An asphalt mixture and a method for producing the same

Abstract

The application discloses asphalt mixture and a preparation method thereof. The asphalt mixture comprises, by weight, 2000 parts of aggregate, 90-110 parts of asphalt, 0.05-0.2 parts of fast-release microcapsules, 0.05-0.2 parts of medium-release microcapsules, 0.05-0.2 parts of inorganic microcapsules, and 0.01-0.1 parts of antioxidant. The fast-release microcapsules and the medium-release microcapsules each independently comprise a capsule core, a capsule wall and a film wrapping material, wherein the capsule wall is wrapped outside the capsule core, and the film wrapping material is wrapped outside the capsule wall. The capsule core comprises an active component, the capsule wall comprises a resin, and the film wrapping material comprises a rubber material. The asphalt mixture can realize slow release of the active component, prolong the action time of the active component, has good compatibility with asphalt, effectively reduces the emission of asphalt fume during construction, and reduces the pollution to the environment.

Description

Technical Field

[0001] This invention relates to a special asphalt mixture and its preparation method, and particularly to a long-life clean asphalt mixture and its preparation method. Background Technology

[0002] As a major type of highway, asphalt pavement still uses the traditional hot-mix hot-paving process in its construction. During construction, asphalt comes into contact with oxygen in the air and reacts: on the one hand, it undergoes a condensation reaction to generate polycyclic aromatic hydrocarbons with larger molecular weights, which further condense into gums and asphaltenes; on the other hand, asphalt molecules will decompose under heating conditions to generate compounds with smaller molecular weights. These small molecule compounds volatilize and form asphalt fumes, which seriously disrupt the ecological balance, pollute the surrounding environment, and harm human health.

[0003] Given that volatile organic compounds (VOCs) are released unorganized during the paving process of asphalt pavement, and it is difficult to collect and treat them throughout the entire process, exploring how to reduce the release of asphalt fumes at the source, achieve clean construction of asphalt pavement, and ensure the harmonious development of the transportation industry and the social economy is an urgent problem to be solved.

[0004] CN101842426A discloses a method for reducing the odor of asphalt-like substances. This method reduces the odor of asphalt-like substances by adding activators and diluents. However, the added activators have poor reactivity and limited action time, making them unable to work for a long time. CN109749466A discloses a smoke suppressant and odor deodorizer additive, its preparation method, and modified asphalt. It reduces the emission of asphalt fumes by using metal-organic framework compounds, inorganic adsorbents, reactive odor inhibitors, and free radical scavengers. However, its inorganic adsorbents have poor compatibility with asphalt, affecting the performance of asphalt. It also suffers from the problem of short action time of the active components.

[0005] In summary, existing technologies simply add inorganic fillers or active components to asphalt, which leads to problems such as segregation and stratification of inorganic fillers and asphalt, poor dispersion, and limited action time of active components, preventing them from exerting their effects for an extended period. Summary of the Invention

[0006] To address the shortcomings of existing technologies, this invention provides an asphalt mixture and its preparation method. The asphalt mixture of this invention encapsulates different active components in microcapsules, enabling the slow release of these active components and prolonging their action time. Simultaneously, it exhibits excellent compatibility with asphalt, effectively reducing asphalt fume emissions and environmental pollution during construction.

[0007] This invention provides an asphalt mixture, comprising the following raw material components by weight:

[0008] Materials collected: 2000 portions;

[0009] Asphalt: 90-110 parts;

[0010] Rapid-release microcapsules: 0.05–0.2 parts;

[0011] Medium-release microcapsules: 0.05–0.2 parts;

[0012] Inorganic microcapsules: 0.05–0.2 parts;

[0013] Antioxidant: 0.01–0.1 parts;

[0014] The fast-release microcapsules and the medium-release microcapsules each independently include a core, a wall, and a membrane encapsulation material, wherein the wall encapsulates the outer layer of the core, and the membrane encapsulation material encapsulates the outer layer of the wall; the core includes an active component, the wall includes a resin, and the membrane encapsulation material includes a rubber material.

[0015] Furthermore, the aggregate can be any of the aggregate raw materials commonly used in the art, such as limestone, basalt, etc.

[0016] Furthermore, the asphalt can be at least one of straight-run asphalt, polymer-modified asphalt, and natural asphalt. Preferably, the asphalt has a penetration of 30–100 1 / 10 mm at 25°C.

[0017] Further, the antioxidant is one or more of 2,2,6,6-tetramethylpiperidinamine, 4-benzoyloxy-2,2,6,6-tetramethylpiperidin, bis[2,2,6,6-tetramethyl-4-piperidinyl] sebacate, and bis[2,2,6,6-tetramethyl-4-piperidinyl]isophthalamide. Further, in the rapid-release microcapsule, the mass ratio of the core, wall, and membrane encapsulation material is 1:(0.7-1):(0.2-0.3).

[0018] Furthermore, in the medium-speed release microcapsule, the mass ratio of the core, the wall, and the membrane encapsulation material is 1:(1.2-1.5):(0.4-0.5).

[0019] Furthermore, the sum of the thickness of the capsule wall and the membrane encapsulation material of the rapid release microcapsule is 0.5–2 μm.

[0020] Furthermore, the sum of the thickness of the capsule wall and the membrane encapsulation material of the medium-speed release microcapsule is 2.1–3 μm.

[0021] Furthermore, in the fast-release microcapsules and medium-release microcapsules, the elastic modulus of the microcapsule and the sum of the thickness of the capsule wall and the membrane encapsulation material satisfy the following formula:

[0022] Y = 0.42X 2 -0.92X+T;

[0023] Wherein, Y is the elastic modulus of the microcapsule, in GPa; X is the sum of the thicknesses of the capsule wall and the membrane encapsulation material, in μm; and T is 1 ± 0.1.

[0024] Furthermore, the elastic modulus of the microcapsule was obtained by testing the mechanical properties of the microcapsule using a nanoindenter, and the thickness of the capsule wall and membrane encapsulation material was obtained by testing the frozen sections of the microcapsule using a scanning electron microscope.

[0025] Furthermore, the size of the fast-release microcapsules and the medium-release microcapsules conforms to the size of conventional microcapsules in the art, each being independently less than 50 micrometers, preferably less than 20 micrometers, and more preferably 3 to 15 μm.

[0026] Furthermore, the active component encapsulated in the rapid-release microcapsule is a first active component, which is one or more of aldehyde compounds and ketone compounds. The aldehyde compounds are selected from one or more of p-methylbenzaldehyde, decanal, o-carboxybenzaldehyde, p-isopropylbenzaldehyde, cinnamaldehyde, p-hydroxybenzaldehyde, p-methoxybenzaldehyde, 2-methyl-3-(3,4-methylene-dioxyphenyl)propanal, 3,4-methylenedioxybenzaldehyde, 3-(4-isopropylphenyl)-2-methylpropanal, ethyl vanillin, phenylacetaldehyde, anisaldehyde, nonadien-2,6-aldehyde, 2,6-dimethyl-2,6-octadienal, vanillin, citronellol, neraldehyde, hydroxymethylpentylcyclohexene acetal, p-diethylaminobenzaldehyde, and undecenal; the ketone compounds are selected from one or more of 6-methyl-3,5-heptadien-2-one, 2-undecenone, acetophenone, ionone, irisone, methyl ionone, damasone, and dihydrodamasone.

[0027] Furthermore, the active component encapsulated in the medium-release microcapsule is a second active component, which is one or more of alcohols and phenols. The alcohols are one or more of cinnamyl alcohol, menthol, cis-3,7-dimethyl-2,6-octadienol, citronellol, geraniol, myrceneol, 2,6,10-trimethyl-2,6,10-dodecanetrien-12-ol, lavenderol, benzyl alcohol, 2-phenylethanol, dihydromyrceneol, tetrahydrogeraniol, and nerolidol. The phenols are one or more of thymol, ethyl maltol, methyl maltol, 3-propenyl-6-ethoxyphenol, and isoeugenol.

[0028] Furthermore, in the capsule wall of the fast-release microcapsule or the medium-release microcapsule, the resin is melamine resin.

[0029] Furthermore, in the fast-release microcapsules or medium-release microcapsules, the membrane encapsulation material is a uniform and dense membrane material.

[0030] Furthermore, in the membrane encapsulation material of the fast-release microcapsules or medium-release microcapsules, the rubber material is one or more of chlorinated rubber, styrene-butadiene rubber, and chloroprene rubber. The membrane encapsulation materials of the fast-release microcapsules and the medium-release microcapsules can be the same or different.

[0031] Furthermore, the inorganic microcapsule includes a core and a wall, wherein the wall wraps around the core; the core includes a third active component, and the wall includes organosilane-modified silica.

[0032] Furthermore, the third active component encapsulated in the inorganic microcapsules is one or more ester compounds. The ester compounds are one or more selected from methyl salicylate, methyl cinnamate, ethyl cinnamate, ethyl phenylacetate, methyl phenylacetate, geraniol phenylacetate, phenethyl phenylacetate, isoamyl phenylacetate, benzyl salicylate, p-methylbenzyl acetate, benzyl acetate, isobutyl benzoate, isoamyl salicylate, benzyl cinnamate, phenethyl cinnamate, linaloyl formate, linaloyl acetate, linaloyl isobutyrate, menthyl acetate, terpineol acetate, and borneol acetate.

[0033] Furthermore, the organosilane is a sulfonylsilane obtained by oxidizing a mercaptosilane. The mercaptosilane is one or more of γ-mercaptopropyltrimethoxysilane, γ-mercaptopropyltriethoxysilane, and γ-mercaptopropylmethyldiethoxysilane.

[0034] Furthermore, the mass ratio of the capsule core to the capsule wall in the inorganic microcapsule is 1:(0.3-0.5).

[0035] Furthermore, the size of the inorganic microcapsule conforms to the size of conventional microcapsules in the art, generally below 50 micrometers, preferably below 20 micrometers, and more preferably 1 to 15 μm.

[0036] The present invention also provides a method for preparing the above-mentioned asphalt mixture, comprising:

[0037] a. Prepare fast-release microcapsules and medium-release microcapsules respectively;

[0038] b. Preparation of inorganic microcapsules;

[0039] c. The fast-release microcapsules, medium-release microcapsules, antioxidants, and asphalt are mixed evenly under heating conditions to obtain purified asphalt;

[0040] d. The purified asphalt, inorganic microcapsules, and aggregates are mixed to obtain an asphalt mixture.

[0041] Further, in step a, the preparation process of the rapid-release microcapsules includes:

[0042] (1) The first active component is mixed with the first emulsifier and water to form an oil-in-water emulsion;

[0043] (2) The water-in-oil emulsion is reacted with the resin prepolymer, and then filtered, washed and dried to obtain the pre-coated material;

[0044] (3) In the presence of a volatile solvent, the rubber material is mixed with the pre-coated material obtained in step (2), and then the resulting mixture is mixed with water and heated until the volatile solvent evaporates to obtain a fast-release microcapsule coated with the first active component.

[0045] Further, in step a, the preparation process of the medium-rate release microcapsules includes:

[0046] (11) The second active component is mixed with the second emulsifier and water to form an oil-in-water emulsion;

[0047] (22) The oil-in-water emulsion is reacted with the resin prepolymer, and then filtered, washed and dried to obtain the pre-coated material;

[0048] (33) In the presence of a volatile solvent, the rubber material is mixed with the pre-coated material obtained in step (22), and then the resulting mixture is mixed with water and heated until the volatile solvent evaporates to obtain medium-speed release microcapsules coated with the second active component.

[0049] Further, in step (1), the weight ratio of the first active component, the first emulsifier, and water is 1:(0.05~0.09):(6~9). Further, in step (11), the weight ratio of the second active component, the second emulsifier, and water is 1:(0.05~0.09):(6~9).

[0050] Further, in step (1) or step (11), the first emulsifier and the second emulsifier are each independently selected from one or more of sodium stearate, sodium dodecyl sulfate, sodium dodecylbenzene sulfonate, hexadecyltrimethylammonium chloride, hexadecyltrimethylammonium bromide, hexadecyldimethylhydroxyethylammonium chloride, nonylphenol polyoxyethylene ether, octylphenol polyoxyethylene ether, and hexadecane polyoxyethylene ether.

[0051] Further, in step (1) or step (11), the mixing process can be carried out in a shearing machine, and the shearing operation conditions may include: a rotation speed of 2000 to 4000 r / min and a time of 20 to 30 min.

[0052] Further, the preferred operation process of step (1) is to dissolve the first active component in water (the water temperature is preferably 60-90°C), then add the first emulsifier and perform high-speed shear emulsification.

[0053] Further, the preferred operation process of step (11) is to dissolve the second active component in water (the water temperature is preferably 60-90°C), then add the second emulsifier and perform high-speed shear emulsification.

[0054] Further, in step (2) or step (22), before the oil-in-water emulsion reacts with the resin prepolymer, the pH value of the oil-in-water emulsion is adjusted to below 5, preferably to 2-4. The reagent used to adjust the pH value can be a conventional inorganic acid solution, such as dilute hydrochloric acid.

[0055] Further, in step (2) or step (22), the weight ratio of the oil-in-water emulsion to the resin prepolymer is 1:(0.08~0.20).

[0056] Further, in step (2) or step (22), the reaction between the oil-in-water emulsion and the resin prepolymer is carried out under stirring. The stirring speed can be 400-1000 r / min, the reaction temperature can be 60-90℃, and the time can be 1-5 h.

[0057] Furthermore, in step (2) or step (22), the resin prepolymer can be prepared by the following method:

[0058] Melamine and formaldehyde solution are mixed and dissolved in water, and the pH value is adjusted to 7.5–9.5. The mixture is then placed in a constant temperature water bath at 60–90°C and reacted with stirring for 0.5–3.5 hours. Further, the mass concentration of the formaldehyde solution is 30%–40%. The weight ratio of melamine, formaldehyde solution, and water is 1:(2–3):(8–10).

[0059] Furthermore, in step (2) or step (22), the washing process may include washing with water and ethanol two or more times respectively.

[0060] Furthermore, in step (2) or step (22), the drying process can be carried out in an oven, and the drying temperature can be 60-90°C for 5-10 hours.

[0061] Further, in step (3) or step (33), the weight ratio of the rubber material to the pre-coated material obtained in step (2) is (0.08~0.25):1.

[0062] Furthermore, in step (3) or step (33), the heating is carried out under stirring, and the stirring speed can be 400-1000 r / min.

[0063] Further, in step (3) or step (33), the volatile solvent is selected from one or more of carbon tetrachloride, dichloromethane, and trichloroethylene.

[0064] Further, in step (3) or step (33), the weight ratio of the rubber material, volatile solvent and water is 1:(10-20):(50-150).

[0065] Furthermore, the preparation process in step b includes:

[0066] (i) The third active component, the third emulsifier and water are mixed and reacted with a silicon source. Then, the mixture is washed, filtered and dried to obtain silica microcapsules coated with the active component.

[0067] (ii) The silica microcapsules coated with the active components, organosilane and organic solvent are mixed to carry out a surface modification reaction, and then cooled, filtered, washed and dried to obtain surface-modified silica microcapsules.

[0068] (iii) After mixing the surface-modified silica microcapsules with hydrogen peroxide solution for oxidation reaction, the microcapsules are washed and dried to obtain inorganic microcapsules.

[0069] Further, in step (i), the silicon source is preferably tetraethyl orthosilicate.

[0070] Further, in step (i), the third emulsifier is selected from one or more of sodium stearate, sodium dodecyl sulfate, sodium dodecylbenzene sulfonate, hexadecyltrimethylammonium chloride, hexadecyltrimethylammonium bromide, hexadecyldimethylhydroxyethylammonium chloride, nonylphenol polyoxyethylene ether, octylphenol polyoxyethylene ether, and hexadecane polyoxyethylene ether.

[0071] Further, the preferred procedure in step (i) is as follows: dissolve the third active component in water (preferably at a temperature of 60–90°C), then add the third emulsifier, perform high-speed shear emulsification, adjust the pH, and then add a silicon source to initiate the reaction. Further, the shearing conditions may include: a rotation speed of 2000–4000 r / min and a time of 20–30 min. Further, the pH adjustment is set to 2.5–5. The pH adjustment can be achieved using commonly used acid-base regulators in the art, such as hydrochloric acid.

[0072] Further, in step (i), the weight ratio of the third active component, the third emulsifier, water, and silicon source is 1:(0.05~0.3):(3~7):(1~5), preferably 1:(0.1~0.2):(4~5):(1~1.5).

[0073] Further, in step (i), the reaction conditions are: a reaction time of 10 to 18 hours and a reaction temperature of 60 to 80°C.

[0074] Furthermore, in step (i), the washing and filtering processes employ conventional methods in the art. The drying temperature can be 80–100°C, and the drying time can be 5–8 hours.

[0075] Further, in step (ii), the weight ratio of the silica microcapsules coated with the active components to the organosilane and the organic solvent is 1:(0.01-0.1):(10-30).

[0076] Further, in step (ii), the organic solvent is preferably one or more of xylene, toluene, cyclohexanone, chlorobenzene and pyridine.

[0077] Further, in step (ii), the surface modification reaction is carried out at a temperature of 100°C to 120°C for a time of 1 to 3 hours.

[0078] Furthermore, in step (ii), the filtration, washing, and drying can all be performed using conventional methods in the art. The washing can be carried out using solvents such as ethanol, chloroform, and acetone, and the drying is performed by allowing the solvent to evaporate. The drying temperature can be 80℃~120℃, and the time can be 0.5~5h.

[0079] Further, in step (iii), the weight ratio of the surface-modified silica microcapsules to the hydrogen peroxide solution is 1:(5-10). The mass fraction of the hydrogen peroxide solution is 10%-30%.

[0080] Furthermore, in step (iii), the oxidation reaction is carried out at a temperature of 50–90°C for 1–5 hours.

[0081] Further, in step (iii), the washing process preferably involves washing with water and ethanol two or more times respectively. The drying temperature is 60–90°C, and the drying time is 6–10 hours.

[0082] Further, in step c, the heating temperature is 140-180℃, and the mixing is carried out by mechanical stirring. Preferably, the stirring speed is 500-1000 r / min, and the stirring time is 1-3 h.

[0083] Furthermore, in step d, the mixing temperature is 150–180°C, and the mixing time is 1–3 min.

[0084] Compared with the prior art, the asphalt mixture and its preparation method of the present invention have the following advantages:

[0085] The microcapsules of the present invention, which encapsulate active components, include a core, a capsule wall encapsulating the core, and a membrane encapsulation material encapsulating the outer layer of the capsule wall. The present invention is the first to use rubber as the membrane encapsulation material. The rubber is encapsulated in the form of a uniform and dense membrane material on the outside of melamine resin, so that the self-healing microcapsule as a whole can not only ensure a certain strength, but also effectively integrate with asphalt and has good compatibility.

[0086] This invention employs microcapsules with varying release rates to encapsulate different active components, achieving slow release and stepwise reaction of the active components. This prolongs the action time of the active components, resulting in a longer storage and service life for the purified asphalt. During the mixing process, the inorganic microcapsules further release the active components, and their acidic sites on the outer surface catalyze and accelerate the reaction, effectively reducing asphalt fume emissions and environmental pollution. The antioxidants added to the long-life purified asphalt contain amine groups, increasing the alkalinity of the asphalt, while the acidic sites of the inorganic microcapsules increase the acidity of the aggregate, resulting in better adhesion between the asphalt and aggregate and improved resistance to water damage. Detailed Implementation

[0087] The technical solution of the present invention is further described below through embodiments, but these embodiments cannot limit the present invention.

[0088] In this invention, the elastic modulus of the microcapsule is obtained by testing the mechanical properties of the microcapsule using a nanoindenter (KLA Corporation iNano), and the thickness of the capsule wall is obtained by testing the frozen sections of the microcapsule using a scanning electron microscope (Hitachi S-4800).

[0089] Unless otherwise specified, the experimental methods used in the following embodiments are conventional methods in the art. Unless otherwise specified, the experimental materials used in the following embodiments are commercially available.

[0090] Example 1

[0091] (1) Add 1 part by weight of 3,4-methylenedioxybenzaldehyde to 9 parts by weight of water at 60°C, add 0.05 parts by weight of hexadecyltrimethylammonium bromide, and shear emulsify using a shear machine at 2000 r / min for 30 min to form an oil-in-water emulsion of the first active component in the aqueous phase.

[0092] Add 1 part by weight of myrcene alcohol to 9 parts by weight of water at 60°C, add 0.05 parts by weight of cetyltrimethylammonium bromide, and shear emulsify using a shear machine at 2000 r / min for 30 min to form an oil-in-water emulsion of the second active component in the aqueous phase.

[0093] (2) Dissolve 1 part by weight of melamine, 2 parts by weight of formaldehyde solution with a concentration of 37 wt.% and 8 parts by weight of deionized water in a three-necked flask, adjust the pH value to 8.5, and then place it in a constant temperature water bath at 60°C and stir at 800 r / min for 0.5 h to obtain melamine resin prepolymer.

[0094] Dilute hydrochloric acid was added dropwise to 1 part by weight of the first active component oil-in-water emulsion to adjust the pH value to 2. 0.10 parts by weight of the prepared melamine resin prepolymer was slowly added dropwise to the oil-in-water emulsion. The mixture was stirred at 700 r / min and reacted at 75°C for 2 h. After the reaction was completed, the resulting mixed solution was filtered, washed twice with water and ethanol respectively, and dried in an oven at 60°C for 10 h to obtain the material with the first active component coated on the inner wall.

[0095] Dilute hydrochloric acid was added dropwise to 1 part by weight of the second active component oil-in-water emulsion to adjust the pH value to 2. 0.12 parts by weight of the prepared melamine resin prepolymer was slowly added dropwise to the oil-in-water emulsion. The mixture was stirred at 700 r / min and reacted at 75℃ for 2 h. After the reaction was completed, the resulting mixed solution was filtered, washed twice with water and ethanol respectively, and dried in an oven at 60℃ for 10 h to obtain the material with the second active component coated on the inner wall.

[0096] (3) Dissolve 0.1 parts by weight of chlorinated rubber in 1 part by weight of dichloromethane, add 1.00 parts by weight of the inner wall coating material for the first active component, and mix thoroughly. Add the resulting mixture to 8 parts by weight of water, stir at 500 r / min, and raise the temperature until the solvent evaporates to obtain fast-release microcapsules coated with the first active component. The capsules have a size of 3-5 μm, an elastic modulus of 0.5 GPa, and a combined thickness of 1.2 μm for the capsule wall and membrane coating material, which conforms to the calculation formula Y = 0.42X. 2 -0.92X+T. Testing revealed that the mass ratio of the core, wall, and membrane encapsulation material in this rapid-release microcapsule was 1:1:0.20.

[0097] 0.1 parts by weight of chlorinated rubber were dissolved in 1 part by weight of dichloromethane, and 0.55 parts by weight of the inner wall coating material for the second active component were added and thoroughly mixed. The resulting mixture was then added to 8 parts by weight of water and stirred at 500 r / min. The temperature was increased until the solvent evaporated, yielding medium-rate release microcapsules coated with the second active component. These microcapsules had a size of 5–7 μm, an elastic modulus of 0.9 GPa, and a combined thickness of 2.1 μm for the capsule wall and membrane coating material, conforming to the calculation formula Y = 0.42X. 2 -0.92X+T. Testing revealed that the mass ratio of the core, wall, and membrane encapsulation material in this medium-release microcapsule was 1:1.21:0.42.

[0098] (4) Add 1 part by weight of ethyl phenylacetate to 5 parts by weight of water at 60℃, add 0.1 part by weight of hexadecyltrimethylammonium bromide, shear emulsify using a shear machine at 2000 r / min for 30 min, adjust the pH value to 2.5, add 1.5 parts by weight of tetraethyl orthosilicate, react for 10 h, and then wash, filter, and dry at 80℃ for 8 h to obtain silica microcapsules coated with active components.

[0099] (5) 1 part by weight of silica microcapsules coated with active components and 0.01 part by weight of γ-mercaptopropyltrimethoxysilane were added to 10 parts by weight of toluene. The surface modification reaction was carried out at 100°C under reflux for 1 hour. After cooling, the surface was filtered and washed with ethanol and dried at 80°C for 5 hours to obtain surface-modified silica microcapsules.

[0100] (6) One part by weight of surface-modified silica microcapsules was added to five parts by weight of a 30% hydrogen peroxide solution. After oxidation at 50°C for 1 hour, the microcapsules were washed twice with water and twice with ethanol, and then dried at 60°C for 6 hours to obtain inorganic microcapsules. The mass ratio of the core to the wall in these inorganic microcapsules was found to be 1:0.43. The size of these inorganic microcapsules was 4–7 μm.

[0101] (7) Add 0.1 parts by weight of the prepared fast-release microcapsules, 0.05 parts by weight of the medium-release microcapsules, and 0.01 parts by weight of 2,2,6,6-tetramethylpiperidinamine to 100 parts by weight of straight-run pitch (with a penetration of 70 at 25°C).

[0102] In 1 / 10mm), under heating conditions of 140℃ and stirring at 800r / min for 3h, clean asphalt is obtained.

[0103] (8) Mix 2000 parts by weight of aggregate, 90 parts by weight of cleaned asphalt and 0.05 parts by weight of inorganic microcapsules at 150°C for 1 min to obtain long-life cleaned asphalt mixture.

[0104] Example 2

[0105] (1) Add 1 part by weight of ionone to 7 parts by weight of water at 60°C, add 0.06 parts by weight of nonylphenol polyoxyethylene ether, and shear emulsify for 25 minutes using a shear machine at 2500 r / min to form an oil-in-water emulsion of the first active component in the aqueous phase.

[0106] Add 1 part by weight of myrcene alcohol to 7 parts by weight of water at 60°C, add 0.06 parts by weight of nonylphenol polyoxyethylene ether, and shear emulsify using a shear mill at 2500 r / min for 25 min to form an oil-in-water emulsion of the second active component in the aqueous phase.

[0107] (2) Dissolve 1 part by weight of melamine, 3 parts by weight of formaldehyde solution with a concentration of 37 wt.% and 10 parts by weight of deionized water in a three-necked flask, adjust the pH value to 7.5, and then place it in a constant temperature water bath at 80℃ and stir at 600 r / min for 1 h to obtain melamine resin prepolymer.

[0108] Dilute hydrochloric acid was added dropwise to 1 part by weight of the first active component oil-in-water emulsion to adjust the pH value to 4. 0.12 parts by weight of the prepared melamine resin prepolymer was slowly added dropwise to the oil-in-water emulsion. The mixture was stirred at 600 r / min and reacted at 70℃ for 3 h. After the reaction was completed, the resulting mixed solution was filtered, washed twice with water and ethanol respectively, and dried in an oven at 70℃ for 8 h to obtain the material with the first active component coated on the inner wall.

[0109] Dilute hydrochloric acid was added dropwise to 1 part by weight of the second active component oil-in-water emulsion to adjust the pH value to 4. 0.17 parts by weight of the prepared melamine resin prepolymer was slowly added dropwise to the oil-in-water emulsion. The mixture was stirred at 600 r / min and reacted at 70 °C for 3 h. After the reaction was completed, the resulting mixed solution was filtered, washed twice with water and ethanol respectively, and dried in an oven at 70 °C for 8 h to obtain the material with the second active component coated on the inner wall.

[0110] (3) Dissolve 0.15 parts by weight of chloroprene rubber in 3 parts by weight of carbon tetrachloride, add 1.40 parts by weight of the inner wall coating material for the first active component, and mix thoroughly. Add the resulting mixture to 10 parts by weight of water, stir at 600 r / min, and raise the temperature until the solvent evaporates to obtain fast-release microcapsules coated with the first active component. The size of these microcapsules is 2–4 μm, the elastic modulus is 0.6 GPa, and the sum of the thickness of the capsule wall and the membrane coating material is 0.7 μm, which conforms to the calculation formula Y = 0.42X. 2 -0.92X+T. Testing revealed that the mass ratio of the core, wall, and membrane encapsulation material in this rapid-release microcapsule was 1:0.96:0.22.

[0111] 0.15 parts by weight of chloroprene rubber were dissolved in 3 parts by weight of carbon tetrachloride, and 0.80 parts by weight of the inner wall coating material for the second active component were added and thoroughly mixed. The resulting mixture was then added to 10 parts by weight of water and stirred at 600 r / min. The temperature was increased until the solvent evaporated, yielding medium-rate release microcapsules coated with the second active component. These microcapsules had a size of 5–7 μm, an elastic modulus of 0.9 GPa, and a combined thickness of 2.1 μm for the capsule wall and membrane coating material, conforming to the calculation formula Y = 0.42X. 2 -0.92X+T. Testing revealed that the mass ratio of the core, wall, and membrane encapsulation material in this medium-release microcapsule was 1:1.33:0.44.

[0112] (4) Add 1 part by weight of benzyl acetate to 5 parts by weight of water at 70°C, add 0.15 parts by weight of sodium stearate, shear emulsify at 3000 r / min for 30 min using a shearing machine, adjust the pH value to 4, add 1.4 parts by weight of tetraethyl orthosilicate, react for 12 h, wash and filter according to routine, and dry at 90°C for 8 h to obtain silica microcapsules coated with active components.

[0113] (5) 1 part by weight of silica microcapsules coated with active components and 0.03 parts by weight of γ-mercaptopropyltriethoxysilane were added to 10 parts by weight of toluene. The surface modification reaction was carried out at 100°C under reflux for 3 hours. After cooling, the surface was filtered and washed with ethanol and dried at 90°C for 5 hours to obtain surface-modified silica microcapsules.

[0114] (6) One part by weight of surface-modified silica microcapsules was added to six parts by weight of a 30% hydrogen peroxide solution. After oxidation at 80°C for 2 hours, the microcapsules were washed three times with water and three times with ethanol, and then dried at 70°C for 6 hours to obtain inorganic microcapsules. The mass ratio of the capsule core to the capsule wall in the inorganic microcapsules was found to be 1:0.41. The size of the inorganic microcapsules was 2–6 μm.

[0115] (7) 0.1 parts by weight of the prepared fast-release microcapsules, 0.1 parts by weight of the medium-release microcapsules and 0.03 parts by weight of 4-benzoyloxy-2,2,6,6-tetramethylpiperidine were added to 100 parts by weight of SBS modified asphalt (penetration of 60 1 / 10 mm at 25°C), and stirred at 800 r / min for 3 h under heating conditions at 150°C to obtain purified asphalt.

[0116] (8) Mix 2000 parts by weight of aggregate, 100 parts by weight of cleaned asphalt and 0.05 parts by weight of inorganic microcapsules at 150°C for 1 min to obtain long-life cleaned asphalt mixture.

[0117] Example 3

[0118] (1) Add 0.5 parts by weight of 2,6-dimethyl-2,6-octadienal and 0.5 parts by weight of nerol to 6 parts by weight of water at 60°C, add 0.09 parts by weight of octylphenol polyoxyethylene ether, and shear emulsify for 20 minutes using a shear machine at 3000 r / min to form an oil-in-water emulsion of the first active component in the aqueous phase.

[0119] Add 1 part by weight of dihydromyrcenol to 6 parts by weight of water at 60°C, add 0.09 parts by weight of octylphenol polyoxyethylene ether, and shear emulsify using a shear machine at 3000 r / min for 20 min to form an oil-in-water emulsion of the second active component in the aqueous phase.

[0120] (2) Dissolve 1 part by weight of melamine, 2 parts by weight of formaldehyde solution with a concentration of 37 wt.% and 9 parts by weight of deionized water in a three-necked flask, adjust the pH value to 8, and then place it in a constant temperature water bath at 70°C and stir at 500 r / min for 2 h to obtain melamine resin prepolymer.

[0121] Dilute hydrochloric acid was added dropwise to 1 part by weight of the first active component oil-in-water emulsion to adjust the pH value to 3. 0.14 parts by weight of the prepared melamine resin prepolymer was slowly added dropwise to the oil-in-water emulsion. The mixture was stirred at 500 r / min and reacted at 65℃ for 3 h. After the reaction was completed, the resulting mixed solution was filtered, washed twice with water and ethanol respectively, and dried in an oven at 90℃ for 6 h to obtain the material with the first active component coated on the inner wall.

[0122] Dilute hydrochloric acid was added dropwise to 1 part by weight of the second active component oil-in-water emulsion to adjust the pH value to 3. 0.18 parts by weight of the prepared melamine resin prepolymer was slowly added dropwise to the oil-in-water emulsion. The mixture was stirred at 500 r / min and reacted at 65℃ for 3 h. After the reaction was completed, the resulting mixed solution was filtered, washed twice with water and ethanol respectively, and dried in an oven at 90℃ for 6 h to obtain the material with the second active component coated on the inner wall.

[0123] (3) Dissolve 0.2 parts by weight of styrene-butadiene rubber in 3 parts by weight of dichloromethane, add 1.34 parts by weight of the inner wall coating material for the first active component, and mix thoroughly. Add the resulting mixture to 15 parts by weight of water, stir at 700 r / min, and raise the temperature until the solvent evaporates to obtain fast-release microcapsules coated with the first active component. The size of these microcapsules is 3–5 μm, the elastic modulus is 0.6 GPa, and the sum of the thickness of the capsule wall and the membrane coating material is 1.3 μm, which conforms to the calculation formula Y = 0.42X. 2 -0.92X+T. Testing revealed that the mass ratio of the core, wall, and membrane encapsulation material in this rapid-release microcapsule was 1:0.98:0.30.

[0124] 0.2 parts by weight of styrene-butadiene rubber was dissolved in 3 parts by weight of dichloromethane, and 0.90 parts by weight of the inner wall coating material for the second active component was added and thoroughly mixed. The resulting mixture was then added to 15 parts by weight of water and stirred at 700 r / min. The temperature was increased until the solvent evaporated, yielding medium-rate release microcapsules coated with the second active component. These microcapsules had a size of 5–7 μm, an elastic modulus of 1.1 GPa, and a combined thickness of 2.3 μm for the capsule wall and membrane coating material, conforming to the calculation formula Y = 0.42X. 2 -0.92X+T. Testing revealed that the mass ratio of the core, wall, and membrane encapsulation material in this medium-release microcapsule was 1:1.28:0.50.

[0125] (4) Add 1 part by weight of ethyl cinnamate to 4 parts by weight of water at 65°C, add 0.1 part by weight of sodium dodecylbenzenesulfonate, shear emulsify at 2000 r / min for 20 min using a shearing machine, adjust the pH value to 5, add 1.3 parts by weight of tetraethyl orthosilicate, react for 14 h, wash and filter according to routine, and dry at 100°C for 6 h to obtain silica microcapsules coated with active components.

[0126] (5) 1 part by weight of silica microcapsules coated with active components and 0.05 parts by weight of γ-mercaptopropyltrimethoxysilane were added to 15 parts by weight of toluene. The surface modification reaction was carried out at 110°C under reflux for 2 hours. After cooling, the surface was filtered and washed with ethanol and dried at 90°C for 4 hours to obtain surface-modified silica microcapsules.

[0127] (6) One part by weight of surface-modified silica microcapsules was added to eight parts by weight of a 30% hydrogen peroxide solution. After oxidation at 80°C for 1 hour, the microcapsules were washed twice with water and ethanol, respectively, and dried at 60°C for 8 hours to obtain inorganic microcapsules. The mass ratio of the capsule core to the capsule wall in the inorganic microcapsules was found to be 1:0.37. The size of the inorganic microcapsules was 3–6 μm.

[0128] (7) 0.2 parts by weight of the prepared fast-release microcapsules, 0.15 parts by weight of the medium-release microcapsules and 0.03 parts by weight of the bis[2,2,6,6-tetramethyl-4-piperidinyl] sebacate were added to 100 parts by weight of natural asphalt (penetration of 501 / 10mm at 25℃), and stirred at 500r / min for 2h under heating conditions at 160℃ to obtain purified asphalt.

[0129] (8) Mix 2000 parts by weight of aggregate, 90 parts by weight of cleaned asphalt and 0.1 parts by weight of inorganic microcapsules at 150°C for 1 min to obtain long-life cleaned asphalt mixture.

[0130] Example 4

[0131] (1) Add 1 part by weight of p-methoxybenzaldehyde to 8 parts by weight of water at 60°C, add 0.06 parts by weight of sodium dodecylbenzenesulfonate, and shear emulsify using a shear machine at 4000 r / min for 20 min to form an oil-in-water emulsion of the first active component in the aqueous phase.

[0132] Add 1 part by weight of thymol to 8 parts by weight of water at 60°C, add 0.06 parts by weight of sodium dodecylbenzenesulfonate, and shear emulsify using a shear machine at 4000 r / min for 20 min to form an oil-in-water emulsion of the second active component in the aqueous phase.

[0133] (2) Dissolve 1 part by weight of melamine, 3 parts by weight of formaldehyde solution with a concentration of 37 wt.% and 9 parts by weight of deionized water in a three-necked flask, adjust the pH value to 7.5, and then place it in a constant temperature water bath at 60℃ and stir at 700 r / min for 2 h to obtain melamine resin prepolymer.

[0134] Dilute hydrochloric acid was added dropwise to 1 part by weight of the first active component oil-in-water emulsion to adjust the pH value to 3. 0.11 parts by weight of the prepared melamine resin prepolymer was slowly added dropwise to the oil-in-water emulsion. The mixture was stirred at 500 r / min and reacted at 60℃ for 5 h. After the reaction was completed, the resulting mixed solution was filtered, washed twice with water and ethanol respectively, and dried in an oven at 90℃ for 6 h to obtain the material with the first active component coated on the inner wall.

[0135] Dilute hydrochloric acid was added dropwise to 1 part by weight of the second active component oil-in-water emulsion to adjust the pH value to 3. 0.15 parts by weight of the prepared melamine resin prepolymer was slowly added dropwise to the oil-in-water emulsion. The mixture was stirred at 500 r / min and reacted at 60℃ for 5 h. After the reaction was completed, the resulting mixed solution was filtered, washed twice with water and ethanol respectively, and dried in an oven at 90℃ for 6 h to obtain the material with the second active component coated on the inner wall.

[0136] (3) Dissolve 0.17 parts by weight of chlorinated rubber in 1.7 parts by weight of dichloromethane, add 1.69 parts by weight of the inner wall coating material for the first active component, and mix thoroughly. Add the resulting mixture to 20 parts by weight of water, stir at 800 r / min, and raise the temperature until the solvent evaporates to obtain fast-release microcapsules coated with the first active component. The capsules have a size of 3-5 μm, an elastic modulus of 0.5 GPa, and a combined thickness of 1.2 μm for the capsule wall and membrane coating material, which conforms to the calculation formula Y = 0.42X. 2 -0.92X+T. Testing revealed that the mass ratio of the core, wall, and membrane encapsulation material in this rapid-release microcapsule was 1:0.98:0.20.

[0137] 0.17 parts by weight of chlorinated rubber were dissolved in 1.7 parts by weight of dichloromethane, and 0.80 parts by weight of the inner wall coating material for the second active component were added and thoroughly mixed. The resulting mixture was then added to 20 parts by weight of water and stirred at 800 r / min. The temperature was increased until the solvent evaporated, yielding medium-rate release microcapsules coated with the second active component. These microcapsules had a size of 5–7 μm, an elastic modulus of 1.2 GPa, and a combined thickness of 2.4 μm for the capsule wall and membrane coating material, conforming to the calculation formula Y = 0.42X. 2 -0.92X+T. Testing revealed that the mass ratio of the core, wall, and membrane encapsulation material in this medium-release microcapsule was 1:1.34:0.5.

[0138] (4) Add 1 part by weight of linaloate formate to 3.5 parts by weight of water at 70°C, add 0.2 parts by weight of nonylphenol polyoxyethylene ether, shear emulsify by shearing at 3000 r / min for 30 min, adjust the pH to 3.5, add 1.2 parts by weight of tetraethyl orthosilicate, react for 18 h, wash and filter according to routine, dry at 85°C for 7 h to obtain silica microcapsules coated with active components.

[0139] (5) 1 part by weight of silica microcapsules coated with active components and 0.08 parts by weight of γ-mercaptopropylmethyldiethoxysilane were added to 20 parts by weight of toluene. The surface modification reaction was carried out at 100°C under reflux for 2 hours. After cooling, the surface was filtered and washed with ethanol and dried at 120°C for 4 hours to obtain surface-modified silica microcapsules.

[0140] (6) One part by weight of surface-modified silica microcapsules was added to eight parts by weight of a 30% hydrogen peroxide solution. After oxidation at 60°C for 4 hours, the microcapsules were washed three times with water and three times with ethanol, and then dried at 90°C for 6 hours to obtain inorganic microcapsules. The mass ratio of the capsule core to the capsule wall in the inorganic microcapsules was found to be 1:0.33. The size of the inorganic microcapsules was 2–5 μm.

[0141] (7) 0.15 parts by weight of the prepared fast-release microcapsules, 0.15 parts by weight of the medium-release microcapsules, and 0.07 parts by weight of bis[2,2,6,6-tetramethyl-4-piperidinyl]isophthalamide were added to 100 parts by weight of straight-run pitch (penetration of 70 1 / 10 mm at 25°C) and stirred at 1000 r / min for 2 h under heating conditions at 150°C to obtain purified pitch.

[0142] (8) Mix 2000 parts by weight of aggregate, 95 parts by weight of clean asphalt and 0.2 parts by weight of inorganic microcapsules at 150°C for 1 min to obtain long-life clean asphalt mixture.

[0143] Example 5

[0144] (1) Add 1 part by weight of methyl ionone to 7 parts by weight of water at 60°C, add 0.08 parts by weight of hexadecyltrimethylammonium chloride, and shear emulsify by shearing at 3000 r / min for 30 min to form an oil-in-water emulsion of the first active component in the aqueous phase.

[0145] Add 1 part by weight of 3-propenyl-6-ethoxyphenol to 7 parts by weight of water at 60°C, add 0.08 parts by weight of hexadecyltrimethylammonium chloride, and shear emulsify using a shear machine at 3000 r / min for 30 min to form an oil-in-water emulsion of the second active component in the aqueous phase.

[0146] (2) Dissolve 1 part by weight of melamine, 2 parts by weight of formaldehyde solution with a mass concentration of 37% and 9 parts by weight of deionized water in a three-necked flask, adjust the pH value to 8, and then place it in a constant temperature water bath at 90℃ and stir at 400r / min for 3.5h to obtain melamine resin prepolymer.

[0147] Dilute hydrochloric acid was added dropwise to 1 part by weight of the first active component oil-in-water emulsion to adjust the pH value to 2. 0.10 parts by weight of the prepared melamine resin prepolymer was slowly added dropwise to the oil-in-water emulsion. The mixture was stirred at 800 r / min and reacted at 90℃ for 1 h. After the reaction was completed, the resulting mixed solution was filtered, washed twice with water and ethanol respectively, and dried in an oven at 60℃ for 9 h to obtain the material with the first active component coated on the inner wall.

[0148] Dilute hydrochloric acid was added dropwise to 1 part by weight of the second active component oil-in-water emulsion to adjust the pH value to 2. 0.15 parts by weight of the prepared melamine resin prepolymer was slowly added dropwise to the oil-in-water emulsion. The mixture was stirred at 800 r / min and reacted at 90℃ for 1 h. After the reaction was completed, the resulting mixed solution was filtered, washed twice with water and ethanol respectively, and dried in an oven at 60℃ for 9 h to obtain the material with the second active component coated on the inner wall.

[0149] (3) Dissolve 0.25 parts by weight of chlorinated rubber in 5 parts by weight of dichloromethane, add 1.48 parts by weight of the inner wall coating material for the first active component, and mix thoroughly. Add the resulting mixture to 25 parts by weight of water, stir at 700 r / min, and raise the temperature until the solvent evaporates to obtain fast-release microcapsules coated with the first active component. The size of these microcapsules is 3–5 μm, the elastic modulus is 0.6 GPa, and the sum of the thickness of the capsule wall and the membrane coating material is 0.8 μm, which conforms to the calculation formula Y = 0.42X. 2 -0.92X+T. Testing revealed that the mass ratio of the core, wall, and membrane encapsulation material in this rapid-release microcapsule was 1:0.79:0.29.

[0150] 0.25 parts by weight of chlorinated rubber were dissolved in 5 parts by weight of dichloromethane, and 1.37 parts by weight of the inner wall coating material for the second active component were added and thoroughly mixed. The resulting mixture was then added to 25 parts by weight of water and stirred at 700 r / min. The temperature was increased until the solvent evaporated, yielding medium-rate release microcapsules coated with the second active component. These microcapsules had a size of 5–7 μm, an elastic modulus of 1.0 GPa, and a combined thickness of 2.2 μm for the capsule wall and membrane coating material, conforming to the calculation formula Y = 0.42X. 2 -0.92X+T. Testing revealed that the mass ratio of the core, wall, and membrane encapsulation material in this medium-release microcapsule was 1:1.22:0.49.

[0151] (4) Add 1 part by weight of terpine acetate to 3 parts by weight of water at 80°C, add 0.2 parts by weight of octylphenol polyoxyethylene ether, shear emulsify at 4000 r / min for 20 min using a shear machine, adjust the pH value to 3, add 1.1 parts by weight of tetraethyl orthosilicate, react for 16 h, wash and filter according to routine, and dry at 90°C for 8 h to obtain silica microcapsules coated with active components.

[0152] (5) 1 part by weight of silica microcapsules coated with active components and 0.1 part by weight of γ-mercaptopropyltrimethoxysilane were added to 30 parts by weight of toluene. The surface modification reaction was carried out at 110°C under reflux for 3 hours. After cooling, the surface was filtered and washed with ethanol and dried at 90°C for 5 hours to obtain surface-modified silica microcapsules.

[0153] (6) One part by weight of surface-modified silica microcapsules was added to 10 parts by weight of a 30% hydrogen peroxide solution. After oxidation at 80°C for 1 hour, the microcapsules were washed twice with water and ethanol, respectively, and dried at 60°C for 10 hours to obtain inorganic microcapsules. The mass ratio of the capsule core to the capsule wall in the inorganic microcapsules was found to be 1:0.32. The size of the inorganic microcapsules was 1–4 μm.

[0154] (7) 0.2 parts by weight of the prepared fast-release microcapsules, 0.2 parts by weight of the medium-release microcapsules, and 0.1 parts by weight of bis[2,2,6,6-tetramethyl-4-piperidinyl]isophthalamide were added to 100 parts by weight of straight-run pitch (701 / 10mm at 25℃), and stirred at 800r / min for 3h under heating conditions at 150℃ to obtain purified pitch.

[0155] (8) Mix 2000 parts by weight of aggregate, 90 parts by weight of cleaned asphalt and 0.15 parts by weight of inorganic microcapsules at 150°C for 1 min to obtain long-life cleaned asphalt mixture.

[0156] Comparative Example 1

[0157] Long-life clean asphalt mixtures were prepared according to the method of Example 1, except that the medium-release microcapsules in step (7) and the inorganic microcapsules in step (8) were replaced with fast-release microcapsules of the same weight.

[0158] Comparative Example 2

[0159] Long-life clean asphalt mixtures were prepared according to the method of Example 1, except that the fast-release microcapsules in step (7) and the inorganic microcapsules in step (8) were replaced with medium-release microcapsules of the same weight.

[0160] Comparative Example 3

[0161] Long-life clean asphalt mixtures were prepared according to the method of Example 1, except that the fast-release microcapsules and medium-release microcapsules mentioned in step (7) were replaced with inorganic microcapsules of the same weight.

[0162] Comparative Example 4

[0163] Long-life clean asphalt mixtures were prepared according to the method of Example 1, except that the antioxidant was not added in step (7).

[0164] Comparative Example 5

[0165] Microcapsules were prepared according to the method of Example 1, except that in step (1), the amount of water was increased to 15 parts by weight and the amount of chlorinated rubber was increased to 0.50 parts by weight.

[0166] Rapid-release microcapsules were obtained, with a size of 4-6 μm, an elastic modulus of 1.0 GPa, and a capsule wall thickness of 1.7 μm, which does not conform to the calculation formula Y = 0.42X. 2 -0.92X+T.

[0167] Medium-release microcapsules were obtained, with a size of 6-8 μm, an elastic modulus of 2.3 GPa, and a capsule wall thickness of 2.7 μm, which does not conform to the calculation formula Y = 0.42X. 2 -0.92X+T.

[0168] (7) 0.1 parts by weight of the prepared fast-release microcapsules, 0.05 parts by weight of the medium-release microcapsules and 0.01 parts by weight of 2,2,6,6-tetramethylpiperidineamine were added to 100 parts by weight of straight-run asphalt (penetration 70 1 / 10 mm), and stirred at 800 r / min for 3 h under heating conditions at 140 °C to obtain purified asphalt.

[0169] (8) Mix 2000 parts by weight of aggregate, 90 parts by weight of cleaned asphalt and 0.05 parts by weight of inorganic microcapsules at 150°C for 1 min to obtain long-life cleaned asphalt mixture.

[0170] Test case

[0171] Asphalt mixtures prepared using straight-run asphalt (70 1 / 10 mm penetration at 25℃), natural asphalt (50 1 / 10 mm penetration at 25℃), and SBS modified asphalt (60 1 / 10 mm penetration at 25℃) as asphalt matrices were tested for asphalt fumes. Specifically, asphalt fumes were enriched by heating at 163℃ for 6 hours. Gas chromatography and a total hydrocarbon analyzer were used to test and analyze the asphalt fumes. The freeze-thaw splitting tensile strength ratio of the asphalt mixtures was also tested to evaluate their resistance to water damage.

[0172] Table 1. Test results of asphalt fumes and mixtures

[0173]

[0174] It should be emphasized that the above-mentioned content is only a specific embodiment of the present invention and should not be construed as limiting the present invention to the above description in specific implementation. For those skilled in the art, any simple deductions and improvements made without departing from the spirit and principles of the present invention should be considered within the scope of protection of the present invention.

Claims

1. An asphalt mixture, characterized in that, By weight, the asphalt mixture comprises the following raw material components: Materials collected: 2000 portions; Asphalt: 90-110 parts; Rapid-release microcapsules: 0.05–0.2 parts; Medium-release microcapsules: 0.05–0.2 parts; Inorganic microcapsules: 0.05–0.2 parts; Antioxidant: 0.01–0.1 parts; The fast-release microcapsules and the medium-release microcapsules each independently include a core, a wall, and a membrane encapsulation material, wherein the wall encapsulates the outer layer of the core, and the membrane encapsulation material encapsulates the outer layer of the wall; the core includes an active component, the wall includes a resin, and the membrane encapsulation material includes a rubber material.

2. The asphalt mixture according to claim 1, characterized in that, The asphalt is at least one of straight-run asphalt, polymer-modified asphalt, and natural asphalt; the penetration of the asphalt at 25°C is 30 to 100 1 / 10 mm. And / or, the antioxidant is one or more of 2,2,6,6-tetramethylpiperidineamine, 4-benzoyloxy-2,2,6,6-tetramethylpiperidine, bis[2,2,6,6-tetramethyl-4-piperidinyl] sebacate, and bis[2,2,6,6-tetramethyl-4-piperidinyl] isophthalamide.

3. The asphalt mixture according to claim 1, characterized in that, In the rapid-release microcapsule, the mass ratio of the core, the wall, and the membrane encapsulation material is 1:(0.7-1):(0.2-0.3); the sum of the thicknesses of the wall and the membrane encapsulation material of the rapid-release microcapsule is 0.5-2 μm. And / or, in the medium-rate release microcapsule, the mass ratio of the core, the wall, and the membrane encapsulation material is 1:(1.2-1.5):(0.4-0.5); the sum of the thicknesses of the wall and the membrane encapsulation material of the medium-rate release microcapsule is 2.1-3 μm.

4. The asphalt mixture according to claim 1, characterized in that, In the fast-release and medium-release microcapsules, the elastic modulus of the microcapsule and the sum of the thickness of the capsule wall and the membrane encapsulation material satisfy the following formula: Y=0.42X 2 -0.92X+T; Wherein, Y is the elastic modulus of the microcapsule, in GPa; X is the sum of the thicknesses of the capsule wall and the membrane encapsulation material, in μm; and T is 1 ± 0.

1.

5. The asphalt mixture according to claim 1, characterized in that, The size of the fast-release microcapsules and the medium-release microcapsules is each independently less than 50 micrometers, preferably less than 20 micrometers, and more preferably 3 to 15 μm.

6. The asphalt mixture according to claim 1, characterized in that, The active component encapsulated in the rapid-release microcapsule is the first active component, which is one or more of aldehyde compounds and ketone compounds; Preferably, the aldehyde compounds are selected from one or more of p-methylbenzaldehyde, decanal, o-carboxybenzaldehyde, p-isopropylbenzaldehyde, cinnamaldehyde, p-hydroxybenzaldehyde, p-methoxybenzaldehyde, 2-methyl-3-(3,4-methylene-dioxyphenyl)propanal, 3,4-methylenedioxybenzaldehyde, 3-(4-isopropylphenyl)-2-methylpropanal, ethyl vanillin, phenylacetaldehyde, anisaldehyde, nonadien-2,6-aldehyde, 2,6-dimethyl-2,6-octadienal, vanillin, citronellol, neraldehyde, hydroxymethylpentylcyclohexene acetal, p-diethylaminobenzaldehyde, and undecenal; the ketone compounds are selected from one or more of 6-methyl-3,5-heptadien-2-one, 2-undecenone, acetophenone, ionone, irisone, methyl ionone, damascone, and dihydrodamascone. And / or, the active component encapsulated in the medium-rate release microcapsule is a second active component, which is one or more of alcohols and phenols; Preferably, the alcohols are one or more selected from cinnamyl alcohol, menthol, cis-3,7-dimethyl-2,6-octadienol, citronellol, geraniol, myrceneol, 2,6,10-trimethyl-2,6,10-dodecanetrien-12-ol, lavenderol, benzyl alcohol, 2-phenylethanol, dihydromyrceneol, tetrahydrogeraniol, and nerolidol; and the phenols are one or more selected from thymol, ethyl maltol, methyl maltol, 3-propenyl-6-ethoxyphenol, and isoeugenol.

7. The asphalt mixture according to claim 1, characterized in that, The resin in the capsule wall of the fast-release microcapsule or the medium-release microcapsule is melamine resin; And / or, in the membrane encapsulation material of the fast-release microcapsules or medium-release microcapsules, the rubber material is one or more of chlorinated rubber, styrene-butadiene rubber, and chloroprene rubber.

8. The asphalt mixture according to claim 1, characterized in that, The inorganic microcapsule includes a core and a wall, wherein the wall is wrapped around the core; the core includes a third active component, and the wall includes organosilane-modified silica. And / or, the third active component encapsulated in the inorganic microcapsule is one or more ester compounds; Preferably, the ester compound is one or more selected from methyl salicylate, methyl cinnamate, ethyl cinnamate, ethyl phenylacetate, methyl phenylacetate, geraniol phenylacetate, phenylethyl phenylacetate, isoamyl phenylacetate, benzyl salicylate, p-methyl benzyl acetate, benzyl acetate, isobutyl benzoate, isoamyl salicylate, benzyl cinnamate, phenylethyl cinnamate, linaloyl formate, linaloyl acetate, linaloyl isobutyrate, menthyl acetate, terpineol acetate, and borneol acetate. And / or, the organosilane is a sulfonylsilane obtained by oxidizing mercaptosilane; the mercaptosilane is one or more of γ-mercaptopropyltrimethoxysilane, γ-mercaptopropyltriethoxysilane and γ-mercaptopropylmethyldiethoxysilane.

9. The asphalt mixture according to claim 8, characterized in that, The mass ratio of the capsule core to the capsule wall in the inorganic microcapsule is 1:(0.3-0.5); And / or, the size of the inorganic microcapsules is less than 50 micrometers, preferably less than 20 micrometers, and more preferably 1 to 15 μm.

10. A method for preparing the asphalt mixture according to any one of claims 1-9, comprising: a. Prepare fast-release microcapsules and medium-release microcapsules respectively; b. Preparation of inorganic microcapsules; c. The fast-release microcapsules, medium-release microcapsules, antioxidants, and asphalt are mixed evenly under heating conditions to obtain purified asphalt; d. The purified asphalt, inorganic microcapsules, and aggregates are mixed to obtain an asphalt mixture.

11. The method according to claim 10, characterized in that, In step a, the preparation process of the rapid-release microcapsules includes: (1) The first active component is mixed with the first emulsifier and water to form an oil-in-water emulsion; (2) The water-in-oil emulsion is reacted with the resin prepolymer, and then filtered, washed and dried to obtain the pre-coated material; (3) In the presence of a volatile solvent, the rubber material is mixed with the pre-coated material obtained in step (2), and then the resulting mixture is mixed with water and heated until the volatile solvent evaporates to obtain a fast-release microcapsule coated with the first active component. And / or, in step a, the preparation process of the medium-rate release microcapsules includes: (11) The second active component is mixed with the second emulsifier and water to form an oil-in-water emulsion; (22) The oil-in-water emulsion is reacted with the resin prepolymer, and then filtered, washed and dried to obtain the pre-coated material; (33) In the presence of a volatile solvent, the rubber material is mixed with the pre-coated material obtained in step (22), and then the resulting mixture is mixed with water and heated until the volatile solvent evaporates to obtain medium-speed release microcapsules coated with the second active component.

12. The method according to claim 11, characterized in that, In step (1), the weight ratio of the first active component, the first emulsifier, and water is 1:(0.05~0.09):(6~9); And / or, in step (11), the weight ratio of the second active component, the second emulsifier, and water is 1:(0.05~0.09):(6~9); And / or, in step (1) or step (11), the first emulsifier and the second emulsifier are each independently selected from one or more of sodium stearate, sodium dodecyl sulfate, sodium dodecylbenzene sulfonate, hexadecyltrimethylammonium chloride, hexadecyltrimethylammonium bromide, hexadecyldimethylhydroxyethylammonium chloride, nonylphenol polyoxyethylene ether, octylphenol polyoxyethylene ether, and hexadecane polyoxyethylene ether.

13. The method according to claim 11, characterized in that, In step (2) or step (22), before the oil-in-water emulsion reacts with the resin prepolymer, the pH value of the oil-in-water emulsion is adjusted to below 5, preferably to 2-4. And / or, in step (2) or step (22), the weight ratio of the oil-in-water emulsion to the resin prepolymer is 1:(0.08~0.20); And / or, in step (2) or step (22), the reaction between the oil-in-water emulsion and the resin prepolymer is carried out under stirring, with a stirring speed of 400-1000 r / min, a reaction temperature of 60-90℃, and a time of 1-5 h.

14. The method according to claim 11, characterized in that, In step (2) or step (22), the resin prepolymer is prepared by the following method: Melamine and formaldehyde solutions are mixed and dissolved in water, and the pH value is adjusted to 7.5-9.

5. Then, the mixture is placed in a constant temperature water bath at 60-90℃ and reacted with stirring for 0.5-3.5 hours. The formaldehyde solution has a mass concentration of 30% to 40%; the weight ratio of melamine, formaldehyde solution, and water is 1:(2 to 3):(8 to 10).

15. The method according to claim 11, characterized in that, In step (3) or step (33), the weight ratio of the rubber material to the pre-coated material obtained in step (2) is (0.08~0.25):1; And / or, in step (3) or step (33), the volatile solvent is selected from one or more of carbon tetrachloride, dichloromethane, and trichloroethylene; And / or, in step (3) or step (33), the weight ratio of the rubber material, volatile solvent and water is 1:(10-20):(50-150).

16. The method according to claim 11, characterized in that, The preparation process in step b includes: (i) The third active component, the third emulsifier and water are mixed and reacted with a silicon source. Then, the mixture is washed, filtered and dried to obtain silica microcapsules coated with the active component. (ii) The silica microcapsules coated with the active components, organosilane and organic solvent are mixed to carry out a surface modification reaction, and then cooled, filtered, washed and dried to obtain surface-modified silica microcapsules. (iii) After mixing the surface-modified silica microcapsules with hydrogen peroxide solution for oxidation reaction, the microcapsules are washed and dried to obtain inorganic microcapsules.

17. The method according to claim 16, characterized in that, In step (i), the silicon source is tetraethyl orthosilicate; And / or, in step (i), the third emulsifier is selected from one or more of sodium stearate, sodium dodecyl sulfate, sodium dodecylbenzene sulfonate, hexadecyltrimethylammonium chloride, hexadecyltrimethylammonium bromide, hexadecyldimethylhydroxyethylammonium chloride, nonylphenol polyoxyethylene ether, octylphenol polyoxyethylene ether, and hexadecane polyoxyethylene ether. And / or, in step (i), the weight ratio of the third active component, the third emulsifier, water, and silicon source is 1:(0.05-0.3):(3-7):(1-5), preferably 1:(0.1-0.2):(4-5):(1-1.5); And / or, in step (i), the reaction conditions are: a reaction time of 10 to 18 hours and a reaction temperature of 60 to 80 degrees Celsius.

18. The method according to claim 16, characterized in that, In step (ii), the weight ratio of the silica microcapsules coated with the active components to the organosilane and the organic solvent is 1:(0.01-0.1):(10-30); And / or, in step (ii), the organic solvent is preferably one or more of xylene, toluene, cyclohexanone, chlorobenzene and pyridine; And / or, in step (ii), the surface modification reaction is carried out at a temperature of 100°C to 120°C for a time of 1 to 3 hours.

19. The method according to claim 16, characterized in that, In step (iii), the weight ratio of the surface-modified silica microcapsules to hydrogen peroxide solution is 1:(5-10); the mass fraction of the hydrogen peroxide solution is 10%-30%. And / or, in step (iii), the oxidation reaction is carried out at a temperature of 50–90°C for a reaction time of 1–5 h.

20. The method according to claim 11, characterized in that, In step c, the heating temperature is 140–180°C; the mixing is performed by mechanical stirring, preferably with a stirring speed of 500–1000 r / min and a stirring time of 1–3 h. And / or, in step d, the mixing temperature is 150-180℃ and the mixing time is 1-3 min.

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