Nettaste temperature control asphalt additive, net taste temperature control asphalt and preparation method thereof

Abstract

The application discloses a kind of net taste temperature control asphalt additives, net taste temperature control asphalt and preparation method thereof.Net taste temperature control asphalt additives of the application includes the following components by weight parts: net taste temperature control microcapsule, 1-5 parts;Auxiliary odor control agent, 1-5 parts;Dispersing agent, 1-5 parts;The net taste temperature control microcapsule includes composite shell material and core material, wherein the composite shell material includes silicon dioxide / nano tourmaline / polydopamine, the core material includes n-alkane with phase transition temperature of 40-60 ℃, and the surface of the composite shell material is loaded with metal chelate and smoke suppression compound containing active alpha-H.Net taste temperature control asphalt additive of the application can efficiently and durably reduce the content of irritating gas in asphalt fumes, reduce the content of volatile organic compounds released at high temperature of asphalt pavement, improve the high-temperature stability of asphalt, and prolong the service life of asphalt pavement, providing a new idea for the long-life and environmentally friendly use of asphalt.

Description

Technical Field

[0001] This invention belongs to the field of special asphalt, specifically relating to an odor-neutralizing and temperature-controlled asphalt additive, odor-neutralizing and temperature-controlled asphalt, and its preparation method. Background Technology

[0002] Currently, asphalt roads are the main type of transportation road due to their advantages such as good road performance, high smoothness, low road noise, and ease of production. However, asphalt faces many problems in production, construction, storage, transportation, and pavement application. For example, the hot-mix and hot-pavement process used in asphalt construction easily generates toxic, harmful, and irritating fumes, affecting the ecological environment and threatening human health. Asphalt has a strong heat absorption capacity; under intense sunlight, the temperature of asphalt pavement can rapidly rise to high levels, causing softening, rutting, swelling, bleeding, and other defects, reducing the service life of the asphalt. It also leads to the release of volatile organic compounds, resulting in smog and photochemical smog, impacting the ecological environment and human health. Furthermore, high-temperature asphalt pavements continuously release large amounts of heat into the environment, exacerbating the urban heat island effect.

[0003] Currently, existing technologies generally address these problems by adding admixtures to asphalt, with phase change materials (PCMs) and neutralizing agents being the two most commonly used. Adding PCMs to the asphalt system can mitigate a series of problems caused by the endothermic heating of asphalt. However, asphalt materials produced using this method often suffer from poor compatibility between the PCMs and asphalt, significantly affecting the basic properties of the asphalt. Furthermore, this method only reduces the amount of volatile organic compounds (VOCs) released from asphalt pavements under high-temperature conditions to a certain extent, and does not reduce the amount of smoke generated during asphalt construction. Adding neutralizing agents to asphalt allows them to react with the volatile light components in the asphalt to generate macromolecular compounds, reducing the amount of smoke generated during asphalt construction to some extent. However, this method only reduces the amount of smoke generated during asphalt construction, not the amount of VOCs released from asphalt pavements under high temperatures. Moreover, the macromolecular compounds generated after the neutralizing agents react with the light components in the asphalt are still relatively unstable: on the one hand, during the thermal storage of asphalt, the molecular chains of these macromolecular compounds may break, causing the light components to detach and subsequently volatilize upon heating, producing asphalt fumes. On the other hand, these macromolecular compounds may directly volatilize and generate asphalt fumes after coming into contact with high-temperature aggregates during asphalt mixing and construction. Summary of the Invention

[0004] To address the problems existing in the prior art, this invention provides an odor-neutralizing and temperature-controlled asphalt additive, odor-neutralizing and temperature-controlled asphalt, 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, achieves a triple objective by utilizing the temperature-controlling effect of the microcapsules and the odor-neutralizing effect of the active odor-neutralizing components on their surface. This results in a significant and lasting reduction in the content of irritating gases in asphalt fumes, a reduction in the content of volatile organic compounds released at high temperatures from asphalt pavements, and an improvement in the high-temperature stability of asphalt, thereby extending the service life of asphalt pavements. This provides a novel approach to extending the lifespan and environmentally friendly utilization of asphalt.

[0005] The first aspect of this invention provides a odor-neutralizing and temperature-controlled asphalt additive, comprising the following components by weight:

[0006] Odor-neutralizing and temperature-controlled microcapsules, 1-5 servings;

[0007] Deodorizing agent, 1-5 parts;

[0008] Dispersant, 1-5 parts;

[0009] The odor-neutralizing and temperature-controlled microcapsule comprises a composite shell and a core material. The composite shell comprises silica / nano-tourmaline / polydopamine, and the core material comprises n-alkanes with a phase transition temperature of 40-60℃. The surface of the composite shell is loaded with metal chelates and smoke-suppressing compounds containing active α-H.

[0010] Furthermore, the auxiliary deodorizing agent is selected from one or more phosphite antioxidants with a boiling point greater than 220°C.

[0011] Furthermore, the phosphite antioxidant with a boiling point greater than 220°C is selected from one or more of the following: tris(2,4-di-tert-butylphenyl) phosphite, 3,9-bis(2,4-di-tert-butylphenoxy)-2,4,8,10-tetraoxa-3,9-bis(5.5)undecane, tris(nonylphenol) phosphite, antioxidant 1500 (4,4'-p-isopropyldiphenyl C12-15-ol phosphite), and pentaerythritol distearate diphosphite.

[0012] Furthermore, the dispersant is selected from one or more of dodecyl dimethyl betaine and 1-hydroxyethyl-carboxymethyl-alkyl imidazoline.

[0013] Furthermore, the particle size of the odor-neutralizing and temperature-controlled microcapsules is 1-5 μm.

[0014] Furthermore, the mass ratio of the composite shell material to the core material of the odor-neutralizing and temperature-controlled microcapsule is 1:(0.5-2).

[0015] Furthermore, the composite shell material of the odor-neutralizing and temperature-controlled microcapsule comprises silica / nano-tourmaline / polydopamine, wherein the mass ratio of silica to nano-tourmaline is (1-5):1, and the mass ratio of silica to polydopamine is 1:(0.1-0.5).

[0016] Furthermore, the n-alkane with a phase transition temperature of 40-60°C is one or more of n-octadecane, n-eicosane, and n-docosahexadecane, preferably n-docosahexadecane.

[0017] Furthermore, the surface of the composite shell material is loaded with a metal chelate, wherein the metal is preferably copper.

[0018] Furthermore, the shell material surface is loaded with metal chelates and smoke-suppressing compounds containing active α-H, with the metal loading accounting for 0.1wt%-15wt% of the total mass of the odor-neutralizing and temperature-controlled microcapsules; and the loading of smoke-suppressing compounds containing active α-H accounting for 0.1wt%-20wt% of the total mass of the odor-neutralizing and temperature-controlled microcapsules.

[0019] Furthermore, the smoke-suppressing compound containing active α-H is selected from one or more aldehyde compounds with more than 9 carbon atoms or ketone compounds with more than 8 carbon atoms.

[0020] Furthermore, the aldehyde compounds with more than 9 carbon atoms are selected from one or more of the following: o-methylcinnamaldehyde, p-methylcinnamaldehyde, anisaldehyde, 2-methylundecaldehyde, 10-undecenaldehyde, ethyl vanillin, benzaldehyde, phenylacetaldehyde, p-hydroxybenzaldehyde, butylphenyl methylpropanal, neraldehyde, hydroxymethylpentylcyclohexene acetal, 3-(4-ethylphenyl)-2,2-dimethylpropanal, vanillin propylene glycol acetal, methylhexylcinnamaldehyde, methylpentylcinnamaldehyde, and diethylaminobenzaldehyde.

[0021] Furthermore, the ketone compound having more than 8 carbon atoms is selected from one or more of carvone, 3-hydroxy-2-butanone, 2,3-butanedione-3-penten-2-one, and 6-methyl-3,5-heptadien-2-one.

[0022] Furthermore, the preparation method of the odor-neutralizing and temperature-controlled microcapsules includes the following steps:

[0023] S1: Nano tourmaline, surfactant and solvent are mixed and modified under stirring. After modification, the mixture is washed and freeze-dried to obtain modified nano tourmaline.

[0024] S2: Heat the core material raw material to melt, then add the solvent and the modified nano-tourmaline obtained in step S1, and stir to mix;

[0025] S3: Add silica precursor to the reaction system of step S2, stir and mix to obtain Pickering emulsion;

[0026] S4: Adjust the pH of the Pickering emulsion obtained in step S3 to 2-5, stir and then age, filter, wash and freeze dry;

[0027] S5: Add the solid powder obtained in step S4 to the buffer solution, add dopamine hydrochloride, stir and process, then filter, wash and freeze dry;

[0028] S6: Add the solid powder obtained in step S5, the smoke suppressant compound containing active α-H, and the strong base to an organic solvent, react under reflux conditions, cool, filter, wash, and freeze-dry.

[0029] S7: The solid powder obtained in step S6 is ultrasonically dispersed in a metal ion salt-formamide solution and reacted under stirring. After the reaction is completed, the powder is filtered, washed, and freeze-dried to obtain the odor-neutralizing temperature-controlled microcapsules.

[0030] Furthermore, in step S1, the diameter of the nano-tourmaline is 10-100 nm.

[0031] Further, in step S1, 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.

[0032] Further, in step S1, 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.

[0033] Further, in step S1, the mass ratio of the nano-tourmaline to the surfactant is (1-10):1, and the mass ratio of the solvent to the surfactant is (5-50):1.

[0034] Further, in step S1, the stirring speed is 200-500 rpm; the modification temperature is 100-190℃; and the modification time is 2-5 hours.

[0035] Furthermore, in step S1, the freeze-drying conditions are: vacuum drying for 4-8 hours at a temperature of -40°C to -20°C.

[0036] Furthermore, in step S2, the core material raw material is heated to a melting temperature of 40-60°C.

[0037] Further, in step S2, 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.

[0038] Further, in step S2, the mass ratio of the core material raw material to the modified nano-tourmaline is (1-10):1, and the mass ratio of the solvent to the modified nano-tourmaline is (20-80):1.

[0039] Furthermore, in step S2, the stirring speed is 400-600 rpm, the stirring temperature is 40-60℃, and the stirring time is 4-6 hours.

[0040] Further, in step S3, the silica precursor is a silicate compound, preferably at least one of methyl silicate, ethyl orthosilicate, tetraethyl orthosilicate, and butyl orthosilicate, and more preferably ethyl orthosilicate.

[0041] Further, in step S3, the mass ratio of the core material raw material to the silicon dioxide precursor is (0.5-1.5):1.

[0042] Furthermore, in step S3, the stirring speed is 400-600 rpm, the stirring temperature is 40-60℃, and the stirring time is 4-6 hours.

[0043] Furthermore, in step S4, pH can be adjusted by adding dilute acid, such as dilute hydrochloric acid.

[0044] Furthermore, in step S4, the stirring speed is 400-600 rpm, the stirring temperature is 40-60℃, and the stirring time is 4-6 hours.

[0045] Further, in step S4, 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.

[0046] Further, in step S5, 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).

[0047] Furthermore, in step S5, the pH value of the buffer solution is preferably 8-10.

[0048] Further, in step S5, the mass ratio of the buffer solution to the solid powder obtained in step S4 is (10-100):1.

[0049] Furthermore, in step S5, after adding dopamine hydrochloride, the mass concentration of dopamine in the reaction system is 2-10 mg / mL.

[0050] Furthermore, in step S5, the stirring speed is 100-300 rpm, the stirring temperature is 20-40℃, and the stirring time is 12-24 hours.

[0051] Furthermore, in step S5, the freeze-drying conditions are: vacuum drying for 4-8 hours at a temperature of -40°C to -20°C.

[0052] Further, in step S6, the organic solvent is selected from one or more of methanol, butanediol, ethylene glycol, n-butanol, and anhydrous ethanol, preferably anhydrous ethanol.

[0053] Further, in step S6, the mass ratio of the solid powder obtained in step S5 to the smoke-suppressing compound containing active α-H is 1:(10-40). The mass ratio of the solid powder obtained in step S5 to the organic solvent is 1:(20-80). The mass ratio of the solid powder obtained in step S5 to the strong base is 1:(0.5-2).

[0054] Furthermore, in step S6, the strong alkali is either solid KOH or solid NaOH, preferably solid KOH.

[0055] Furthermore, in step S6, the reaction conditions for heating and reflux are: a reaction temperature of 80-220℃ and a reaction time of 5-10 hours.

[0056] Furthermore, in step S6, the freeze-drying conditions are: vacuum drying for 4-8 hours at a temperature of -40°C to -20°C.

[0057] Further, in step S7, the metal ion salt is preferably a copper ion salt, and more preferably anhydrous copper sulfate.

[0058] Further, in step S7, the mass ratio of the metal ion salt to formamide in the metal ion salt-formamide solution is (0.5-1.5):1.

[0059] Further, in step S7, the mass ratio of the metal ion salt-formamide solution to the solid powder obtained in step S6 is (5-30):1.

[0060] Furthermore, in step S7, the stirring speed is 200-450 rpm, the reaction temperature is 100-190℃, and the reaction time is 2-5 hours.

[0061] Furthermore, in step S7, the freeze-drying conditions are: vacuum drying for 4-8 hours at a temperature of -40°C to -20°C.

[0062] Furthermore, the auxiliary deodorizing agent is added to the dispersant and stirred at 400-500 rpm for 1-3 hours at 25-45℃. Then, deodorizing and temperature-controlled microcapsules are added, and stirring is continued for 1-2 hours to obtain the deodorizing and temperature-controlled asphalt additive.

[0063] A second aspect of the present invention provides an odor-neutralizing and temperature-controlled asphalt, comprising the following components by weight:

[0064] Base bitumen, 50-500 parts;

[0065] The above-mentioned odor-neutralizing and temperature-controlled asphalt additive, 1-50 parts.

[0066] Furthermore, the base asphalt is commercially available No. 50, No. 70 and No. 90 road asphalt, preferably No. 70 Grade A asphalt.

[0067] Further, heat the base asphalt to 133-153℃, add the odor-neutralizing and temperature-controlled asphalt additive at a speed of 400-600 rpm, and stir for 2-4 hours to obtain the odor-neutralizing and temperature-controlled asphalt.

[0068] Compared with the prior art, the present invention has the following advantages:

[0069] (1) The odor-neutralizing and temperature-controlled microcapsules in the odor-neutralizing and temperature-controlled asphalt additive of the present invention have a composite shell material with three functions. The first function is that during the preparation process, nano-tourmaline serves as a template agent for the synthesis of microcapsules, which can maintain the stability of n-alkane droplets. The second function is that during the metal ion modification process of the microcapsule composite shell material, the negative ion field released by nano-tourmaline under high temperature conditions is used to adsorb a large number of metal ions onto the surface of the microcapsules, effectively increasing the metal ion loading of the microcapsule shell material and further enhancing the smoke suppression ability of the odor-neutralizing and temperature-controlled microcapsules. The third function is that during the asphalt heat storage, mixing, and road use processes, under high temperature, the nano-tourmaline contained inside the odor-neutralizing and temperature-controlled microcapsule shell material will release a negative ion field, further attracting the compounds released by the asphalt under high temperature to the vicinity of the odor-neutralizing and temperature-controlled microcapsules. While increasing the difficulty of volatilization of these compounds, it can also cause the metal ions and smoke suppression compounds on the surface of the microcapsules to react with more of the above compounds, thereby effectively reducing the impact of irritating gases released during asphalt mixing and asphalt pavement service on the human body.

[0070] (2) The odor-neutralizing and temperature-controlled microcapsules of the present invention have a large number of active sites on the surface of their polydopamine shell. These active sites can undergo a Michael addition reaction with the smoke-suppressing compound containing active α-H as described in the present invention, so that the smoke-suppressing compound containing active α-H is firmly fixed on the surface of the microcapsule, preventing its physical migration and volatilization, and further enhancing the binding ability of the microcapsule with asphalt. This improves the storage stability of the odor-neutralizing and temperature-controlled asphalt without affecting other properties of the asphalt. In addition, after reacting with the smoke-suppressing compound containing active α-H, a large number of catechol groups are generated on the surface of the polydopamine, providing a large number of active sites for the subsequent chelation of metal ions.

[0071] (3) The odor-neutralizing and temperature-controlled microcapsule of the present invention has the disadvantages of poor odor-neutralizing effect, poor storage stability and poor high temperature stability of the chemical odor-neutralizing agent used in traditional odor-neutralizing asphalt. The smoke-suppressing compound containing α-H modified by chemical reaction on its surface has extremely strong stability because it is connected to the microcapsule wall material. It will not volatilize or degrade due to high temperature, thus reducing the odor-neutralizing effect.

[0072] (4) The odor-neutralizing and temperature-controlled microcapsules of the present invention have a large number of metal ions modified on their surface through chelation. These metal ions have empty orbitals. After the microcapsules enter the asphalt system, the metal ions can directly accept the unshared electrons of some more active sulfur-containing and nitrogen-containing pollutants with irritating odors in the asphalt and form coordinate bonds, thus stably fixing the above compounds on the surface of the microcapsules. This effectively prevents them from volatilizing into the air under high temperature conditions, further reducing the harm of asphalt fumes to the environment and human body.

[0073] (5) The odor-neutralizing and temperature-controlled asphalt additive of the present invention can regulate the temperature of the road surface in situ, which can not only effectively improve the high-temperature performance of asphalt, but also reduce the damage to the road surface caused by temperature changes and extend the service life of asphalt pavement.

[0074] (6) The odor-neutralizing and temperature-controlled asphalt additive of the present invention can reduce the road surface temperature without affecting the low-temperature performance of the road surface after being added to the asphalt material. It can not only effectively reduce the urban heat island effect, but also prevent the asphalt road surface from releasing volatile organic compounds due to excessive temperature, thereby avoiding the generation of photochemical smog and haze. Attached Figure Description

[0075] Figure 1 It is the odor-neutralizing and temperature-controlled microcapsule obtained in Example 1 of this invention;

[0076] Figure 2 These are the temperature control performance test data of the odor-free temperature-controlled asphalt and the base asphalt obtained in Example 1 and Comparative Example 6 of this invention. Detailed Implementation

[0077] To further illustrate the technical solution of the present invention, the present invention will be clearly and thoroughly described below in conjunction with embodiments.

[0078] The odor-neutralizing and temperature-controlled microcapsules of this invention were subjected to morphological testing using a scanning electron microscope with an accelerating voltage of 20kV. Since the microcapsule wall material is non-conductive, the samples need to be sputter-coated with gold before testing.

[0079] The surface elemental analysis of the odor-neutralizing and temperature-controlled microcapsules described in this invention was performed using an X-ray energy dispersive spectroscopy (EDS) instrument to confirm that metal ions were successfully modified onto the surface of the microcapsules. The sulfides in the odor-neutralizing asphalt flue gas described in this invention were tested using gas chromatography according to the national standard GB / T 14678-1993, "Determination of Hydrogen Sulfide, Methanethiol, Dimethyl Sulfide and Dimethyl Disulfide in Air Quality," using an Agilent 7890 gas chromatograph.

[0080] The base asphalt used in the following examples and comparative examples is Sinopec Donghai brand No. 70 Grade A asphalt.

[0081] Example 1

[0082] S1: Add 90nm nano-tourmaline, hexadecyltrimethylammonium bromide and formamide to the first container in a mass ratio of 5:1:50. Stir at 180℃ and 400 rpm for 5 hours, then wash with ethanol multiple times and vacuum dry at -30℃ for 5 hours to obtain modified nano-tourmaline for later use.

[0083] S2: Add n-dodecane to the second container and heat it to melt at 50°C. Then add formamide and the modified nano-tourmaline obtained in step S1. The mass ratio of n-dodecane, modified nano-tourmaline obtained in step S1 and formamide is 4:1:50. Stir for 5 hours at 50°C and 400 rpm.

[0084] S3: Add tetraethyl orthosilicate to the reaction system of step S2. The mass ratio of n-dodecane to tetraethyl orthosilicate is 1:1. Continue stirring at 400 rpm for 5 hours at 50°C to obtain Pickering emulsion.

[0085] S4: Slowly add 10wt% dilute hydrochloric acid to the reaction system in step S3 using a peristaltic pump until the pH of the reaction system is 4. Continue stirring at 400 rpm for 5 hours at 50°C, then stop stirring and age at the same temperature for 24 hours. After that, filter and wash the solid powder in the reaction system and vacuum dry it at -30°C for 5 hours.

[0086] S5: Add the solid powder obtained in step S4 to Tris buffer solution with a pH of 8.5. The mass ratio of Tris buffer solution to solid powder is 50:1. Then add dopamine hydrochloride to make the concentration of dopamine in the reaction system 4 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.

[0087] S6: Mix the smoke-suppressing compounds 2-methylundecaldehyde, 10-undecenaldehyde, carvone, and 3-hydroxy-2-butanone in equal mass ratio by hand until homogeneous. Then add the solid powder obtained in step S5, anhydrous ethanol, and solid KOH. The mass ratio of the solid powder obtained in step S5 to the smoke-suppressing compound, anhydrous ethanol, and KOH is 1:20:40:1. React under reflux at 90°C for 6 hours. Then filter and wash the bottom solid powder and vacuum dry it at -30°C for 5 hours.

[0088] S7: The solid powder obtained in step S6 was ultrasonically dispersed in a 50 wt% anhydrous copper sulfate-formamide solution. The mass ratio of the solid powder to the anhydrous copper sulfate-formamide solution was 1:30. The mixture was stirred at 400 rpm and 140°C for 2 hours. After the reaction was completed, the bottom solid powder was filtered and washed, and then vacuum dried at -30°C for 5 hours to obtain the deodorizing and temperature-controlled microcapsules. The electron micrograph is shown below. Figure 1 .

[0089] Add the auxiliary deodorizing agent and antioxidant 1500 to dodecyl dimethyl betaine, and stir at 300 rpm for 3 hours at 45°C. Then add the deodorizing and temperature-controlled microcapsules prepared above, and continue stirring for 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 is 1:1:1.

[0090] Heat 50 parts by weight of base asphalt to 143°C, add 6 parts by weight of odor-neutralizing and temperature-controlled asphalt additive at a speed of 500 rpm, and stir for 4 hours to obtain odor-neutralizing and temperature-controlled asphalt.

[0091] Example 2

[0092] Except that the smoke-suppressing compounds in step S6 are neraldehyde, anisaldehyde, 2,3-butanedione, 3-penten-2-one, and 6-methyl-3,5-heptadien-2-one in equal mass ratios, the rest are the same as in Example 1.

[0093] Example 3

[0094] Except that the auxiliary deodorizing agent used in the preparation of the deodorizing and temperature-controlled asphalt additive is tris(nonylphenol) phosphite, the rest is the same as in Example 1.

[0095] Example 4

[0096] Except for step S2, where the mass ratio of n-dodecane, the modified nano-tourmaline obtained in step S1, and formamide is 6:1:50, the rest is the same as in Example 1.

[0097] Example 5

[0098] Except for step S7, where the mass ratio of solid powder to anhydrous copper sulfate-formamide solution is 1:20, the rest is the same as in Example 1.

[0099] Example 6

[0100] Except for step S6, in which the mass ratio of the solid powder, smoke suppressant compound, anhydrous ethanol, and KOH obtained in step S5 is 1:10:40:1, the rest is the same as in Example 1.

[0101] Example 7

[0102] When using the deodorizing and temperature-controlled asphalt additive, the mass ratio of the auxiliary deodorizing agent, deodorizing and temperature-controlled microcapsules, and dodecyl dimethyl betaine is 2.5:1:2.5, and the rest is the same as in Example 1.

[0103] Comparative Example 1

[0104] Steps S1-S6 are the same as in Example 1, except that step S7 is omitted, and the solid powder obtained in step S6 is directly used to prepare a odor-neutralizing and temperature-controlled asphalt additive, as follows:

[0105] Add the auxiliary deodorizing agent and antioxidant 1500 to dodecyl dimethyl betaine, and stir and mix at 300 rpm for 3 hours at 45°C. Then add the solid powder obtained in step S6, and continue stirring for 1 hour to obtain the deodorizing and temperature-controlled asphalt additive. The mass ratio of the auxiliary deodorizing agent, the solid powder obtained in S6, and dodecyl dimethyl betaine is 1:1:1.

[0106] Heat 50 parts by weight of base asphalt to 143°C, add 6 parts by weight of odor-neutralizing and temperature-controlled asphalt additive at a speed of 500 rpm, and stir for 4 hours to obtain odor-neutralizing and temperature-controlled asphalt.

[0107] Comparative Example 2

[0108] S1: Add 90nm nano-tourmaline, hexadecyltrimethylammonium bromide and formamide to the first container in a mass ratio of 5:1:50. Stir at 180℃ and 400 rpm for 5 hours, then wash with ethanol multiple times and vacuum dry at -30℃ for 5 hours to obtain modified nano-tourmaline for later use.

[0109] S2: Add n-dodecane to the second container and heat it to melt at 50°C. Then add formamide and the modified nano-tourmaline obtained in step S1. The mass ratio of n-dodecane, modified nano-tourmaline obtained in step S1 and formamide is 4:1:50. Stir for 5 hours at 50°C and 400 rpm.

[0110] S3: Add tetraethyl orthosilicate to the reaction system of step S2. The mass ratio of n-dodecane to tetraethyl orthosilicate is 1:1. Continue stirring at 400 rpm for 5 hours at 50°C to obtain Pickering emulsion.

[0111] S4: Slowly add 10wt% dilute hydrochloric acid to the reaction system in step S3 using a peristaltic pump until the pH of the reaction system is 4. Continue stirring at 400 rpm for 5 hours at 50°C, then stop stirring and age at the same temperature for 24 hours. After that, filter and wash the solid powder in the reaction system and vacuum dry it at -30°C for 5 hours.

[0112] S5: Add the solid powder obtained in step S4 to Tris buffer solution with a pH of 8.5. The mass ratio of Tris buffer solution to solid powder is 50:1. Then add dopamine hydrochloride to make the concentration of dopamine in the reaction system 4 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.

[0113] S6: The solid powder obtained in step S5 is ultrasonically dispersed in a 50wt% anhydrous copper sulfate-formamide solution. The mass ratio of the solid powder to the anhydrous copper sulfate-formamide solution is 1:30. The mixture is stirred and reacted at 400 rpm and 140°C for 2 hours. After the reaction is completed, the bottom solid powder is filtered and washed, and then vacuum dried at -30°C for 5 hours to obtain the odor-neutralizing and temperature-controlled microcapsules.

[0114] Add the auxiliary deodorizing agent and antioxidant 1500 to dodecyl dimethyl betaine, and mix at 300 rpm for 3 hours at 45°C. Then add the deodorizing and temperature-controlled microcapsules and continue mixing for 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 is 1:1:1.

[0115] Heat 50 parts by weight of base asphalt to 143°C, add 6 parts by weight of odor-neutralizing and temperature-controlled asphalt additive at a speed of 500 rpm, and stir for 4 hours to obtain odor-neutralizing and temperature-controlled asphalt.

[0116] Comparative Example 3

[0117] The method for preparing the odor-neutralizing and temperature-controlled microcapsules is the same as in Example 1.

[0118] The odor-neutralizing and temperature-controlled asphalt additive is prepared by stirring the auxiliary odor neutralizer and antioxidant 1500 with the above-mentioned odor-neutralizing and temperature-controlled microcapsules at 45°C and 300 rpm for 1 hour. The mass ratio of the auxiliary odor neutralizer to the odor-neutralizing and temperature-controlled microcapsules is 1:1.

[0119] Heat 50 parts by weight of base asphalt to 143°C, add 4 parts by weight of odor-neutralizing and temperature-controlled asphalt additive at a speed of 500 rpm, and stir for 4 hours to obtain odor-neutralizing and temperature-controlled asphalt.

[0120] Comparative Example 4

[0121] When preparing the odor-neutralizing and temperature-controlled microcapsules, steps S5-S7 are omitted, and steps S1-S4 are the same as in Example 1, to obtain a solid powder.

[0122] Add the auxiliary deodorizing agent and antioxidant 1500 to dodecyl dimethyl betaine, and stir and mix at 300 rpm for 3 hours at 45°C. Then add the solid powder obtained from S4, and continue stirring for 1 hour to obtain the deodorizing and temperature-controlled asphalt additive. The mass ratio of the auxiliary deodorizing agent, the solid powder obtained from S4, and dodecyl dimethyl betaine is 1:1:1.

[0123] Heat 50 parts by weight of base asphalt to 143°C, add 6 parts by weight of odor-neutralizing and temperature-controlled asphalt additive at a speed of 500 rpm, and stir for 4 hours to obtain odor-neutralizing and temperature-controlled asphalt.

[0124] Comparative Example 5

[0125] S1: Add n-dodecane to the container and heat it to melt at 50°C. Then add formamide and hexadecyltrimethylammonium bromide. The mass ratio of n-dodecane, hexadecyltrimethylammonium bromide and formamide is 4:1:50. Stir for 5 hours at 50°C and 400 rpm.

[0126] S2: Add tetraethyl orthosilicate to the reaction system of step S1. The mass ratio of n-dodecane to tetraethyl orthosilicate is 1:1. Continue stirring at 400 rpm for 5 hours at 50°C to obtain Pickering emulsion.

[0127] S3: Slowly add 10wt% dilute hydrochloric acid to the reaction system in step S2 using a peristaltic pump until the pH of the reaction system is 4. Continue stirring at 400 rpm for 5 hours at 50°C, then stop stirring and age at the same temperature for 24 hours. After that, filter and wash the solid powder in the reaction system and vacuum dry it at -30°C for 5 hours.

[0128] S4: Add the solid powder obtained in step S3 to Tris buffer solution with a pH of 8.5. The mass ratio of Tris buffer solution to solid powder is 50:1. Then add dopamine hydrochloride to make the concentration of dopamine in the reaction system 4 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.

[0129] S5: Mix the smoke-suppressing compounds 2-methylundecaldehyde, 10-undecenaldehyde, carvone, and 3-hydroxy-2-butanone in equal mass ratio by hand until homogeneous. Then add the solid powder obtained in S4, anhydrous ethanol, and KOH. The mass ratio of the solid powder obtained in S4, the smoke-suppressing compound, anhydrous ethanol, and KOH is 1:20:40:1. Further react under reflux at 90°C for 6 hours. Then filter and wash the bottom solid powder and vacuum dry it at -30°C for 5 hours.

[0130] S6: The solid powder obtained in step S5 is ultrasonically dispersed in a 50wt% anhydrous copper sulfate-formamide solution. The mass ratio of the solid powder to the anhydrous copper sulfate-formamide solution is 1:30. The mixture is stirred and reacted at 400 rpm and 140°C for 2 hours. After the reaction is completed, the bottom solid powder is filtered and washed, and then vacuum dried at -30°C for 5 hours to obtain the odor-neutralizing and temperature-controlled microcapsules.

[0131] Add the auxiliary deodorizing agent and antioxidant 1500 to dodecyl dimethyl betaine, and mix at 300 rpm for 3 hours at 45°C. Then add the deodorizing and temperature-controlled microcapsules and continue mixing for 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 is 1:1:1.

[0132] Heat 50 parts by weight of base asphalt to 143°C, add 6 parts by weight of odor-neutralizing and temperature-controlled asphalt additive at a speed of 500 rpm, and stir for 4 hours to obtain odor-neutralizing and temperature-controlled asphalt.

[0133] Comparative Example 6

[0134] The odor-neutralizing and temperature-controlled asphalt additive is prepared by adding the auxiliary odor neutralizer and antioxidant 1500 to dodecyl dimethyl betaine and stirring at 300 rpm for 3 hours at 45°C. The mass ratio of the auxiliary odor neutralizer to dodecyl dimethyl betaine is 1:1.

[0135] Heat 50 parts by weight of base asphalt to 143°C, add 4 parts by weight of odor-neutralizing and temperature-controlled asphalt additive at a speed of 500 rpm, and stir for 4 hours to obtain odor-neutralizing and temperature-controlled asphalt.

[0136] Test Example 1

[0137] Sulfides are the main cause of the pungent odor in asphalt fumes. Odor-neutralizing temperature-controlled asphalt was prepared using Sinopec Donghai brand No. 70 Grade A asphalt. The odor-neutralizing temperature-controlled asphalt prepared in the examples and comparative examples was stored at 143°C for 0 days and 14 days, respectively. Then, equal masses of the stored asphalt were transferred to a sealed container, and fumes were enriched at 163°C with stirring at 300 rpm for 4 hours. After enrichment, the gas in the sealed container was extracted, and the sulfide content in the gas was tested using gas chromatography. The data are shown in Table 1 below.

[0138] Table 1 Gas chromatography sulfide test data

[0139]

[0140] Test Example 2

[0141] 100g of the odor-free temperature-controlled asphalt samples obtained in Example 1 and Comparative Example 6, along with the base asphalt, were respectively injected into 100mL beakers. The sensor probe of a multi-channel temperature acquisition and recording instrument was then inserted into the middle of the asphalt system. After the asphalt cooled for 24 hours, the beakers were placed in a 60°C water bath to record the temperature changes of the asphalt system. The obtained data are shown in the attached figure. Figure 2 As shown.

Claims

1. A taste-free temperature control asphalt additive characterized in that: By weight parts comprising the following components: Net taste temperature control microcapsules, 1-5 parts; Auxiliary net taste agents, 1-5 parts; Dispersants, 1-5 parts; The net taste temperature control microcapsules comprise a composite shell material and a core material, wherein the composite shell material comprises silicon dioxide / nano tourmaline / polydopamine, the core material comprises n-alkane with a phase transition temperature of 40-60℃, and the surface of the composite shell material is loaded with metal chelates and smoke suppression compounds containing active α-H; The auxiliary net taste agent is selected from one or more of phosphite antioxidants with a boiling point greater than 220℃; The surface of the composite shell material is loaded with metal chelates, and the metal is copper; The smoke suppression compound containing active α-H is selected from one or more of aldehyde compounds with more than 9 carbon atoms or ketone compounds with more than 8 carbon atoms; The net taste temperature control microcapsules are prepared by the following method, comprising: S1: Mix nano tourmaline, surfactant and solvent, modify under stirring, wash after modification, freeze-dry to obtain modified nano tourmaline; S2: Heat the core material raw material to melt, then add solvent and modified nano tourmaline prepared in step S1, and stir to mix; S3: Add silicon dioxide precursor to the reaction system of step S2, stir to mix, and obtain Pickering emulsion; S4: Adjust the pH value of the Pickering emulsion obtained in step S3 to 2-5, stir, then age, filter, wash, and freeze-dry; S5: Add the solid powder prepared in step S4 to a buffer solution, add dopamine hydrochloride, treat under stirring, then filter, wash, and freeze-dry; S6: Add the solid powder prepared in step S5, smoke suppression compounds containing active α-H, and strong base to an organic solvent, react under heating reflux condition, cool, filter, wash, and freeze-dry; S7: Ultrasonically disperse the solid powder prepared in step S6 in a copper ion salt-formamide solution, react under stirring, after the reaction is completed, filter, wash, and freeze-dry to obtain the net taste temperature control microcapsules.

2. The taste-free temperature control asphalt additive according to claim 1, characterized in that: The phosphite antioxidant with a boiling point greater than 220℃ is selected from one or more of tris(2,4-di-tert-butylphenyl) phosphite, 3,9-bis(2,4-di-tert-butylphenoxy)-2,4,8,10-tetraoxa-3,9-diphospha-spiro[5.5]undecane, tris(nonylphenyl) phosphite, antioxidant 1500 (4,4'-di-tert-propyl biphenyl C12-15-alcohol phosphite), and distearyl pentaerythritol diphosphite.

3. The taste-free temperature control asphalt additive according to claim 1, characterized in that: The dispersant is selected from one or more of dodecyl dimethyl betaine and 1-hydroxyethyl-carboxymethyl-alkyl imidazoline.

4. The taste-free temperature control asphalt additive of claim 1, wherein: The particle size of the net taste temperature control microcapsules is 1-5 μm.

5. The taste-free temperature control asphalt additive of claim 1, wherein: The mass ratio of the composite shell material to the core material of the net taste temperature control microcapsules is 1:(0.5-2).

6. The taste-free temperature-control asphalt additive according to claim 1, characterized in that: The composite shell material of the net taste temperature control microcapsules comprises silicon dioxide / nano tourmaline / polydopamine, wherein the mass ratio of silicon dioxide to nano tourmaline is (1-5):1, and the mass ratio of silicon dioxide to polydopamine is 1:(0.1-0.5).

7. The taste-free temperature-control asphalt additive according to claim 1, characterized in that: The n-alkane with a phase transition temperature of 40-60℃ is one or more of n-octadecane, n-eicosane, and n-docosane.

8. The taste-free temperature control asphalt additive according to claim 7, characterized in that: The phase transition temperature is n-dodecane.

9. The taste-free temperature control asphalt additive of claim 1, wherein: The surface of the composite shell contains 0.1wt%-15wt% of metal load and 0.1wt%-20wt% of active alpha-H containing smoke suppression compound.

10. The taste-free temperature-control asphalt additive according to claim 1, characterized in that: The aldehyde compound with more than 9 carbon atoms is selected from one or more of o-methyl cinnamic aldehyde, p-methyl cinnamic aldehyde, anisic aldehyde, 2-methyl undecanal, 10-undecenal, ethyl vanillin, benzaldehyde, phenylacetaldehyde, p-hydroxybenzaldehyde, butylphenyl methyl propyl aldehyde, neral, hydroxymethyl pentyl cyclohexene acetal, 3-(4-ethylphenyl)-2,2-dimethyl propionaldehyde, vanillin propylene glycol acetal, methyl hexyl guaiacol aldehyde, methyl pentyl cinnamic aldehyde, diethylaminobenzaldehyde; The ketone compound with more than 8 carbon atoms is selected from one or more of carvone, 3-hydroxy-2-butanone, 2,3-butanedione 3-penten-2-one, 6-methyl-3,5-heptadien-2-one.

11. The taste-free temperature-control asphalt additive according to claim 1, characterized in that: In step S1, the surfactant is a cationic surfactant, and the solvent is an aprotic solvent with a boiling point >100℃. And / or, in step S1, the mass ratio of the nanotourmaline to the surfactant is (1-10):1, and the mass ratio of the solvent to the surfactant is (5-50):

1.

12. The taste-free temperature-control asphalt additive according to claim 11, characterized in that: In step S1, the surfactant is at least one of cetyltrimethylammonium bromide, cetyltrimethylammonium chloride, dodecyl dimethyl benzyl ammonium chloride, and octadecyl trimethyl ammonium chloride; and the solvent is at least one of formamide, N,N-dimethylformamide, dimethylacetamide, and dimethylphosphoryl amide.

13. The taste-free temperature-control asphalt additive according to claim 1, characterized in that: In step S1, the stirring speed is 200-500 rpm, the modification temperature is 100-190℃, and the modification time is 2-5 hours. And / or, in step S2, the stirring speed is 400-600 rpm, the stirring temperature is 40-60℃, and the stirring time is 4-6 hours. And / or, in step S3, the stirring speed is 400-600 rpm, the stirring temperature is 40-60℃, and the stirring time is 4-6 hours. And / or, in step S4, the stirring speed is 400-600 rpm, the stirring temperature is 40-60℃, and the stirring time is 4-6 hours. And / or, in step S5, the stirring speed is 100-300 rpm, the stirring temperature is 20-40℃, and the stirring time is 12-24 hours. And / or, in step S7, the stirring speed is 200-450 rpm, the reaction temperature is 100-190℃, and the reaction time is 2-5 hours.

14. The taste-free temperature-control asphalt additive according to claim 1, characterized in that: In step S2, the solvent is an aprotic solvent with a boiling point >100℃. And / or, in step S2, the mass ratio of the core material to the modified nanotourmaline is (1-10):1, and the mass ratio of the solvent to the modified nanotourmaline is (20-80):

1.

15. The taste-free temperature control asphalt additive of claim 14, wherein: In step S2, the solvent is at least one of formamide, N,N-dimethylformamide, dimethylacetamide, and dimethylphosphoryl amide.

16. The taste-free temperature-control asphalt additive according to claim 1, characterized in that: In step S3, the silica precursor is a silicate compound; And / or, the mass ratio of the core material raw material to the silica precursor is (0.5-1.5):

1.

17. The taste-free temperature-control asphalt additive according to claim 16, characterized in that: In step S3, the silica precursor is at least one of methyl silicate, ethyl silicate, tetraethyl silicate, and butyl silicate.

18. The taste-free temperature-control asphalt additive according to claim 1, characterized in that: In step S5, the buffer solution is one or more of a phosphate buffer, a carbonate buffer, and a tris-hydroxymethyl aminomethane hydrochloride buffer. And / or, the mass ratio of the buffer solution to the solid powder prepared in step S4 is (10-100):

1.

19. The taste-free temperature-control asphalt additive according to claim 18, characterized in that: In step S5, the pH value of the buffer solution is 8-10.

20. The taste-free temperature-control asphalt additive according to claim 1, characterized in that: In step S5, after adding dopamine hydrochloride, the mass concentration of dopamine in the reaction system is 2-10 mg / mL.

21. The taste-free temperature-control asphalt additive according to claim 1, characterized in that: In step S6, the organic solvent is selected from one or more of methanol, butanediol, ethylene glycol, n-butanol, and anhydrous ethanol. And / or, in step S6, the mass ratio of the solid powder prepared in step S5 to the smoke-suppressing compound containing active α-H is 1:(10-40); the mass ratio of the solid powder prepared in step S5 to the organic solvent is 1:(20-80); and the mass ratio of the solid powder prepared in step S5 to the strong base is 1:(0.5-2). And / or, in step S6, the strong base is one of solid KOH and solid NaOH. And / or, in step S6, the heating reflux reaction condition is that the reaction temperature is 80-220°C and the reaction time is 5-10 hours.

22. The taste-free temperature-control asphalt additive according to claim 1, characterized in that: In step S7, the metal copper ion salt is anhydrous copper sulfate. And / or, the mass ratio of the metal copper ion salt-formamide solution to the solid powder prepared in step S6 is (5-30):

1.

23. A tasteless temperature-controlled asphalt, comprising the following components by weight parts: Base asphalt, 50-500 parts; The tasteless temperature-controlled asphalt additive of any one of claims 1-22, 1-50 parts.

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