CN117943264A - Waterproof and heat-insulating modified asphalt coiled material and preparation method thereof - Google Patents

Waterproof and heat-insulating modified asphalt coiled material and preparation method thereof Download PDF

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CN117943264A
CN117943264A CN202410349939.2A CN202410349939A CN117943264A CN 117943264 A CN117943264 A CN 117943264A CN 202410349939 A CN202410349939 A CN 202410349939A CN 117943264 A CN117943264 A CN 117943264A
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modified
heat
coiled material
gel
mixing
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CN117943264B (en
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祝兴洲
王黎
李金丽
谷民军
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Jinxiu Waterproof Technology Co ltd
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Jinxiu Waterproof Technology Co ltd
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B05SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05DPROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05D7/00Processes, other than flocking, specially adapted for applying liquids or other fluent materials to particular surfaces or for applying particular liquids or other fluent materials
    • B05D7/02Processes, other than flocking, specially adapted for applying liquids or other fluent materials to particular surfaces or for applying particular liquids or other fluent materials to macromolecular substances, e.g. rubber
    • B05D7/04Processes, other than flocking, specially adapted for applying liquids or other fluent materials to particular surfaces or for applying particular liquids or other fluent materials to macromolecular substances, e.g. rubber to surfaces of films or sheets
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B05SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05DPROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05D5/00Processes for applying liquids or other fluent materials to surfaces to obtain special surface effects, finishes or structures
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B05SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05DPROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05D7/00Processes, other than flocking, specially adapted for applying liquids or other fluent materials to particular surfaces or for applying particular liquids or other fluent materials
    • B05D7/24Processes, other than flocking, specially adapted for applying liquids or other fluent materials to particular surfaces or for applying particular liquids or other fluent materials for applying particular liquids or other fluent materials
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09DCOATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D195/00Coating compositions based on bituminous materials, e.g. asphalt, tar, pitch
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09DCOATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D7/00Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
    • C09D7/40Additives
    • C09D7/60Additives non-macromolecular
    • C09D7/61Additives non-macromolecular inorganic
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09DCOATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D7/00Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
    • C09D7/40Additives
    • C09D7/60Additives non-macromolecular
    • C09D7/61Additives non-macromolecular inorganic
    • C09D7/62Additives non-macromolecular inorganic modified by treatment with other compounds
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09DCOATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D7/00Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
    • C09D7/40Additives
    • C09D7/65Additives macromolecular

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  • Chemical & Material Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Wood Science & Technology (AREA)
  • Materials Engineering (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Compositions Of Macromolecular Compounds (AREA)

Abstract

The invention discloses a modified asphalt waterproof heat-insulating coiled material and a preparation method thereof, and the modified asphalt waterproof heat-insulating coiled material comprises the following steps: weighing the following raw materials in parts by weight: 80-100 parts of matrix asphalt, 10-13 parts of modified resin, 5-8 parts of modified filler and 2-4 parts of montmorillonite are mixed to prepare a coating material, the coating material is poured on a PY polyester tire and naturally cooled to prepare a waterproof heat-insulating coiled material, the modified filler has good heat-insulating effect, the mechanical effect of internal heat-insulating gel is enhanced by compounding with a metal organic frame and graphene oxide and wrapping with a polyacrylamide shell, the coiled material is prevented from being impacted in the using process, the porous structure of the heat-insulating gel collapses and cannot achieve the heat-insulating effect, and the water absorption of the modified filler is reduced due to the fact that a large number of hydrophobic groups are contained on the surface, so that the coiled material has good heat-insulating effect and the waterproof effect is not reduced.

Description

Waterproof and heat-insulating modified asphalt coiled material and preparation method thereof
Technical Field
The invention relates to the technical field of asphalt coiled material preparation, in particular to a modified asphalt waterproof heat-insulating coiled material and a preparation method thereof.
Background
The base of the polymer modified asphalt waterproof coiled material is glass fiber felt, jute cloth, polyester non-woven fabric and the like, the synthetic polymer mixture modified asphalt is used as a dip-coating material, mineral materials on sheets, grains or powder are used as coating materials to synthesize polymer films and the like, and the prepared coiled sheet waterproof material is characterized in that the property of the polymer modified asphalt is used for determining the quality of the waterproof coiled material prepared by the polymer modified asphalt, the polymer modified asphalt is favorable for improving the heat resistance of the asphalt, reducing the low-temperature brittleness of the asphalt, and improving the elasticity, the low-temperature deformability and the plasticity of the asphalt, and the polymer modified asphalt is increasingly enhanced in future application as an advanced representative of pavement asphalt technology.
Disclosure of Invention
The invention aims to provide a modified asphalt waterproof heat-insulating coiled material and a preparation method thereof, which solve the problems that the asphalt coiled material at the present stage has poor heat-insulating effect and the waterproof and heat-insulating effects are reduced after being impacted.
The aim of the invention can be achieved by the following technical scheme:
The preparation method of the modified asphalt waterproof heat-insulating coiled material specifically comprises the following steps:
Weighing the following raw materials in parts by weight: 80-100 parts of matrix asphalt, 10-13 parts of modified resin, 5-8 parts of modified filler and 2-4 parts of montmorillonite, stirring the raw materials for 1.5-2 hours at the rotation speed of 4000-5000r/min and the temperature of 170-180 ℃ to prepare a coating material, pouring the coating material on a PY polyester tire, and naturally cooling to prepare the waterproof heat-insulating coiled material.
Further, the modified resin is prepared by the following steps:
step A1: mixing 4-aminophenylboric acid and tetrahydrofuran, introducing nitrogen for protection, reacting for 3-5 hours at the rotating speed of 150-200r/min and the temperature of 50-60 ℃, adding 3-isocyanatopropyl trimethoxy silane, and continuing to react for 1-3 hours to obtain a modifier;
Step A2: mixing aminopropyl end-capped polydimethylsiloxane, dodecyl ethylene oxide and DMF (dimethyl formamide), and reacting for 2-3h under the conditions of the rotating speed of 150-200r/min, the temperature of 40-50 ℃ and the pH value of 10-11 to obtain a modified monomer;
Step A3: mixing polycaprolactone diol and diphenylmethane diisocyanate, introducing nitrogen for protection, reacting for 2-4 hours at the rotation speed of 60-80r/min and the temperature of 85-90 ℃, adding modified monomer, dimethylolpropionic acid and 1, 4-butanediol, reacting for 2-4 hours, cooling to 40-45 ℃, adding triethylamine, reacting for 30-40 minutes, adding KH550, reacting for 30-40 minutes, adding modifier and deionized water, mixing uniformly, heating and drying to obtain the modified resin.
Further, the molar ratio of the 4-aminophenylboronic acid to the 3-isocyanatopropyl trimethoxysilane in the step A1 is 1:1.
Further, the molar ratio of the aminopropyl terminated polydimethylsiloxane to the dodecyloxirane described in step A2 is 1:4.
Further, the dosage ratio of polycaprolactone diol, diphenylmethane diisocyanate, modified monomer, dimethylolpropionic acid, 1, 4-butanediol, triethylamine, KH550, modifier, and deionized water in step A3 is 40g:25g:3.4g:2.04g:4.33g:2.11mL:0.5mL:5g:50mL.
Further, the modified filler is prepared by the following steps:
Mixing hexafluorodianhydride, 4' -diaminodiphenyl ether, aminopropyl end-capped polydimethylsiloxane and DMF, introducing nitrogen, stirring for 3-5 hours at the temperature of 40-50 ℃ at the rotating speed of 200-300r/min, adding heat-insulating gel, uniformly mixing, freeze-drying at the temperature of minus 70 ℃ to prepare a precursor, preserving the heat of the precursor for 1-1.5 hours at the temperature of 220-230 ℃, and then heating to 280-300 ℃ for 1-1.5 hours to prepare the modified filler.
Further, the dosage ratio of the hexafluorodianhydride, the 4,4' -diaminodiphenyl ether, the aminopropyl end-capped polydimethylsiloxane and the heat-insulating gel is 8mmol, 1mmol, 5mmol and 2g, and the molecular weight of the aminopropyl end-capped polydimethylsiloxane is 2000.
Further, the heat insulation gel is prepared by the following steps:
Step B1: mixing 2-aminoimidazole, 3-isocyanatopropyl trimethoxy silane and DMF (dimethyl formamide), reacting for 2-3 hours at the rotation speed of 120-150r/min and the temperature of 40-50 ℃ to obtain an intermediate 1, mixing sodium silicate and deionized water, adding hydrochloric acid solution, and stirring for 10-15 minutes at the rotation speed of 120-150r/min and the temperature of 20-25 ℃ to obtain silica sol;
Step B2: mixing the intermediate 1, perfluorodecyl triethoxysilane and deionized water, adding hydrochloric acid solution, stirring at the rotation speed of 200-300r/min and the temperature of 20-25 ℃ for 30-40min, heating to 45-50 ℃, standing for 30-40min, adding silica sol, uniformly mixing, adjusting the pH value to 6.5, preserving heat for 20-25h, and freeze-drying at the temperature of minus 80 ℃ to obtain gel;
Step B3: dispersing the gel in a methanol solution of zinc nitrate hexahydrate, stirring for 10-15 hours at the rotating speed of 300-500r/min to obtain modified gel, mixing graphene oxide, ascorbic acid, modified gel and deionized water, performing ultrasonic treatment for 10-15 minutes at the frequency of 20-30kHz, heating to 90-95 ℃, preserving heat for 1-1.5 hours, cooling to-70 ℃, and freeze-drying to obtain the heat-insulating gel.
Further, the molar ratio of the 2-aminoimidazole to the 3-isocyanatopropyl trimethoxysilane in the step B1 is 1:1, the volume ratio of the water glass, the deionized water and the hydrochloric acid solution is 1:4:5, and the concentration of the hydrochloric acid solution is 0.75mol/L.
Further, the intermediate 1, perfluorodecyl triethoxysilane, deionized water, hydrochloric acid solution and silica sol described in step B2 are used in the same ratio of 0.5mol:0.5mol:800mL:5mL:300mL, and the hydrochloric acid solution is the same as the hydrochloric acid solution in step B1.
Further, the dosage ratio of the gel to the methanol solution of the zinc nitrate hexahydrate in the step B3 is 1g to 12mL, the concentration of the methanol solution of the zinc nitrate hexahydrate is 0.05mol/L, and the dosage ratio of the graphene oxide, the ascorbic acid, the modified gel and the deionized water is 1g to 10g to 50mL to 200mL.
The invention has the beneficial effects that: the modified asphalt waterproof heat-insulating coiled material is prepared by pouring a coating material on a PY polyester tire and naturally cooling, wherein the coating material comprises the following raw materials in parts by weight: 80-100 parts of matrix asphalt, 10-13 parts of modified resin, 5-8 parts of modified filler and 2-4 parts of montmorillonite, wherein the modified resin takes 4-aminophenylboric acid and 3-isocyanatopropyl trimethoxy silane as raw materials to prepare a modifier, aminopropyl-terminated polydimethylsiloxane and dodecyl ethylene oxide are reacted to enable amino groups on the aminopropyl-terminated polydimethylsiloxane to react with epoxy groups on the dodecyl ethylene oxide to generate new hydroxyl groups to prepare a modified monomer, polycaprolactone diol, diphenylmethane diisocyanate, the modified monomer, dimethylol propionic acid and 1, 4-butanediol are reacted to form hyperbranched polyurethane prepolymer, triethylamine is used for neutralization, KH550 is added for blocking, finally the modified resin is condensed with the modifier in deionized water to prepare the modified resin, the modified resin contains organosilicon hyperbranched grid, long-chain alkyl groups are contained between the grid, the mechanical strength of the resin can be enhanced due to the fact that the amino groups on the aminopropyl-terminated polydimethylsiloxane are contained on the molecular chain, a B-O six-membered cyclic dynamic cross-linking network structure is formed by the modifier, the modified resin is subjected to the reaction of polycaprolactone diol, the diaminotoluene ring and the 3' -diaminopropyl-terminated polyamide is subjected to the reaction under the condition of 3-diaminopropyl-silane, the thermal insulation condition is further prolonged, the thermal insulation coiled material is prepared by the thermal insulation, the thermal insulation coiled material is subjected to the thermal insulation condition of 3-diaminopropyl-3-terminated polyol, 3-diaminopropyl silane, the thermal-terminated polyurethane is subjected to the thermal insulation, and the thermal insulation coiled material is subjected to the thermal insulation reaction, after the thermal insulation condition is subjected to the thermal insulation, and the thermal insulation reaction is subjected to the thermal insulation reaction with the thermal insulation, and the thermal insulation is prepared, the method comprises the steps of preparing an intermediate 1, treating water glass with hydrochloric acid solution to form silica sol, hydrolyzing the intermediate 1 and perfluorodecyl triethoxysilane, adding the silica sol for further polycondensation, and finally freeze-drying to obtain gel, wherein the surface of the gel contains imidazolyl and long-chain halothane, the gel is dispersed in methanol solution of zinc nitrate hexahydrate, imidazolyl on the surface of the gel is matched with zinc ions, a metal organic framework is formed on the surface of the gel to prepare modified gel, pi-pi accumulation is enhanced through reduction of ascorbic acid, graphene oxide and the modified gel are assembled into a three-dimensional structure, and the modified filler has good heat insulation 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
The preparation method of the modified asphalt waterproof heat-insulating coiled material specifically comprises the following steps:
weighing the following raw materials in parts by weight: 80 parts of matrix asphalt, 10 parts of modified resin, 5 parts of modified filler and 2 parts of montmorillonite, stirring the raw materials for 1.5 hours at the temperature of 170 ℃ at the rotation speed of 4000r/min to obtain a coating material, pouring the coating material on a PY polyester tire, and naturally cooling to obtain the waterproof heat-insulating coiled material.
The model of the matrix asphalt is 90# and the mesh number of the montmorillonite is 200.
The modified resin is prepared by the following steps:
Step A1: mixing 4-aminophenylboric acid and tetrahydrofuran, introducing nitrogen for protection, reacting for 3 hours at the rotation speed of 150r/min and the temperature of 50 ℃, adding 3-isocyanatopropyl trimethoxy silane, and continuing to react for 1 hour to obtain a modifier;
Step A2: mixing aminopropyl end-capped polydimethylsiloxane, dodecyl ethylene oxide and DMF (dimethyl formamide), and reacting for 2 hours under the conditions of the rotating speed of 150r/min, the temperature of 40 ℃ and the pH value of 10 to obtain a modified monomer;
Step A3: mixing polycaprolactone diol and diphenylmethane diisocyanate, introducing nitrogen for protection, reacting for 2 hours at the rotation speed of 60r/min and the temperature of 85 ℃, adding a modified monomer, dimethylolpropionic acid and 1, 4-butanediol for reacting for 2 hours, cooling to 40 ℃, adding triethylamine for reacting for 30 minutes, adding KH550 for reacting for 30 minutes, adding a modifier and deionized water for uniform mixing, and heating and drying to obtain the modified resin.
The molar ratio of the 4-aminophenylboronic acid to the 3-isocyanatopropyl trimethoxysilane in the step A1 is 1:1.
The molar ratio of the aminopropyl terminated polydimethylsiloxane to the dodecyl ethylene oxide described in step A2 was 1:4.
The dosage ratio of polycaprolactone diol, diphenylmethane diisocyanate, modified monomer, dimethylolpropionic acid, 1, 4-butanediol, triethylamine, KH550, modifier and deionized water in step A3 is 40g:25g:3.4g:2.04g:4.33g:2.11mL:0.5mL:5g:50mL.
The modified filler is prepared by the following steps:
Mixing hexafluorodianhydride, 4' -diaminodiphenyl ether, aminopropyl end-capped polydimethylsiloxane and DMF, introducing nitrogen, stirring for 3 hours at the temperature of 40 ℃ at the rotation speed of 200r/min, adding heat-insulating gel, uniformly mixing, freeze-drying at the temperature of minus 70 ℃ to prepare a precursor, preserving the heat of the precursor at the temperature of 220 ℃ for 1 hour, and then heating to 280 ℃ and preserving the heat for 1 hour to prepare the modified filler.
The dosage ratio of the hexafluorodianhydride, the 4,4' -diaminodiphenyl ether, the aminopropyl end-capped polydimethylsiloxane to the heat insulation gel is 8mmol, 1mmol, 5mmol and 2g, and the molecular weight of the aminopropyl end-capped polydimethylsiloxane is 2000.
The heat insulation gel is prepared by the following steps:
step B1: mixing 2-aminoimidazole, 3-isocyanatopropyl trimethoxy silane and DMF (dimethyl formamide), reacting for 2 hours at the rotation speed of 120r/min and the temperature of 40 ℃ to obtain an intermediate 1, mixing sodium silicate and deionized water, adding hydrochloric acid solution, and stirring for 10 minutes at the rotation speed of 120r/min and the temperature of 20 ℃ to obtain silica sol;
Step B2: mixing the intermediate 1, perfluorodecyl triethoxysilane and deionized water, adding hydrochloric acid solution, stirring at a rotation speed of 200r/min and a temperature of 20 ℃ for 30min, heating to 45 ℃, standing for 30min, adding silica sol, uniformly mixing, adjusting the pH value to 6.5, preserving heat for 20h, and freeze-drying at a temperature of minus 80 ℃ to obtain gel;
Step B3: dispersing the gel in a methanol solution of zinc nitrate hexahydrate, stirring for 10 hours at the rotating speed of 300r/min to obtain modified gel, mixing graphene oxide, ascorbic acid, the modified gel and deionized water, performing ultrasonic treatment for 10 minutes at the frequency of 20kHz, heating to 90 ℃, preserving heat for 1 hour, cooling to minus 70 ℃, and performing freeze drying to obtain the heat insulation gel.
The mol ratio of the 2-aminoimidazole to the 3-isocyanatopropyl trimethoxysilane in the step B1 is 1:1, the volume ratio of the water glass to the deionized water to the hydrochloric acid solution is 1:4:5, and the concentration of the hydrochloric acid solution is 0.75mol/L.
The dosage ratio of the intermediate 1, the perfluorodecyl triethoxysilane, the deionized water, the hydrochloric acid solution and the silica sol in the step B2 is 0.5mol:0.5mol:800mL:5mL:300mL, and the hydrochloric acid solution is the same as the hydrochloric acid solution in the step B1.
The dosage ratio of the gel to the methanol solution of the zinc nitrate hexahydrate in the step B3 is 1g to 12mL, the concentration of the methanol solution of the zinc nitrate hexahydrate is 0.05mol/L, and the dosage ratio of the graphene oxide, the ascorbic acid, the modified gel and the deionized water is 1g to 10g to 50mL to 200mL.
Example 2
The preparation method of the modified asphalt waterproof heat-insulating coiled material specifically comprises the following steps:
Weighing the following raw materials in parts by weight: 90 parts of matrix asphalt, 12 parts of modified resin, 6 parts of modified filler and 3 parts of montmorillonite, stirring the raw materials for 2 hours at the temperature of 175 ℃ at the rotation speed of 4000r/min to obtain a coating material, pouring the coating material on a PY polyester tire, and naturally cooling to obtain the waterproof heat-insulating coiled material.
The model of the matrix asphalt is 90# and the mesh number of the montmorillonite is 200.
The modified resin is prepared by the following steps:
Step A1: mixing 4-aminophenylboric acid and tetrahydrofuran, introducing nitrogen for protection, reacting for 4 hours at the rotation speed of 150r/min and the temperature of 55 ℃, adding 3-isocyanatopropyl trimethoxy silane, and continuing to react for 2 hours to obtain a modifier;
step A2: mixing aminopropyl end-capped polydimethylsiloxane, dodecyl ethylene oxide and DMF (dimethyl formamide), and reacting for 2 hours under the conditions of the rotating speed of 150r/min, the temperature of 45 ℃ and the pH value of 11 to obtain a modified monomer;
Step A3: mixing polycaprolactone diol and diphenylmethane diisocyanate, introducing nitrogen for protection, reacting for 3 hours at the rotation speed of 60r/min and the temperature of 90 ℃, adding a modified monomer, dimethylolpropionic acid and 1, 4-butanediol for reacting for 3 hours, cooling to 45 ℃, adding triethylamine for reacting for 35 minutes, adding KH550 for reacting for 35 minutes, adding a modifier and deionized water for uniform mixing, and heating and drying to obtain the modified resin.
The molar ratio of the 4-aminophenylboronic acid to the 3-isocyanatopropyl trimethoxysilane in the step A1 is 1:1.
The molar ratio of the aminopropyl terminated polydimethylsiloxane to the dodecyl ethylene oxide described in step A2 was 1:4.
The dosage ratio of polycaprolactone diol, diphenylmethane diisocyanate, modified monomer, dimethylolpropionic acid, 1, 4-butanediol, triethylamine, KH550, modifier and deionized water in step A3 is 40g:25g:3.4g:2.04g:4.33g:2.11mL:0.5mL:5g:50mL.
The modified filler is prepared by the following steps:
Mixing hexafluorodianhydride, 4' -diaminodiphenyl ether, aminopropyl end-capped polydimethylsiloxane and DMF, introducing nitrogen, stirring for 4 hours at the temperature of 45 ℃ at the rotation speed of 300r/min, adding heat-insulating gel, uniformly mixing, freeze-drying at the temperature of minus 70 ℃ to obtain a precursor, preserving the heat of the precursor at the temperature of 225 ℃ for 1.5 hours, and then heating to 290 ℃ for 1.5 hours to obtain the modified filler.
The dosage ratio of the hexafluorodianhydride, the 4,4' -diaminodiphenyl ether, the aminopropyl end-capped polydimethylsiloxane to the heat insulation gel is 8mmol, 1mmol, 5mmol and 2g, and the molecular weight of the aminopropyl end-capped polydimethylsiloxane is 2000.
The heat insulation gel is prepared by the following steps:
Step B1: mixing 2-aminoimidazole, 3-isocyanatopropyl trimethoxy silane and DMF (dimethyl formamide), reacting for 3 hours at the temperature of 45 ℃ at the speed of 120r/min to obtain an intermediate 1, mixing sodium silicate and deionized water, adding hydrochloric acid solution, and stirring for 15 minutes at the temperature of 20 ℃ at the speed of 150r/min to obtain silica sol;
Step B2: mixing the intermediate 1, perfluorodecyl triethoxysilane and deionized water, adding hydrochloric acid solution, stirring at a rotation speed of 200r/min and a temperature of 25 ℃ for 35min, heating to 48 ℃, standing for 35min, adding silica sol, uniformly mixing, adjusting the pH value to 6.5, preserving heat for 23h, and freeze-drying at a temperature of minus 80 ℃ to obtain gel;
Step B3: dispersing the gel in a methanol solution of zinc nitrate hexahydrate, stirring for 15 hours at the rotating speed of 300r/min to obtain modified gel, mixing graphene oxide, ascorbic acid, the modified gel and deionized water, performing ultrasonic treatment for 15 minutes at the frequency of 25kHz, heating to 95 ℃, preserving heat for 1.5 hours, cooling to minus 70 ℃, and performing freeze drying to obtain the heat insulation gel.
The mol ratio of the 2-aminoimidazole to the 3-isocyanatopropyl trimethoxysilane in the step B1 is 1:1, the volume ratio of the water glass to the deionized water to the hydrochloric acid solution is 1:4:5, and the concentration of the hydrochloric acid solution is 0.75mol/L.
The dosage ratio of the intermediate 1, the perfluorodecyl triethoxysilane, the deionized water, the hydrochloric acid solution and the silica sol in the step B2 is 0.5mol:0.5mol:800mL:5mL:300mL, and the hydrochloric acid solution is the same as the hydrochloric acid solution in the step B1.
The dosage ratio of the gel to the methanol solution of the zinc nitrate hexahydrate in the step B3 is 1g to 12mL, the concentration of the methanol solution of the zinc nitrate hexahydrate is 0.05mol/L, and the dosage ratio of the graphene oxide, the ascorbic acid, the modified gel and the deionized water is 1g to 10g to 50mL to 200mL.
Example 3
The preparation method of the modified asphalt waterproof heat-insulating coiled material specifically comprises the following steps:
Weighing the following raw materials in parts by weight: 100 parts of matrix asphalt, 13 parts of modified resin, 8 parts of modified filler and 4 parts of montmorillonite, stirring the raw materials for 2 hours at the rotation speed of 5000r/min and the temperature of 180 ℃ to obtain a coating material, pouring the coating material on a PY polyester tire, and naturally cooling to obtain the waterproof heat-insulating coiled material.
The model of the matrix asphalt is 90# and the mesh number of the montmorillonite is 200.
The modified resin is prepared by the following steps:
Step A1: mixing 4-aminophenylboric acid and tetrahydrofuran, introducing nitrogen for protection, reacting for 5 hours at the rotation speed of 200r/min and the temperature of 60 ℃, adding 3-isocyanatopropyl trimethoxy silane, and continuing to react for 3 hours to obtain a modifier;
Step A2: mixing aminopropyl end-capped polydimethylsiloxane, dodecyl ethylene oxide and DMF, and reacting for 3 hours under the conditions of the rotating speed of 200r/min, the temperature of 50 ℃ and the pH value of 11 to obtain a modified monomer;
Step A3: mixing polycaprolactone diol and diphenylmethane diisocyanate, introducing nitrogen for protection, reacting for 4 hours at the rotation speed of 80r/min and the temperature of 90 ℃, adding a modified monomer, dimethylolpropionic acid and 1, 4-butanediol for reacting for 4 hours, cooling to 45 ℃, adding triethylamine for reacting for 40 minutes, adding KH550 for reacting for 40 minutes, adding a modifier and deionized water for uniformly mixing, and heating and drying to obtain the modified resin.
The molar ratio of the 4-aminophenylboronic acid to the 3-isocyanatopropyl trimethoxysilane in the step A1 is 1:1.
The molar ratio of the aminopropyl terminated polydimethylsiloxane to the dodecyl ethylene oxide described in step A2 was 1:4.
The dosage ratio of polycaprolactone diol, diphenylmethane diisocyanate, modified monomer, dimethylolpropionic acid, 1, 4-butanediol, triethylamine, KH550, modifier and deionized water in step A3 is 40g:25g:3.4g:2.04g:4.33g:2.11mL:0.5mL:5g:50mL.
The modified filler is prepared by the following steps:
Mixing hexafluorodianhydride, 4' -diaminodiphenyl ether, aminopropyl end-capped polydimethylsiloxane and DMF, introducing nitrogen, stirring for 5 hours at the temperature of 50 ℃ at the rotating speed of 300r/min, adding heat-insulating gel, uniformly mixing, freeze-drying at the temperature of minus 70 ℃ to prepare a precursor, preserving the heat of the precursor at the temperature of 230 ℃ for 1.5 hours, and then heating to 300 ℃ and preserving the heat for 1.5 hours to prepare the modified filler.
The dosage ratio of the hexafluorodianhydride, the 4,4' -diaminodiphenyl ether, the aminopropyl end-capped polydimethylsiloxane to the heat insulation gel is 8mmol, 1mmol, 5mmol and 2g, and the molecular weight of the aminopropyl end-capped polydimethylsiloxane is 2000.
The heat insulation gel is prepared by the following steps:
Step B1: mixing 2-aminoimidazole, 3-isocyanatopropyl trimethoxy silane and DMF (dimethyl formamide), reacting for 3 hours at the speed of 150r/min and the temperature of 50 ℃ to obtain an intermediate 1, mixing sodium silicate and deionized water, adding hydrochloric acid solution, and stirring for 15 minutes at the speed of 150r/min and the temperature of 25 ℃ to obtain silica sol;
Step B2: mixing the intermediate 1, perfluorodecyl triethoxysilane and deionized water, adding hydrochloric acid solution, stirring at a rotation speed of 300r/min and a temperature of 25 ℃ for 40min, heating to 50 ℃, standing for 40min, adding silica sol, uniformly mixing, adjusting the pH value to 6.5, preserving heat for 25h, and freeze-drying at a temperature of minus 80 ℃ to obtain gel;
Step B3: dispersing the gel in methanol solution of zinc nitrate hexahydrate, stirring for 15 hours at the rotating speed of 500r/min to obtain modified gel, mixing graphene oxide, ascorbic acid, modified gel and deionized water, performing ultrasonic treatment for 15 minutes at the frequency of 30kHz, heating to 95 ℃, preserving heat for 1.5 hours, cooling to minus 70 ℃, and freeze-drying to obtain the heat-insulating gel.
The mol ratio of the 2-aminoimidazole to the 3-isocyanatopropyl trimethoxysilane in the step B1 is 1:1, the volume ratio of the water glass to the deionized water to the hydrochloric acid solution is 1:4:5, and the concentration of the hydrochloric acid solution is 0.75mol/L.
The dosage ratio of the intermediate 1, the perfluorodecyl triethoxysilane, the deionized water, the hydrochloric acid solution and the silica sol in the step B2 is 0.5mol:0.5mol:800mL:5mL:300mL, and the hydrochloric acid solution is the same as the hydrochloric acid solution in the step B1.
The dosage ratio of the gel to the methanol solution of the zinc nitrate hexahydrate in the step B3 is 1g to 12mL, the concentration of the methanol solution of the zinc nitrate hexahydrate is 0.05mol/L, and the dosage ratio of the graphene oxide, the ascorbic acid, the modified gel and the deionized water is 1g to 10g to 50mL to 200mL.
Comparative example 1
This comparative example was identical to example 1 in that no modifier was added and the remainder.
Comparative example 2
This comparative example was identical to example 1 except that no modifying monomer was added.
Comparative example 3
Compared with the comparative example 1, the comparative example is prepared by mixing methyltrimethoxysilane and deionized water, adding hydrochloric acid solution, stirring for 30min at the rotation speed of 200r/min and the temperature of 20 ℃, heating to 45 ℃, standing for 30min, adding silica sol, uniformly mixing, adjusting the pH value to 6.5, preserving heat for 20h, and freeze-drying at the temperature of minus 80 ℃ to obtain a product which replaces heat insulation gel, wherein the rest steps are the same.
Comparative example 4
This comparative example uses a heat insulating gel instead of the modified filler as compared with example 1, and the rest of the procedure is the same.
The coiled materials prepared in examples 1-3 and comparative examples 1-4 were prepared into 25mm×25mm×5mm samples, and the coiled materials were tested for thermal conductivity at different ambient temperatures and after cyclic compression using a TPS2500s thermal conductivity meter, with a compression strength of 300kPa, and the waterproof effect was measured in accordance with the mode B in GB/T328.10-2007, and the measurement results are shown in the following table.
As can be seen from the above table, the present application has good waterproof and heat-insulating 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 (10)

1. A preparation method of a modified asphalt waterproof heat-insulating coiled material is characterized by comprising the following steps: the method specifically comprises the following steps:
Weighing the following raw materials in parts by weight: 80-100 parts of matrix asphalt, 10-13 parts of modified resin, 5-8 parts of modified filler and 2-4 parts of montmorillonite, uniformly mixing the raw materials to prepare a coating material, pouring the coating material on a PY polyester tire, and naturally cooling to prepare a waterproof heat-insulating coiled material;
The modified resin is prepared by the following steps:
Step A1: mixing 4-aminophenylboric acid and tetrahydrofuran for reaction, adding 3-isocyanatopropyl trimethoxy silane, and continuing the reaction to obtain a modifier;
step A2: mixing and reacting aminopropyl end-capped polydimethylsiloxane, dodecyl ethylene oxide and DMF to prepare a modified monomer;
Step A3: mixing polycaprolactone diol and diphenylmethane diisocyanate for reaction, adding modified monomer, dimethylolpropionic acid and 1, 4-butanediol for reaction, cooling, adding triethylamine for reaction, adding KH550 for reaction, adding modifier and deionized water for uniform mixing, heating and drying to obtain modified resin;
The modified filler is prepared by the following steps:
And mixing and stirring hexafluorodianhydride, 4' -diaminodiphenyl ether, aminopropyl end-capped polydimethylsiloxane and DMF, adding heat-insulating gel, uniformly mixing, freeze-drying to obtain a precursor, and carrying out high-temperature heat preservation on the precursor to obtain the modified filler.
2. The method for preparing the modified asphalt waterproof heat-insulating coiled material according to claim 1, which is characterized in that: the molar ratio of the 4-aminophenylboronic acid to the 3-isocyanatopropyl trimethoxysilane in the step A1 is 1:1.
3. The method for preparing the modified asphalt waterproof heat-insulating coiled material according to claim 1, which is characterized in that: the molar ratio of the aminopropyl terminated polydimethylsiloxane to the dodecyl ethylene oxide described in step A2 was 1:4.
4. The method for preparing the modified asphalt waterproof heat-insulating coiled material according to claim 1, which is characterized in that: the dosage ratio of polycaprolactone diol, diphenylmethane diisocyanate, modified monomer, dimethylolpropionic acid, 1, 4-butanediol, triethylamine, KH550, modifier and deionized water in step A3 is 40g:25g:3.4g:2.04g:4.33g:2.11mL:0.5mL:5g:50mL.
5. The method for preparing the modified asphalt waterproof heat-insulating coiled material according to claim 1, which is characterized in that: the dosage ratio of the hexafluorodianhydride, the 4,4' -diaminodiphenyl ether, the aminopropyl end-capped polydimethylsiloxane and the heat insulation gel is 8mmol, 1mmol, 5mmol and 2g.
6. The method for preparing the modified asphalt waterproof heat-insulating coiled material according to claim 1, which is characterized in that: the heat insulation gel is prepared by the following steps:
step B1: mixing 2-aminoimidazole, 3-isocyanatopropyl trimethoxy silane and DMF for reaction to prepare an intermediate 1, mixing water glass and deionized water, adding hydrochloric acid solution, and stirring for treatment to prepare silica sol;
Step B2: mixing the intermediate 1, perfluorodecyl triethoxysilane and deionized water, adding hydrochloric acid solution, stirring, heating and standing, adding silica sol, mixing uniformly, adjusting pH to be acidic, heat-preserving, and freeze-drying to obtain gel;
step B3: dispersing the gel in a methanol solution of zinc nitrate hexahydrate, stirring to obtain modified gel, mixing graphene oxide, ascorbic acid, modified gel and deionized water, performing ultrasonic treatment, heating, preserving heat, and freeze-drying to obtain the heat-insulating gel.
7. The method for preparing the modified asphalt waterproof heat-insulating coiled material according to claim 6, which is characterized in that: the mol ratio of the 2-aminoimidazole to the 3-isocyanatopropyl trimethoxysilane in the step B1 is 1:1, and the volume ratio of the water glass to the deionized water to the hydrochloric acid solution is 1:4:5.
8. The method for preparing the modified asphalt waterproof heat-insulating coiled material according to claim 6, which is characterized in that: the dosage ratio of the intermediate 1, the perfluorodecyl triethoxysilane, the deionized water, the hydrochloric acid solution and the silica sol in the step B2 is 0.5mol:0.5mol:800mL:5mL:300mL.
9. The method for preparing the modified asphalt waterproof heat-insulating coiled material according to claim 6, which is characterized in that: the dosage ratio of the gel to the methanol solution of the zinc nitrate hexahydrate in the step B3 is 1g to 12mL, and the dosage ratio of the graphene oxide, the ascorbic acid, the modified gel and the deionized water is 1g to 10g to 50mL to 200mL.
10. A modified asphalt waterproof heat-insulating coiled material is characterized in that: the preparation method according to any one of claims 1 to 9.
CN202410349939.2A 2024-03-26 2024-03-26 Waterproof and heat-insulating modified asphalt coiled material and preparation method thereof Active CN117943264B (en)

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CN108084880A (en) * 2017-12-11 2018-05-29 四川蜀羊防水材料有限公司 Thermal insulation elastic modified asphalt coat material and preparation method thereof, waterproof roll
CN111038024A (en) * 2019-12-13 2020-04-21 安徽亿脉通讯科技有限公司 Composite polymer modified asphalt waterproof coiled material and preparation method thereof
CN114395927A (en) * 2022-02-09 2022-04-26 江苏贝施特防水科技有限公司 Anti-aging elastomer SBS (styrene butadiene styrene) modified asphalt waterproof coiled material and preparation method thereof
CN115572525A (en) * 2022-10-12 2023-01-06 夏德祥 Heat-preservation and heat-insulation coiled material and preparation process thereof
CN116102878A (en) * 2023-03-02 2023-05-12 南京富顺塑业有限公司 High-strength and high-toughness plastic film and preparation method thereof
CN116253882A (en) * 2022-09-05 2023-06-13 南京大学 Preparation method of amino hyperbranched siloxane and modified polyimide aerogel material thereof
CN117304800A (en) * 2023-09-28 2023-12-29 嘉兴富瑞邦新材料科技有限公司 Aerogel ceramic coating and preparation process thereof

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105038273A (en) * 2015-07-28 2015-11-11 蚌埠南自仪表有限公司 Silica gel asphalt waterproof coiled material
CN108084880A (en) * 2017-12-11 2018-05-29 四川蜀羊防水材料有限公司 Thermal insulation elastic modified asphalt coat material and preparation method thereof, waterproof roll
CN111038024A (en) * 2019-12-13 2020-04-21 安徽亿脉通讯科技有限公司 Composite polymer modified asphalt waterproof coiled material and preparation method thereof
CN114395927A (en) * 2022-02-09 2022-04-26 江苏贝施特防水科技有限公司 Anti-aging elastomer SBS (styrene butadiene styrene) modified asphalt waterproof coiled material and preparation method thereof
CN116253882A (en) * 2022-09-05 2023-06-13 南京大学 Preparation method of amino hyperbranched siloxane and modified polyimide aerogel material thereof
CN115572525A (en) * 2022-10-12 2023-01-06 夏德祥 Heat-preservation and heat-insulation coiled material and preparation process thereof
CN116102878A (en) * 2023-03-02 2023-05-12 南京富顺塑业有限公司 High-strength and high-toughness plastic film and preparation method thereof
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