A deodorized temperature control asphalt additive, an asphalt composition and a preparation method thereof

Abstract

The application discloses a kind of net taste temperature control asphalt additive, asphalt composition and preparation method thereof.Net taste temperature control asphalt additive of the application includes the following components by weight parts: auxiliary odor control agent, 1-5 parts;Dispersing agent, 1-10 parts;Odor control temperature microcapsule, 1-5 parts;The odor control temperature microcapsule includes composite shell material and core material, wherein the composite shell material includes inorganic base layer shell, barium titanate nanoparticles, polydopamine and cuprous oxide, the core material includes n-alkane with phase transition temperature of 40-60 DEG C, and the composite shell material surface is loaded with active smoke suppression compound.The net taste temperature control asphalt prepared by adding odor control temperature microcapsule into asphalt can efficiently and durably reduce the content of irritating gas in asphalt fume, reduce the content of volatile organic compounds released by asphalt pavement at high temperature, improve the high-temperature stability of asphalt, and prolong the service life of asphalt pavement by the temperature control effect of microcapsule and the odor control effect of active components on the surface of microcapsule.

Description

Technical Field

[0001] This invention belongs to the field of special asphalt, specifically relating to an odor-neutralizing and temperature-controlled asphalt additive, an asphalt composition, and a method for preparing the same. Background Technology

[0002] Asphalt pavement, with its superior road performance, high smoothness, and low noise characteristics, dominates urban roads and highways, especially highways, where over 90% of the pavement is asphalt. However, as a temperature-sensitive material, asphalt is prone to rutting, swelling, bleeding, and cracking under high temperatures and heavy loads, significantly shortening pavement life. In hot regions such as Guangxi, Guangdong, and Xiamen, high summer temperatures soften asphalt, further exacerbating rutting and other problems and intensifying the urban heat island effect. At the same time, asphalt pavement also faces multiple environmental challenges: the release of pollutants such as sulfides and volatile organic compounds caused by the hot-mix hot-lay process urgently needs to be addressed.

[0003] Existing technologies attempt to address the aforementioned problems by adding phase change materials and odor neutralizers, but both have limitations. While phase change materials can mitigate the effects of high temperatures, their control over flue gas is limited; while odor neutralizers can reduce flue gas emissions during construction, their thermal stability is poor, and the large molecular compounds generated in the reaction are also unstable, still posing potential environmental risks.

[0004] CN115322752A discloses a method for preparing phase change microcapsules for autonomously temperature-regulating asphalt pavement in areas with large temperature differences. After being added to the asphalt system, the microcapsules can effectively reduce the impact of high temperature on the performance of asphalt pavement, but the microcapsules have little effect on suppressing asphalt fumes.

[0005] Therefore, developing more efficient and environmentally friendly asphalt modification technologies to comprehensively improve the weather resistance of asphalt pavements and reduce the environmental impact of flue gas has become a current research hotspot and challenge. Summary of the Invention

[0006] To address the problems existing in the prior art, this invention provides an odor-neutralizing and temperature-controlled asphalt additive, an asphalt composition, and a method for preparing the same. The odor-neutralizing and temperature-controlled asphalt, prepared by adding odor-neutralizing and temperature-controlled microcapsules to asphalt, utilizes the temperature-controlling effect of the microcapsules and the odor-neutralizing effect of the active odor-neutralizing components on their surface. This effectively and persistently reduces the content of irritating gases in asphalt fumes, reduces the content of volatile organic compounds released at high temperatures from asphalt pavements, improves the high-temperature stability of asphalt, and extends the service life of asphalt pavements, providing a novel approach for the long-life and environmentally friendly utilization of asphalt.

[0007] The first aspect of this invention provides a odor-neutralizing and temperature-controlled asphalt additive, comprising the following components by weight:

[0008] Deodorizing agent, 1-5 parts;

[0009] Dispersant, 1-10 parts;

[0010] Odor-neutralizing and temperature-controlled microcapsules, 1-5 servings;

[0011] The odor-neutralizing and temperature-controlled microcapsule comprises a composite shell and a core material. The composite shell comprises an inorganic base shell, barium titanate nanoparticles, polydopamine, and cuprous oxide. The core material comprises n-alkanes with a phase transition temperature of 40-60°C. The surface of the composite shell is loaded with an active smoke-suppressing compound.

[0012] 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.

[0013] 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).

[0014] 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.

[0015] Furthermore, the dispersant is one or more of dodecyl dimethyl betaine and 1-hydroxyethyl-carboxymethyl-alkyl imidazoline.

[0016] Furthermore, the particle size of the odor-neutralizing and temperature-controlled microcapsules is 1-12 μm.

[0017] Furthermore, the mass ratio of the composite shell material to the core material of the odor-neutralizing and temperature-controlled microcapsule is 1:(0.2-2).

[0018] Further, 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 is 1:(0.2-0.8), the mass ratio of the inorganic base shell to the polydopamine is 1:(0.1-0.5), and the mass ratio of the inorganic base shell to the cuprous oxide is 1:(0.5-2).

[0019] Furthermore, the inorganic base shell is made of at least one material selected from silicon dioxide and titanium dioxide, preferably silicon dioxide.

[0020] Furthermore, the n-alkane with a phase transition temperature of 40-60℃ is one or more of n-octadecane, n-eicosane, and n-docosahexadecane.

[0021] Furthermore, the loading of the active smoke-suppressing compound accounts for 0.1wt%-20wt% of the total mass of the odor-neutralizing and temperature-controlled microcapsules.

[0022] Furthermore, the active smoke-suppressing compound is selected from one or more aldehyde compounds with a molecular weight greater than 160 and / or ketone compounds with a molecular weight greater than 150.

[0023] Furthermore, the aldehyde compound with a molecular weight greater than 160 is selected from one or more of 2-methylundecaldehyde, 10-undecenaldehyde, neojasmine aldehyde, citronellol, and citronellol.

[0024] Furthermore, the ketone compound with a molecular weight greater than 150 is selected from one or more of methyl nonyl ketone, geranylacetone, farnesyl acetone, dihydrodamastone, menthone, and allyl ionone.

[0025] A second aspect of the present invention provides a method for preparing the above-mentioned odor-neutralizing and temperature-controlled asphalt additive, comprising:

[0026] The auxiliary odor neutralizer is added to the dispersant, stirred for the first time, and then the prepared odor neutralizing and temperature-controlled microcapsules are added. After stirring for the second time, the asphalt additive is obtained.

[0027] Furthermore, the conditions for the first stirring are: stirring at 400-500 rpm for 1-3 hours at 25-45℃.

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

[0029] Furthermore, the preparation method of the odor-neutralizing and temperature-controlled microcapsules includes:

[0030] (1) Preparation of barium titanate nanoparticles;

[0031] (2) Heat the core material raw material to melt, and mix it with solvent and barium titanate nanoparticles obtained in step (1);

[0032] (3) Add the inorganic base shell precursor to the reaction system of step (2), stir and mix to obtain Pickering emulsion;

[0033] (4) Adjust the pH value of the Pickering emulsion, continue stirring, then age, filter, wash, and freeze dry;

[0034] (5) Add the solid material obtained in step (4) to the buffer solution, add dopamine hydrochloride, stir and process, then filter, wash and freeze dry;

[0035] (6) Add the solid particles and copper ion solution obtained in step (5) into the reaction vessel and carry out the reaction with stirring;

[0036] (7) Mix the reducing agent with the buffer solution, stir to dissolve, and then add it to the reaction system of step (6). Stir to carry out the reaction, then filter, wash, and freeze dry.

[0037] (8) Mix the solid particles obtained in step (7) with water, adjust the pH, and then heat and stir; then add silane coupling agent, continue to react under stirring, and then filter, wash and freeze dry.

[0038] (9) The solid material obtained in step (8), the active smoke-suppressing compound, and the strong alkali are added to an organic solvent to react. After cooling, filtering, washing, and freeze-drying, the odor-neutralizing temperature-controlled microcapsules are obtained.

[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 core material raw material is heated to a melting temperature of 40-80℃.

[0066] Further, in step (2), the solvent is an aprotic solvent with a boiling point >100℃, preferably at least one of formamide, N,N-dimethylformamide, dimethylacetamide, and dimethylphosphoramide, and more preferably formamide.

[0067] Further, in step (2), the mass ratio of the solvent to the barium titanate nanoparticles is (20-80):1.

[0068] Furthermore, in step (2), the stirring speed is 400-600 rpm, the stirring temperature is 40-80℃, and the stirring time is 4-6 hours.

[0069] Further, in step (3), 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 preferably at least one of methyl silicate, tetraethyl orthosilicate, tetraethyl orthosilicate, and tetraethyl orthosilicate, more preferably tetraethyl orthosilicate.

[0070] Furthermore, in step (3), the stirring speed is 400-600 rpm, the stirring temperature is 40-80℃, and the stirring time is 4-6 hours.

[0071] Further, in step (4), the pH value is adjusted to 3-6. The pH can be adjusted using a dilute acid, such as dilute hydrochloric acid.

[0072] Furthermore, in step (4), the stirring speed is 400-600 rpm, the stirring temperature is 40-80℃, and the stirring time is 4-6 hours.

[0073] Further, in step (4), the aging conditions are: standing at 40-80℃ for 12-30 hours. The freeze-drying conditions are: vacuum drying at -40---20℃ for 4-8 hours.

[0074] Further, in step (5), the buffer solution is one or more of phosphate buffer, carbonate buffer, and tris(hydroxymethyl)aminomethane hydrochloride buffer (Tris buffer), preferably tris(hydroxymethyl)aminomethane hydrochloride buffer (Tris buffer).

[0075] Furthermore, in step (5), the pH value of the buffer solution is preferably 8-10.

[0076] Further, in step (5), the mass ratio of the buffer solution to the solid material obtained in step (4) is (10-100):1.

[0077] Furthermore, in step (5), after adding dopamine hydrochloride, the mass concentration of dopamine in the reaction system is 2-10 mg / mL.

[0078] Furthermore, in step (5), the stirring speed is 100-300 rpm, the stirring temperature is 20-40℃, and the stirring time is 12-24 hours.

[0079] Furthermore, in step (5), the freeze-drying conditions are: vacuum drying for 4-8 hours at a temperature of -40°C to -20°C.

[0080] Further, in step (6), the copper ion solution is prepared by mixing copper ion salt and deionized water, and the copper ion salt is preferably anhydrous copper sulfate.

[0081] Further, in step (6), the concentration of copper ions in the copper ion solution is 0.05-0.5 mol / L.

[0082] Further, in step (6), the mass ratio of the solid particles and copper ion solution obtained in step (5) is 1:(50-200).

[0083] Furthermore, in step (6), the stirring speed is 100-450 rpm, the reaction temperature is 100-190℃, and the reaction time is 1-5 hours.

[0084] Further, in step (7), the reducing agent is a sulfite reducing agent, preferably selected from at least one of potassium sulfite and sodium sulfite.

[0085] Further, in step (7), the buffer solution is selected from one of acetate buffer and phosphate buffer, preferably acetate buffer; the pH value of the buffer solution is 4.5-6.5.

[0086] Further, in step (7), the mass ratio of the reducing agent to the buffer solution is 1:(10-20).

[0087] Furthermore, in step (7), when stirring to dissolve, the stirring speed is 200-450 rpm, the stirring temperature is 40-80℃, and the stirring time is 1-5 hours.

[0088] Furthermore, in step (7), the stirring speed is 100-450 rpm, the reaction temperature is 60-95℃, and the reaction time is 2-5 hours.

[0089] Further, in step (7), the freeze-drying conditions are: vacuum drying for 4-8 hours at a temperature of -40°C to -20°C.

[0090] Furthermore, in step (8), the stirring speed is 300-500 rpm, the stirring temperature is 20-90℃, and the stirring time is 1-6h.

[0091] Furthermore, in step (8), the pH is adjusted to 9-11. The pH can be adjusted using a conventional dilute alkaline solution, such as at least one of dilute sodium hydroxide solution or dilute potassium hydroxide solution.

[0092] Further, in step (8), the mass ratio of the solid particles obtained in step (7) to water is 1:(10-50).

[0093] Furthermore, in step (8), the added silane coupling agent is selected from one or more of chloropropyltriethoxysilane, chloromethyltriethoxysilane, dichloromethyltriethoxysilane, and chloromethyltriisopropoxysilane.

[0094] Further, in step (8), the mass ratio of the solid particles obtained in step (7) to the silane coupling agent is 1:(0.5-4).

[0095] Further, in step (8), the stirring speed is 300-500 rpm, the stirring temperature is 20-90℃, and the stirring time is 1-8h.

[0096] 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.

[0097] Further, in step (9), the organic solvent is selected from one or more of methanol, butanediol, ethylene glycol, n-butanol, and ethanol, preferably ethanol, and all organic solvents are anhydrous solvents.

[0098] Further, in step (9), the mass ratio of the solid material obtained in step (8) to the organic solvent is 1:(20-80). The mass ratio of the solid material obtained in step (8) to the strong alkali is 1:(0.5-2).

[0099] Furthermore, in step (9), the strong alkali is either solid KOH or solid NaOH, preferably solid KOH.

[0100] Furthermore, in step (9), the reaction is carried out under reflux and the reaction conditions are: reaction temperature of 80-210℃ and reaction time of 5-10 hours.

[0101] Further, in step (9), the freeze-drying conditions are: vacuum drying for 4-8 hours at a temperature of -40°C to -20°C.

[0102] A third aspect of the present invention provides an asphalt composition comprising, by weight, the following components:

[0103] 50-200 parts of base bitumen;

[0104] The above-mentioned odor-neutralizing and temperature-controlled asphalt additive is used in quantities of 0.1-20 parts, preferably 1.5-5 parts.

[0105] Furthermore, the penetration of the base asphalt at 25°C is 30-210 1 / 10 mm.

[0106] A fourth aspect of the present invention provides a method for preparing the above-mentioned asphalt composition, comprising:

[0107] The base asphalt is heated to a molten state, and then a neutral-odor asphalt additive is added while stirring to obtain an asphalt composition.

[0108] Furthermore, the temperature at which the base asphalt is heated to a molten state is 133-153℃.

[0109] Furthermore, the stirring speed is 400-600 rpm, and the stirring time is 2-4 hours.

[0110] Compared with the prior art, the present invention has the following advantages:

[0111] (1) The odor-neutralizing and temperature-controlled asphalt additive of the present invention contains an inorganic base shell, barium titanate nanoparticles, polydopamine and cuprous oxide as the composite shell material of the odor-neutralizing and temperature-controlled microcapsules, 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 application, it can attract compounds released from 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 on the surface of the microcapsules to react with more of the above-mentioned compounds, thereby effectively reducing the impact of irritating gases released by asphalt during application on the human body.

[0112] (2) The odor-neutralizing and temperature-controlled asphalt additive of the present invention comprises an inorganic base shell, barium titanate nanoparticles, polydopamine and cuprous oxide as the composite shell material of the odor-neutralizing and temperature-controlled microcapsules. 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 application 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 microcapsules, which effectively improves the adsorption capacity of cuprous oxide for 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 on the surface of the odor-neutralizing and temperature-controlled microcapsules and pollutants, further improving the smoke-suppressing ability of the odor-neutralizing and temperature-controlled microcapsules.

[0113] (3) The odor-neutralizing and temperature-controlled asphalt additive of the present invention contains odor-neutralizing and temperature-controlled microcapsules that can regulate the temperature of asphalt pavement in situ. This not only effectively improves the high-temperature performance of asphalt pavement, but also reduces the damage to asphalt pavement caused by temperature changes and extends the service life of asphalt pavement.

[0114] (4) The odor-neutralizing and temperature-controlled asphalt additive of the present invention contains odor-neutralizing and temperature-controlled microcapsules, which can reduce the temperature of asphalt pavement during application after being added to asphalt. This can not only effectively reduce the urban heat island effect, but also prevent asphalt pavement from releasing various harmful substances due to excessive temperature, thereby avoiding the generation of photochemical smog and haze.

[0115] (5) The odor-neutralizing and temperature-controlled asphalt additive of the present invention contains an auxiliary odor-neutralizing agent that can quickly and effectively reduce the asphalt fumes generated by the action of heat and oxygen during the production, construction and service of asphalt. This agent can be used in the window period when the odor-neutralizing and temperature-controlled asphalt additive is added to asphalt and the odor-neutralizing and temperature-controlled microcapsules are not yet effective. Detailed Implementation

[0116] To further illustrate the technical solution of the present invention, the present invention will be clearly and thoroughly described below in conjunction with embodiments.

[0117] The hydrogen sulfide in the asphalt fumes described in this invention was tested using a TESTO 350 flue gas analyzer. During the test, the pipeline was kept at 120°C to prevent moisture from affecting the test results.

[0118] The volatile organic compounds in the asphalt fumes described in this invention are determined according to standard HJ 734-2014, "Determination of Volatile Organic Compounds in Waste Gas from Stationary Sources: Solid Phase Adsorption-Thermal Desorption Gas Chromatography-Mass Spectrometry," and are tested using a gas chromatography-mass spectrometer.

[0119] The benzene series compounds in the asphalt flue gas described in this invention are tested according to the solid adsorption thermal desorption-gas chromatography method for the determination of benzene series compounds in ambient air, as specified in HJ 583-2010.

[0120] Example 1

[0121] Preparation of asphalt additives:

[0122] (1): Preparation of barium titanate nanoparticles:

[0123] S1: Weigh 22 parts by weight of tetrabutyl titanate and 15 parts by weight of anhydrous ethanol and add them to a flask. Stir for 2 hours at 50°C and 400 rpm to obtain a titanium precursor solution.

[0124] S2: Slowly add 10wt% ammonia to the S1 solution until the pH of the reaction system is 10.5, and continue stirring at 400 rpm for 2 hours at 50℃ to obtain the titanium precursor sol.

[0125] S3: Add 18.5 parts by weight of Ba(OH)2·H2O and 18.5 parts by weight of deionized water to the reactor, and heat and stir at 400 rpm for 2 hours at 85°C.

[0126] S4: Add the sol obtained in S2 to the reaction vessel in S3, close the reaction vessel lid, heat to 160℃, stir at 400 rpm for 16 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.

[0127] S5: Add 1 part by weight of the primary barium titanate nanoparticles obtained in step S4 and 3 parts by weight of hexadecyltrimethylammonium bromide to 45 parts by weight of dimethylphosphoramide. Modify by stirring at 200 rpm for 5 hours at 140°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 30-50 nm).

[0128] (2): 4 parts by mass of n-dodecane were heated and melted at 50°C, and 60 parts by mass of formamide and 1.5 parts by mass of barium titanate nanoparticles prepared in step (1) were added. The mixture was stirred at 50°C and 400 rpm for 5 hours.

[0129] (3): Keeping the conditions of the reaction system in step (2) unchanged, slowly add 3 parts by mass of tetraethyl orthosilicate to the reaction system in step (2). After the addition is completed, continue stirring at 50°C and 400 rpm for 5 hours to obtain Pickering emulsion.

[0130] (4): Slowly add 10wt% dilute hydrochloric acid to the reaction system in step (3) using a peristaltic pump until the pH of the reaction system is 3.5. Continue stirring at 500 rpm for 4.5 hours at 50°C. Stop stirring and keep the temperature constant for 24 hours. Then filter and wash the solid powder in the reaction system and vacuum dry it at -30°C for 5 hours.

[0131] (5): Add the solid material obtained in step (4) to a Tris buffer solution with a pH of 8.5. The mass ratio of Tris buffer solution to solid powder is 80:1. Then add dopamine hydrochloride to make the concentration of dopamine in the reaction system 6 mg / mL. Stir at 200 rpm for 12 hours at 25°C and then stop stirring. Filter and wash the bottom solid powder and vacuum dry it at -30°C for 5 hours.

[0132] (6): 1.35 parts by mass of anhydrous copper sulfate and 80 parts by mass of deionized water were manually stirred and mixed at room temperature to prepare a copper sulfate solution. 1 part by mass of the solid particles obtained in step (5) and the prepared copper sulfate solution were added to the reactor, the reactor lid was closed, and the mixture was stirred at 300 rpm for 1 h at a temperature of 130°C.

[0133] (7): Add 6 parts by mass of sodium sulfite to 70 parts by mass of pH=5 acetate buffer solution and stir at 200 rpm for 1 h at 50 °C; add the prepared mixed solution to the reaction vessel in step (6), close the vessel lid, stir at 300 rpm for 4 h at 75 °C, and finally filter and wash the bottom solid powder and vacuum dry at -30 °C for 5 h.

[0134] (8): Add 1 part by mass of the solid particles obtained in step (7) to 40 parts by mass of deionized water, then adjust the pH of the system to 10 using dilute potassium hydroxide solution, and stir for 2 hours at 70°C and 200 rpm. Keeping the temperature and stirring conditions unchanged, slowly add 3 parts by mass of chloromethyltriethoxysilane to the reaction system in step (8), and continue stirring for 4 hours. Finally, filter and wash the bottom solid powder, and vacuum dry it for 5 hours at -30°C.

[0135] (9): 6 parts by mass of the smoke-suppressing compound 10-undecenal and methyl nonyl ketone were stirred evenly and then added to 50 parts by mass of the solid material obtained in step (8). Then 1 part by mass of KOH was added and the mixture was refluxed at 95°C for 6 hours. The bottom solid powder was then filtered and washed and vacuum dried at -30°C for 5 hours to obtain the odor-neutralizing temperature-controlled microcapsules. The particle size of the microcapsules was 3.64-8.63 μm and the loading of the active smoke-suppressing compound accounted for 12.35 wt% of the total mass of the odor-neutralizing temperature-controlled microcapsules.

[0136] The auxiliary deodorizing agent hexadecyl maleimide, 2,6-di-tert-butyl-p-methylphenol, and tris(nonylphenol) phosphite were mixed in equal mass ratios and dispersed in dodecyl dimethyl betaine. The mixture was stirred at 400 rpm for 1 hour at 25°C. Then, the deodorizing and temperature-controlled microcapsules prepared in step (9) were added, and stirring was continued for another hour to obtain the deodorizing and temperature-controlled asphalt additive. The mass ratio of the auxiliary deodorizing agent, the deodorizing and temperature-controlled microcapsules, and dodecyl dimethyl betaine was 1:1:1.

[0137] Preparation of the asphalt composition:

[0138] Heat 100 parts by weight of base asphalt with a penetration of 52 at 25°C to 143°C, add 1.8 parts by weight of odor-neutralizing and temperature-controlled asphalt additive at a rotation speed of 500 rpm, and stir for 4 hours to obtain odor-neutralizing and temperature-controlled asphalt.

[0139] Example 2

[0140] Preparation of asphalt additives:

[0141] (1): Preparation of barium titanate nanoparticles:

[0142] S1: Weigh 15.5 parts by weight of tetrabutyl titanate and 15 parts by weight of anhydrous ethanol and add them to a flask. Stir at 50°C and 400 rpm for 3 hours to obtain a titanium precursor solution.

[0143] 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 3 hours at 50℃ to obtain titanium precursor sol.

[0144] S3: Add 12.9 parts by weight of Ba(OH)2·H2O and 15 parts by weight of deionized water to the reactor, and heat and stir at 400 rpm for 4 hours at 95°C.

[0145] S4: Add the sol obtained in S2 to the reaction vessel in S3, close the reaction vessel lid, heat to 170℃, stir at 400 rpm for 13 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.

[0146] S5: Add 1 part by weight of the primary barium titanate nanoparticles obtained in step S4 and 5 parts by weight of octadecyltrimethylammonium chloride to 80 parts by weight of dimethylacetamide. Modify by stirring at 200 rpm for 4 hours at 150°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 30-50 nm).

[0147] (2): 3 parts by mass of n-eicosane were heated and melted at 50°C, and 60 parts by mass of formamide and 1.5 parts by mass of barium titanate nanoparticles prepared in step (1) were added. The mixture was stirred at 50°C and 400 rpm for 5 hours.

[0148] (3): Keeping the conditions of the reaction system in step (2) unchanged, slowly add 3 parts by mass of methyl silicate to the reaction system in step (2). After the addition is completed, continue stirring at 50°C and 400 rpm for 5 hours to obtain Pickering emulsion.

[0149] (4): Slowly add 10wt% dilute hydrochloric acid to the reaction system in step (3) using a peristaltic pump until the pH of the reaction system is 3.5. Continue stirring at 500 rpm for 4.5 hours at 50°C. Stop stirring and keep the temperature constant for 24 hours. Then filter and wash the solid powder in the reaction system and vacuum dry it at -30°C for 5 hours.

[0150] (5): Add the solid material obtained in step (4) to a Tris buffer solution with a pH of 8.5. The mass ratio of Tris buffer solution to solid powder is 80:1. Then add dopamine hydrochloride to make the concentration of dopamine in the reaction system 6 mg / mL. Stir at 200 rpm for 12 hours at 25°C and then stop stirring. Filter and wash the bottom solid powder and vacuum dry it at -30°C for 5 hours.

[0151] (6): 1.35 parts by mass of anhydrous copper sulfate and 80 parts by mass of deionized water were manually stirred and mixed at room temperature to prepare a copper sulfate solution. 1 part by mass of the solid particles obtained in step (5) and the prepared copper sulfate solution were added to the reactor, the reactor lid was closed, and the mixture was stirred at 300 rpm for 1 h at a temperature of 130°C.

[0152] (7): Add 6 parts by mass of sodium sulfite to 70 parts by mass of pH=5 acetate buffer solution and stir at 200 rpm for 1 h at 50 °C; add the prepared mixed solution to the reaction vessel in step (6), close the vessel lid, stir at 300 rpm for 4 h at 75 °C, and finally filter and wash the bottom solid powder and vacuum dry at -30 °C for 5 h.

[0153] (8): Add 1 part by mass of the solid particles obtained in step (7) to 40 parts by mass of deionized water, then adjust the pH of the system to 10 using dilute potassium hydroxide solution, and stir for 2 hours at 70°C and 200 rpm. Keeping the temperature and stirring conditions unchanged, slowly add 3 parts by mass of chloromethyltriethoxysilane to the reaction system in step (8), and continue stirring for 4 hours. Finally, filter and wash the bottom solid powder, and vacuum dry it for 5 hours at -30°C.

[0154] (9): 6 parts by mass of the smoke-suppressing compound 10-undecenal and methyl nonyl ketone were stirred evenly and then added to 50 parts by mass of the solid material obtained in step (8). Then 1 part by mass of KOH was added and the mixture was refluxed at 95°C for 6 hours. The bottom solid powder was then filtered and washed and vacuum dried at -30°C for 5 hours to obtain the odor-neutralizing temperature-controlled microcapsules. The particle size of the microcapsules was 3.45-8.09 μm and the loading of the active smoke-suppressing compound accounted for 11.50 wt% of the total mass of the odor-neutralizing temperature-controlled microcapsules.

[0155] The auxiliary deodorizing agent hexadecyl maleimide, 2,6-di-tert-butyl-p-methylphenol, and tris(nonylphenol) phosphite were mixed in equal mass ratios and dispersed in dodecyl dimethyl betaine. The mixture was stirred at 400 rpm for 1 hour at 25°C. Then, the deodorizing and temperature-controlled microcapsules prepared in step (9) were added, and stirring was continued for another hour to obtain the deodorizing and temperature-controlled asphalt additive. The mass ratio of the auxiliary deodorizing agent, the deodorizing and temperature-controlled microcapsules, and dodecyl dimethyl betaine was 1:1:1.

[0156] Preparation of the asphalt composition:

[0157] Heat 100 parts by weight of base asphalt with a penetration of 52 at 25°C to 143°C, add 1.8 parts by weight of odor-neutralizing and temperature-controlled asphalt additive at a rotation speed of 500 rpm, and stir for 4 hours to obtain odor-neutralizing and temperature-controlled asphalt.

[0158] Example 3

[0159] Preparation of asphalt additives:

[0160] (1): Preparation of barium titanate nanoparticles:

[0161] S1: Weigh 17.3 parts by weight of tetrabutyl titanate and 12 parts by weight of ethylene glycol and add them to a flask. Stir at 55°C and 400 rpm for 2 hours to obtain a titanium precursor solution.

[0162] 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 2 hours at 55℃ to obtain titanium precursor sol.

[0163] S3: Add 14.5 parts by weight of Ba(OH)2·H2O and 16 parts by weight of deionized water to the reactor, and heat and stir at 400 rpm for 2 hours at 85°C.

[0164] S4: Add the sol obtained in S2 to the reaction vessel in S3, close the reaction vessel lid, heat to 160℃, stir at 400 rpm for 16 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.

[0165] S5: Add 1 part by weight of the primary barium titanate nanoparticles obtained in step S4 and 3 parts by weight of hexadecyltrimethylammonium bromide to 45 parts by weight of dimethylphosphoramide. Modify by stirring at 200 rpm for 5 hours at 140°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 30-50 nm).

[0166] (2): 4 parts by mass of n-dodecane were heated and melted at 50°C, and 60 parts by mass of formamide and 1.5 parts by mass of barium titanate nanoparticles prepared in step (1) were added. The mixture was stirred at 50°C and 400 rpm for 5 hours.

[0167] (3): Keeping the conditions of the reaction system in step (2) unchanged, slowly add 3 parts by mass of tetraethyl orthosilicate to the reaction system in step (2). After the addition is completed, continue stirring at 50°C and 400 rpm for 5 hours to obtain Pickering emulsion.

[0168] (4): Slowly add 10wt% dilute hydrochloric acid to the reaction system in step (3) using a peristaltic pump until the pH of the reaction system is 3.5. Continue stirring at 500 rpm for 4.5 hours at 50°C. Stop stirring and keep the temperature constant for 24 hours. Then filter and wash the solid powder in the reaction system and vacuum dry it at -30°C for 5 hours.

[0169] (5): Add the solid material obtained in step (4) to a Tris buffer solution with a pH of 8.5. The mass ratio of Tris buffer solution to solid powder is 80:1. Then add dopamine hydrochloride to make the concentration of dopamine in the reaction system 6 mg / mL. Stir at 200 rpm for 12 hours at 25°C and then stop stirring. Filter and wash the bottom solid powder and vacuum dry it at -30°C for 5 hours.

[0170] (6): 1.2 parts by mass of anhydrous copper sulfate and 80 parts by mass of deionized water were manually stirred and mixed at room temperature to prepare a copper sulfate solution. 1 part by mass of the solid particles obtained in step (5) and the prepared copper sulfate solution were added to the reactor, the reactor lid was closed, and the mixture was stirred at 300 rpm for 1 h at a temperature of 130°C.

[0171] (7): Add 6 parts by mass of potassium sulfite to 70 parts by mass of pH=5 acetate buffer solution and stir at 200 rpm for 1 h at 50 °C; add the prepared mixed solution to the reaction vessel in step (6), close the vessel lid, stir at 300 rpm for 4 h at 75 °C, and finally filter and wash the bottom solid powder and vacuum dry at -30 °C for 5 h.

[0172] (8): Add 1 part by mass of the solid particles obtained in step (7) to 40 parts by mass of deionized water, then adjust the pH of the system to 10 using dilute potassium hydroxide solution, and stir for 2 hours at 70°C and 200 rpm. Keeping the temperature and stirring conditions unchanged, slowly add 3 parts by mass of chloromethyltriethoxysilane to the reaction system in step (8), and continue stirring for 4 hours. Finally, filter and wash the bottom solid powder, and vacuum dry it for 5 hours at -30°C.

[0173] (9): 6 parts by mass of the smoke-suppressing compound: oxalicum aldehyde and farnesyl acetone in equal mass ratio were stirred evenly and then added to 50 parts by mass of the solid material obtained in step (8) with 1 part by mass of n-butanol. Then 1 part by mass of KOH was added and the mixture was refluxed at 130°C for 8 hours. The bottom solid powder was then filtered and washed and vacuum dried at -30°C for 5 hours to obtain the odor-neutralizing temperature-controlled microcapsules. The particle size of the microcapsules was 3.57 to 8.36 μm and the loading of the active smoke-suppressing compound accounted for 11.15 wt% of the total mass of the odor-neutralizing temperature-controlled microcapsules.

[0174] The auxiliary deodorizing agent hexadecyl maleimide, 2,6-di-tert-butyl-p-methylphenol, and tris(nonylphenol) phosphite were mixed in equal mass ratios and dispersed in dodecyl dimethyl betaine. The mixture was stirred at 400 rpm for 1 hour at 25°C. Then, the deodorizing and temperature-controlled microcapsules prepared in step (9) were added, and stirring was continued for another hour to obtain the deodorizing and temperature-controlled asphalt additive. The mass ratio of the auxiliary deodorizing agent, the deodorizing and temperature-controlled microcapsules, and dodecyl dimethyl betaine was 1:1:1.

[0175] Preparation of the asphalt composition:

[0176] Heat 100 parts by weight of base asphalt with a penetration of 52 at 25°C to 143°C, add 1.8 parts by weight of odor-neutralizing and temperature-controlled asphalt additive at a rotation speed of 500 rpm, and stir for 4 hours to obtain odor-neutralizing and temperature-controlled asphalt.

[0177] Example 4

[0178] Preparation of asphalt additives:

[0179] (1): Preparation of barium titanate nanoparticles:

[0180] S1: Weigh 19.7 parts by weight of tetrabutyl titanate and 14 parts by weight of n-butanol and add them to a flask. Stir at 50°C and 400 rpm for 3 hours to obtain a titanium precursor solution.

[0181] S2: Slowly add 10wt% ammonia water to the S1 solution until the pH of the reaction system is 11.5, and continue stirring at 400 rpm for 3 hours at 50℃ to obtain titanium precursor sol.

[0182] S3: Add 16.5 parts by weight of Ba(OH)2·H2O and 16.5 parts by weight of deionized water to the reactor, and heat and stir at 400 rpm for 2 hours at 85°C.

[0183] S4: Add the sol obtained in S2 to the reaction vessel in S3, close the reaction vessel lid, heat to 150℃, stir at 400 rpm for 17 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.

[0184] S5: Add 1 part by weight of the primary barium titanate nanoparticles obtained in step S4 and 6 parts by weight of dodecyl dimethyl benzyl ammonium chloride to 60 parts by weight of N,N-dimethylformamide. Modify by stirring at 200 rpm for 5 hours at 150°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 30-50 nm).

[0185] (2): 4 parts by mass of n-dodecane were heated and melted at 50°C, and 60 parts by mass of formamide and 1.5 parts by mass of barium titanate nanoparticles prepared in step (1) were added. The mixture was stirred at 50°C and 400 rpm for 5 hours.

[0186] (3): Keeping the conditions of the reaction system in step (2) unchanged, slowly add 3 parts by mass of tetraethyl orthosilicate to the reaction system in step (2). After the addition is completed, continue stirring at 50°C and 400 rpm for 5 hours to obtain Pickering emulsion.

[0187] (4): Slowly add 10wt% dilute hydrochloric acid to the reaction system in step (3) using a peristaltic pump until the pH of the reaction system is 3.5. Continue stirring at 500 rpm for 4.5 hours at 50°C. Stop stirring and keep the temperature constant for 24 hours. Then filter and wash the solid powder in the reaction system and vacuum dry it at -30°C for 5 hours.

[0188] (5): Add the solid material obtained in step (4) to a Tris buffer solution with a pH of 8.5. The mass ratio of Tris buffer solution to solid powder is 80:1. Then add dopamine hydrochloride to make the concentration of dopamine in the reaction system 6 mg / mL. Stir at 200 rpm for 12 hours at 25°C and then stop stirring. Filter and wash the bottom solid powder and vacuum dry it at -30°C for 5 hours.

[0189] (6): 1.35 parts by mass of anhydrous copper sulfate and 80 parts by mass of deionized water were manually stirred and mixed at room temperature to prepare a copper sulfate solution. 1 part by mass of the solid particles obtained in step (5) and the prepared copper sulfate solution were added to the reactor, the reactor lid was closed, and the mixture was stirred at 300 rpm for 1 h at a temperature of 130°C.

[0190] (7): Add 6 parts by mass of sodium sulfite to 70 parts by mass of pH=5 acetate buffer solution and stir at 200 rpm for 1 h at 50 °C; add the prepared mixed solution to the reaction vessel in step (6), close the vessel lid, stir at 300 rpm for 4 h at 75 °C, and finally filter and wash the bottom solid powder and vacuum dry at -30 °C for 5 h.

[0191] (8): Add 1 part by mass of the solid particles obtained in step (7) to 40 parts by mass of deionized water, then adjust the pH of the system to 10 using dilute potassium hydroxide solution, and stir for 2 hours at 70°C and 200 rpm. Keeping the temperature and stirring conditions unchanged, slowly add 3 parts by mass of chloromethyltriethoxysilane to the reaction system in step (8), and continue stirring for 4 hours. Finally, filter and wash the bottom solid powder, and vacuum dry it for 5 hours at -30°C.

[0192] (9): 6 parts by mass of the smoke-suppressing compound 10-undecenal and methyl nonyl ketone were stirred evenly and then added to 50 parts by mass of the solid material obtained in step (8). Then 1 part by mass of KOH was added and the mixture was refluxed at 95°C for 6 hours. The bottom solid powder was then filtered and washed and vacuum dried at -30°C for 5 hours to obtain the odor-neutralizing temperature-controlled microcapsules. The particle size of the microcapsules was 3.64 to 8.63 μm and the loading of the active smoke-suppressing compound accounted for 12.35 wt% of the total mass of the odor-neutralizing temperature-controlled microcapsules.

[0193] The auxiliary deodorizing agent tris(2-maleimide ethyl)amine, 2,2'-methylenebis(4-ethyl-6-tert-butylphenol), and pentaerythritol distearate diphosphite were mixed in equal mass ratios and dispersed in 1-hydroxyethyl-carboxymethyl-alkylimidazoline. The mixture was stirred at 400 rpm for 1 hour at 25°C. Then, the deodorizing and temperature-controlled microcapsules prepared in step (9) were added, and stirring was continued for another hour to obtain the deodorizing and temperature-controlled asphalt additive. The mass ratio of the auxiliary deodorizing agent, the deodorizing and temperature-controlled microcapsules, and dodecyl dimethyl betaine was 1:2:2.

[0194] Preparation of the asphalt composition:

[0195] Heat 100 parts by weight of base asphalt with a penetration of 52 at 25°C to 143°C, add 1.2 parts by weight of odor-neutralizing and temperature-controlled asphalt additive at a rotation speed of 500 rpm, and stir for 4 hours to obtain odor-neutralizing and temperature-controlled asphalt.

[0196] Comparative Example 1

[0197] The base asphalt control sample can be obtained by heating 100 parts by weight of base asphalt with a penetration of 52 at 25°C to 143°C and stirring at 500 rpm for 4 hours.

[0198] Comparative Example 2

[0199] Preparation of asphalt additives:

[0200] (1): Preparation of barium titanate nanoparticles:

[0201] S1: Weigh 22 parts by weight of tetrabutyl titanate and 15 parts by weight of anhydrous ethanol and add them to a flask. Stir for 2 hours at 50°C and 400 rpm to obtain a titanium precursor solution.

[0202] S2: Slowly add 10wt% ammonia to the S1 solution until the pH of the reaction system is 10.5, and continue stirring at 400 rpm for 2 hours at 50℃ to obtain the titanium precursor sol.

[0203] S3: Add 18.5 parts by weight of Ba(OH)2·H2O and 18.5 parts by weight of deionized water to the reactor, and heat and stir at 400 rpm for 2 hours at 85°C.

[0204] S4: Add the sol obtained in S2 to the reaction vessel in S3, close the reaction vessel lid, heat to 160℃, stir at 400 rpm for 16 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.

[0205] S5: Add 1 part by weight of the primary barium titanate nanoparticles obtained in step S4 and 3 parts by weight of hexadecyltrimethylammonium bromide to 45 parts by weight of dimethylphosphoramide. Modify by stirring at 200 rpm for 5 hours at 140°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 30-50 nm).

[0206] (2): 4 parts by mass of n-dodecane were heated and melted at 50°C, and 60 parts by mass of formamide and 1.5 parts by mass of barium titanate nanoparticles prepared in step (1) were added. The mixture was stirred at 50°C and 400 rpm for 5 hours.

[0207] (3): Keeping the conditions of the reaction system in step (2) unchanged, slowly add 3 parts by mass of tetraethyl orthosilicate to the reaction system in step (2). After the addition is completed, continue stirring at 50°C and 400 rpm for 5 hours to obtain Pickering emulsion.

[0208] (4): Slowly add 10wt% dilute hydrochloric acid to the reaction system in step (3) using a peristaltic pump until the pH of the reaction system is 3.5. Continue stirring at 500 rpm for 4.5 hours at 50°C. Stop stirring and keep the temperature constant for 24 hours. Then filter and wash the solid powder in the reaction system and vacuum dry it at -30°C for 5 hours.

[0209] The auxiliary deodorizing agent hexadecyl maleimide, 2,6-di-tert-butyl-p-methylphenol, and tris(nonylphenol) phosphite were mixed in equal mass ratios and dispersed in dodecyl dimethyl betaine. The mixture was stirred at 400 rpm for 1 hour at 25°C. Then, the solid powder obtained in step (4) was added, and stirring was continued for another 1 hour to obtain the deodorizing and temperature-controlled asphalt additive. The mass ratio of the auxiliary deodorizing agent, the deodorizing and temperature-controlled microcapsules, and the dodecyl dimethyl betaine was 1:1:1.

[0210] Preparation of the asphalt composition:

[0211] Heat 100 parts by weight of base asphalt with a penetration of 52 at 25°C to 143°C, add 1.8 parts by weight of odor-neutralizing and temperature-controlled asphalt additive at a rotation speed of 500 rpm, and stir for 4 hours to obtain odor-neutralizing and temperature-controlled asphalt.

[0212] Test Example 1

[0213] Hydrogen sulfide and benzene compounds are harmful substances that are produced during the service of asphalt pavement and have a significant impact on human health. The asphalt samples prepared in Examples 1-4 and Comparative Examples 1-2 were subjected to flue gas enrichment at a temperature of 168°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.

[0214] Table 1

[0215] Test sample Hydrogen sulfide content, ppm <![CDATA[Benzene series content, mg·m -3 > Example 1 128.11 235.04 Example 2 189.63 295.77 Example 3 174.69 293.80 Example 4 212.92 346.13 Comparative Example 1 582.30 839.42 Comparative Example 2 460.02 693.36

[0216] Test Example 2

[0217] The asphalt samples prepared in Examples 1-4 and Comparative Examples 1-2 were subjected to flue gas enrichment at a temperature of 80°C for 24 hours. After enrichment, the gas in the sealed container was extracted and tested. The data obtained are shown in Table 2 below.

[0218] Table 2

[0219]

[0220]

[0221] 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. A deodorizing and temperature-controlled asphalt additive, characterized in that, The odor-neutralizing and temperature-controlled asphalt additive comprises the following components by weight: Deodorizing agent, 1-5 parts; Dispersant, 1-10 parts; Odor-neutralizing and temperature-controlled microcapsules, 1-5 servings; The odor-neutralizing and temperature-controlled microcapsule comprises a composite shell and a core material. The composite shell comprises an inorganic base shell, barium titanate nanoparticles, polydopamine, and cuprous oxide. The core material comprises n-alkanes with a phase transition temperature of 40-60°C. The surface of the composite shell is loaded with an active smoke-suppressing compound.

2. The odor-neutralizing and temperature-controlled asphalt additive according to claim 1, characterized in that, The auxiliary deodorizing agent is selected from one or more imide compounds with a molecular weight greater than 170 and antioxidants with a molecular weight greater than 200.

3. The odor-neutralizing and temperature-controlled asphalt additive according to claim 1, characterized in that, The dispersant is one or more of dodecyl dimethyl betaine and 1-hydroxyethyl-carboxymethyl-alkyl imidazoline.

4. The odor-neutralizing and temperature-controlled asphalt additive according to claim 1, characterized in that, The particle size of the odor-neutralizing and temperature-controlled microcapsules is 1-12 μm; And / or, the mass ratio of the composite shell material to the core material of the odor-neutralizing and temperature-controlled microcapsule 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 is 1:(0.2-0.8), the mass ratio of the inorganic base shell to the polydopamine is 1:(0.1-0.5), and the mass ratio of the inorganic base shell to the cuprous oxide is 1:(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; And / or, the n-alkane with a phase transition temperature of 40-60°C is one or more of n-octadecane, n-eicosane, and n-docosahexadecane; And / or, the loading of the active smoke-suppressing compound accounts for 0.1wt%-20wt% of the total mass of the odor-neutralizing and temperature-controlled microcapsules; And / or, the active smoke-suppressing compound is selected from one or more aldehyde compounds with a molecular weight greater than 160 and ketone compounds with a molecular weight greater than 150.

5. A method for preparing the odor-neutralizing and temperature-controlled asphalt additive according to any one of claims 1-4, comprising: The auxiliary odor neutralizer is added to the dispersant, stirred for the first time, and then the prepared odor neutralizing and temperature-controlled microcapsules are added. After stirring for the second time, the asphalt additive is obtained.

6. The method according to claim 5, 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.

7. The method according to claim 5, characterized in that, The method for preparing the odor-neutralizing and temperature-controlled microcapsules includes: (1) Preparation of barium titanate nanoparticles; (2) Heat the core material raw material to melt, and mix it with solvent and barium titanate nanoparticles obtained in step (1); (3) Add the inorganic base shell precursor to the reaction system of step (2), stir and mix to obtain Pickering emulsion; (4) Adjust the pH value of the Pickering emulsion, continue stirring, then age, filter, wash, and freeze dry; (5) Add the solid material obtained in step (4) to the buffer solution, add dopamine hydrochloride, stir and process, then filter, wash and freeze dry; (6) Add the solid particles and copper ion solution obtained in step (5) into the reaction vessel and carry out the reaction with stirring; (7) Mix the reducing agent with the buffer solution, stir to dissolve, and then add it to the reaction system of step (6). Stir to carry out the reaction, then filter, wash, and freeze dry. (8) Mix the solid particles obtained in step (7) with water, adjust the pH, and then heat and stir; then add silane coupling agent, continue to react under stirring, and then filter, wash and freeze dry. (9) The solid material obtained in step (8), the active smoke-suppressing compound, and the strong alkali are added to an organic solvent to react. After cooling, filtering, washing, and freeze-drying, the odor-neutralizing temperature-controlled microcapsules are obtained.

8. The method according to claim 7, 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.

9. The method according to claim 8, 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.

10. The method according to claim 8, 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.

11. The method according to claim 8, 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.

12. The method according to claim 8, 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.

13. The method according to claim 8, 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.

14. The method according to claim 7, characterized in that, In step (2), 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 (2), the mass ratio of the solvent to the barium titanate nanoparticles is (20-80):1; And / or, in step (2), the stirring speed is 400-600 rpm, the stirring temperature is 40-80℃, and the stirring time is 4-6 hours.

15. The method according to claim 7, characterized in that, In step (3), 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 preferably at least one of methyl silicate, tetraethyl orthosilicate, tetraethyl orthosilicate, and tetrabutyl orthosilicate. And / or, in step (3), the stirring speed is 400-600 rpm, the stirring temperature is 40-80℃, and the stirring time is 4-6 hours.

16. The method according to claim 7, characterized in that, In step (4), adjust the pH value to 3-6; And / or, in step (4), the stirring speed is 400-600 rpm, the stirring temperature is 40-80℃, and the stirring time is 4-6 hours; And / or, in step (4), the aging conditions are: standing at 40-80°C for 12-30 hours.

17. The method according to claim 7, characterized in that, In step (5), the buffer solution is one or more of phosphate buffer, carbonate buffer, and tris(hydroxymethyl)aminomethane hydrochloride buffer; And / or, in step (5), the pH value of the buffer solution is 8-10; And / or, in step (5), the mass ratio of the buffer solution to the solid material obtained in step (4) is (10-100):1; And / or, in step (5), after adding dopamine hydrochloride, the mass concentration of dopamine in the reaction system is 2-10 mg / mL; And / or, in step (5), the stirring speed is 100-300 rpm, the stirring temperature is 20-40℃, and the stirring time is 12-24 hours.

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

19. The method according to claim 7, characterized in that, In step (7), the reducing agent is a sulfite reducing agent, preferably selected from at least one of potassium sulfite and sodium sulfite; the pH value of the buffer solution is 4.5-6.5; And / or, in step (7), the mass ratio of the reducing agent to the buffer solution is 1:(10-20); And / or, in step (7), when stirring to dissolve, the stirring speed is 200-450 rpm, the stirring temperature is 40-80℃, and the stirring time is 1-5 hours; And / or, in step (7), the stirring speed is 100-450 rpm, the reaction temperature is 60-95°C, and the reaction time is 2-5 hours.

20. The method according to claim 7, characterized in that, In step (8), the stirring speed is 300-500 rpm, the stirring temperature is 20-90℃, and the stirring time is 1-6h; And / or, in step (8), adjust the pH to 9-11; And / or, in step (8), the mass ratio of the solid particles obtained in step (7) to water is 1:(10-50); And / or, in step (8), the added silane coupling agent is selected from one or more of chloropropyltriethoxysilane, chloromethyltriethoxysilane, dichloromethyltriethoxysilane, and chloromethyltriisopropoxysilane; And / or, in step (8), the mass ratio of the solid particles obtained in step (7) to the silane coupling agent is 1:(0.5-4); And / or, in step (8), the stirring speed is 300-500 rpm, the stirring temperature is 20-90℃, and the stirring time is 1-8h.

21. The method according to claim 7, characterized in that, In step (9), the organic solvent is selected from one or more of methanol, butanediol, ethylene glycol, n-butanol, and ethanol; And / or, in step (9), the mass ratio of the solid material obtained in step (8) to the organic solvent is 1:(20-80); the mass ratio of the solid material obtained in step (8) to the strong alkali is 1:(0.5-2); And / or, in step (9), the reaction conditions are: a reaction temperature of 80-210℃ and a reaction time of 5-10 hours.

22. An asphalt composition, comprising, by weight, the following components: 50-200 parts of base bitumen; The odor-neutralizing and temperature-controlled asphalt additive according to any one of claims 1-4 is used in an amount of 0.1-20 parts, preferably 1.5-5 parts.

23. A method for preparing the asphalt composition of claim 22, comprising: The base asphalt is heated to a molten state, and then a neutral-odor asphalt additive is added while stirring to obtain an asphalt composition.

Images