutrality to obtain a precursor;
Step B2: uniformly mixing the precursor, aluminum hydroxide, sodium hydroxide and deionized water, reacting for 2-3 hours at the rotating speed of 150-200r/min and the temperature of 200-220 ℃ and the pH value of 11-12 to obtain a modified precursor, uniformly mixing the modified precursor, KH570, n-butyllithium and DMF, and reacting for 3-5 hours under the ultraviolet irradiation at the rotating speed of 120-150r/min and the ultraviolet irradiation at 365nm to obtain the pretreated filler.
Further, the dosage ratio of the cetyltrimethylammonium bromide, the ammonia water, the ethanol, the deionized water, the tetraethyl orthosilicate and the 3-mercaptotrimethoxysilane in the step B1 is 0.34g:1mL:100mL:6mL:1.67g:0.39g, and the mass fraction of the ethanol solution of the hydrochloric acid is 15%.
Further, the mass ratio of the precursor to the aluminum hydroxide in the step B2 is 1:1.1, the mol ratio of the mercapto group on the precursor to the KH570 is 1:1, and the dosage of the n-butyllithium is 0.5-1% of the mass of KH 570.
The invention has the beneficial effects that: the invention discloses a multifunctional fireproof anti-riot board which comprises the following raw materials: cement, modified filler, silicon carbide, quartz sand, silica micropowder and water, wherein the modified filler takes 4-formylphenylboric acid and pentaerythritol as raw materials to react, boric acid groups on the 4-formylphenylboric acid and hydroxyl groups on the pentaerythritol react to prepare an intermediate 1, P-hydroxyaniline reacts with the intermediate 1 to react amino groups on the P-hydroxyaniline with aldehyde groups on the intermediate 1, DOPO is added to react P-H bonds on the DOPO with N=C bonds to prepare a modified monomer, the modified monomer, polytetrahydrofuran ether glycol and diphenylmethane diisocyanate react to prepare polyurethane prepolymer, KH550 is used for end capping to prepare modified polyurethane, the modified filler, KH560 and the modified polyurethane are subjected to hydrolytic condensation to form cage-type silsesquioxane between the modified filler and the modified polyurethane, and the cage-type silsesquioxane structurally contains epoxy groups, adding 2-aminobenzimidazole, reacting under alkaline condition to make amino on 2-aminobenzimidazole react with epoxy group, then making it coordinate with molybdenum trioxide to form metal organic frame to obtain modified filler, using tetraethyl orthosilicate and 3-mercaptopropyl trimethoxy silane as raw material to form mercapto mesoporous silica to obtain precursor, making precursor and aluminium hydroxide undergo the process of hydrothermal reaction under alkaline condition to make aluminium hydroxide grow in micropores of precursor to obtain modified precursor, making modified precursor react with KH570 under the condition of irradiation of ultraviolet light to make mercapto group on modified precursor react with double bond on KH570 to obtain pretreated filler, the modified filler is core-shell structure of polyurethane-coated mesoporous silica, and its surface contains metal organic frame, so that it can raise mechanical property of fire-resisting and anti-riot plate, and then prevent under the high temperature condition that the panel appears bursting, the polyurethane cladding on surface contains elements such as phosphorus, boron, nitrogen and silicon, can produce dense carbon layer and adhere to the base member surface when burning, reaches thermal-insulated oxygen effect that separates, and the cladding can reduce the possibility that the panel bursts at the base member surface, can release a large amount of steam when aluminium hydroxide is heated simultaneously, and then reaches fire prevention fire-retardant effect.
Detailed Description
The following description of the technical solutions in the embodiments of the present invention will be clear and complete, and it is obvious that the described embodiments are only some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
Example 1
A multifunctional fireproof antiriot plate and a preparation method thereof specifically comprise the following steps:
weighing the following powder raw materials by weight: 15 parts of cement, 5 parts of modified filler, 8 parts of silicon carbide, 3 parts of quartz sand, 2 parts of silicon micropowder and 12 parts of water, uniformly mixing the raw materials, pouring the raw materials into a mold, and performing compression molding to obtain the multifunctional fireproof anti-riot plate.
The cement is 32.5 silicate cement, the particle size of the modified filler is 3mm, the particle size of the silicon carbide is 30 mu m, the particle size of the quartz sand is 1mm, and the particle size of the silicon micropowder is 0.1 mu m.
The modified filler is prepared by the following steps:
Step A1: uniformly mixing 4-formylphenylboric acid, pentaerythritol and benzene, carrying out reflux reaction for 6 hours at the rotation speed of 120r/min and the temperature of 81 ℃ to obtain an intermediate 1, uniformly mixing parahydroxyaniline and absolute ethyl alcohol, stirring and adding the intermediate 1 at the rotation speed of 150r/min and the temperature of 65 ℃ to react for 10 hours, adding DOPO, and continuing to react for 10 hours to obtain a modified monomer;
step A2: uniformly mixing a modified monomer, polytetrahydrofuran ether glycol, dibutyl tin dilaurate and DMF (dimethyl formamide), stirring and adding diphenylmethane diisocyanate under the condition of the rotating speed of 150r/min and the temperature of 70 ℃, reacting for 1h, adding KH550, and continuously reacting for 1h to obtain modified polyurethane;
Step A3: dispersing pretreated filler in DMF, adding KH560 and modified polyurethane, reacting for 10h at a speed of 120r/min and a temperature of 60 ℃, cooling to room temperature, adding ammonium fluoride, continuing to react for 20h, filtering to remove filtrate, dispersing substrate in DMF, adding 2-aminobenzimidazole, stirring for 6h at a speed of 60r/min and a temperature of 30 ℃ and a pH value of 11, adjusting the pH value to be neutral, adding molybdenum trioxide at a temperature of 110 ℃, and reacting for 10h to obtain the modified filler.
The molar ratio of the 4-formylphenylboric acid to the pentaerythritol in the step A1 is 2:1, and the molar ratio of the parahydroxyaniline to the intermediate 1 to the DOPO is 2:1:2.
The dosage ratio of the modified monomer to the polytetrahydrofuran ether glycol to the diphenyl diisocyanate to the KH550 in the step A2 is 1:2:4:2, the molecular weight of the polytetrahydrofuran ether glycol is 2000, and the dosage of the dibutyl tin dilaurate is 1% of the mass of the modified monomer.
The dosage ratio of the pretreatment filler, KH560, modified polyurethane and ammonium fluoride in the step A3 is 2g to 3mL to 6g to 0.3g, and the molar ratio of epoxy groups, 2-aminobenzimidazole and molybdenum trioxide on the substrate is 2 to 1.
The pretreatment filler is prepared by the following steps:
Step B1: uniformly mixing cetyl trimethyl ammonium bromide, ammonia water, ethanol and deionized water, stirring at the rotation speed of 1200r/min and the temperature of 55 ℃, adding tetraethyl orthosilicate and 3-mercaptopropyl trimethoxy silane, reacting for 20 hours, filtering to remove filtrate, adding into hydrochloric acid solution, soaking for 3 minutes, centrifuging to remove supernatant, and washing with deionized water to neutrality to obtain a precursor;
step B2: uniformly mixing the precursor, aluminum hydroxide, sodium hydroxide and deionized water, reacting for 2 hours at the rotating speed of 150r/min and the temperature of 200 ℃ and the pH value of 11 to obtain a modified precursor, uniformly mixing the modified precursor, KH570, n-butyllithium and DMF, and reacting for 3 hours under the ultraviolet irradiation condition with the rotating speed of 120r/min and the ultraviolet irradiation of 365nm to obtain the pretreated filler.
The dosage ratio of the cetyl trimethyl ammonium bromide, the ammonia water, the ethanol, the deionized water, the tetraethyl orthosilicate and the 3-mercaptotrimethoxysilane in the step B1 is 0.34g:1mL:100mL:6mL:1.67g:0.39g, and the mass fraction of the ethanol solution of the hydrochloric acid is 15%.
The mass ratio of the precursor to the aluminum hydroxide in the step B2 is 1:1.1, the mol ratio of the mercapto group on the precursor to KH570 is 1:1, and the dosage of the n-butyllithium is 0.5% of the mass of KH 570.
Example 2
A multifunctional fireproof antiriot plate and a preparation method thereof specifically comprise the following steps:
weighing the following powder raw materials by weight: 18 parts of cement, 8 parts of modified filler, 9 parts of silicon carbide, 4 parts of quartz sand, 2.5 parts of silicon micropowder and 13.5 parts of water, and the raw materials are uniformly mixed, poured into a mold and pressed for molding to prepare the multifunctional fireproof anti-riot board.
The cement is 32.5 silicate cement, the particle size of the modified filler is 4mm, the particle size of the silicon carbide is 40 mu m, the particle size of the quartz sand is 2mm, and the particle size of the silicon micropowder is 0.2 mu m.
The modified filler is prepared by the following steps:
Step A1: uniformly mixing 4-formylphenylboric acid, pentaerythritol and benzene, carrying out reflux reaction for 7 hours at the rotation speed of 120r/min and the temperature of 82 ℃ to obtain an intermediate 1, uniformly mixing parahydroxyaniline and absolute ethyl alcohol, stirring and adding the intermediate 1 at the rotation speed of 150r/min and the temperature of 68 ℃ to react for 11 hours, adding DOPO, and continuing to react for 13 hours to obtain a modified monomer;
step A2: uniformly mixing a modified monomer, polytetrahydrofuran ether glycol, dibutyl tin dilaurate and DMF (dimethyl formamide), stirring and adding diphenylmethane diisocyanate under the condition of the rotating speed of 150r/min and the temperature of 73 ℃, reacting for 1.5 hours, adding KH550, and continuously reacting for 1.5 hours to obtain modified polyurethane;
Step A3: dispersing pretreated filler in DMF, adding KH560 and modified polyurethane, reacting for 13h at a rotation speed of 150r/min and a temperature of 63 ℃, cooling to room temperature, adding ammonium fluoride, continuing to react for 25h, filtering to remove filtrate, dispersing a substrate in DMF, adding 2-aminobenzimidazole, stirring for 7h at a rotation speed of 60r/min and a temperature of 35 ℃ and a pH value of 12, adjusting the pH value to be neutral, adding molybdenum trioxide at a temperature of 115 ℃, and reacting for 13h to obtain the modified filler.
The molar ratio of the 4-formylphenylboric acid to the pentaerythritol in the step A1 is 2:1, and the molar ratio of the parahydroxyaniline to the intermediate 1 to the DOPO is 2:1:2.
The dosage ratio of the modified monomer to the polytetrahydrofuran ether glycol to the diphenyl diisocyanate to the KH550 in the step A2 is 1:2:4:2, the molecular weight of the polytetrahydrofuran ether glycol is 2000, and the dosage of the dibutyl tin dilaurate is 1.3 percent of the mass of the modified monomer.
The dosage ratio of the pretreatment filler, KH560, modified polyurethane and ammonium fluoride in the step A3 is 2g to 3mL to 6g to 0.3g, and the molar ratio of epoxy groups, 2-aminobenzimidazole and molybdenum trioxide on the substrate is 2 to 1.
The pretreatment filler is prepared by the following steps:
Step B1: uniformly mixing cetyl trimethyl ammonium bromide, ammonia water, ethanol and deionized water, stirring at the rotation speed of 1200r/min and the temperature of 58 ℃, adding tetraethyl orthosilicate and 3-mercaptopropyl trimethoxy silane, reacting for 23 hours, filtering to remove filtrate, adding into hydrochloric acid solution, soaking for 4 minutes, centrifuging to remove supernatant, and washing with deionized water to neutrality to obtain a precursor;
Step B2: uniformly mixing the precursor, aluminum hydroxide, sodium hydroxide and deionized water, reacting for 3 hours at the rotating speed of 150r/min and the temperature of 210 ℃ and the pH value of 12 to obtain a modified precursor, uniformly mixing the modified precursor, KH570, n-butyllithium and DMF, and reacting for 4 hours under the ultraviolet irradiation condition with the rotating speed of 120r/min and the ultraviolet irradiation of 365nm to obtain the pretreated filler.
The dosage ratio of the cetyl trimethyl ammonium bromide, the ammonia water, the ethanol, the deionized water, the tetraethyl orthosilicate and the 3-mercaptotrimethoxysilane in the step B1 is 0.34g:1mL:100mL:6mL:1.67g:0.39g, and the mass fraction of the ethanol solution of the hydrochloric acid is 15%.
The mass ratio of the precursor to the aluminum hydroxide in the step B2 is 1:1.1, the mol ratio of the mercapto group on the precursor to KH570 is 1:1, and the dosage of the n-butyllithium is 1% of the mass of KH 570.
Example 3
A multifunctional fireproof antiriot plate and a preparation method thereof specifically comprise the following steps:
Weighing the following powder raw materials by weight: 20 parts of cement, 10 parts of modified filler, 10 parts of silicon carbide, 5 parts of quartz sand, 3 parts of silicon micropowder and 15 parts of water, uniformly mixing the raw materials, pouring the raw materials into a mold, and performing compression molding to obtain the multifunctional fireproof anti-riot plate.
The cement is 32.5 silicate cement, the particle size of the modified filler is 5mm, the particle size of the silicon carbide is 50 mu m, the particle size of the quartz sand is 3mm, and the particle size of the silicon micropowder is 0.3 mu m.
The modified filler is prepared by the following steps:
Step A1: uniformly mixing 4-formylphenylboric acid, pentaerythritol and benzene, carrying out reflux reaction for 8 hours at the rotation speed of 150r/min and the temperature of 83 ℃ to obtain an intermediate 1, uniformly mixing parahydroxyaniline and absolute ethyl alcohol, stirring and adding the intermediate 1 at the rotation speed of 200r/min and the temperature of 70 ℃ to react for 12 hours, adding DOPO, and continuing to react for 15 hours to obtain a modified monomer;
Step A2: uniformly mixing a modified monomer, polytetrahydrofuran ether glycol, dibutyl tin dilaurate and DMF (dimethyl formamide), stirring and adding diphenylmethane diisocyanate under the condition of the rotating speed of 200r/min and the temperature of 75 ℃, reacting for 2 hours, adding KH550, and continuously reacting for 1.5 hours to obtain modified polyurethane;
Step A3: dispersing pretreated filler in DMF, adding KH560 and modified polyurethane, reacting for 15h at a rotation speed of 150r/min and a temperature of 65 ℃, cooling to room temperature, adding ammonium fluoride, continuing to react for 25h, filtering to remove filtrate, dispersing a substrate in DMF, adding 2-aminobenzimidazole, stirring for 8h at a rotation speed of 80r/min and a temperature of 40 ℃ and a pH value of 12, adjusting the pH value to be neutral, adding molybdenum trioxide at a temperature of 120 ℃, and reacting for 15h to obtain the modified filler.
The molar ratio of the 4-formylphenylboric acid to the pentaerythritol in the step A1 is 2:1, and the molar ratio of the parahydroxyaniline to the intermediate 1 to the DOPO is 2:1:2.
The dosage ratio of the modified monomer to the polytetrahydrofuran ether glycol to the diphenyl diisocyanate to the KH550 in the step A2 is 1:2:4:2, the molecular weight of the polytetrahydrofuran ether glycol is 2000, and the dosage of the dibutyl tin dilaurate is 1.5 percent of the mass of the modified monomer.
The dosage ratio of the pretreatment filler, KH560, modified polyurethane and ammonium fluoride in the step A3 is 2g to 3mL to 6g to 0.3g, and the molar ratio of epoxy groups, 2-aminobenzimidazole and molybdenum trioxide on the substrate is 2 to 1.
The pretreatment filler is prepared by the following steps:
Step B1: uniformly mixing cetyl trimethyl ammonium bromide, ammonia water, ethanol and deionized water, stirring at a rotating speed of 1500r/min and a temperature of 60 ℃, adding tetraethyl orthosilicate and 3-mercaptopropyl trimethoxy silane, reacting for 25 hours, filtering to remove filtrate, adding into hydrochloric acid solution, soaking for 5 minutes, centrifuging to remove supernatant, and washing with deionized water to neutrality to obtain a precursor;
Step B2: uniformly mixing the precursor, aluminum hydroxide, sodium hydroxide and deionized water, reacting for 3 hours at the rotation speed of 200r/min and the temperature of 220 ℃ and the pH value of 12 to obtain a modified precursor, uniformly mixing the modified precursor, KH570, n-butyllithium and DMF, and reacting for 5 hours under the ultraviolet irradiation condition with the rotation speed of 150r/min and the pH value of 365nm to obtain the pretreated filler.
The dosage ratio of the cetyl trimethyl ammonium bromide, the ammonia water, the ethanol, the deionized water, the tetraethyl orthosilicate and the 3-mercaptotrimethoxysilane in the step B1 is 0.34g:1mL:100mL:6mL:1.67g:0.39g, and the mass fraction of the ethanol solution of the hydrochloric acid is 15%.
The mass ratio of the precursor to the aluminum hydroxide in the step B2 is 1:1.1, the mol ratio of the mercapto group on the precursor to KH570 is 1:1, and the dosage of the n-butyllithium is 1% of the mass of KH 570.
Comparative example 1
Compared with the comparative example 1, the pretreatment filler is dispersed in DMF, modified polyurethane is added, the reaction is carried out for 10 hours under the conditions of the rotating speed of 120r/min and the temperature of 60 ℃, the temperature is reduced to the room temperature, ammonium fluoride is added, and the reaction is continued for 20 hours, so that the product is obtained to replace the modified filler.
Comparative example 2
This comparative example was compared to example 1 without the addition of pretreatment filler, and the rest of the procedure was the same.
Comparative example 3
This comparative example uses the precursor instead of the modified precursor as compared to example 1, with the rest of the procedure being the same.
The panels prepared in examples 1-3 and comparative examples 1-3 were tested for fire resistance according to the GB/T9978.1-2008 standard, the back surface temperature was measured and recorded until the average back temperature rise was greater than 140℃, the maximum rise was greater than 180℃, and the tensile strength was measured, with the test results shown in the following table.
The table shows that the application has good fireproof and antiriot effects.
The foregoing is merely illustrative and explanatory of the principles of the invention, as various modifications and additions may be made to the specific embodiments described, or similar thereto, by those skilled in the art, without departing from the principles of the invention or beyond the scope of the appended claims.

Claims (9)

1. The preparation method of the multifunctional fireproof anti-riot board is characterized by comprising the following steps of: the method specifically comprises the following steps:
Weighing the following powder raw materials by weight: 15-20 parts of cement, 5-10 parts of modified filler, 8-10 parts of silicon carbide, 3-5 parts of quartz sand, 2-3 parts of silicon micropowder and 12-15 parts of water, uniformly mixing the raw materials, pouring the raw materials into a mold, and performing compression molding to obtain the multifunctional fireproof anti-riot board.
2. The method for preparing the multifunctional fireproof and antiriot plate material according to claim 1, wherein the method comprises the following steps: the modified filler is prepared by the following steps:
Step A1: mixing 4-formylphenylboric acid, pentaerythritol and benzene, carrying out reflux reaction to obtain an intermediate 1, mixing and stirring p-hydroxyaniline and absolute ethyl alcohol, adding the intermediate 1, carrying out reaction, adding DOPO, and carrying out continuous reaction to obtain a modified monomer;
Step A2: mixing and stirring a modified monomer, polytetrahydrofuran ether glycol, dibutyl tin dilaurate and DMF, adding diphenylmethane diisocyanate, reacting, adding KH550, and continuing reacting to obtain modified polyurethane;
step A3: dispersing the pretreated filler in DMF, adding KH560 and modified polyurethane, reacting, cooling to room temperature, adding ammonium fluoride, continuing the reaction, filtering to remove filtrate, dispersing the substrate in DMF, adding 2-aminobenzimidazole, stirring, adjusting pH to be neutral, heating, adding molybdenum trioxide, and reacting to obtain the modified filler.
3. The method for preparing the multifunctional fireproof and antiriot plate material according to claim 2, wherein the method comprises the following steps: the molar ratio of the 4-formylphenylboric acid to the pentaerythritol in the step A1 is 2:1, and the molar ratio of the parahydroxyaniline to the intermediate 1 to the DOPO is 2:1:2.
4. The method for preparing the multifunctional fireproof and antiriot plate material according to claim 2, wherein the method comprises the following steps: the dosage ratio of the modified monomer to the polytetrahydrofuran ether glycol to the diphenyl diisocyanate to the KH550 in the step A2 is 1:2:4:2, the molecular weight of the polytetrahydrofuran ether glycol is 2000, and the dosage of the dibutyl tin dilaurate is 1-1.5% of the mass of the modified monomer.
5. The method for preparing the multifunctional fireproof and antiriot plate material according to claim 2, wherein the method comprises the following steps: the dosage ratio of the pretreatment filler, KH560, modified polyurethane and ammonium fluoride in the step A3 is 2g to 3mL to 6g to 0.3g, and the molar ratio of epoxy groups, 2-aminobenzimidazole and molybdenum trioxide on the substrate is 2 to 1.
6. The method for preparing the multifunctional fireproof and antiriot plate material according to claim 2, wherein the method comprises the following steps: the pretreatment filler is prepared by the following steps:
Step B1: mixing cetyl trimethyl ammonium bromide, ammonia water, ethanol and deionized water, stirring, adding tetraethyl orthosilicate and 3-mercaptopropyl trimethoxy silane, reacting, filtering to remove filtrate, adding into hydrochloric acid solution, soaking, centrifuging to remove supernatant, and washing with deionized water to neutrality to obtain a precursor;
Step B2: mixing and reacting the precursor, aluminum hydroxide, sodium hydroxide and deionized water to obtain a modified precursor, and mixing and reacting the modified precursor, KH570, n-butyllithium and DMF to obtain the pretreated filler.
7. The method for preparing the multifunctional fireproof and antiriot plate material according to claim 6, wherein the method comprises the following steps: the dosage ratio of cetyltrimethylammonium bromide, ammonia water, ethanol, deionized water, tetraethyl orthosilicate and 3-mercaptotrimethoxysilane described in step B1 was 0.34g:1mL:100mL:6mL:1.67g:0.39g.
8. The method for preparing the multifunctional fireproof and antiriot plate material according to claim 6, wherein the method comprises the following steps: the mass ratio of the precursor to the aluminum hydroxide in the step B2 is 1:1.1, the mol ratio of the mercapto group on the precursor to KH570 is 1:1, and the dosage of the n-butyllithium is 0.5-1% of the mass of KH 570.
9. Multifunctional fireproof and antiriot plate, which is characterized in that: the preparation method according to any one of claims 1-8.
CN202410167918.9A 2024-02-06 2024-02-06 Multifunctional fireproof and explosion-proof plate and preparation method thereof Active CN117964313B (en)

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Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20140367105A1 (en) * 2013-06-14 2014-12-18 Halliburton Energy Services, Inc. Filler Particles with Enhanced Suspendability for Use in Hardenable Resin Compositions
CN114292515A (en) * 2022-01-12 2022-04-08 安徽冠泓塑业有限公司 High-wear-resistance and high-strength protective boot and preparation method thereof
CN115368813A (en) * 2021-05-19 2022-11-22 黄建发 Scratch-resistant double-component polyurethane varnish
CN116041945A (en) * 2023-01-30 2023-05-02 湖州高裕家居科技有限公司 Polyurethane material and preparation method thereof

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20140367105A1 (en) * 2013-06-14 2014-12-18 Halliburton Energy Services, Inc. Filler Particles with Enhanced Suspendability for Use in Hardenable Resin Compositions
CN115368813A (en) * 2021-05-19 2022-11-22 黄建发 Scratch-resistant double-component polyurethane varnish
CN114292515A (en) * 2022-01-12 2022-04-08 安徽冠泓塑业有限公司 High-wear-resistance and high-strength protective boot and preparation method thereof
CN116041945A (en) * 2023-01-30 2023-05-02 湖州高裕家居科技有限公司 Polyurethane material and preparation method thereof

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