CN115109423A - Anti-aging durable asphalt and preparation method thereof - Google Patents
Anti-aging durable asphalt and preparation method thereof Download PDFInfo
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- CN115109423A CN115109423A CN202210671672.XA CN202210671672A CN115109423A CN 115109423 A CN115109423 A CN 115109423A CN 202210671672 A CN202210671672 A CN 202210671672A CN 115109423 A CN115109423 A CN 115109423A
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- C08L95/00—Compositions of bituminous materials, e.g. asphalt, tar, pitch
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- C—CHEMISTRY; METALLURGY
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Abstract
The invention discloses anti-aging durable asphalt, which belongs to the technical field of asphalt preparation and comprises the following raw materials in parts by weight: 120 parts of matrix asphalt, 10-13 parts of cosolvent and 8-10 parts of additive; the invention also discloses a preparation method of the asphalt, which solves the problems that the ultraviolet absorbent in the existing asphalt has small molecular weight, is easy to migrate, has low light stability, is easy to be inhaled by human bodies and the like, and comprises the following steps: firstly, adding matrix asphalt and a cosolvent into a reaction kettle, and stirring at the temperature of 140 ℃ to obtain a molten material; and secondly, adding an additive into the molten material, heating to 180 ℃, shearing at a high speed for 40min, stirring for 20min by using a magnetic stirrer, and finally standing for 2h in a 120 ℃ blast drying oven to obtain the anti-aging durable asphalt.
Description
Technical Field
The invention belongs to the technical field of asphalt preparation, and particularly relates to anti-aging durable asphalt and a preparation method thereof.
Background
The asphalt is a black brown complex mixture composed of hydrocarbons with different molecular weights and nonmetal derivatives thereof, is one of high-viscosity organic liquids, mostly exists in a liquid or semisolid petroleum form, has a black surface, and is a waterproof, moistureproof and anticorrosive organic cementing material; the material is widely applied to projects such as buildings, roads, bridges and the like, and is mainly used for waterproof materials and cementing materials for paving pavement structures. However, asphalt is also an organic mixture, and if exposed to air for a long time, a series of physical and chemical changes, such as evaporation, deoxidation, condensation, oxidation, etc., occur under the action of natural conditions such as wind, rain, temperature change, etc. At this time, besides the increase of oxygen-containing functional groups, other chemical compositions also change, and finally, the asphalt is gradually hardened, embrittled and cracked, so that the original bonding or sealing function cannot be continuously exerted.
The Chinese patent with publication number CN103275502B discloses an anti-aging asphalt and a preparation method thereof, wherein the anti-aging asphalt is prepared from the following raw materials in percentage by weight: 93-98.9% of asphalt, 1-6% of organic vermiculite and 0.1-1% of ultraviolet absorbent, wherein the surface of the organic vermiculite is oleophilic, can be compatible with asphalt matrix, and can exert the synergistic oxidation resistance and ultraviolet resistance with the ultraviolet absorbent, but the traditional ultraviolet absorbent has the problems of small molecular weight, easy migration, low light stability, easy human body inhalation and the like, so that the asphalt material with good compatibility and lasting aging resistance is provided.
Disclosure of Invention
The invention aims to provide anti-aging durable asphalt and a preparation method thereof.
The technical problems to be solved by the invention are as follows:
the traditional ultraviolet absorbent has the problems of small molecular weight, easy migration, low light stability, easy human body inhalation and the like, has poor compatibility with asphalt matrix and is difficult to play an anti-aging role for a long time.
The purpose of the invention can be realized by the following technical scheme:
the anti-aging durable asphalt comprises the following raw materials in parts by weight: 120 parts of matrix asphalt, 10-13 parts of cosolvent and 8-10 parts of additive;
the anti-aging durable asphalt is prepared by the following steps:
firstly, adding matrix asphalt and a cosolvent into a reaction kettle, and stirring for 20min at the temperature of 140 ℃ and the rotating speed of 2000r/min to obtain a molten material;
and secondly, adding an additive into the molten material, heating to 180 ℃, shearing for 40min at the rotating speed of 4500r/min under the action of a high-speed shearing machine, stirring for 20min at the rotating speed of 2000r/min and the temperature of 120 ℃ by using a magnetic stirrer after shearing is finished, and finally standing for 2h in a 120 ℃ blast drying box to obtain the anti-aging durable asphalt.
Further, the additive is prepared by the following steps:
step 1, adding cyanuric chloride and resorcinol into a three-neck flask, adding nitrobenzene, magnetically stirring for 10min at 40 ℃, adding an aluminum trichloride catalyst into the three-neck flask, heating to 80 ℃, carrying out heat preservation reaction for 2h, carrying out suction filtration while hot after the reaction is finished, washing a filter cake with deionized water for 3-5 times, combining filtrates, separating the combined filtrates by using a separating funnel, and obtaining an organic phase as an intermediate 1;
the reaction process is as follows:
step 2, adding the intermediate 1, acetone and epichlorohydrin into a three-neck flask, heating to 80 ℃, then dropwise adding a sodium hydroxide aqueous solution with the mass concentration of 2.5 wt%, dropwise adding at the speed of 2 drops/second, stirring at the rotation speed of 100 plus one liter of water for reaction for 2 hours after the dropwise adding is finished, adding ethyl acetate for extraction after the reaction is finished, removing an organic solvent through a rotary evaporator, purifying through a silica gel chromatographic column, and performing vacuum drying at 50 ℃ for 12 hours to obtain an intermediate 2;
the reaction process is as follows:
step 3, adding the intermediate 2 and tetrahydrofuran into a beaker, stirring for 10min at the rotating speed of 60-80r/min, dropwise adding an ethanol solution of p-aminodiphenylamine into the beaker, reacting for 30-60min under magnetic stirring at room temperature after dropwise adding, filtering after the reaction is finished, and removing the organic solvent from the filtrate in a rotary evaporator to obtain an intermediate 3;
the reaction process is as follows:
step 4, under the protection of nitrogen, adding the intermediate 3 and tetrahydrofuran into a three-neck flask, stirring for 5min, adding diphenylmethane diisocyanate and dibutyl tin dilaurate, refluxing and stirring at 70 ℃ for reaction for 3h, cooling to room temperature after the reaction is finished, and carrying out reduced pressure distillation to obtain an intermediate 4;
the reaction process is as follows:
step 5, adding the intermediate 4 and dimethylformamide into a three-neck flask in a water bath, then adding 2,2,6, 6-tetramethylpiperidine, stirring at the temperature of 70 ℃ for reaction for 1 hour, and obtaining an intermediate 5 after the reaction is finished; adding a sodium methoxide methanol solution with the mass fraction of 30% into a three-neck flask, mixing for 10min at the rotation speed of 60r/min, adding gamma-chloropropyltrimethoxysilane, controlling the temperature to be 65 ℃, heating and stirring for 5min to remove methanol, then heating to 134 ℃ and 136 ℃, carrying out reflux reaction for 10h, cooling and standing overnight after the reaction is finished, carrying out suction filtration, and carrying out reduced pressure distillation on the filtrate under the protection of nitrogen to obtain an intermediate 6;
the reaction process is as follows:
and 6, adding the magnesium-aluminum hydrotalcite and an ethanol solution with the mass fraction of 50% into a three-neck flask under the protection of nitrogen, stirring and reacting for 1h at 70 ℃, dropwise adding the ethanol solution of the intermediate 6 into the three-neck flask, after dropwise adding, adding a hydrochloric acid solution with the mass fraction of 17% to adjust the pH value to 3, stirring and reacting for 3h, cooling to room temperature after reaction, filtering, washing a filter cake with deionized water until a washing solution is neutral, and finally drying at 65 ℃ to constant weight to obtain the additive.
Further, the dosage ratio of the cyanuric chloride, the resorcinol, the nitrobenzene and the aluminum trichloride catalyst in the step 1 is 30 mmol: 90 mmol: 170-180 mL: 0.5-0.8 g;
in the step 2, the using ratio of the intermediate 1, acetone, epichlorohydrin to the sodium hydroxide aqueous solution is 0.01 mol: 30-38 mL: 4.63 g: 20 mL;
in the step 3, the dosage ratio of the intermediate 1, the tetrahydrofuran and the ethanol solution of the p-aminodiphenylamine is 0.01 mol: 62-68 mL: 10 mL; wherein the ethanol solution of the p-aminodiphenylamine is prepared from the p-aminodiphenylamine and absolute ethanol according to the weight ratio of 1.84-1.85 g: 10mL of the mixture is mixed;
in the step 4, the dosage ratio of the intermediate 3, tetrahydrofuran, diphenylmethane diisocyanate and dibutyl tin dilaurate is 0.01 mol: 68-72 mL: 0.01 mol: 1 mL;
in the step 5, the dosage ratio of the intermediate 4, the dimethylformamide, the 2,2,6,6, -tetramethylpiperidine, the sodium methoxide methanol solution and the gamma-chloropropyltrimethoxysilane is 0.08 mol: 140mL of: 0.08 mol: 10.5-14.4 g: 0.08-0.09 mol;
in the step 6, the dosage ratio of the magnesium aluminum hydrotalcite to the ethanol solution of the intermediate 6 is 7 g: 200mL of: 4-5 mL; the dosage ratio of the ethanol solution of the intermediate 6 is that the intermediate 6 and ethanol are mixed according to the mass of 1 g: 4-5 mL.
Furthermore, the cosolvent is one or more of epoxy natural rubber, polyethylene resin, normal hexane and xylene which are mixed according to any proportion.
The anti-aging durable asphalt is prepared by the following steps:
firstly, adding matrix asphalt and a cosolvent into a reaction kettle, and stirring for 20min at the temperature of 140 ℃ and the rotating speed of 2000r/min to obtain a molten material;
and secondly, adding an additive into the molten material, heating to 180 ℃, shearing for 40min at the rotating speed of 4500r/min under the action of a high-speed shearing machine, stirring for 20min at the rotating speed of 2000r/min and the temperature of 120 ℃ by using a magnetic stirrer after shearing is finished, and finally standing for 2h in a 120 ℃ blast drying box to obtain the anti-aging durable asphalt.
The invention has the beneficial effects that:
the invention takes matrix asphalt, cosolvent and additive as raw materials, obtains an anti-aging durable asphalt by melting and shearing, takes cyanuric chloride and resorcinol as substrates, obtains triazine intermediate 1 under the catalytic action of aluminum trichloride, takes the intermediate 1 as a substrate, leads phenolic hydroxyl of the intermediate 1 to have substitution reaction with epichlorohydrin under alkaline environment, obtains intermediate 2 containing epoxy group, leads p-aminodiphenylamine to be grafted on the intermediate 2 by utilizing the characteristic that the epoxy group and amino are easy to have ring-opening reaction, obtains intermediate 3 containing diphenylamine structure, leads the intermediate to have grafting reaction with alcoholic hydroxyl of the intermediate 3 by utilizing the characteristic of diphenylmethane diisocyanate, obtains intermediate 4, then leads the intermediate to have grafting reaction with secondary amine of 2,2,6,6, -tetramethylpiperidine, obtains intermediate 5, then using gamma-chloropropyltrimethoxysilane as a modifier to replace phenolic hydroxyl on the intermediate 5 to obtain an intermediate 6 grafted with a silane coupling agent, finally dispersing the magnesium-aluminum hydrotalcite in an ethanol solution, and then adding the intermediate 6 and the-Si-O-CH of the intermediate 6 3 Hydrolysis reaction is carried out, the additive is combined with hydroxyl on the surface of the magnalium hydrotalcite through chemical bonds to obtain the additive, the additive contains all characteristics of triazine ultraviolet absorbent, can absorb ultraviolet with the wavelength of 280-380nm, has wide absorption range, has large molecular weight, is not easy to migrate and has good light stability, the additive contains diphenylamine structure, can capture free radicals and exert the anti-aging performance, 2,6, 6-tetramethylpiperidine is grafted on the additive, contains hindered amine structure, can capture free radicals, decompose peroxides and quench singlet oxygen, and enhance the light stability of the additive, wherein the magnalium hydrotalcite is a layered silicate material, not only can realize the obstruction of oxygen and heat, but also has the performance of shielding ultraviolet light, and can play a role in the aspects of heat, oxygen and ultraviolet aging resistance of asphalt, the additive belongs to an organic-inorganic composite material, can improve the aging resistance of asphalt in many aspects, and has higher aging resistance.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all 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.
Example 1
The additive is prepared by the following steps:
step 1, adding 30mmol of cyanuric chloride and 90mmol of resorcinol into a three-neck flask, then adding 170mL of nitrobenzene, magnetically stirring at 40 ℃ for 10min, adding 0.5g of aluminum trichloride catalyst into the three-neck flask, heating to 80 ℃, carrying out heat preservation reaction for 2h, after the reaction is finished, carrying out suction filtration while hot, washing a filter cake with deionized water for 3 times, combining filtrates, separating the combined filtrates by using a separating funnel, and obtaining an organic phase as an intermediate 1;
step 2, adding 0.01mol of the intermediate 1, 30mL of acetone and 4.63g of epoxy chloropropane into a three-neck flask, heating to 80 ℃, then dropwise adding 20mL of a 2.5 wt% sodium hydroxide aqueous solution at a dropping speed of 2 drops/second, stirring and reacting for 2 hours at a rotating speed of 100r/min after the dropwise adding is finished, adding ethyl acetate for extraction after the reaction is finished, removing an organic solvent through a rotary evaporator, purifying through a silica gel chromatographic column, and performing vacuum drying for 12 hours at 50 ℃ to obtain an intermediate 2;
step 3, adding 0.01mol of the intermediate 2 and 62mL of tetrahydrofuran into a beaker, stirring for 10min at the rotating speed of 60r/min, dropwise adding 10mL of ethanol solution of p-aminodiphenylamine into the beaker, after dropwise adding, magnetically stirring at room temperature for reaction for 30min, after the reaction, filtering, and removing the organic solvent from the filtrate in a rotary evaporator to obtain an intermediate 3; wherein the ethanol solution of the p-aminodiphenylamine is prepared from the p-aminodiphenylamine and absolute ethanol according to the weight ratio of 1.84 g: 10mL of the mixture is mixed;
step 4, under the protection of nitrogen, adding 0.01mol of the intermediate 3 and 68mL of tetrahydrofuran into a three-neck flask, stirring for 5min, adding 0.01mol of diphenylmethane diisocyanate and 1mL of dibutyl tin dilaurate, refluxing and stirring at 70 ℃ for reaction for 3h, cooling to room temperature after the reaction is finished, and carrying out reduced pressure distillation to obtain an intermediate 4;
step 5, adding 0.08mol of the intermediate 4 and 140mL of dimethylformamide into a three-neck flask in a water bath, then adding 0.08mol of 2,2,6, 6-tetramethylpiperidine, stirring at 70 ℃ for reaction for 1h, and obtaining an intermediate 5 after the reaction is finished; then adding 10.5g of sodium methoxide methanol solution with the mass fraction of 30% into a three-neck flask, mixing for 10min at the rotating speed of 60r/min, adding 0.08mol of gamma-chloropropyltrimethoxysilane, heating and stirring at the controlled temperature of 65 ℃ for 5min to remove methanol, heating to 134 ℃, carrying out reflux reaction for 10h, cooling and standing overnight after the reaction is finished, carrying out suction filtration, and carrying out reduced pressure distillation on the filtrate under the protection of nitrogen to obtain an intermediate 6;
step 6, under the protection of nitrogen, adding 7g of magnesium-aluminum hydrotalcite and 200mL of 50% ethanol solution in mass fraction into a three-neck flask, stirring and reacting for 1h at 70 ℃, dropwise adding 4mL of the ethanol solution of the intermediate 6 into the three-neck flask, after dropwise adding, adding 17% hydrochloric acid solution in mass fraction to adjust the pH value to 3, stirring and reacting for 3h, after reacting, cooling to room temperature, filtering, washing a filter cake with deionized water until the washing solution is neutral, and finally drying to constant weight at 65 ℃ to obtain an additive, wherein the dosage ratio of the ethanol solution of the intermediate 6 is that the intermediate 6 and ethanol are 1g by mass: 4mL of the mixture was mixed.
Example 2
The additive is prepared by the following steps:
step 1, adding 30mmol of cyanuric chloride and 90mmol of resorcinol into a three-neck flask, then adding 170mL of nitrobenzene, magnetically stirring at 40 ℃ for 10min, adding 0.5g of aluminum trichloride catalyst into the three-neck flask, heating to 80 ℃, carrying out heat preservation reaction for 2h, after the reaction is finished, carrying out suction filtration while hot, washing a filter cake with deionized water for 3 times, combining filtrates, separating the combined filtrates by using a separating funnel, and obtaining an organic phase as an intermediate 1;
step 2, adding 0.01mol of the intermediate 1, 30mL of acetone and 4.63g of epoxy chloropropane into a three-neck flask, heating to 80 ℃, then dropwise adding 20mL of a 2.5 wt% sodium hydroxide aqueous solution at a dropping speed of 2 drops/second, stirring and reacting for 2 hours at a rotating speed of 100r/min after the dropwise adding is finished, adding ethyl acetate for extraction after the reaction is finished, removing an organic solvent through a rotary evaporator, purifying through a silica gel chromatographic column, and performing vacuum drying for 12 hours at 50 ℃ to obtain an intermediate 2;
step 3, adding 0.01mol of the intermediate 2 and 62mL of tetrahydrofuran into a beaker, stirring for 10min at the rotating speed of 60r/min, dropwise adding 10mL of ethanol solution of p-aminodiphenylamine into the beaker, after dropwise adding, magnetically stirring at room temperature for reaction for 30min, after the reaction, filtering, and removing the organic solvent from the filtrate in a rotary evaporator to obtain an intermediate 3; wherein the ethanol solution of the p-aminodiphenylamine is prepared from the p-aminodiphenylamine and absolute ethanol according to the weight ratio of 1.84 g: 10mL of the mixture is mixed;
step 4, under the protection of nitrogen, adding 0.01mol of the intermediate 3 and 70mL of tetrahydrofuran into a three-neck flask, stirring for 5min, adding 0.01mol of diphenylmethane diisocyanate and 1mL of dibutyl tin dilaurate, refluxing and stirring at 70 ℃ for reaction for 3h, cooling to room temperature after the reaction is finished, and carrying out reduced pressure distillation to obtain an intermediate 4;
step 5, adding 0.08mol of the intermediate 4 and 140mL of dimethylformamide into a three-neck flask in a water bath, then adding 0.08mol of 2,2,6, 6-tetramethylpiperidine, stirring at 70 ℃ for reaction for 1h, and obtaining an intermediate 5 after the reaction is finished; then adding 12.4g of sodium methoxide methanol solution with the mass fraction of 30% into a three-neck flask, mixing for 10min at the rotating speed of 60r/min, adding 0.08mol of gamma-chloropropyltrimethoxysilane, heating and stirring at the controlled temperature of 65 ℃ for 5min to remove methanol, heating to 135 ℃, carrying out reflux reaction for 10h, cooling and standing overnight after the reaction is finished, carrying out suction filtration, and carrying out reduced pressure distillation on the filtrate under the protection of nitrogen to obtain an intermediate 6;
step 6, under the protection of nitrogen, adding 7g of magnesium-aluminum hydrotalcite and 200mL of 50% ethanol solution in mass fraction into a three-neck flask, stirring and reacting for 1h at 70 ℃, dropwise adding 4.5mL of ethanol solution of intermediate 6 into the three-neck flask, after dropwise adding, adding 17% hydrochloric acid solution in mass fraction to adjust the pH value to 3, stirring and reacting for 3h, after reacting, cooling to room temperature, filtering, washing a filter cake with deionized water until the washing solution is neutral, and finally drying at 65 ℃ to constant weight to obtain an additive, wherein the dosage ratio of the ethanol solution of the intermediate 6 is that the intermediate 6 and ethanol are 1g by mass: 4mL of the mixture was mixed.
Example 3
The additive is prepared by the following steps:
step 1, adding 30mmol of cyanuric chloride and 90mmol of resorcinol into a three-neck flask, then adding 175mL of nitrobenzene, magnetically stirring at 40 ℃ for 10min, adding 0.7g of aluminum trichloride catalyst into the three-neck flask, heating to 80 ℃, carrying out heat preservation reaction for 2h, after the reaction is finished, carrying out suction filtration while hot, washing a filter cake with deionized water for 4 times, combining filtrates, separating the combined filtrates by using a separating funnel, and obtaining an organic phase as an intermediate 1;
step 2, adding 0.01mol of the intermediate 1, 38mL of acetone and 4.63g of epoxy chloropropane into a three-neck flask, heating to 80 ℃, then dropwise adding 20mL of a 2.5 wt% sodium hydroxide aqueous solution at a dropping speed of 2 drops/second, stirring and reacting for 2 hours at a rotating speed of 200r/min after the dropwise adding is finished, adding ethyl acetate for extraction after the reaction is finished, removing an organic solvent through a rotary evaporator, purifying through a silica gel chromatographic column, and performing vacuum drying for 12 hours at 50 ℃ to obtain an intermediate 2;
step 3, adding 0.01mol of the intermediate 2 and 68mL of tetrahydrofuran into a beaker, stirring for 10min at the rotating speed of 80r/min, dropwise adding 10mL of ethanol solution of p-aminodiphenylamine into the beaker, after dropwise adding, magnetically stirring at room temperature for reaction for 60min, after the reaction, filtering, and removing the organic solvent from the filtrate in a rotary evaporator to obtain an intermediate 3; wherein the ethanol solution of the p-aminodiphenylamine is prepared from the p-aminodiphenylamine and absolute ethanol according to the weight ratio of 1.85 g: 10mL of the mixture is mixed;
step 4, under the protection of nitrogen, adding 0.01mol of the intermediate 3 and 72mL of tetrahydrofuran into a three-neck flask, stirring for 5min, adding 0.01mol of diphenylmethane diisocyanate and 1mL of dibutyl tin dilaurate, refluxing and stirring at 70 ℃ for reaction for 3h, cooling to room temperature after the reaction is finished, and carrying out reduced pressure distillation to obtain an intermediate 4;
step 5, adding 0.08mol of the intermediate 4 and 140mL of dimethylformamide into a three-neck flask in a water bath, then adding 0.08mol of 2,2,6, 6-tetramethylpiperidine, stirring at 70 ℃ for reaction for 1h, and obtaining an intermediate 5 after the reaction is finished; then adding 14.4g of sodium methoxide methanol solution with the mass fraction of 30% into a three-neck flask, mixing for 10min at the rotating speed of 60r/min, adding 0.09mol of gamma-chloropropyltrimethoxysilane, heating and stirring at the controlled temperature of 65 ℃ for 5min to remove methanol, heating to 136 ℃, carrying out reflux reaction for 10h, cooling and standing overnight after the reaction is finished, carrying out suction filtration, and carrying out reduced pressure distillation on the filtrate under the protection of nitrogen to obtain an intermediate 6;
step 6, under the protection of nitrogen, adding 7g of magnesium-aluminum hydrotalcite and 200mL of 50% ethanol solution in mass fraction into a three-neck flask, stirring and reacting for 1h at 70 ℃, dropwise adding 5mL of the ethanol solution of the intermediate 6 into the three-neck flask, after dropwise adding, adding 17% hydrochloric acid solution in mass fraction to adjust the pH value to 3, stirring and reacting for 3h, after reacting, cooling to room temperature, filtering, washing a filter cake with deionized water until the washing solution is neutral, and finally drying to constant weight at 65 ℃ to obtain an additive, wherein the dosage ratio of the ethanol solution of the intermediate 6 is that the intermediate 6 and ethanol are 1g by mass: 5mL of the above-mentioned components were mixed.
Comparative example 1
This comparative example is UV-0, an ultraviolet absorber sold by Nantong Runfeng petrochemical Co., Ltd.
Comparative example 2
This comparative example is a magnesium aluminum hydrotalcite sold by Noojia plastication Co., Ltd, Dongguan.
Example 4
The anti-aging durable asphalt comprises the following raw materials in parts by weight: 120 parts of matrix asphalt, 10 parts of epoxy natural rubber and 8 parts of the additive in the embodiment 1;
the anti-aging durable asphalt is prepared by the following steps:
firstly, adding matrix asphalt and epoxy natural rubber into a reaction kettle, and stirring for 20min at the temperature of 140 ℃ and the rotating speed of 2000r/min to obtain molten materials;
and secondly, adding the additive in the embodiment 1 into the molten material, heating to 180 ℃, shearing for 40min at the rotating speed of 4500r/min under the action of a high-speed shearing machine, stirring for 20min at the rotating speed of 2000r/min and at the temperature of 120 ℃ by using a magnetic stirrer after shearing is finished, and finally standing for 2h in a 120 ℃ blast drying box to obtain the anti-aging durable asphalt.
Example 5
The anti-aging durable asphalt comprises the following raw materials in parts by weight: 120 parts of matrix asphalt, 12 parts of epoxy natural rubber and 9 parts of the additive of the embodiment 2;
the anti-aging durable asphalt is prepared by the following steps:
firstly, adding matrix asphalt and epoxy natural rubber into a reaction kettle, and stirring for 20min at the temperature of 140 ℃ and the rotating speed of 2000r/min to obtain molten materials;
and secondly, adding the additive in the embodiment 2 into the molten material, heating to 180 ℃, shearing for 40min at the rotating speed of 4500r/min under the action of a high-speed shearing machine, stirring for 20min at the rotating speed of 2000r/min and the temperature of 120 ℃ by using a magnetic stirrer after shearing is finished, and finally standing for 2h in a 120 ℃ blast drying box to obtain the anti-aging durable asphalt.
Example 6
The anti-aging durable asphalt comprises the following raw materials in parts by weight: 120 parts of matrix asphalt, 13 parts of epoxy natural rubber and 10 parts of the additive of example 3;
the anti-aging durable asphalt is prepared by the following steps:
firstly, adding matrix asphalt and epoxy natural rubber into a reaction kettle, and stirring for 20min at the temperature of 140 ℃ and the rotating speed of 2000r/min to obtain molten materials;
and secondly, adding the additive in the embodiment 3 into the molten material, heating to 180 ℃, shearing for 40min at the rotating speed of 4500r/min under the action of a high-speed shearing machine, stirring for 20min at the rotating speed of 2000r/min and the temperature of 120 ℃ by using a magnetic stirrer after shearing is finished, and finally standing for 2h in a 120 ℃ blast drying box to obtain the anti-aging durable asphalt.
Comparative example 3
Compared with example 4, the additive in example 4 is replaced by UV-0 in comparative example 1, and the rest of raw materials and preparation process are unchanged.
Comparative example 4
Compared with the example 5, the additive in the example 5 is replaced by the magnesium-aluminum hydrotalcite in the proportion 2, and the rest raw materials and the preparation process are unchanged.
Comparative example 5
Compared with the example 6, the additive in the example 6 is removed, and the rest raw materials and the preparation process are unchanged.
The bituminous materials of examples 4 to 6 and comparative examples 3 to 5 were subjected to a performance test:
softening point: according to the standard GB/T4507-2014, placing a certain mass of steel balls on the surface of a copper ring grinding tool filled with asphalt in an environment of 5 +/-0.5 ℃, observing the temperature of the steel balls sinking to a bottom baffle, and recording the temperature as a softening point;
ductility: determining a ductility value according to a standard GB/T4508-2010, selecting an 8-shaped die, and performing a tensile test on the die at 10 ℃, wherein the ductility of the asphalt is the length of the test sample when the test sample breaks;
TFOT aging and UV aging: each group of asphalt is subjected to a film oven test and an ultraviolet oven irradiation test (ultraviolet light intensity 1200 mu W/cm) 2 Aging at 60 deg.C for 6 days);
using the softening point increment delta T as the softening point after aging-the softening point before aging; ductility retention ratio K D -aged post-ductility/aged pre-ductility;
the test results are shown in table 1:
TABLE 1
As can be seen from Table 1, the increases in softening points Δ T after TFOT aging and UV aging for the bitumens of examples 4 to 6 are smaller than those of comparative examples 3 to 5; ductility retention ratio K D Are all larger than comparative examples 3-5, which shows that the asphalt of examples 4-6 has better aging resistance and has greater application value in the fields of road construction and the like.
The foregoing is merely exemplary and illustrative of the principles of the present invention and various modifications, additions and substitutions of the specific embodiments described herein may be made by those skilled in the art without departing from the principles of the present invention or exceeding the scope of the claims set forth herein.
Claims (6)
1. The anti-aging durable asphalt is characterized by comprising the following raw materials in parts by weight: 120 parts of matrix asphalt, 10-13 parts of cosolvent and 8-10 parts of additive;
wherein, the additive is prepared by the following steps:
step 1, adding cyanuric chloride and resorcinol into a three-neck flask, then adding nitrobenzene, magnetically stirring for 10min at the temperature of 40 ℃, adding aluminum trichloride, heating to 80 ℃, carrying out heat preservation reaction for 2h, carrying out suction filtration while hot, washing filter cakes, combining filtrates, separating liquid, and obtaining an organic phase as an intermediate 1;
step 2, adding the intermediate 1, acetone and epichlorohydrin into a three-neck flask, heating to 80 ℃, dropwise adding a sodium hydroxide aqueous solution, stirring for reacting for 2 hours, extracting with ethyl acetate, performing rotary evaporation, purifying with a silica gel chromatographic column, and drying to obtain an intermediate 2;
step 3, adding the intermediate 2 and tetrahydrofuran into a beaker, stirring for 10min, then dropwise adding an ethanol solution of p-aminodiphenylamine, stirring for reacting for 30-60min, filtering, and rotatably steaming the filtrate to obtain an intermediate 3;
step 4, under the protection of nitrogen, adding the intermediate 3 and tetrahydrofuran into a three-neck flask, stirring for 5min, adding diphenylmethane diisocyanate and dibutyl tin dilaurate, refluxing and stirring at the temperature of 70 ℃, reacting for 3h, cooling to room temperature, and distilling under reduced pressure to obtain an intermediate 4;
step 5, adding the intermediate 4 and dimethylformamide into a three-neck flask in a water bath, then adding 2,2,6, 6-tetramethylpiperidine, and stirring at the temperature of 70 ℃ for reacting for 1h to obtain an intermediate 5; adding a sodium methoxide methanol solution, mixing for 10min, adding gamma-chloropropyltrimethoxysilane, heating and stirring for 5min at the temperature of 65 ℃, heating to 136 ℃ and carrying out reflux reaction for 10h, cooling, carrying out suction filtration, and carrying out reduced pressure distillation on the filtrate to obtain an intermediate 6;
and 6, adding the magnesium-aluminum hydrotalcite and the ethanol solution into a three-neck flask under the protection of nitrogen, stirring at 70 ℃ for reaction for 1h, then dropwise adding the ethanol solution of the intermediate 6, adding a hydrochloric acid solution to adjust the pH value to 3, stirring for reaction for 3h, then cooling to room temperature, filtering, washing a filter cake, and drying to obtain the additive.
2. The anti-aging durable asphalt as claimed in claim 1, wherein the dosage ratio of cyanuric chloride, resorcinol, nitrobenzene and aluminum trichloride catalyst in step 1 is 30 mmol: 90mmo l: 170-180 mL: 0.5-0.8g, wherein the using ratio of the intermediate 1, the acetone, the epichlorohydrin and the sodium hydroxide aqueous solution in the step 2 is 0.01 mol: 30-38 mL: 4.63 g: 20 mL.
3. The anti-aging durable asphalt as claimed in claim 1, wherein the ratio of the amount of the ethanol solution of the intermediate 1, tetrahydrofuran and p-aminodiphenylamine used in step 3 is 0.01 mol: 62-68 mL: 10 mL; in the step 4, the dosage ratio of the intermediate 3, tetrahydrofuran, diphenylmethane diisocyanate and dibutyl tin dilaurate is 0.01 mol: 68-72 mL: 0.01 mol: 1 mL.
4. The anti-aging durable asphalt as claimed in claim 1, wherein the amount ratio of the intermediate 4, dimethylformamide, 2,6,6, -tetramethylpiperidine, sodium methoxide methanol solution and gamma-chloropropyltrimethoxysilane in step 5 is 0.08 mol: 140mL of: 0.08 mol: 10.5-14.4 g: 0.08-0.09 mol; in the step 6, the dosage ratio of the magnesium aluminum hydrotalcite, the ethanol solution and the ethanol solution of the intermediate 6 is 7 g: 200mL of: 4-5 mL.
5. The anti-aging durable asphalt as claimed in claim 1, wherein the cosolvent is one or more of epoxy natural rubber, polyethylene resin, n-hexane and xylene mixed in any proportion.
6. The method for preparing the anti-aging durable asphalt as claimed in claim 1, wherein the method comprises the following steps:
firstly, adding matrix asphalt and a cosolvent into a reaction kettle, and stirring for 20min at the temperature of 140 ℃ to obtain a molten material;
and secondly, adding an additive into the molten material, heating to 180 ℃, shearing for 40min under the action of a high-speed shearing machine, stirring for 20min at the temperature of 120 ℃ by using a magnetic stirrer after shearing is finished, and finally standing for 2h in a 120 ℃ blast drying box to obtain the anti-aging durable asphalt.
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| CN116656412A (en) * | 2023-05-26 | 2023-08-29 | 深圳市合诚润滑材料有限公司 | Multifunctional lubricating grease and preparation method thereof |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN116656412A (en) * | 2023-05-26 | 2023-08-29 | 深圳市合诚润滑材料有限公司 | Multifunctional lubricating grease and preparation method thereof |
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