Asphalt additives, asphalt compositions and methods for their preparation

By encapsulating odor-neutralizing active components in environmentally friendly microcapsules and utilizing the slow-release and catalytic effects of the composite shell material, the problem of harmful gas emissions during asphalt pavement construction has been solved, achieving stable and efficient emission reduction and improving the environmental performance of asphalt pavements.

CN122145886APending Publication Date: 2026-06-05CHINA PETROLEUM & CHEMICAL CORP +1

Patent Information

Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
CHINA PETROLEUM & CHEMICAL CORP
Filing Date
2024-12-05
Publication Date
2026-06-05

AI Technical Summary

Technical Problem

In existing asphalt pavement construction, additives are prone to volatilization at high temperatures, affecting emission reduction effects. Furthermore, the reaction products are not stable enough during high-temperature storage, making it impossible to effectively control the emission of harmful gases.

Method used

The odor-neutralizing active ingredients are encapsulated in environmentally friendly microcapsules. The microcapsules are formed by a composite shell material including an inorganic base shell, barium titanate nanoparticles, polydopamine, and cuprous oxide. These microcapsules adsorb and catalyze harmful substances in asphalt fumes, generating highly stable compounds.

Benefits of technology

It effectively reduces the content of irritating gases in asphalt fumes, improves road performance, ensures stable release of odor-neutralizing active components at high temperatures, reduces emissions of harmful substances, and improves safety in use.

✦ Generated by Eureka AI based on patent content.

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Abstract

The application discloses a kind of asphalt additives, asphalt composition and preparation method thereof.The asphalt additive of the application includes the following components by weight parts: auxiliary odorless agent, 1-5 parts;Environment-friendly microcapsule, 1-5 parts;Dispersing agent, 1-10 parts;The environment-friendly microcapsule includes composite shell material and core material, the composite shell material includes silicon dioxide, barium titanate nanoparticles, polydopamine and cuprous oxide, and the core material includes one or more of aldehydes, alcohols, esters, enes.The odorless asphalt additive prepared by adding environment-friendly microcapsule to asphalt, with the help of slow-release effect of microcapsule, can efficiently and durably reduce the content of irritating gas in asphalt fume and emit pleasant fragrance, while also having good road performance.
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Description

Technical Field

[0001] This invention belongs to the field of environmentally friendly asphalt, specifically relating to an asphalt additive, an asphalt composition, and a method for preparing the same. Background Technology

[0002] Currently, the world is facing severe environmental challenges, and rapid urbanization has intensified the expansion of urban road networks. Although traditional asphalt pavements efficiently support traffic, the asphalt fumes released during their production are rich in harmful substances, which not only challenge environmental protection principles but also hinder sustainable development and pose a threat to human health.

[0003] Given the growing global consensus on energy conservation and emission reduction, the research and optimization of harmful gas control technologies in asphalt pavement construction are particularly crucial.

[0004] Currently, additive modification technology is the main means of emission reduction. This involves reacting highly reactive compound additives with volatile components in asphalt to improve asphalt stability and reduce harmful gas emissions during high-temperature construction. However, additives are prone to premature volatilization at high temperatures, affecting emission reduction effectiveness; furthermore, the reaction products lack stability during high-temperature storage and may decompose over a long period, weakening emission reduction performance.

[0005] CN118222107A discloses a high-efficiency odor-neutralizing modified asphalt and its preparation method. However, this method is limited to directly adding the odor-neutralizing active component into the asphalt system, and cannot cope with the loss of active component during storage and transportation.

[0006] Therefore, continuous technological optimization and innovation to improve the stability of the active ingredients for odor neutralization are crucial for the future. Summary of the Invention

[0007] To address the problems existing in the prior art, this invention provides an asphalt additive, an asphalt composition, and a method for preparing the same. The odor-neutralizing asphalt additive, prepared by adding environmentally friendly microcapsules to asphalt, achieves the purpose of efficiently and persistently reducing the content of irritating gases in asphalt fumes and emitting a pleasant aroma through the slow-release effect of the microcapsules, while also exhibiting good road performance. This provides a brand-new approach for the environmentally friendly utilization of asphalt.

[0008] The first aspect of this invention provides an asphalt additive, comprising, by weight, the following components:

[0009] Deodorizing agent, 1-5 parts;

[0010] Environmentally friendly microcapsules, 1-5 servings;

[0011] Dispersant, 1-10 parts;

[0012] The environmentally friendly microcapsule comprises a composite shell material and a core material. The composite shell material comprises silicon dioxide, barium titanate nanoparticles, polydopamine, and cuprous oxide. The core material comprises one or more of aldehydes, alcohols, esters, and alkenes.

[0013] Furthermore, the auxiliary deodorizing agent is selected from one or more of imide compounds with a molecular weight greater than 170 and antioxidants with a molecular weight greater than 200.

[0014] Furthermore, the imide compound with a molecular weight greater than 170 is selected from one or more of N-phenylmaleimide, hexadecylmaleimide, tris(2-maleimide ethyl)amine, and 4,4′-methylenebis(N-phenylmaleimide).

[0015] Further, the antioxidant with a molecular weight greater than 200 is a hindered phenolic antioxidant and / or a phosphite antioxidant. The hindered phenolic antioxidant is selected from one or more of 2,6-di-tert-butyl-p-methylphenol, pentaerythritol tetrakis(dibutylhydroxyhydrocinnamic acid) ester, 2,5-di-tert-butylhydroquinone, 4-(1,1-dimethylethyl)-1,2-benzenediphenol, and 2,2′-methylenebis(4-ethyl-6-tert-butylphenol). The phosphite antioxidant is selected from one or more of tris(2,4-di-tert-butylphenyl) phosphite, tris(nonylphenol) phosphite, and pentaerythritol distearate diphosphite.

[0016] Furthermore, the dispersant is one or more of dodecyl dimethyl betaine and 1-hydroxyethyl-carboxymethyl-alkyl imidazoline.

[0017] Furthermore, the particle size of the environmentally friendly microcapsules is 1-10 μm.

[0018] Furthermore, the mass ratio of the composite shell material to the core material is 1:(0.2-2).

[0019] Furthermore, the core material preferably includes aldehydes, alcohols, esters, and alkenes simultaneously.

[0020] Further, the aldehydes are selected from one or more aromatic aldehydes with a molecular weight greater than 120 and cyclic terpene aldehydes with a molecular weight greater than 170. The aromatic aldehydes with a molecular weight greater than 120 are selected from one or more of cinnamaldehyde, jasmine aldehyde, vanillin, neojasmine aldehyde, and methylpentylcinnamaldehyde; the cyclic terpene aldehydes with a molecular weight greater than 170 are selected from one or more of crocinnamaldehyde and β-cyclocitral.

[0021] Further, the alcohols are selected from one or more of terpenols with a molecular weight greater than 140 and cyclic terpenols with a molecular weight greater than 150. The terpenols with a molecular weight greater than 140 are selected from one or more of geraniol, linalool, citronellol, nerol, tetrahydrogeraniol, nerolidol, and 3,7-dimethyl-octen-2-ol; the cyclic terpenols with a molecular weight greater than 150 are selected from one or more of neomenthol, α-terpineol, borneol, vetiverol, and santalol.

[0022] Further, the esters are selected from one or more of fatty acid esters with a molecular weight greater than 130 and salicylate esters with a molecular weight greater than 200. The fatty acid esters with a molecular weight greater than 130 are selected from one or more of isoamyl acetate, leaf ester acetate, butyl butyrate, ethyl hexanoate, methyl laurate, and methyl 2-octynoate; the salicylate esters with a molecular weight greater than 200 are selected from one or more of isoamyl salicylate, leaf ester salicylate, and benzyl salicylate.

[0023] Further, the alkene is selected from cyclic terpenes with a molecular weight greater than 130. It is further selected from one or more of limonene, α-terpinene, α-phellandrene, α-pinene, thujone, juniperene, and longleafene.

[0024] Furthermore, the composite shell material comprises an inorganic base shell / barium titanate nanoparticles / polydopamine / cuprous oxide, wherein the mass ratio of the inorganic base shell to barium titanate nanoparticles, polydopamine, and cuprous oxide is 1:(0.2-0.8):(0.1-0.5):(0.5-2).

[0025] Furthermore, the inorganic base shell is made of at least one material selected from silicon dioxide and titanium dioxide, preferably silicon dioxide.

[0026] A second aspect of the present invention provides a method for preparing the above-mentioned asphalt additive, comprising:

[0027] The auxiliary deodorizing agent is added to the dispersant, stirred for the first time, and then the prepared environmentally friendly microcapsules are added. After stirring for the second time, the asphalt additive is obtained.

[0028] Furthermore, the conditions for the first stirring are: stirring at 400-500 rpm for 1-3 hours at 25-45℃.

[0029] Furthermore, the second stirring conditions are: stirring at 400-500 rpm for 1-3 hours at 25-45℃.

[0030] Furthermore, the method for preparing the environmentally friendly microcapsules includes:

[0031] (1) Preparation of barium titanate nanoparticles;

[0032] (2) Stir and mix one or more deodorizing agents to obtain a core material mixture;

[0033] (3) The core material mixture and barium titanate nanoparticles are stirred and mixed in a solvent;

[0034] (4) Add the inorganic base shell precursor to the reaction system of step (3), stir and mix to obtain Pickering emulsion;

[0035] (5) Adjust the pH value of the Pickering emulsion obtained in step (4), continue stirring, then age, filter, freeze dry, and obtain an environmentally friendly microcapsule matrix;

[0036] (6) Disperse the environmentally friendly microcapsule matrix obtained in step (5) in a buffer solution, add dopamine hydrochloride, process with stirring, then filter, wash, freeze dry to obtain solid particles;

[0037] (7) Add the solid particles and copper ion solution obtained in step (6) into the reaction vessel and carry out the reaction with stirring;

[0038] (8) Mix the reducing agent with the buffer solution, stir to dissolve, and then add it to the reaction system of step (7). Stir to carry out the reaction, then filter, wash, freeze dry, and obtain environmentally friendly microcapsules.

[0039] Furthermore, the method for preparing barium titanate nanoparticles in step (1) includes:

[0040] S1: Stir and mix the titanium precursor and solvent;

[0041] S2: Adjust the pH of the mixed solution obtained in S1 and stir until a titanium precursor sol is obtained;

[0042] S3: Mix the barium precursor with water;

[0043] S4: The titanium precursor sol obtained in S2 is mixed with the mixture obtained in S3 and reacted under stirring. After the reaction is completed, the mixture is filtered, washed, freeze-dried, and ground to obtain primary barium titanate nanoparticles.

[0044] S5: Primary barium titanate nanoparticles, surfactants and solvents are mixed and modified under stirring. After modification, the mixture is washed and freeze-dried to obtain barium titanate nanoparticles.

[0045] Further, in step S1, the titanium precursor is selected from at least one of tetraethyl titanate, n-propyl titanate, and tetrabutyl titanate.

[0046] Further, in step S1, the solvent is an alcohol compound with a boiling point >60°C, and the alcohol compound is an anhydrous alcohol compound, preferably at least one of methanol, butanediol, ethylene glycol, n-butanol, and ethanol.

[0047] Furthermore, in step S1, the stirring temperature is 25-60℃; the stirring speed is 200-500 rpm; and the stirring time is 0.5-3 hours.

[0048] Further, in step S1, the mass ratio of the titanium precursor to the solvent is (1-20):1.

[0049] Further, in step S2, the pH of the mixed solution from S1 is adjusted to pH = 9-12.

[0050] Further, in step S2, the pH of the S1 mixed solution is adjusted by adding an alkaline solution dropwise to the S1 solution. The alkaline solution is at least one of ammonia, sodium hydroxide solution, and potassium hydroxide solution.

[0051] Furthermore, in step S2, the stirring temperature is 25-60℃; the stirring speed is 200-500 rpm; and the stirring time is 0.5-3 hours.

[0052] Further, in step S3, the barium precursor is at least one of Ba(OH)2, Ba(OH)2·H2O, and Ba(OH)2·8H2O.

[0053] Further, in step S3, the barium precursor and water are added to the reaction vessel and stirred. The water is deionized water. The mass ratio of the barium precursor to deionized water is (0.5-4):1.

[0054] Furthermore, in step S3, the stirring temperature is 80-120℃; the stirring speed is 200-500 rpm; and the stirring time is 2-5 hours.

[0055] Further, in step S4, the molar ratio of the mixture obtained in S3 (based on barium) to the titanium precursor sol obtained in S2 (based on titanium) is 1:(0.5-5).

[0056] Furthermore, in step S4, the stirring speed is 200-500 rpm; the reaction temperature is 100-200℃; and the reaction time is 2-48 hours.

[0057] Furthermore, in step S4, the freeze-drying conditions are: vacuum drying for 4-8 hours at a temperature of -40°C to -20°C.

[0058] Furthermore, in step S4, the grinding specifically means grinding until there are no obvious lumps.

[0059] Furthermore, in step S5, the diameter of the barium titanate nanoparticles is 20-100 nm.

[0060] Further, in step S5, the surfactant is a cationic surfactant, preferably at least one of hexadecyltrimethylammonium bromide, hexadecyltrimethylammonium chloride, dodecyldimethylbenzylammonium chloride, and octadecyltrimethylammonium chloride, and more preferably hexadecyltrimethylammonium bromide.

[0061] Further, in step S5, the solvent is an aprotic solvent with a boiling point >100℃, preferably at least one of formamide, N,N-dimethylformamide, dimethylacetamide, and dimethylphosphoramide.

[0062] Further, in step S5, the mass ratio of the primary barium titanate nanoparticles to the surfactant is 1:(0.1-10), and the mass ratio of the solvent to the primary barium titanate nanoparticles is (5-50):1.

[0063] Furthermore, in step S5, the stirring speed is 200-500 rpm; the modification temperature is 70-180℃; and the modification time is 2-8 hours.

[0064] Furthermore, in step S5, the freeze-drying conditions are: vacuum drying for 4-8 hours at a temperature of -40°C to -20°C.

[0065] Furthermore, in step (2), the stirring speed is 400-600 rpm, the stirring temperature is 30-70℃, and the stirring time is 3-10 minutes.

[0066] Further, in step (3), the solvent is an aprotic solvent with a boiling point >100℃, preferably at least one of formamide, N,N-dimethylformamide, dimethylacetamide, and dimethylphosphoramide.

[0067] Further, in step (3), the mass ratio of the solvent to the barium titanate nanoparticles is (10-40):1.

[0068] Furthermore, in step (3), the stirring speed is 400-600 rpm, the stirring temperature is 30-60℃, and the stirring time is 4-6 hours.

[0069] Further, in step (4), the inorganic base shell precursor is at least one of silicate ester compounds and titanate ester compounds, preferably a silicate ester compound; the silicate ester compound is at least one of methyl silicate, ethyl orthosilicate, tetraethyl orthosilicate, and butyl orthosilicate.

[0070] Furthermore, in step (4), the stirring speed is 400-600 rpm, the stirring temperature is 30-60℃, and the stirring time is 4-6 hours.

[0071] Further, in step (5), the pH is adjusted to 3-6. The pH can be adjusted using a dilute acid, such as dilute hydrochloric acid. The stirring speed is 400-600 rpm, the stirring temperature is 30-60℃, and the stirring time is 4-6 hours.

[0072] Further, in step (5), the aging conditions are: standing at 40-60℃ for 12-30 hours. The freeze-drying conditions are: vacuum drying at -40 to -20℃ for 4-8 hours.

[0073] Further, in step (6), the buffer solution is at least one of phosphate buffer, carbonate buffer, and tris(hydroxymethyl)aminomethane hydrochloride buffer (Tris buffer), preferably tris(hydroxymethyl)aminomethane hydrochloride buffer (Tris buffer).

[0074] Furthermore, in step (6), the pH value of the buffer solution is preferably 8-10.

[0075] Further, in step (6), the mass ratio of the buffer solution to the environmentally friendly microcapsule matrix obtained in step (5) is (10-100):1.

[0076] Furthermore, in step (6), after adding dopamine hydrochloride, the mass concentration of dopamine in the reaction system is 2-10 mg / mL.

[0077] Furthermore, in step (6), the stirring speed is 100-300 rpm, the stirring temperature is 20-40℃, and the stirring time is 12-24 hours.

[0078] Furthermore, in step (6), the freeze-drying conditions are: vacuum drying for 4-8 hours at a temperature of -40°C to -20°C.

[0079] Further, in step (7), the copper ion solution is prepared by mixing copper ion salt and deionized water, and the copper ion salt is preferably anhydrous copper sulfate.

[0080] Further, in step (7), the concentration of copper ions in the copper ion solution is 0.05-0.5 mol / L.

[0081] Further, in step (7), the mass ratio of the solid particles obtained in step (6) to the copper ion solution is 1:(50-200).

[0082] Furthermore, the stirring speed in step (7) is 100-450 rpm, the reaction temperature is 100-190℃, and the reaction time is 1-5 hours.

[0083] Further, the reducing agent in step (8) is a sulfite reducing agent, preferably selected from at least one of potassium sulfite and sodium sulfite.

[0084] Further, the buffer solution in step (8) is selected from at least one of acetate buffer and phosphate buffer, preferably acetate buffer; the pH value of the buffer solution is 4.5-6.5.

[0085] Further, the mass ratio of the reducing agent to the buffer solution in step (8) is 1:(10-20).

[0086] Furthermore, during step (8) of stirring and dissolving, the stirring speed is 200-450 rpm, the stirring temperature is 40-80℃, and the stirring time is 1-5 hours.

[0087] Furthermore, in step (8), when the reaction is carried out under stirring, the stirring speed is 100-450 rpm, the reaction temperature is 60-95℃, and the reaction time is 2-5 hours.

[0088] Furthermore, the freeze-drying conditions described in step (8) are: vacuum drying for 4-8 hours at a temperature of -40°C to -20°C.

[0089] A third aspect of the present invention provides an asphalt composition comprising, by weight, the following components:

[0090] Base bitumen, 50-500 parts;

[0091] The above-mentioned asphalt additive is used in quantities of 1-50 parts, preferably 2-50 parts.

[0092] Furthermore, the base asphalt is at least one of straight-run asphalt, polymer-modified asphalt, and natural asphalt.

[0093] Furthermore, the penetration of the asphalt at 25°C is 30-210 1 / 10 mm.

[0094] A fourth aspect of the present invention provides a method for preparing the above-mentioned asphalt composition, comprising:

[0095] The base asphalt is heated to a molten state, and the asphalt additive is added while stirring to obtain an asphalt composition.

[0096] Furthermore, the temperature at which the base asphalt is heated to a molten state is 133-153℃.

[0097] Furthermore, the stirring speed is 400-600 rpm, and the stirring time is 2-4 hours.

[0098] Compared with the prior art, the present invention has the following advantages:

[0099] (1) The environmentally friendly microcapsule of the present invention has a composite shell material comprising an inorganic base shell, barium titanate nanoparticles, polydopamine and cuprous oxide, wherein the barium titanate nanoparticles have multiple functions. Firstly, during the preparation process, the modified barium titanate nanoparticles, due to their nanoscale size, can stably exist between the water and oil interfaces, and can further serve as template agents for microcapsule synthesis, maintaining the stability of the core material mixed droplets. Secondly, under the influence of high temperature, the crystal axis of the barium titanate nanoparticles will be distorted, leading to spontaneous polarization without any external electric field, generating permanent electrodes. On the one hand, during the synthesis of cuprous oxide in the microcapsule composite shell, copper ions can be adsorbed onto the surface of the polydopamine film, effectively increasing the copper ion loading of the microcapsule shell, thus generating a porous cuprous oxide structure with a large specific surface area during the subsequent copper ion reduction process. On the other hand, during the asphalt mixing and construction process, the high temperature attracts compounds released by the asphalt to the vicinity of the slow-release modified microcapsules, increasing the difficulty of these compounds volatilizing while allowing the cuprous oxide shell of the microcapsules to adsorb more harmful compounds, and causing the smoke-suppressing active components released by the microcapsules to react with more of the above compounds, thereby effectively reducing the impact of irritating gases released from asphalt pavements on the human body.

[0100] (2) The environmentally friendly microcapsule of the present invention comprises an inorganic base shell, barium titanate nanoparticles, polydopamine, and cuprous oxide. Cuprous oxide has multiple functions. The first function is that cuprous oxide itself has extremely high adsorption capacity for sulfur-containing compounds, which can effectively reduce the malodorous sulfides generated during the production and construction of asphalt. The second function is that after being synthesized by the method described in the present invention, cuprous oxide will form a porous structure with a large specific surface area on the surface of the microcapsule, which effectively improves the adsorption capacity of cuprous oxide for various harmful substances in asphalt fumes. The third function is that cuprous oxide has extremely strong catalytic activity, which can catalyze the reaction between the smoke-suppressing compounds released by the microcapsule and various pollutants in the asphalt fumes, further improving the smoke-suppressing ability of the environmentally friendly microcapsule.

[0101] (3) The asphalt additive of the present invention incorporates environmentally friendly microcapsules, which encapsulate low-boiling-point odor-neutralizing active components in a composite shell. These active components can be slowly released from the microcapsules during asphalt storage and construction, and undergo nucleophilic reactions with compounds in asphalt that have irritating odors to generate compounds with higher stability and boiling points. These compounds are difficult to decompose and volatilize during high-temperature asphalt construction, thereby reducing the irritating odor of asphalt fumes. At the same time, microencapsulating the odor-neutralizing active components can also effectively prevent them from reacting in time due to rapid volatilization at high temperatures. This not only prolongs the action time of the odor-neutralizing active components, but also further improves their safety of use.

[0102] (4) The asphalt additive of the present invention can also undergo nucleophilic reaction with compounds in asphalt that have irritating odor to generate compounds with higher stability and boiling point, thereby reducing the irritating odor of asphalt fumes. Moreover, the auxiliary deodorizing agent has a higher boiling point and can exert its maximum deodorizing effect faster than environmentally friendly microcapsules. While ensuring safety and deodorizing effect, it makes up for the defect that environmentally friendly microcapsules cannot play a role immediately after being added to asphalt. Detailed Implementation

[0103] To further illustrate the technical solution of the present invention, the present invention will be clearly and thoroughly described below in conjunction with embodiments.

[0104] The sulfides in the asphalt flue gas described in this invention are tested according to the standard GB_T 33318-2016 Determination of Sulfides by Gas Analysis using the sulfur chemiluminescence gas chromatography method.

[0105] The non-methane total hydrocarbons in the asphalt flue gas described in this invention are tested using a portable total hydrocarbon analyzer in accordance with the technical requirements and detection methods for portable monitoring instruments for total hydrocarbons, methane and non-methane total hydrocarbons in ambient air and exhaust gas, as specified in HJ 1012-2018.

[0106] The asphalt fumes described in this invention were tested using the asphalt fumes enrichment and collection device described in Example 1 of Chinese Patent CN220912767U.

[0107] Example 1

[0108] Preparation of asphalt additives:

[0109] (1): Preparation of barium titanate nanoparticles:

[0110] S1: Weigh 18 parts by weight of tetrapropyl titanate and 14 parts by weight of anhydrous ethanol and add them to a flask. Stir at 60°C and 400 rpm for 1 hour to obtain a titanium precursor solution.

[0111] S2: Slowly add 10wt% ammonia to the S1 solution until the pH of the reaction system is 10, and continue stirring at 400 rpm for 1 hour at 60℃ to obtain titanium precursor sol.

[0112] S3: Add 9.7 parts by weight of Ba(OH)2·H2O and 9 parts by weight of deionized water to the reactor, and heat and stir at 400 rpm for 2 hours at 85°C.

[0113] S4: Add the sol obtained in S2 to the reaction vessel in S3, close the reaction vessel lid, heat to 130℃, stir at 400 rpm for 28 hours, then filter and wash the solid powder in the reaction system, and vacuum dry at -30℃ for 5 hours. After grinding until there are no obvious lumps in the system, the primary barium titanate nanoparticles are obtained.

[0114] S5: Add 1 part by weight of the primary barium titanate nanoparticles obtained in step S4 and 2 parts by weight of hexadecyltrimethylammonium bromide to 30 parts by weight of formamide. Modify by stirring at 200 rpm for 5 hours at 160°C. Then filter and wash the bottom solid powder and vacuum dry it at -30°C for 5 hours to obtain barium titanate nanoparticles (particle size of 40-60 nm).

[0115] (2): Vanillin, tetrahydrogeraniol, methyl lauryl ester and cypressene are mixed in equal weight ratios and stirred at 550 rpm for 10 minutes at 70°C to obtain the core material mixture.

[0116] (3): 3.5 parts by weight of the core material mixture obtained in step (2), 1.5 parts by weight of the barium titanate nanoparticles obtained in step (1) and 20 parts by weight of N,N-dimethylformamide were stirred at 400 rpm for 5 hours at 50°C.

[0117] (4): Add butyl orthosilicate to the reaction system in step (3). The mass ratio of the core material mixture to butyl orthosilicate is 7:5. Continue stirring at 400 rpm for 5 hours at 50°C to obtain Pickering emulsion.

[0118] (5): Slowly add 10wt% dilute hydrochloric acid to the reaction system in step (4) using a peristaltic pump until the pH of the reaction system is 3.5. Continue stirring at 400 rpm for 4.5 hours at 50°C, then stop stirring and age at the same temperature for 24 hours. Then filter and wash the solid powder in the reaction system and vacuum dry it at -30°C for 5 hours to obtain an environmentally friendly microcapsule matrix.

[0119] (6): The environmentally friendly microcapsule matrix obtained in step (5) was added to a Tris buffer solution with a pH of 8.5. The mass ratio of the Tris buffer solution to the deodorizing environmentally friendly microcapsule matrix was 60:1. Then, dopamine hydrochloride was added to make the concentration of dopamine in the reaction system 6.5 mg / mL. The mixture was stirred at 200 rpm for 12 hours at 25°C. The stirring was then stopped. The bottom solid powder was filtered and washed, and then vacuum dried at -30°C for 5 hours.

[0120] (7): 1.35 parts by weight of anhydrous copper sulfate and 50 parts by weight of deionized water were mixed manually at room temperature to prepare a copper sulfate solution. 1 part by weight of the solid particles obtained after drying in step (6) and the copper sulfate solution were added to the reactor. The reactor lid was closed and the mixture was stirred at 200 rpm for 1 hour at 110°C.

[0121] (8): Add 4 parts by weight of sodium sulfite to 40 parts by weight of acetate buffer solution with pH=6, and stir at 200 rpm for 1 h at 50 °C; add the resulting mixed solution to the reaction vessel (7), close the vessel lid, and stir at 200 rpm for 4 h at 90 °C. Finally, filter and wash the bottom solid powder, and vacuum dry it at -30 °C for 5 h to obtain environmentally friendly microcapsules with a particle size of 2.81~7.43 μm.

[0122] The auxiliary deodorizing agent hexadecyl maleimide, 2,6-di-tert-butyl-p-methylphenol, and tris(nonylphenol) phosphite were mixed in a mass ratio and dispersed in 1-hydroxyethyl-carboxymethyl-alkylimidazoline. The mixture was stirred at 400 rpm for 1 hour at 25°C. Then, the environmentally friendly microcapsules prepared in step (8) were added and stirred for another hour under the same conditions to obtain the asphalt additive. The mass ratio of the auxiliary deodorizing agent, the environmentally friendly microcapsules, and 1-hydroxyethyl-carboxymethyl-alkylimidazoline was 1:1:2.

[0123] Preparation of the asphalt composition:

[0124] Add 2 parts by weight of asphalt additive to 100 parts of base asphalt with a penetration of 54 at 25°C and heated to 143°C, and stir at 400 rpm for 4 hours to obtain odorless and environmentally friendly asphalt.

[0125] Example 2

[0126] Preparation of asphalt additives:

[0127] (1): Preparation of barium titanate nanoparticles:

[0128] S1: Weigh 12.5 parts by weight of tetrapropyl titanate and 12 parts by weight of n-butanol and add them to a flask. Stir at 50°C and 400 rpm for 1 hour to obtain a titanium precursor solution.

[0129] S2: Slowly add 10wt% ammonia to the S1 solution until the pH of the reaction system is 10, and continue stirring at 400 rpm for 1 hour at 50℃ to obtain titanium precursor sol.

[0130] S3: Add 6.7 parts by weight of Ba(OH)2·H2O and 9 parts by weight of deionized water to the reactor, and heat and stir at 400 rpm for 2 hours at 85°C.

[0131] S4: Add the sol obtained in S2 to the reaction vessel in S3, close the reaction vessel lid, heat to 145℃, stir at 300 rpm for 24 hours, then filter and wash the solid powder in the reaction system, and vacuum dry at -30℃ for 5 hours. After grinding until there are no obvious lumps in the system, the primary barium titanate nanoparticles are obtained.

[0132] S5: 1 part by weight of the primary barium titanate nanoparticles obtained in step S4 and 7 parts by weight of dodecyl dimethyl benzyl ammonium chloride were added to 20 parts by weight of dimethylacetamide. The mixture was stirred and modified at 200 rpm for 5 hours at 150°C. The bottom solid powder was then filtered and washed, and vacuum dried at -30°C for 5 hours to obtain barium titanate nanoparticles.

[0133] (2): Cinnamaldehyde, α-terpineol, isoamyl salicylate, and α-pinene are mixed in equal weight ratios and stirred at 600 rpm for 10 minutes at 70°C to obtain a core material mixture.

[0134] (3): 3.5 parts by weight of the core material mixture obtained in step (2), 1.5 parts by weight of the barium titanate nanoparticles obtained in step (1) and 20 parts by weight of N,N-dimethylformamide were stirred at 400 rpm for 5 hours at 50°C.

[0135] (4): Add butyl orthosilicate to the reaction system in step (3). The mass ratio of the core material mixture to butyl orthosilicate is 7:5. Continue stirring at 400 rpm for 5 hours at 50°C to obtain Pickering emulsion.

[0136] (5): Slowly add 10wt% dilute hydrochloric acid to the reaction system in step (4) using a peristaltic pump until the pH of the reaction system is 3.5. Continue stirring at 400 rpm for 4.5 hours at 50°C, then stop stirring and age at the same temperature for 24 hours. Then filter and wash the solid powder in the reaction system and vacuum dry it at -30°C for 5 hours to obtain an environmentally friendly microcapsule matrix.

[0137] (6): The environmentally friendly microcapsule matrix obtained in step (5) was added to a Tris buffer solution with a pH of 8.5. The mass ratio of the Tris buffer solution to the deodorizing environmentally friendly microcapsule matrix was 60:1. Then, dopamine hydrochloride was added to make the concentration of dopamine in the reaction system 6.5 mg / mL. The mixture was stirred at 200 rpm for 12 hours at 25°C. The stirring was then stopped. The bottom solid powder was filtered and washed, and then vacuum dried at -30°C for 5 hours.

[0138] (7): 1.35 parts by weight of anhydrous copper sulfate and 50 parts by weight of deionized water were mixed manually at room temperature to prepare a copper sulfate solution. 1 part by weight of the solid particles obtained after drying in step (6) and the copper sulfate solution were added to the reactor. The reactor lid was closed and the mixture was stirred at 200 rpm for 1 hour at 110°C.

[0139] (8): Add 4 parts by weight of sodium sulfite to 40 parts by weight of acetate buffer solution with pH=6, and stir at 200 rpm for 1 h at 50 °C; add the resulting mixed solution to the reaction vessel (7), close the vessel lid, and stir at 200 rpm for 4 h at 90 °C. Finally, filter and wash the bottom solid powder, and vacuum dry it at -30 °C for 5 h to obtain environmentally friendly microcapsules with a particle size of 2.81~7.43 μm.

[0140] The auxiliary deodorizing agent hexadecyl maleimide, 2,6-di-tert-butyl-p-methylphenol, and tris(nonylphenol) phosphite were mixed in a mass ratio and dispersed in 1-hydroxyethyl-carboxymethyl-alkylimidazoline. The mixture was stirred at 400 rpm for 1 hour at 25°C. Then, the environmentally friendly microcapsules obtained in step (8) were added and the mixture was stirred for another 1 hour to obtain the asphalt additive. The mass ratio of the auxiliary deodorizing agent, the environmentally friendly microcapsules, and 1-hydroxyethyl-carboxymethyl-alkylimidazoline was 1:1:2.

[0141] Preparation of the asphalt composition:

[0142] Add 2 parts by weight of asphalt additive to 100 parts of base asphalt with a penetration of 54 at 25°C and heated to 143°C, and stir at 400 rpm for 4 hours to obtain odorless and environmentally friendly asphalt.

[0143] Example 3

[0144] Preparation of asphalt additives:

[0145] (1): Preparation of barium titanate nanoparticles:

[0146] S1: Weigh 14.5 parts by weight of n-propyl titanate and 12 parts by weight of n-butanol and add them to a flask. Stir at 55°C and 400 rpm for 2 hours to obtain a titanium precursor solution.

[0147] S2: Slowly add 10wt% ammonia to the S1 solution until the pH of the reaction system is 9.5, and continue stirring at 400 rpm for 1.5 hours at 55℃ to obtain titanium precursor sol;

[0148] S3: Add 7.8 parts by weight of Ba(OH)2·H2O and 8 parts by weight of deionized water to the reactor, and heat and stir at 400 rpm for 2 hours at 80°C.

[0149] S4: Add the sol obtained in S2 to the reaction vessel in S3, close the reaction vessel lid, heat to 140℃, stir at 400 rpm for 26 hours, then filter and wash the solid powder in the reaction system, and vacuum dry at -30℃ for 5 hours. After grinding until there are no obvious lumps in the system, the primary barium titanate nanoparticles are obtained.

[0150] S5: Add 1 part by weight of the primary barium titanate nanoparticles obtained in step S4 and 2 parts by weight of octadecyltrimethylammonium chloride to 30 parts by weight of formamide. Modify by stirring at 200 rpm for 4 hours at 160°C. Then filter and wash the bottom solid powder and vacuum dry it at -30°C for 5 hours to obtain barium titanate nanoparticles (particle size of 40-60 nm).

[0151] (2): Vanillin, tetrahydrogeraniol, methyl lauryl ester and cypressene are mixed in equal weight ratios and stirred at 550 rpm for 10 minutes at 70°C to obtain the core material mixture.

[0152] (3): 3.5 parts by weight of the core material mixture obtained in step (2), 1.5 parts by weight of the barium titanate nanoparticles obtained in step (1) and 30 parts by weight of dimethylacetamide were stirred at 400 rpm for 5 hours at 50°C.

[0153] (4): Add methyl silicate to the reaction system of step (3). The mass ratio of the core material mixture to methyl silicate is 7:6. Continue stirring at 400 rpm for 5 hours at 50°C to obtain Pickering emulsion.

[0154] (5): Slowly add 10wt% dilute hydrochloric acid to the reaction system in step (4) using a peristaltic pump until the pH of the reaction system is 4.5. Continue stirring at 450 rpm for 4 hours at 45°C, then stop stirring and age for 24 hours at the same temperature. Then filter and wash the solid powder in the reaction system and vacuum dry it at -30°C for 5 hours to obtain an environmentally friendly microcapsule matrix.

[0155] (6): The environmentally friendly microcapsule matrix obtained in step (5) was added to a Tris buffer solution with a pH of 8.5. The mass ratio of the Tris buffer solution to the deodorizing environmentally friendly microcapsule matrix was 60:1. Then, dopamine hydrochloride was added to make the concentration of dopamine in the reaction system 6.5 mg / mL. The mixture was stirred at 200 rpm for 12 hours at 25°C. The stirring was then stopped. The bottom solid powder was filtered and washed, and then vacuum dried at -30°C for 5 hours.

[0156] (7): 1.35 parts by weight of anhydrous copper sulfate and 50 parts by weight of deionized water were mixed manually at room temperature to prepare a copper sulfate solution. 1 part by weight of the solid particles obtained after drying in step (6) and the copper sulfate solution were added to the reactor. The reactor lid was closed and the mixture was stirred at 200 rpm for 1 hour at 110°C.

[0157] (8): Add 4 parts by weight of sodium sulfite to 40 parts by weight of acetate buffer solution with pH=6, and stir at 200 rpm for 1 h at 50 °C; add the resulting mixed solution to the reaction vessel (7), close the vessel lid, and stir at 200 rpm for 4 h at 90 °C. Finally, filter and wash the bottom solid powder, and vacuum dry it at -30 °C for 5 h to obtain environmentally friendly microcapsules with a particle size of 2.94~7.78 μm.

[0158] The auxiliary deodorizing agent hexadecyl maleimide, 2,6-di-tert-butyl-p-methylphenol, and tris(nonylphenol) phosphite were mixed in a mass ratio and dispersed in 1-hydroxyethyl-carboxymethyl-alkylimidazoline. The mixture was stirred at 400 rpm for 1 hour at 25°C. Then, the environmentally friendly microcapsules obtained in step (8) were added and the mixture was stirred for another 1 hour to obtain the asphalt additive. The mass ratio of the auxiliary deodorizing agent, the environmentally friendly microcapsules, and 1-hydroxyethyl-carboxymethyl-alkylimidazoline was 1:1:2.

[0159] Preparation of the asphalt composition:

[0160] Add 2 parts by weight of asphalt additive to 100 parts of base asphalt with a penetration of 54 at 25°C and heated to 143°C, and stir at 400 rpm for 4 hours to obtain odorless and environmentally friendly asphalt.

[0161] Example 4

[0162] Preparation of asphalt additives:

[0163] (1): Preparation of barium titanate nanoparticles:

[0164] S1: Weigh 16 parts by weight of tetrapropyl titanate and 12 parts by weight of methanol and add them to a flask. Stir at 40°C and 400 rpm for 2 hours to obtain a titanium precursor solution.

[0165] S2: Slowly add 10wt% ammonia water to the S1 solution until the pH of the reaction system is 10.5, and continue stirring at 400 rpm for 2 hours at 40℃ to obtain titanium precursor sol.

[0166] S3: Add 8.5 parts by weight of Ba(OH)2·H2O and 8.5 parts by weight of deionized water to the reactor, and heat and stir at 400 rpm for 2 hours at 85°C.

[0167] S4: Add the sol obtained in S2 to the reaction vessel in S3, close the reaction vessel lid, heat to 130℃, stir at 400 rpm for 28 hours, then filter and wash the solid powder in the reaction system, and vacuum dry at -30℃ for 5 hours. After grinding until there are no obvious lumps in the system, the primary barium titanate nanoparticles are obtained.

[0168] S5: Add 1 part by weight of the primary barium titanate nanoparticles obtained in step S4 and 2 parts by weight of hexadecyltrimethylammonium bromide to 30 parts by weight of formamide. Modify by stirring at 200 rpm for 5 hours at 160°C. Then filter and wash the bottom solid powder and vacuum dry it at -30°C for 5 hours to obtain barium titanate nanoparticles (particle size of 40-60 nm).

[0169] (2): Mix jasmine aldehyde, geraniol, butyl butyrate and phellandrene in equal weight ratios, and stir at 500 rpm for 10 minutes at 50°C to obtain core material mixture.

[0170] (3): 3.5 parts by weight of the core material mixture obtained in step (2), 1.5 parts by weight of the barium titanate nanoparticles obtained in step (1) and 20 parts by weight of N,N-dimethylformamide were stirred at 400 rpm for 5 hours at 50°C.

[0171] (4): Add butyl orthosilicate to the reaction system in step (3). The mass ratio of the core material mixture to butyl orthosilicate is 7:5. Continue stirring at 400 rpm for 5 hours at 50°C to obtain Pickering emulsion.

[0172] (5): Slowly add 10wt% dilute hydrochloric acid to the reaction system in step (4) using a peristaltic pump until the pH of the reaction system is 3.5. Continue stirring at 400 rpm for 4.5 hours at 50°C, then stop stirring and age at the same temperature for 24 hours. Then filter and wash the solid powder in the reaction system and vacuum dry it at -30°C for 5 hours to obtain an environmentally friendly microcapsule matrix.

[0173] (6): The environmentally friendly microcapsule matrix obtained in step (5) was added to a Tris buffer solution with a pH of 8.5. The mass ratio of the Tris buffer solution to the deodorizing environmentally friendly microcapsule matrix was 60:1. Then, dopamine hydrochloride was added to make the concentration of dopamine in the reaction system 5.0 mg / mL. The mixture was stirred at 150 rpm for 15 hours at 30°C. The stirring was then stopped. The bottom solid powder was filtered and washed, and then vacuum dried at -30°C for 5 hours.

[0174] (7): 1.35 parts by weight of anhydrous copper sulfate and 50 parts by weight of deionized water were mixed manually at room temperature to prepare a copper sulfate solution. 1 part by weight of the solid particles obtained after drying in step (6) and the copper sulfate solution were added to the reactor. The reactor lid was closed and the mixture was stirred at 200 rpm for 1 hour at 110°C.

[0175] (8): Add 4 parts by weight of sodium sulfite to 40 parts by weight of acetate buffer solution with pH=6, and stir at 200 rpm for 1 h at 50 °C; add the resulting mixed solution to the reaction vessel (7), close the vessel lid, stir at 200 rpm for 4 h at 90 °C, and finally filter and wash the bottom solid powder, and vacuum dry at -30 °C for 5 h to obtain environmentally friendly microcapsules with a particle size of 2.79~7.38 μm;

[0176] The auxiliary deodorizing agent hexadecyl maleimide, 2,6-di-tert-butyl-p-methylphenol, and tris(nonylphenol) phosphite were mixed in a mass ratio and dispersed in 1-hydroxyethyl-carboxymethyl-alkylimidazoline. The mixture was stirred at 400 rpm for 1 hour at 25°C. Then, the environmentally friendly microcapsules obtained in step (8) were added and the mixture was stirred for another 1 hour to obtain the asphalt additive. The mass ratio of the auxiliary deodorizing agent, the environmentally friendly microcapsules, and 1-hydroxyethyl-carboxymethyl-alkylimidazoline was 1:1:2.

[0177] Preparation of the asphalt composition:

[0178] Add 2 parts by weight of asphalt additive to 100 parts of base asphalt with a penetration of 54 at 25°C and heated to 143°C, and stir at 400 rpm for 4 hours to obtain odorless and environmentally friendly asphalt.

[0179] Example 5

[0180] Preparation of asphalt additives:

[0181] (1): Preparation of barium titanate nanoparticles:

[0182] S1: Weigh 10 parts by weight of tetrapropyl titanate and 8 parts by weight of anhydrous ethanol and add them to a flask. Stir at 60°C and 400 rpm for 1 hour to obtain a titanium precursor solution.

[0183] S2: Slowly add 10wt% ammonia water to the S1 solution until the pH of the reaction system is 10.5, and continue stirring at 400 rpm for 1 hour at 60℃ to obtain titanium precursor sol.

[0184] S3: Add 5.5 parts by weight of Ba(OH)2·H2O and 6 parts by weight of deionized water to the reactor, and heat and stir at 400 rpm for 2 hours at 90°C.

[0185] S4: Add the sol obtained in S2 to the reaction vessel in S3, close the reaction vessel lid, heat to 130℃, stir at 400 rpm for 28 hours, then filter and wash the solid powder in the reaction system, and vacuum dry at -30℃ for 5 hours. After grinding until there are no obvious lumps in the system, the primary barium titanate nanoparticles are obtained.

[0186] S5: Add 1 part by weight of the primary barium titanate nanoparticles obtained in step S4 and 2 parts by weight of hexadecyltrimethylammonium bromide to 30 parts by weight of formamide. Modify by stirring at 200 rpm for 5 hours at 160°C. Then filter and wash the bottom solid powder and vacuum dry it at -30°C for 5 hours to obtain barium titanate nanoparticles.

[0187] (2): Vanillin, tetrahydrogeraniol, methyl lauryl ester and cypressene are mixed in equal weight ratios and stirred at 550 rpm for 10 minutes at 70°C to obtain the core material mixture.

[0188] (3): 3.5 parts by weight of the core material mixture obtained in step (2), 1.5 parts by weight of the barium titanate nanoparticles obtained in step (1) and 20 parts by weight of N,N-dimethylformamide were stirred at 400 rpm for 5 hours at 50°C.

[0189] (4): Add butyl orthosilicate to the reaction system in step (3). The mass ratio of the core material mixture to butyl orthosilicate is 7:5. Continue stirring at 400 rpm for 5 hours at 50°C to obtain Pickering emulsion.

[0190] (5): Slowly add 10wt% dilute hydrochloric acid to the reaction system in step (4) using a peristaltic pump until the pH of the reaction system is 3.5. Continue stirring at 400 rpm for 4.5 hours at 50°C, then stop stirring and age at the same temperature for 24 hours. Then filter and wash the solid powder in the reaction system and vacuum dry it at -30°C for 5 hours to obtain an environmentally friendly microcapsule matrix.

[0191] (6): The environmentally friendly microcapsule matrix obtained in step (5) was added to a Tris buffer solution with a pH of 8.5. The mass ratio of the Tris buffer solution to the deodorizing environmentally friendly microcapsule matrix was 60:1. Then, dopamine hydrochloride was added to make the concentration of dopamine in the reaction system 6.5 mg / mL. The mixture was stirred at 200 rpm for 12 hours at 25°C. The stirring was then stopped. The bottom solid powder was filtered and washed, and then vacuum dried at -30°C for 5 hours.

[0192] (7): 0.95 parts by weight of anhydrous copper sulfate and 80 parts by weight of deionized water were manually stirred and mixed at room temperature to prepare a copper sulfate solution. 1 part by weight of the solid particles obtained after drying in step (6) and the copper sulfate solution were added to the reactor. The reactor lid was closed and the mixture was stirred at 300 rpm for 2 hours at 120°C.

[0193] (8): Add 4 parts by weight of sodium sulfite to 40 parts by weight of acetate buffer solution with pH=6, and stir at 200 rpm for 1 h at 50 °C; add the resulting mixed solution to the reaction vessel (7), close the vessel lid, and stir at 200 rpm for 4 h at 90 °C. Finally, filter and wash the bottom solid powder, and vacuum dry it at -30 °C for 5 h to obtain environmentally friendly microcapsules with a particle size of 2.62~6.92 μm.

[0194] The auxiliary deodorizing agent hexadecyl maleimide, 2,6-di-tert-butyl-p-methylphenol, and tris(nonylphenol) phosphite were mixed in a mass ratio and dispersed in 1-hydroxyethyl-carboxymethyl-alkylimidazoline. The mixture was stirred at 400 rpm for 1 hour at 25°C. Then, the environmentally friendly microcapsules obtained in step (8) were added and the mixture was stirred for another 1 hour to obtain the asphalt additive. The mass ratio of the auxiliary deodorizing agent, the environmentally friendly microcapsules, and 1-hydroxyethyl-carboxymethyl-alkylimidazoline was 1:1:2.

[0195] Preparation of the asphalt composition:

[0196] Add 2 parts by weight of asphalt additive to 100 parts of base asphalt with a penetration of 54 at 25°C and heated to 143°C, and stir at 400 rpm for 4 hours to obtain odorless and environmentally friendly asphalt.

[0197] Example 6

[0198] Preparation of asphalt additives:

[0199] (1): Preparation of barium titanate nanoparticles:

[0200] S1: Weigh 8 parts by weight of tetrapropyl titanate and 8 parts by weight of n-butanol and add them to a flask. Stir at 55°C and 400 rpm for 3 hours to obtain a titanium precursor solution.

[0201] S2: Slowly add 10wt% ammonia to the S1 solution until the pH of the reaction system is 10, and continue stirring at 400 rpm for 3 hours at 55℃ to obtain titanium precursor sol.

[0202] S3: Add 4.3 parts by weight of Ba(OH)2·H2O and 5 parts by weight of deionized water to the reactor, and heat and stir at 400 rpm for 2 hours at 85°C.

[0203] S4: Add the sol obtained in S2 to the reaction vessel in S3, close the reaction vessel lid, heat to 130℃, stir at 400 rpm for 28 hours, then filter and wash the solid powder in the reaction system, and vacuum dry at -30℃ for 5 hours. After grinding until there are no obvious lumps in the system, the primary barium titanate nanoparticles are obtained.

[0204] S5: Add 1 part by weight of the primary barium titanate nanoparticles obtained in step S4 and 2 parts by weight of hexadecyltrimethylammonium bromide to 30 parts by weight of formamide. Modify by stirring at 200 rpm for 5 hours at 160°C. Then filter and wash the bottom solid powder and vacuum dry it at -30°C for 5 hours to obtain barium titanate nanoparticles.

[0205] (2): Vanillin, tetrahydrogeraniol, methyl lauryl ester and cypressene are mixed in equal weight ratios and stirred at 550 rpm for 10 minutes at 70°C to obtain the core material mixture.

[0206] (3): 3.5 parts by weight of the core material mixture obtained in step (2), 1.5 parts by weight of the barium titanate nanoparticles obtained in step (1) and 20 parts by weight of N,N-dimethylformamide were stirred at 400 rpm for 5 hours at 50°C.

[0207] (4): Add butyl orthosilicate to the reaction system in step (3). The mass ratio of the core material mixture to butyl orthosilicate is 7:5. Continue stirring at 400 rpm for 5 hours at 50°C to obtain Pickering emulsion.

[0208] (5): Slowly add 10wt% dilute hydrochloric acid to the reaction system in step (4) using a peristaltic pump until the pH of the reaction system is 3.5. Continue stirring at 400 rpm for 4.5 hours at 50°C, then stop stirring and age at the same temperature for 24 hours. Then filter and wash the solid powder in the reaction system and vacuum dry it at -30°C for 5 hours to obtain an environmentally friendly microcapsule matrix.

[0209] (6): The environmentally friendly microcapsule matrix obtained in step (5) was added to a Tris buffer solution with a pH of 8.5. The mass ratio of the Tris buffer solution to the deodorizing environmentally friendly microcapsule matrix was 60:1. Then, dopamine hydrochloride was added to make the concentration of dopamine in the reaction system 6.5 mg / mL. The mixture was stirred at 200 rpm for 12 hours at 25°C. The stirring was then stopped. The bottom solid powder was filtered and washed, and then vacuum dried at -30°C for 5 hours.

[0210] (7): 1.35 parts by weight of anhydrous copper sulfate and 50 parts by weight of deionized water were mixed manually at room temperature to prepare a copper sulfate solution. 1 part by weight of the solid particles obtained after drying in step (6) and the copper sulfate solution were added to the reactor. The reactor lid was closed and the mixture was stirred at 200 rpm for 1 hour at 110°C.

[0211] (8): Add 4 parts by weight of sodium sulfite to 40 parts by weight of acetate buffer solution with pH=6, and stir at 200 rpm for 1 h at 50 °C; add the resulting mixed solution to the reaction vessel (7), close the vessel lid, and stir at 200 rpm for 4 h at 90 °C. Finally, filter and wash the bottom solid powder, and vacuum dry it at -30 °C for 5 h to obtain environmentally friendly microcapsules with a particle size of 2.81~7.43 μm.

[0212] The auxiliary deodorizing agent 4,4′-methylenebis(N-phenylmaleimide), tetrakis 2,5-ditert-butylhydroquinone, and distearate pentaerythritol diphosphite were mixed in a mass ratio and dispersed in dodecyl dimethyl betaine. The mixture was stirred at 450 rpm for 1.5 h at 35 °C. Then, the environmentally friendly microcapsules obtained in step (8) were added and the mixture was stirred for another 2 h to obtain the asphalt additive. The mass ratio of the auxiliary deodorizing agent, the environmentally friendly microcapsules, and 1-hydroxyethyl-carboxymethyl-alkylimidazoline was 1:1:2.

[0213] Preparation of the asphalt composition:

[0214] Add 1 part by weight of asphalt additive to 100 parts of base asphalt with a penetration of 54 at 25°C and heated to 143°C, and stir at 400 rpm for 4 hours to obtain odorless and environmentally friendly asphalt.

[0215] Comparative Example 1

[0216] One hundred portions of base asphalt with a penetration of 54 at 25°C were heated to 143°C and stirred at 400 rpm for 4 hours to obtain a base asphalt control sample.

[0217] Comparative Example 2

[0218] Preparation of asphalt additives:

[0219] The deodorizing agents vanillin, tetrahydrogeraniol, methyl laurylate, and cedrene were mixed in equal mass ratios; the auxiliary deodorizing agents hexadecyl maleimide, 2,6-di-tert-butyl-p-methylphenol, and tris(nonylphenol) phosphite were mixed in equal mass ratios; the deodorizing agents and auxiliary deodorizing agents were dispersed in 1-hydroxyethyl-carboxymethyl-alkylimidazoline, and stirred and mixed at 400 rpm for 1 hour at 25°C to obtain the asphalt additive. The mass ratio of the deodorizing agent, auxiliary deodorizing agent, and 1-hydroxyethyl-carboxymethyl-alkylimidazoline was 1:1:2.

[0220] Preparation of the asphalt composition:

[0221] Add 2 parts by weight of asphalt additive to 100 parts of base asphalt with a penetration of 54 at 25°C and heated to 143°C, and stir at 400 rpm for 4 hours to obtain odorless and environmentally friendly asphalt.

[0222] Test case

[0223] Sulfides and hydrocarbons are harmful substances in asphalt fumes that have a significant impact on human health. The asphalt samples prepared in Examples 1-6 and Comparative Examples 1-2 were stored at 143°C for 7 days. After storage, an equal mass of the stored asphalt was transferred to an asphalt fume enrichment and collection device, where fume enrichment was carried out at 163°C for 4 hours. After enrichment, the gas in the sealed container was extracted and tested. The data obtained are shown in Table 1 below.

[0224] Table 1

[0225]

[0226] The specific embodiments of the present invention have been described in detail above; however, the present invention is not limited thereto. Within the scope of the inventive concept, various simple modifications can be made to the technical solutions of the present invention, including combining the various technical features in any other suitable manner. These simple modifications and combinations should also be considered as the content disclosed in the present invention and are all within the protection scope of the present invention.

Claims

1. An asphalt additive, characterized in that, The asphalt additive, by weight, comprises the following components: Deodorizing agent, 1-5 parts; Environmentally friendly microcapsules, 1-5 servings; Dispersant, 1-10 parts; The environmentally friendly microcapsule comprises a composite shell material and a core material. The composite shell material comprises silicon dioxide, barium titanate nanoparticles, polydopamine, and cuprous oxide. The core material comprises one or more of aldehydes, alcohols, esters, and alkenes.

2. The asphalt additive according to claim 1, characterized in that, The auxiliary deodorizing agent is selected from one or more of imide compounds with a molecular weight greater than 170 and antioxidants with a molecular weight greater than 200. And / or, the imide compound with a molecular weight greater than 170 is selected from one or more of N-phenylmaleimide, hexadecylmaleimide, tris(2-maleimide ethyl)amine, and 4,4′-methylenebis(N-phenylmaleimide); And / or, the antioxidant with a molecular weight greater than 200 is a hindered phenolic antioxidant and / or a phosphite antioxidant; the hindered phenolic antioxidant is selected from one or more of 2,6-di-tert-butyl-p-methylphenol, pentaerythritol tetrakis(dibutylhydroxy-hydrocinnamic acid) ester, 2,5-di-tert-butylhydroquinone, 4-(1,1-dimethylethyl)-1,2-benzenediol, and 2,2′-methylenebis(4-ethyl-6-tert-butylphenol); the phosphite antioxidant is selected from one or more of tris(2,4-di-tert-butylphenyl) phosphite, tris(nonylphenol) phosphite, and pentaerythritol distearate diphosphite. And / or, the dispersant is one or more of dodecyl dimethyl betaine and 1-hydroxyethyl-carboxymethyl-alkyl imidazoline.

3. The asphalt additive according to claim 1, characterized in that, The environmentally friendly microcapsules have a particle size of 1-10 μm; And / or, the mass ratio of the composite shell material to the core material is 1:(0.2-2); And / or, the composite shell material comprises an inorganic base shell / barium titanate nanoparticles / polydopamine / cuprous oxide, wherein the mass ratio of the inorganic base shell to the barium titanate nanoparticles, polydopamine, and cuprous oxide is 1:(0.2-0.8):(0.1-0.5):(0.5-2); And / or, the material of the inorganic base shell is selected from at least one of silicon dioxide and titanium dioxide, preferably silicon dioxide.

4. A method for preparing the asphalt additive according to any one of claims 1-3, comprising: The auxiliary deodorizing agent is added to the dispersant, stirred for the first time, and then the prepared environmentally friendly microcapsules are added. After stirring for the second time, the asphalt additive is obtained.

5. The method according to claim 4, characterized in that, The first stirring conditions are: stirring at 400-500 rpm for 1-3 hours at 25-45℃; And / or, the second stirring conditions are: stirring at 400-500 rpm for 1-3 hours at 25-45°C.

6. The method according to claim 4, characterized in that, The method for preparing the environmentally friendly microcapsules includes: (1) Preparation of barium titanate nanoparticles; (2) Stir and mix one or more deodorizing agents to obtain a core material mixture; (3) The core material mixture and barium titanate nanoparticles are stirred and mixed in a solvent; (4) Add the inorganic base shell precursor to the reaction system of step (3), stir and mix to obtain Pickering emulsion; (5) Adjust the pH value of the Pickering emulsion obtained in step (4), continue stirring, then age, filter, freeze dry, and obtain an environmentally friendly microcapsule matrix; (6) Disperse the environmentally friendly microcapsule matrix obtained in step (5) in a buffer solution, add dopamine hydrochloride, process with stirring, then filter, wash, freeze dry to obtain solid particles; (7) Add the solid particles and copper ion solution obtained in step (6) into the reaction vessel and carry out the reaction with stirring; (8) Mix the reducing agent with the buffer solution, stir to dissolve, and then add it to the reaction system of step (7). Stir to carry out the reaction, then filter, wash, freeze dry, and obtain environmentally friendly microcapsules.

7. The method according to claim 6, characterized in that, Step (1) of preparing barium titanate nanoparticles includes: S1: Stir and mix the titanium precursor and solvent; S2: Adjust the pH of the mixed solution obtained in S1 and stir until a titanium precursor sol is obtained; S3: Mix the barium precursor with water; S4: The titanium precursor sol obtained in S2 is mixed with the mixture obtained in S3 and reacted under stirring. After the reaction is completed, the mixture is filtered, washed, freeze-dried, and ground to obtain primary barium titanate nanoparticles. S5: Primary barium titanate nanoparticles, surfactants and solvents are mixed and modified under stirring. After modification, the mixture is washed and freeze-dried to obtain barium titanate nanoparticles.

8. The method according to claim 7, characterized in that, In step S1, the titanium precursor is selected from at least one of tetraethyl titanate, n-propyl titanate, and tetrabutyl titanate. And / or, in step S1, the solvent is an alcohol compound with a boiling point >60°C, and the alcohol compound is an anhydrous alcohol compound, preferably at least one of methanol, butanediol, ethylene glycol, n-butanol, and ethanol; And / or, in step S1, the stirring temperature is 25-60℃; the stirring speed is 200-500 rpm; and the stirring time is 0.5-3 hours. And / or, in step S1, the mass ratio of the titanium precursor to the solvent is (1-20):

1.

9. The method according to claim 7, characterized in that, In step S2, the pH of the S1 mixed solution is adjusted to pH = 9-12; And / or, in step S2, the stirring temperature is 25-60℃; the stirring speed is 200-500 rpm; and the stirring time is 0.5-3 hours.

10. The method according to claim 7, characterized in that, In step S3, the barium precursor is at least one of Ba(OH)2, Ba(OH)2·H2O, and Ba(OH)2·8H2O. And / or, in step S3, the stirring temperature is 80-120℃; the stirring speed is 200-500 rpm; and the stirring time is 2-5 hours.

11. The method according to claim 7, characterized in that, In step S4, the molar ratio of the mixture obtained in S3 (based on barium) to the titanium precursor sol obtained in S2 (based on titanium) is 1:(0.5-5). And / or, the stirring speed is 200-500 rpm; the reaction temperature is 100-200℃; and the reaction time is 2-48 hours. And / or, in step S4, the freeze-drying conditions are: vacuum drying for 4-8 hours at a temperature of -40°C to -20°C.

12. The method according to claim 7, characterized in that, In step S5, the diameter of the barium titanate nanoparticles is 20-100 nm; And / or, in step S5, the surfactant is an anionic surfactant, preferably at least one of sodium dodecylbenzenesulfonate, sodium dodecyl sulfate, and 2-morpholine ethanesulfonic acid; And / or, in step S5, the solvent is an aprotic solvent with a boiling point >100℃, preferably at least one of formamide, N,N-dimethylformamide, dimethylacetamide, and dimethylphosphoramide; And / or, in step S5, the stirring speed is 200-500 rpm; The modification temperature is 70-180℃, and the modification time is 2-8 hours; And / or, in step S5, the freeze-drying conditions are: vacuum drying for 4-8 hours at a temperature of -40°C to -20°C.

13. The method according to claim 6, characterized in that, In step (3), the solvent is an aprotic solvent with a boiling point >100℃, preferably at least one of formamide, N,N-dimethylformamide, dimethylacetamide, and dimethylphosphoramide; And / or, in step (3), the mass ratio of the solvent to the barium titanate nanoparticles is (10-40):1; And / or, in step (3), the stirring speed is 400-600 rpm, the stirring temperature is 30-60℃, and the stirring time is 4-6 hours.

14. The method according to claim 6, characterized in that, In step (4), the inorganic base shell precursor is at least one of silicate ester compounds and titanate compounds, preferably a silicate ester compound; the silicate ester compound is at least one of methyl silicate, tetraethyl orthosilicate, tetraethyl orthosilicate, and tetrabutyl orthosilicate. And / or, in step (4), the stirring speed is 400-600 rpm, the stirring temperature is 30-60℃, and the stirring time is 4-6 hours.

15. The method according to claim 6, characterized in that, In step (5), the pH is adjusted to 3-6; the stirring speed is 400-600 rpm, the stirring temperature is 30-60℃, and the stirring time is 4-6 hours. And / or, in step (5), the aging conditions are: standing at 40-60°C for 12-30 hours; the freeze-drying conditions are: vacuum drying at -40-20°C for 4-8 hours.

16. The method according to claim 6, characterized in that, In step (6), the buffer solution is at least one of phosphate buffer, carbonate buffer, and tris(hydroxymethyl)aminomethane hydrochloride buffer. And / or, in step (6), the pH value of the buffer solution is 8-10; And / or, in step (6), the mass ratio of the buffer solution to the environmentally friendly microcapsule matrix obtained in step (5) is (10-100):1; And / or, in step (6), after adding dopamine hydrochloride, the mass concentration of dopamine in the reaction system is 2-10 mg / mL; And / or, in step (6), the stirring speed is 100-300 rpm, the stirring temperature is 20-40°C, and the stirring time is 12-24 hours; And / or, in step (6), the freeze-drying conditions are: vacuum drying for 4-8 hours at a temperature of -40°C to -20°C.

17. The method according to claim 6, characterized in that, In step (7), the copper ion solution has a copper ion concentration of 0.05-0.5 mol / L; And / or, in step (7), the mass ratio of the solid particles and copper ion solution obtained in step (6) is 1:(50-200); And / or, in step (7), the stirring speed is 100-450 rpm, the reaction temperature is 100-190°C, and the reaction time is 1-5 hours.

18. The method according to claim 6, characterized in that, In step (8), the reducing agent is a sulfite reducing agent, preferably selected from at least one of potassium sulfite and sodium sulfite; And / or, in step (8), the buffer solution is selected from at least one of acetate buffer and phosphate buffer, preferably acetate buffer; the pH value of the buffer solution is 4.5-6.5; And / or, in step (8), the mass ratio of the reducing agent to the buffer solution is 1:(10-20); And / or, in step (8), when stirring to dissolve, the stirring speed is 200-450 rpm, the stirring temperature is 40-80°C, and the stirring time is 1-5 hours; And / or, in step (8), when the reaction is carried out under stirring, the stirring speed is 100-450 rpm, the reaction temperature is 60-95°C, and the reaction time is 2-5 hours; And / or, in step (8), the freeze-drying conditions are: vacuum drying for 4-8 hours at a temperature of -40°C to -20°C.

19. An asphalt composition, comprising, by weight, the following components: Base bitumen, 50-500 parts; The asphalt additive according to any one of claims 1-3, 1-50 parts, preferably 2-50 parts.

20. A method for preparing the asphalt composition of claim 19, comprising: The base asphalt is heated to a molten state, and the asphalt additive is added while stirring to obtain an asphalt composition.