CN114686014A - Modified asphalt with good high-temperature cohesiveness and preparation method thereof - Google Patents
Modified asphalt with good high-temperature cohesiveness and preparation method thereof Download PDFInfo
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Abstract
The invention discloses modified asphalt with good high-temperature cohesiveness and a preparation method thereof, and relates to the technical field of asphalt preparation. The modified asphalt with good high-temperature cohesiveness, which is prepared by the invention, comprises modified carbon nanotubes, styrene-butadiene-styrene block copolymers, tackifiers, aromatic oil and matrix asphalt, wherein the modified carbon nanotubes are prepared by coating pre-modified carbon nanotubes with aqueous tackifying resin; phenolic resin and modified polyether form a cross-linking structure to enhance the toughness of the aqueous tackifying resin, and then the hydroxylated multi-walled carbon nanotubes grafted with 4,4' -diphenylmethane diisocyanate are coated to enhance the impact resistance of the modified asphalt; the tackifier is modified polyethylene naphthalate, so that the steric hindrance is large, the movement of calcium carbonate and the modified carbon nano tubes is limited, and the cohesiveness of the modified asphalt is enhanced.
Description
Technical Field
The invention relates to the technical field of asphalt preparation materials, in particular to modified asphalt with good high-temperature cohesiveness and a preparation method thereof.
Background
The asphalt pavement has the defects of cracks, looseness, pits and the like in the long-term service process, and the defects are related to the aging of asphalt besides design and construction factors; meanwhile, oxygen can chemically react with various components in the asphalt, and functional groups in the asphalt are changed under the combined action of heat and oxygen to generate carbonyl and sulfoxide groups; the change of the components and the functional groups of the asphalt causes the asphalt to be hardened and the flexibility to be reduced, so that the flow property of the asphalt is poor, and the asphalt pavement gradually generates micro cracks, and then diseases such as cracks, pits and the like are formed in an expanding mode.
Therefore, the used asphalt is required to have high cohesiveness and impact resistance, and the common modified asphalt is difficult to meet the requirements; and the occurrence of diseases can be reduced only if the rubber has higher viscosity and impact resistance; therefore, the invention researches and prepares the modified asphalt with good cohesiveness, impact resistance and good high-temperature cohesiveness.
Disclosure of Invention
The invention aims to provide modified asphalt with good high-temperature cohesiveness and a preparation method thereof, so as to solve the problems in the background technology.
A modified asphalt with good high-temperature cohesiveness comprises a modified carbon nano tube prepared by coating a pre-modified carbon nano tube with an aqueous tackifying resin, a styrene-butadiene-styrene block copolymer, a tackifier, aromatic oil and matrix asphalt; the modified carbon nano tube is prepared by coating a pre-modified carbon nano tube with aqueous tackifying resin; the tackifier is modified polyethylene naphthalate.
Preferably, the aqueous tackifying resin is prepared by introducing modified polyether during the preparation of phenolic resin and performing amination; the modified polyether is prepared by introducing polyethylene oxide containing benzene rings to active polyether; the pre-modified carbon nano tube is prepared by grafting and modifying 4,4' -diphenylmethane diisocyanate and a hydroxylated multi-wall carbon nano tube.
Preferably, the modified polyethylene naphthalate is prepared by connecting polyethylene glycol phosphate with calcium carbonate and performing esterification reaction with dimethyl 2, 6-naphthalene dicarboxylate.
Preferably, the base asphalt is imported No. 70 base asphalt; the cosolvent is aromatic oil.
Preferably, the preparation method of the modified asphalt with good high-temperature cohesiveness comprises the following specific steps:
(1) mixing polyethylene glycol and tetrahydrofuran according to a mass ratio of 1: 2-1: 4, placing the mixture in an ice bath at 0-2 ℃, adding initiator boron trifluoride diethyl etherate with the mass of 0.003-0.005 time of that of the polyethylene glycol in a nitrogen atmosphere, stirring the mixture at 30-50 rpm for reaction for 15-30 min, dropwise adding propylene oxide with the mass of 0.05-0.2 time of that of the polyethylene glycol at a speed of 10-15 drops/s, after the reaction is carried out for 4-8 h, adjusting the pH to 7 by using sodium bicarbonate, adding trihydroxymethyl propane with the mass of 0.05-0.1 time of the polyethylene glycol and polyethylene oxide with the mass of 0.1-0.2 time of the polyethylene glycol and containing benzene rings, continuing the reaction for 5-8 h, finally adding deionized water with the temperature of 80-90 ℃ for layering, and carrying out reduced pressure distillation in an oil bath at the temperature of 100 ℃ to prepare modified polyether;
(2) mixing phenol and triethylamine according to the mass ratio of 8: 1-10: 1, heating to 60-70 ℃, stirring until the mixture is dissolved, adding a formaldehyde water solution with the mass fraction of 37-40% and the mass fraction of 3-5 times of that of the phenol, cooling to 40-43 ℃, stirring at the speed of 50-100 rpm, dropwise adding a sodium hydroxide solution with the mass fraction of 40-50% at the speed of 3-5 ml/min, adjusting the temperature to 50-52 ℃ after dropwise adding, adding modified polyether with the mass fraction of 0.2-0.5 time of that of the phenol, reacting for 1-3 h, heating to 80-82 ℃, reacting for 2-4 h, cooling to 30-40 ℃, adjusting the pH to 6.8-7.2 with hydrochloric acid, and preparing a water-based tackifying resin;
(3) mixing aqueous tackifying resin, dimethylolpropionic acid, acetone and pre-modified carbon nano tubes according to the mass ratio of 0.8:2:10: 3-2: 3:20:5, adding hydroxyethyl methacrylate with the mass of 0.02-0.04 time of that of the aqueous tackifying resin, heating to 40-50 ℃, reacting for 6-8 hours, adding triethylamine with the mass of 0.005-0.008 time of that of the aqueous tackifying resin, adding deionized water with the mass of 2-4 times of that of the aqueous tackifying resin at 50-100 rpm for emulsification and rotary evaporation, and finally performing vacuum drying at 55-60 ℃ to prepare modified carbon nano tubes;
(4) mixing dimethyl 2, 6-naphthalene dicarboxylate and a composite material according to a mass ratio of 1.2: 1-1.5: 1, preheating for 40-50 min at 80-100 ℃, transferring to a reaction kettle, heating to 140-160 ℃ in a nitrogen atmosphere, adding a catalyst zinc acetate 0.002-0.008 times of the mass of the composite material, stirring and reacting for 18-20 h at 50-100 rpm, cooling to room temperature, washing with deionized water for 10-20 min, and preparing a tackifier;
(5) uniformly mixing the component A and the component B according to the mass ratio of 14: 5-18: 8, placing the mixture in a high-speed shearing machine, shearing the mixture for 1-2 hours at the temperature of 145-155 ℃ at 4000-5000 rpm, transferring the mixture to a common stirrer, and continuously stirring the mixture for 1-2 hours at the temperature of 1000-2000 rpm to prepare the modified asphalt with good high-temperature cohesiveness.
Preferably, in the step (1): the preparation method of the polyethylene oxide containing the benzene ring comprises the following steps: mixing cyclohexane, polyethylene glycol monomethyl ether, sodium hydroxide, anhydrous sodium sulfate and deionized water according to the mass ratio of 2:3:0.5:0.02: 6-2: 4:0.8:0.05:8, purging with argon for 3-5 min, reacting at 40-50 ℃ for 1-2 h, dropwise adding p-chloromethyl styrene with the mass 0.2-0.5 times that of cyclohexane at the rate of 3-5 ml/min, heating to 60-65 ℃, continuing to react for 2-3 h, extracting once with deionized water, extracting 3-5 times with dichloromethane, and performing rotary evaporation to obtain the polyethylene oxide containing benzene rings.
Preferably, in the step (3): the preparation method of the pre-modified carbon nano tube comprises the following steps: mixing a hydroxylated carbon nanotube and N, N-dimethylformamide according to a mass ratio of 1: 50-1: 100, ultrasonically dispersing for 30-50 min at 40-50 kHz to prepare a hydroxylated carbon nanotube dispersion liquid, mixing the hydroxylated carbon nanotube dispersion liquid and a N, N-dimethylformamide solution of 4,4' -diphenylmethane diisocyanate with the mass fraction of 30-50% according to a mass ratio of 5: 2-5: 3, then dropwise adding dibutyltin dilaurate with the mass of 0.01-0.03 time of that of the hydroxylated carbon nanotube at the speed of 3-8 ml/min, heating to 50-60 ℃, reacting for 12-16 h, centrifuging after the reaction is finished, washing for 5-8 times by using N, N-dimethylformamide, and finally drying for 4-6 h in a vacuum drying box with the temperature of 50-60 ℃ to prepare the pre-modified carbon nanotube.
Preferably, in the step (4): the preparation method of the composite material comprises the following steps: dispersing calcium oxide into boiling deionized water with the mass 15-20 times that of the calcium oxide, stirring to obtain calcium hydroxide slurry, standing for 12-24 h, filtering, adding polyethylene glycol phosphate with the mass 0.2-0.4 time that of the calcium oxide, stirring at 30-50 rpm, reacting for 30-50 min, introducing mixed gas of carbon dioxide and nitrogen with the volume ratio of 2: 1-3: 1 at the flow rate of 800-1000 sscm, keeping the reaction temperature at 15-20 ℃, reacting for 3-6 h, filtering, washing and drying to obtain the composite material.
Preferably, in the step (5): the preparation process of the component A comprises the following steps: heating the matrix asphalt to 140-150 ℃, keeping the temperature for 0.5-1 h, adding a styrene-butadiene-styrene block copolymer with the mass of 0.12-0.14 time of that of the matrix asphalt, shearing the mixture in a high-speed shearing machine at 4000-5000 rpm and 145-155 ℃ for 10-20 min, and cooling to room temperature to obtain the component A.
Preferably, in the step (5): the preparation process of the component B comprises the following steps: and mixing the modified carbon nano tube, the tackifier and the aromatic oil according to the mass ratio of 3:5: 20-8: 10:24, and uniformly stirring to obtain the component B.
Compared with the prior art, the invention has the following beneficial effects:
the modified asphalt with good high-temperature cohesiveness, which is prepared by the invention, comprises modified carbon nanotubes, styrene-butadiene-styrene block copolymers, tackifiers, aromatic oil and matrix asphalt, wherein the modified carbon nanotubes are prepared by coating pre-modified carbon nanotubes with aqueous tackifying resin;
the aqueous tackifying resin is prepared by introducing modified polyether during the preparation of phenolic resin and carrying out amination; the modified polyether is prepared by introducing polyethylene oxide containing benzene rings to active polyether, and secondary hydroxyl on the active polyether is converted into primary hydroxyl to improve reaction activity; hydroxyl on the modified polyether can react with hydroxymethyl on a phenolic resin polycondensate to graft the modified polyether onto the phenolic resin, and the hydroxymethyl on the phenolic resin polycondensate can also react with hydrogen on a phenol ring to generate methylene, so that the phenolic resin and the modified polyether form a cross-linked structure, the toughness of the aqueous tackifying resin is enhanced, and the cohesiveness of the modified asphalt is enhanced; the pre-modified carbon nano tube is prepared by grafting and modifying 4,4' -diphenylmethane diisocyanate and hydroxylated multi-wall carbon nano tube, so that polyurethane is formed between the aqueous tackifying resin and the pre-modified carbon nano tube, a buffer layer is formed on the surface of the pre-modified carbon nano tube, the dispersibility is improved, and the impact resistance of the modified asphalt is enhanced;
the tackifier is modified polyethylene naphthalate which is prepared by connecting polyethylene glycol phosphate with calcium carbonate and carrying out esterification reaction with dimethyl 2, 6-naphthalene dicarboxylate; one end of the polyethylene glycol phosphate forms a chemical bond with the surface of calcium carbonate to reduce the surface energy, and then the polyethylene glycol phosphate and the 2, 6-dimethyl naphthalate are subjected to esterification reaction to form polyethylene naphthalate with calcium carbonate, the calcium carbonate is uniformly dispersed while a benzene ring is introduced, the large steric hindrance in the polyethylene naphthalate limits the movement of the calcium carbonate and the modified carbon nanotube, and the cohesiveness of the modified asphalt is enhanced.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
In order to more clearly illustrate the method of the present invention, the following examples are given, and the method for testing each index of the modified asphalt with good high-temperature adhesion prepared in the examples and comparative examples is as follows:
impact resistance: the modified asphalt with good high-temperature cohesiveness prepared in the examples and the comparative examples are subjected to penetration, ductility and softening point tests according to GB/T4509, GB/T4508 and GB/T4507;
adhesion: the modified asphalt with good high-temperature cohesiveness prepared in the examples and the comparative examples is subjected to dynamic viscosity test at 60 ℃ by referring to SH/T0557.
Example 1
(1) Mixing cyclohexane, polyethylene glycol monomethyl ether, sodium hydroxide, anhydrous sodium sulfate and deionized water according to the mass ratio of 2:3:0.5:0.02:6, purging with argon for 3min, reacting at 40 ℃ for 1h, dropwise adding p-chloromethyl styrene with the mass of 0.2 time of that of the cyclohexane at the speed of 3ml/min, heating to 60 ℃, continuing to react for 2h, extracting once with deionized water, extracting for 3 times with dichloromethane and carrying out rotary evaporation to prepare polyethylene oxide containing benzene rings; mixing polyethylene glycol and tetrahydrofuran according to a mass ratio of 1:2, placing the mixture in an ice bath at 0 ℃, adding boron trifluoride diethyl etherate as an initiator with the mass of 0.003 time that of the polyethylene glycol in the nitrogen atmosphere, stirring the mixture at 30rpm for reaction for 15min, dropwise adding propylene oxide with the mass of 0.05 time that of the polyethylene glycol at the speed of 10 drops/s, after the reaction is carried out for 4h, adjusting the pH to 7 by using sodium bicarbonate, adding trihydroxymethyl propane with the mass of 0.05 time that of the polyethylene glycol and polyethylene oxide with the mass of 0.1 time that of the polyethylene glycol and containing benzene rings, continuing the reaction for 5h, finally adding deionized water at 80 ℃ for layering, and carrying out reduced pressure distillation in an oil bath at 100 ℃ to obtain modified polyether;
(2) mixing phenol and triethylamine according to the mass ratio of 8:1, heating to 60 ℃, stirring until the phenol and the triethylamine are dissolved, adding a formaldehyde water solution with the mass fraction of 37% and the mass fraction of 3 times of that of the phenol, cooling to 40 ℃, stirring at the speed of 50rpm, dropwise adding a sodium hydroxide solution with the mass fraction of 40% at the speed of 3ml/min, adjusting the temperature to 50 ℃ after the dropwise adding is finished, adding modified polyether with the mass of 0.2 time of that of the phenol, heating to 80 ℃ after the reaction is carried out for 1h, reacting for 2h, cooling to 30 ℃, and adjusting the pH to 6.8 with hydrochloric acid to obtain the aqueous tackifying resin;
(3) mixing a hydroxylated carbon nanotube with N, N-dimethylformamide according to a mass ratio of 1:50, ultrasonically dispersing for 30min at 40kHz to prepare a hydroxylated carbon nanotube dispersion liquid, mixing the hydroxylated carbon nanotube dispersion liquid with a 30 mass percent N, N-dimethylformamide solution of 4,4' -diphenylmethane diisocyanate according to a mass ratio of 5:2, dropwise adding dibutyltin dilaurate with the mass of 0.01 time that of the hydroxylated carbon nanotube at the speed of 3ml/min, heating to 50 ℃, reacting for 12h, centrifuging after the reaction is finished, washing for 5 times by using N, N-dimethylformamide, and finally drying for 4h in a vacuum drying oven at 50 ℃ to prepare a pre-modified carbon nanotube; mixing aqueous tackifying resin, dimethylolpropionic acid, acetone and pre-modified carbon nano tubes according to the mass ratio of 0.8:2:10:3, adding hydroxyethyl methacrylate with the mass of 0.02 time of that of the aqueous tackifying resin, heating to 40 ℃, reacting for 6 hours, adding triethylamine with the mass of 0.005 time of that of the aqueous tackifying resin, adding deionized water with the mass of 2 times of that of the aqueous tackifying resin at 50rpm for emulsification and rotary evaporation, and finally performing vacuum drying at 55 ℃ to prepare modified carbon nano tubes;
(4) dispersing calcium oxide into boiling deionized water with the mass 15 times that of the calcium oxide, stirring to prepare calcium hydroxide slurry, standing for 12h, filtering, adding polyethylene glycol phosphate with the mass 0.2 times that of the calcium oxide, stirring at 30rpm for reaction for 30min, introducing mixed gas of carbon dioxide and nitrogen with the volume ratio of 2:1 at the flow rate of 800sscm, keeping the reaction temperature at 15 ℃, reacting for 3h, filtering, washing and drying to prepare the composite material; mixing dimethyl 2, 6-naphthalene dicarboxylate and a composite material according to a mass ratio of 1.2:1, preheating for 40min at 80 ℃, transferring to a reaction kettle, heating to 140 ℃ in a nitrogen atmosphere, adding a catalyst zinc acetate with the mass of 0.002 times that of the composite material, stirring and reacting for 18h at 50rpm, cooling to room temperature, and washing for 10min with deionized water to prepare a tackifier;
(5) heating the matrix asphalt to 140 ℃, preserving heat for 0.5h, adding a styrene-butadiene-styrene block copolymer with the mass of 0.12 time that of the matrix asphalt, shearing in a high-speed shearing machine at 4000rpm and 145 ℃ for 10min, and cooling to room temperature to prepare a component A; mixing the modified carbon nano tube, the tackifier and the aromatic oil according to the mass ratio of 3:5:20, and uniformly stirring to obtain a component B; uniformly mixing the component A and the component B according to the mass ratio of 14:5, placing the mixture in a high-speed shearing machine, shearing the mixture for 1h at 4000rpm and 145 ℃, transferring the mixture to a common stirrer, and continuously stirring the mixture for 1h at 1000rpm to prepare the modified asphalt with good high-temperature cohesiveness.
Example 2
(1) Mixing cyclohexane, polyethylene glycol monomethyl ether, sodium hydroxide, anhydrous sodium sulfate and deionized water according to the mass ratio of 2:3.5:0.6:0.04:7, purging with argon for 4min, reacting at 45 ℃ for 1.5h, dropwise adding p-chloromethyl styrene with the mass of 0.4 time of that of the cyclohexane at the speed of 4ml/min, heating to 63 ℃, continuing to react for 2.5h, extracting once with deionized water, extracting 4 times with dichloromethane and carrying out rotary evaporation to prepare polyethylene oxide containing benzene rings; mixing polyethylene glycol and tetrahydrofuran according to a mass ratio of 1:3, placing the mixture in an ice bath at 1 ℃, adding an initiator boron trifluoride diethyl etherate with the mass of 0.0034 times that of the polyethylene glycol in the nitrogen atmosphere, stirring the mixture at 40rpm for reaction for 25min, dropwise adding propylene oxide with the mass of 0.1.3 times that of the polyethylene glycol at a speed of 13 drops/s, after the reaction for 6h, adjusting the pH value to 7 by using sodium bicarbonate, adding trihydroxymethyl propane with the mass of 0.08 times that of the polyethylene glycol and polyethylene oxide with the mass of 0.15 times that of the polyethylene glycol and containing benzene rings, continuing the reaction for 6h, finally adding deionized water at 85 ℃ for layering, and carrying out reduced pressure distillation in an oil bath at 100 ℃ to obtain modified polyether;
(2) mixing phenol and triethylamine according to the mass ratio of 9:1, heating to 65 ℃, stirring until the phenol and the triethylamine are dissolved, adding a formaldehyde water solution with mass fraction of 38% and 4 times of the mass of the phenol, cooling to 42 ℃, stirring at the speed of 80rpm, dropwise adding a sodium hydroxide solution with mass fraction of 45% at the speed of 4ml/min, adjusting the temperature to 51 ℃ after the dropwise adding is finished, adding modified polyether with mass of 0.4 time of the mass of the phenol, heating to 81 ℃ after the reaction is carried out for 2 hours, reacting for 3 hours, cooling to 35 ℃, and adjusting the pH to 7 with hydrochloric acid to obtain the aqueous tackifying resin;
(3) mixing a hydroxylated carbon nanotube with N, N-dimethylformamide according to a mass ratio of 1:80, ultrasonically dispersing for 40min at 40-50 kHz to prepare a hydroxylated carbon nanotube dispersion liquid, mixing the hydroxylated carbon nanotube dispersion liquid with a 40 mass percent N, N-dimethylformamide solution of 4,4' -diphenylmethane diisocyanate according to a mass ratio of 5:2.5, dropwise adding dibutyltin dilaurate with the mass of 0.02 time of that of the hydroxylated carbon nanotube at the speed of 3-8 ml/min, heating to 55 ℃, reacting for 14h, centrifuging after the reaction is finished, washing for 6 times by using N, N-dimethylformamide, and finally drying for 5h in a vacuum drying oven at 55 ℃ to prepare a pre-modified carbon nanotube; mixing aqueous tackifying resin, dimethylolpropionic acid, acetone and pre-modified carbon nano tubes according to the mass ratio of 1.3:2:15:4, adding hydroxyethyl methacrylate with the mass of 0.03 time of that of the aqueous tackifying resin, heating to 45 ℃, reacting for 7 hours, adding triethylamine with the mass of 0.006 time of that of the aqueous tackifying resin, adding deionized water with the mass of 3 times of that of the aqueous tackifying resin at 70rpm for emulsification and rotary evaporation, and finally performing vacuum drying at 58 ℃ to prepare modified carbon nano tubes;
(4) dispersing calcium oxide into boiling deionized water with the mass 17 times that of the calcium oxide, stirring to prepare calcium hydroxide slurry, standing for 18h, filtering, adding polyethylene glycol phosphate with the mass 0.4 time that of the calcium oxide, stirring at 40rpm for reaction for 40min, introducing mixed gas of carbon dioxide and nitrogen with the volume ratio of 2.5:1 at the flow rate of 900sscm, keeping the reaction temperature at 18 ℃, reacting for 5h, filtering, washing and drying to prepare the composite material; mixing dimethyl 2, 6-naphthalene dicarboxylate and a composite material according to a mass ratio of 1.4:1, preheating for 45min at 90 ℃, transferring to a reaction kettle, heating to 150 ℃ in a nitrogen atmosphere, adding a catalyst zinc acetate with the mass of 0.005 time of that of the composite material, stirring and reacting for 19h at 80rpm, cooling to room temperature, and washing for 15min with deionized water to obtain a tackifier;
(5) heating the matrix asphalt to 145 ℃, preserving heat for 0.5h, adding a styrene-butadiene-styrene block copolymer with the mass of 0.13 time of that of the matrix asphalt, shearing for 15min at 4500rpm and 150 ℃ in a high-speed shearing machine, and cooling to room temperature to obtain a component A; mixing the modified carbon nano tube, the tackifier and the aromatic oil according to the mass ratio of 6:9:23, and uniformly stirring to obtain a component B; uniformly mixing the component A and the component B according to the mass ratio of 16:6, placing the mixture in a high-speed shearing machine, shearing the mixture for 1.5h at 4500rpm and 150 ℃, transferring the mixture to a common stirrer, and continuously stirring the mixture for 1.5h at 150rpm to prepare the modified asphalt with good high-temperature cohesiveness.
Example 3
(1) Mixing cyclohexane, polyethylene glycol monomethyl ether, sodium hydroxide, anhydrous sodium sulfate and deionized water according to the mass ratio of 2:4:0.8:0.05:8, purging with argon for 5min, reacting at 50 ℃ for 2h, dropwise adding p-chloromethyl styrene with the mass of 0.5 time of that of the cyclohexane at the speed of 5ml/min, heating to 65 ℃, continuing to react for 3h, extracting once with deionized water, extracting for 5 times with dichloromethane and carrying out rotary evaporation to prepare polyethylene oxide containing benzene rings; mixing polyethylene glycol and tetrahydrofuran according to a mass ratio of 1:4, placing the mixture in an ice bath at 2 ℃, adding an initiator boron trifluoride diethyl etherate with the mass of 0.005 time that of the polyethylene glycol into the ice bath under the nitrogen atmosphere, stirring the mixture at 50rpm for reaction for 30min, dropwise adding propylene oxide with the mass of 0.2 time that of the polyethylene glycol at a speed of 15 drops/s, after the reaction is carried out for 8h, adjusting the pH to 7 by using sodium bicarbonate, adding trihydroxymethyl propane with the mass of 0.1 time that of the polyethylene glycol and polyethylene oxide with the mass of 0.2 time that of the polyethylene glycol and containing benzene rings, continuing the reaction for 8h, finally adding deionized water at 90 ℃ for layering, and carrying out reduced pressure distillation in an oil bath at 100 ℃ to obtain modified polyether;
(2) mixing phenol and triethylamine according to the mass ratio of 10:1, heating to 70 ℃, stirring until the phenol and the triethylamine are dissolved, adding a formaldehyde water solution with the mass fraction of 40% and the mass fraction of 5 times of that of the phenol, cooling to 43 ℃, stirring at the speed of 100rpm, dropwise adding a sodium hydroxide solution with the mass fraction of 50% at the speed of 5ml/min, adjusting the temperature to 52 ℃ after the dropwise adding is finished, adding modified polyether with the mass of 0.5 time of the phenol, heating to 82 ℃ after the reaction is carried out for 3 hours, reacting for 4 hours, cooling to 40 ℃, and adjusting the pH to 7.2 with hydrochloric acid to obtain the aqueous tackifying resin;
(3) mixing a hydroxylated carbon nanotube with N, N-dimethylformamide according to a mass ratio of 1:100, ultrasonically dispersing for 50min at 50kHz to prepare a hydroxylated carbon nanotube dispersion liquid, mixing the hydroxylated carbon nanotube dispersion liquid with a 50% mass fraction N, N-dimethylformamide solution of 4,4' -diphenylmethane diisocyanate according to a mass ratio of 5:3, dropwise adding dibutyltin dilaurate with the mass of 0.03 time of that of the hydroxylated carbon nanotube at a speed of 3-8 ml/min, heating to 60 ℃, reacting for 16h, centrifuging after the reaction is finished, washing for 8 times with N, N-dimethylformamide, and finally drying for 6h in a vacuum drying oven at 60 ℃ to prepare a pre-modified carbon nanotube; mixing aqueous tackifying resin, dimethylolpropionic acid, acetone and pre-modified carbon nano tubes according to the mass ratio of 2:3:20:5, adding hydroxyethyl methacrylate with the mass of 0.04 time of that of the aqueous tackifying resin, heating to 50 ℃, reacting for 8 hours, adding triethylamine with the mass of 0.008 time of that of the aqueous tackifying resin, adding deionized water with the mass of 4 times of that of the aqueous tackifying resin at 100rpm for emulsification and rotary evaporation, and finally performing vacuum drying at 60 ℃ to prepare modified carbon nano tubes;
(4) dispersing calcium oxide into boiling deionized water with the mass 20 times that of the calcium oxide, stirring to prepare calcium hydroxide slurry, standing for 24h, filtering, adding polyethylene glycol phosphate with the mass 0.4 time that of the calcium oxide, stirring at 50rpm for reaction for 50min, introducing mixed gas of carbon dioxide and nitrogen with the volume ratio of 3:1 at the flow rate of 1000sscm, keeping the reaction temperature at 20 ℃, reacting for 6h, filtering, washing and drying to prepare the composite material; mixing dimethyl 2, 6-naphthalene dicarboxylate and a composite material according to a mass ratio of 1.5:1, preheating for 50min at 100 ℃, transferring to a reaction kettle, heating to 140-160 ℃ in a nitrogen atmosphere, adding a catalyst zinc acetate 0.008 times of the mass of the composite material, stirring and reacting for 20h at 100rpm, cooling to room temperature, washing for 20min with deionized water, and preparing a tackifier;
(5) heating the matrix asphalt to 150 ℃, preserving heat for 1h, adding a styrene-butadiene-styrene block copolymer with the mass of 0.14 time of that of the matrix asphalt, shearing the mixture in a high-speed shearing machine at 5000rpm and 155 ℃ for 20min, and cooling to room temperature to obtain a component A; mixing the modified carbon nano tube, the tackifier and aromatic oil according to the mass ratio of 8:10:24, and uniformly stirring to obtain a component B; uniformly mixing the component A and the component B according to the mass ratio of 18:8, placing the mixture in a high-speed shearing machine, shearing the mixture for 2 hours at the temperature of 145-155 ℃ at 5000rpm, transferring the mixture to a common stirrer, and continuously stirring the mixture for 2 hours at 2000rpm to prepare the modified asphalt with good high-temperature cohesiveness.
Comparative example 1
(1) Mixing a hydroxylated carbon nanotube with N, N-dimethylformamide according to a mass ratio of 1:80, performing ultrasonic dispersion for 40min at 40-50 kHz to obtain a hydroxylated carbon nanotube dispersion liquid, mixing the hydroxylated carbon nanotube dispersion liquid with a 40% mass fraction N, N-dimethylformamide solution of 4,4' -diphenylmethane diisocyanate according to a mass ratio of 5:2.5, then dropwise adding dibutyltin dilaurate with the mass of 0.02 time of that of the hydroxylated carbon nanotube at a rate of 3-8 ml/min, heating to 55 ℃, reacting for 14h, centrifuging after the reaction is finished, washing for 6 times by using N, N-dimethylformamide, and finally drying for 5h in a vacuum drying oven at 55 ℃ to obtain a pre-modified carbon nanotube;
(2) dispersing calcium oxide into boiling deionized water with the mass 17 times that of the calcium oxide, stirring to prepare calcium hydroxide slurry, standing for 18h, filtering, adding polyethylene glycol phosphate with the mass 0.4 time that of the calcium oxide, stirring at 40rpm for reaction for 40min, introducing mixed gas of carbon dioxide and nitrogen with the volume ratio of 2.5:1 at the flow rate of 900sscm, keeping the reaction temperature at 18 ℃, reacting for 5h, filtering, washing and drying to prepare the composite material; mixing dimethyl 2, 6-naphthalene dicarboxylate and a composite material according to a mass ratio of 1.4:1, preheating for 45min at 90 ℃, transferring to a reaction kettle, heating to 150 ℃ in a nitrogen atmosphere, adding a catalyst zinc acetate with the mass of 0.005 time of that of the composite material, stirring and reacting for 19h at 80rpm, cooling to room temperature, and washing for 15min with deionized water to obtain a tackifier;
(3) heating the matrix asphalt to 145 ℃, preserving heat for 0.5h, adding a styrene-butadiene-styrene block copolymer with the mass of 0.13 time of that of the matrix asphalt, shearing for 15min at 4500rpm and 150 ℃ in a high-speed shearing machine, and cooling to room temperature to obtain a component A; mixing the pre-modified carbon nano tube, the tackifier and aromatic oil according to the mass ratio of 6:9:23, and uniformly stirring to obtain a component B; uniformly mixing the component A and the component B according to the mass ratio of 16:6, placing the mixture in a high-speed shearing machine, shearing the mixture for 1.5h at 4500rpm and 150 ℃, transferring the mixture to a common stirrer, and continuously stirring the mixture for 1.5h at 150rpm to prepare the modified asphalt with good high-temperature cohesiveness.
Comparative example 2
Comparative example 2 was formulated in the same manner as in example 2. The preparation method of the modified asphalt with good high-temperature caking property is different from the preparation method of the embodiment 2 only in the step (3), and the step (3) is modified as follows: mixing aqueous tackifying resin, dimethylolpropionic acid, acetone and carbon nano tubes according to the mass ratio of 1.3:2:15:4, adding hydroxyethyl methacrylate with the mass of 0.03 time of that of the aqueous tackifying resin, heating to 45 ℃, reacting for 7 hours, adding triethylamine with the mass of 0.006 time of that of the aqueous tackifying resin, adding deionized water with the mass of 3 times of that of the aqueous tackifying resin at 70rpm for emulsification and rotary evaporation, and finally performing vacuum drying at 58 ℃ to prepare the modified carbon nano tubes.
Comparative example 3
The formulation of comparative example 3 was the same as that of example 2. The preparation method of the modified asphalt with good high-temperature caking property is different from the preparation method of the embodiment 2 only in the difference of the step (1), and the step (1) is modified as follows: mixing polyethylene glycol and tetrahydrofuran according to the mass ratio of 1:3, placing the mixture in an ice bath at 1 ℃, adding an initiator boron trifluoride diethyl ether with the mass of 0.0034 times that of the polyethylene glycol in the nitrogen atmosphere, stirring and reacting for 25min at 40rpm, dropwise adding propylene oxide with the mass of 0.1.3 times that of the polyethylene glycol at the speed of 13 drops/s, reacting for 6h, adjusting the pH to 7 by using sodium bicarbonate, finally adding deionized water at 85 ℃ for layering, and distilling under reduced pressure in an oil bath at 100 ℃ to obtain the modified polyether.
Comparative example 4
Comparative example 4 was formulated as in example 2. The preparation method of the modified asphalt with good high-temperature caking property is different from the preparation method of the modified asphalt in the example 2 only in the difference of (2), and the step (2) is modified as follows: (2) adding formaldehyde aqueous solution with mass fraction of 38% 4 times of the mass of phenol into the phenol, cooling to 42 ℃, stirring at 80rpm, dropwise adding sodium hydroxide solution with mass fraction of 45% at 4ml/min, adjusting the temperature to 51 ℃ after dropwise adding, adding modified polyether with mass fraction of 0.4 time of the mass of phenol, reacting for 2h, then heating to 81 ℃, reacting for 3h, cooling to 35 ℃, and adjusting the pH to 7 with hydrochloric acid to obtain the aqueous tackifying resin.
Comparative example 5
Comparative example 5 was formulated as in example 2. The preparation method of the modified asphalt with good high-temperature caking property is different from the preparation method of the modified asphalt in the embodiment 2 only in that the treatments of (1), (2) and (3) are not carried out, and the step (5) is modified as follows: heating the matrix asphalt to 145 ℃, preserving heat for 0.5h, adding a styrene-butadiene-styrene block copolymer with the mass of 0.13 time of that of the matrix asphalt, shearing for 15min at 4500rpm and 150 ℃ in a high-speed shearing machine, and cooling to room temperature to obtain a component A; mixing the carbon nano tube, the tackifier and aromatic oil according to the mass ratio of 6:9:23, and uniformly stirring to obtain a component B; uniformly mixing the component A and the component B according to the mass ratio of 16:6, placing the mixture in a high-speed shearing machine, shearing the mixture for 1.5h at 4500rpm and 150 ℃, transferring the mixture to a common stirrer, and continuously stirring the mixture for 1.5h at 150rpm to prepare the modified asphalt with good high-temperature cohesiveness.
Comparative example 6
Comparative example 6 was formulated as in example 2. The preparation method of the modified asphalt with good high-temperature caking property is different from the embodiment 2 only in the step (4), and the step (4) is modified as follows: mixing dimethyl 2, 6-naphthalene dicarboxylate and ethylene glycol according to the mass ratio of 1.4:1, preheating for 45min at 90 ℃, transferring to a reaction kettle, heating to 150 ℃ in the nitrogen atmosphere, adding a catalyst zinc acetate with the mass of 0.005 time of that of the composite material, stirring and reacting for 19h at 80rpm, cooling to room temperature, and washing for 15min with deionized water to obtain the tackifier.
Comparative example 7
Comparative example 7 was formulated as in example 2. The preparation method of the modified asphalt with good high-temperature cohesiveness is different from the embodiment 2 only in that the treatment of the step (4) is not carried out, and the step (5) is modified as follows: heating the matrix asphalt to 145 ℃, preserving heat for 0.5h, adding a styrene-butadiene-styrene block copolymer with the mass of 0.13 time of that of the matrix asphalt, shearing for 15min at 4500rpm and 150 ℃ in a high-speed shearing machine, and cooling to room temperature to obtain a component A; mixing the modified carbon nano tube and aromatic oil according to the mass ratio of 6:23, and uniformly stirring to obtain a component B; uniformly mixing the component A and the component B according to the mass ratio of 16:6, placing the mixture in a high-speed shearing machine, shearing the mixture for 1.5h at 4500rpm and 150 ℃, transferring the mixture to a common stirrer, and continuously stirring the mixture for 1.5h at 150rpm to prepare the modified asphalt with good high-temperature cohesiveness.
Examples of effects
The following table 1 shows the results of performance analysis of the modified asphalts excellent in high-temperature adhesion using examples 1, 2, and 3 of the present invention and comparative examples 1, 2, 3, 4, 5, and 6/7.
TABLE 1
It is obvious from the comparison of the experimental data of the examples and the comparative examples in table 1 that the modified asphalts prepared in examples 1, 2 and 3 have good high-temperature cohesiveness, and are good in elasticity, heat resistance, air permeability, antibacterial property and stain resistance;
from the comparison of experimental data of examples 1, 2 and 3 and comparative examples 1, 2, 3 and 4/5, it can be seen that the modified polyether is introduced into the phenolic resin and aminated to prepare the waterborne tackifying resin, the modified polyether is grafted onto the phenolic resin, the methylol on the phenolic resin polycondensate can also react with the hydrogen on the phenol ring to generate methylene, so that the phenolic resin and the modified polyether form a cross-linked structure, the toughness of the waterborne tackifying resin is enhanced, and the adhesiveness of the modified asphalt is enhanced; 4,4' -diphenylmethane diisocyanate and hydroxylated multi-walled carbon nanotubes are used for grafting modification to prepare pre-modified carbon nanotubes, polyurethane is formed between the aqueous tackifying resin and the pre-modified carbon nanotubes, and a buffer layer is formed on the surface of the pre-modified carbon nanotubes, so that the dispersibility is improved, and the impact resistance of the modified asphalt is enhanced; from the comparison of the experimental data of example 1, example 2, example 3 and comparative examples 5 and 6, it can be seen that the modified polyethylene naphthalate obtained by connecting polyethylene glycol phosphate with calcium carbonate and further performing esterification reaction with dimethyl 2, 6-naphthalate introduces benzene ring, and at the same time, disperses calcium carbonate uniformly, and the polyethylene naphthalate has large steric hindrance, so that the movement of calcium carbonate and modified carbon nanotubes is limited, and the adhesiveness of the modified asphalt is enhanced.
It will be evident to those skilled in the art that the invention is not limited to the details of the foregoing illustrative embodiments, and that the present invention may be embodied in other specific forms without departing from the spirit or essential attributes thereof. The present embodiments are therefore to be considered in all respects as illustrative and not restrictive, the scope of the invention being indicated by the appended claims rather than by the foregoing description, and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein. Any reference sign in a claim should not be construed as limiting the claim concerned.
Claims (10)
1. The modified asphalt with good high-temperature cohesiveness is characterized by comprising modified carbon nanotubes prepared by coating pre-modified carbon nanotubes with aqueous tackifying resin, styrene-butadiene-styrene block copolymer, tackifier, aromatic oil and matrix asphalt; the modified carbon nano tube is prepared by coating a pre-modified carbon nano tube with aqueous tackifying resin; the tackifier is modified polyethylene naphthalate.
2. The modified asphalt with good high-temperature cohesiveness as claimed in claim 1, wherein the aqueous tackifying resin is prepared by introducing modified polyether during preparation of phenolic resin and performing amination; the modified polyether is prepared by introducing polyethylene oxide containing benzene rings to active polyether; the pre-modified carbon nano tube is prepared by grafting and modifying 4,4' -diphenylmethane diisocyanate and a hydroxylated multi-wall carbon nano tube.
3. The modified asphalt with good high-temperature cohesiveness as claimed in claim 1, wherein the modified polyethylene naphthalate is prepared by connecting polyethylene glycol phosphate with calcium carbonate and performing esterification reaction with dimethyl 2, 6-naphthalate.
4. The modified asphalt with good high-temperature caking property according to claim 1, wherein the base asphalt is imported No. 70 base asphalt; the cosolvent is aromatic oil.
5. The preparation method of the modified asphalt with good high-temperature cohesiveness is characterized by comprising the following specific steps of:
(1) mixing polyethylene glycol and tetrahydrofuran according to a mass ratio of 1: 2-1: 4, placing the mixture in an ice bath at 0-2 ℃, adding initiator boron trifluoride diethyl etherate with the mass of 0.003-0.005 time of that of the polyethylene glycol in a nitrogen atmosphere, stirring the mixture at 30-50 rpm for reaction for 15-30 min, dropwise adding propylene oxide with the mass of 0.05-0.2 time of that of the polyethylene glycol at a speed of 10-15 drops/s, after the reaction is carried out for 4-8 h, adjusting the pH to 7 by using sodium bicarbonate, adding trihydroxymethyl propane with the mass of 0.05-0.1 time of the polyethylene glycol and polyethylene oxide with the mass of 0.1-0.2 time of the polyethylene glycol and containing benzene rings, continuing the reaction for 5-8 h, finally adding deionized water with the temperature of 80-90 ℃ for layering, and carrying out reduced pressure distillation in an oil bath at the temperature of 100 ℃ to prepare modified polyether;
(2) mixing phenol and triethylamine according to the mass ratio of 8: 1-10: 1, heating to 60-70 ℃, stirring until the mixture is dissolved, adding a formaldehyde water solution with the mass fraction of 37-40% and the mass fraction of 3-5 times of that of the phenol, cooling to 40-43 ℃, stirring at the speed of 50-100 rpm, dropwise adding a sodium hydroxide solution with the mass fraction of 40-50% at the speed of 3-5 ml/min, adjusting the temperature to 50-52 ℃ after dropwise adding, adding modified polyether with the mass fraction of 0.2-0.5 time of that of the phenol, reacting for 1-3 h, heating to 80-82 ℃, reacting for 2-4 h, cooling to 30-40 ℃, adjusting the pH to 6.8-7.2 with hydrochloric acid, and preparing a water-based tackifying resin;
(3) mixing aqueous tackifying resin, dimethylolpropionic acid, acetone and pre-modified carbon nano tubes according to the mass ratio of 0.8:2:10: 3-2: 3:20:5, adding hydroxyethyl methacrylate with the mass of 0.02-0.04 time of that of the aqueous tackifying resin, heating to 40-50 ℃, reacting for 6-8 hours, adding triethylamine with the mass of 0.005-0.008 time of that of the aqueous tackifying resin, adding deionized water with the mass of 2-4 times of that of the aqueous tackifying resin at 50-100 rpm for emulsification and rotary evaporation, and finally performing vacuum drying at 55-60 ℃ to prepare modified carbon nano tubes;
(4) mixing dimethyl 2, 6-naphthalene dicarboxylate and a composite material according to a mass ratio of 1.2: 1-1.5: 1, preheating for 40-50 min at 80-100 ℃, transferring to a reaction kettle, heating to 140-160 ℃ in a nitrogen atmosphere, adding a catalyst zinc acetate 0.002-0.008 times of the mass of the composite material, stirring and reacting for 18-20 h at 50-100 rpm, cooling to room temperature, washing with deionized water for 10-20 min, and preparing a tackifier;
(5) uniformly mixing the component A and the component B according to the mass ratio of 14: 5-18: 8, placing the mixture in a high-speed shearing machine, shearing the mixture for 1-2 hours at the temperature of 145-155 ℃ at 4000-5000 rpm, transferring the mixture to a common stirrer, and continuously stirring the mixture for 1-2 hours at the temperature of 1000-2000 rpm to prepare the modified asphalt with good high-temperature cohesiveness.
6. The method for producing a modified asphalt having good high-temperature adhesion according to claim 5, wherein in the step (1): the preparation method of the polyethylene oxide containing the benzene ring comprises the following steps: mixing cyclohexane, polyethylene glycol monomethyl ether, sodium hydroxide, anhydrous sodium sulfate and deionized water according to the mass ratio of 2:3:0.5:0.02: 6-2: 4:0.8:0.05:8, purging with argon for 3-5 min, reacting at 40-50 ℃ for 1-2 h, dropwise adding p-chloromethyl styrene with the mass 0.2-0.5 times that of cyclohexane at the rate of 3-5 ml/min, heating to 60-65 ℃, continuing to react for 2-3 h, extracting once with deionized water, extracting 3-5 times with dichloromethane, and performing rotary evaporation to obtain the polyethylene oxide containing benzene rings.
7. The method for producing a modified asphalt having good high-temperature adhesion according to claim 5, wherein in the step (3): the preparation method of the pre-modified carbon nano tube comprises the following steps: mixing a hydroxylated carbon nanotube and N, N-dimethylformamide according to a mass ratio of 1: 50-1: 100, ultrasonically dispersing for 30-50 min at 40-50 kHz to prepare a hydroxylated carbon nanotube dispersion liquid, mixing the hydroxylated carbon nanotube dispersion liquid and a N, N-dimethylformamide solution of 4,4' -diphenylmethane diisocyanate with the mass fraction of 30-50% according to a mass ratio of 5: 2-5: 3, then dropwise adding dibutyltin dilaurate with the mass of 0.01-0.03 time of that of the hydroxylated carbon nanotube at the speed of 3-8 ml/min, heating to 50-60 ℃, reacting for 12-16 h, centrifuging after the reaction is finished, washing for 5-8 times by using N, N-dimethylformamide, and finally drying for 4-6 h in a vacuum drying box with the temperature of 50-60 ℃ to prepare the pre-modified carbon nanotube.
8. The method for producing a modified asphalt having good high-temperature adhesion according to claim 5, wherein in the step (4): the preparation method of the composite material comprises the following steps: dispersing calcium oxide into boiling deionized water with the mass 15-20 times that of the calcium oxide, stirring to obtain calcium hydroxide slurry, standing for 12-24 h, filtering, adding polyethylene glycol phosphate with the mass 0.2-0.4 time that of the calcium oxide, stirring at 30-50 rpm, reacting for 30-50 min, introducing mixed gas of carbon dioxide and nitrogen with the volume ratio of 2: 1-3: 1 at the flow rate of 800-1000 sscm, keeping the reaction temperature at 15-20 ℃, reacting for 3-6 h, filtering, washing and drying to obtain the composite material.
9. The method for preparing modified asphalt with good high-temperature caking property according to claim 5, wherein in the step (5): the preparation process of the component A comprises the following steps: heating the matrix asphalt to 140-150 ℃, keeping the temperature for 0.5-1 h, adding a styrene-butadiene-styrene block copolymer with the mass of 0.12-0.14 time of that of the matrix asphalt, shearing the mixture in a high-speed shearing machine at 4000-5000 rpm and 145-155 ℃ for 10-20 min, and cooling to room temperature to obtain the component A.
10. The method for producing a modified asphalt having good high-temperature adhesion according to claim 5, wherein in the step (5): the preparation process of the component B comprises the following steps: and mixing the modified carbon nano tube, the tackifier and the aromatic oil according to the mass ratio of 3:5: 20-8: 10:24, and uniformly stirring to obtain the component B.
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