Low-noise water damage resistant asphalt mixture and preparation method thereof

Abstract

The application discloses a kind of low-noise water disaster resistant asphalt mixture and preparation method thereof, it is related to bitumen technical field.The mixture is composed of modified basalt porous ceramic hybrid aggregate and self-repairing gel modified asphalt material composite;Among them, modified basalt porous ceramic hybrid aggregate is crushed after basalt ore, by the synergistic effect of foaming agent, cosolvent, in the vacuum gradient sintering, carbon dioxide is inhaled to optimize pore structure, then by pickling, plasma activation and polyurethane impregnation strengthen mixed aggregate and filler are prepared;Self-repairing gel modified asphalt is three (2-mercaptoethyl) cyanuric acid ester as precursor, by thiol-epoxy click chemistry reaction to form crosslinked gel network, then with matrix asphalt composite;The scheme is through the acoustic wave dissipation of porous ceramic, hydrophobic interface and the dynamic self-repairing synergistic effect of gel network, significantly improve the water disaster resistance and noise reduction performance of mixture.

Description

TECHNICAL FIELD

[0001] The present application relates to the technical field of asphalt, in particular to a low-noise water damage resistant asphalt mixture and a preparation method thereof. BACKGROUND

[0002] As a key material for road engineering, asphalt mixture has two major technical bottlenecks in long-term service: on the one hand, rainwater penetration leads to a decrease in the adhesion of the aggregate-asphalt interface, which easily causes water damage and significantly weakens the overall durability of the pavement structure; on the other hand, with the acceleration of urbanization, traffic noise problems are becoming increasingly prominent, and the impact of road noise on the environment and residents' health is becoming increasingly severe; although existing technologies have improved water damage and noise pollution respectively, such as by adding anti-stripping agents to enhance interface adhesion or using porous aggregate to absorb noise, it is difficult to balance both: porous aggregate can significantly reduce noise, but is prone to water absorption, increasing the risk of water damage; water damage design usually sacrifices porosity and acoustic performance; in addition, asphalt mixture is prone to micro-cracks under long-term load and environmental changes, and lacks effective self-repairing ability, further shortening the service life of the pavement; therefore, there is an urgent need to propose a new type of asphalt mixture that has low noise, high water damage resistance and self-repairing function, to overcome the defects of existing technologies that cannot simultaneously balance these three aspects of performance, and to meet the comprehensive needs of modern road engineering for environmental protection, durability and sustainability. SUMMARY

[0003] The present application aims to provide a low-noise water damage resistant asphalt mixture and a preparation method thereof to solve the problems in the prior art.

[0004] To solve the above technical problems, the present application provides the following technical solution: a low-noise water damage resistant asphalt mixture, which is a mixture of modified basalt porous ceramic hybrid aggregate and self-repairing gel modified asphalt material.

[0005] Further, the modified basalt porous ceramic hybrid aggregate is obtained by treating basalt ore, vacuum sintering, introducing carbon dioxide in the late sintering stage, vacuum impregnating polyurethane liquid after surface activation and immersion of coupling agent, and mixing with fine aggregate and filler.

[0006] Further, the self-repairing gel modified asphalt material is obtained by combining tris(2-mercaptoethyl) cyanurate with glycerol triglycidyl ether to obtain a gel master particle composite asphalt by oxygenation.

[0007] Further, the tris(2-mercaptoethyl) cyanurate is prepared by reacting phosphorus oxychloride with cyanuric acid and preparing cyanuric acid trichloride by vacuum distillation, followed by nucleophilic substitution reaction with 2-(acetylmercapto) ethyl dichlorophosphate to obtain tris(2-acetylmercaptoethyl) cyanurate, and then reducing the acetylmercapto group.

[0008] Further, the 2-(acetylmercapto)ethyl dichlorophosphate is prepared by dissolving 2-mercaptoethanol in anhydrous reagent, adding acetyl chloride dropwise, and then distilling under reduced pressure, adding anhydrous reagent and adding phosphorus oxychloride dropwise in an ice bath.

[0009] Further, a low-noise water damage resistant asphalt mixture comprises the following preparation steps:

[0010] (1) Taking 100 parts of basalt ore as a base body, first crushing to 100-200 mesh, adding 3-8 parts of foaming agent and 5-12 parts of cosolvent for dry mixing, sintering at 900-1000°C for 1-2h in a vacuum environment, and in the middle of sintering, increasing the temperature to 1000-1100°C and introducing 1-3L / min of carbon dioxide to regenerate the oxides into carbonates, and continuing to heat for 2-3h; then increasing the temperature to 1100-1200°C for 2-3h; after cooling, screening 2-3mm particles to obtain porous basalt ceramic;

[0011] (2) Adding 10-20% mass fraction of dilute hydrochloric acid to soak the porous basalt ceramic for 30-60min to dissolve the surface metal oxides, washing with deionized water until neutral, then exposing the hydroxyl group by hot drying at 60°C, and irradiating with argon atmosphere plasma for 1-3min to obtain a pre-modified porous basalt ceramic;

[0012] (3) Under nitrogen protection, a polyurethane prepolymer is prepared by polymerization of polyether polyol and isocyanate; 1-3 parts of coupling agent is mixed with the pre-modified porous basalt ceramic particles, soaked for 1-2h; then 10-30 parts of polyurethane prepolymer is added for further mixing and degassing; maintaining under vacuum for 30-50min; finally, gradient temperature curing to obtain modified porous basalt ceramic; then adding 20-30 parts of fine aggregate and 8-10 parts of filler to obtain modified porous basalt ceramic hybrid aggregate;

[0013] (4) Under nitrogen protection, 100 parts of cyanuric acid is mixed with 260-340 parts of phosphorus oxychloride, and reacted at 80-100°C for 3-5h; after the reaction is completed, the excess phosphorus oxychloride is recovered by reduced pressure distillation, and cyanuric acid trichloride is prepared; then 400 parts of anhydrous THF is added, followed by the addition of 210 parts of 2-(acetylmercapto)ethyl dichlorophosphate, and stirred at 60-80°C for 6-8h; after the reaction is completed, the inorganic salt is removed by filtration, and the filtrate is concentrated and evaporated to obtain tris(2-acetylmercaptoethyl) cyanurate; then 300 parts of anhydrous methanol, 180 parts of potassium carbonate and 1 part of BHT are added, 40 parts of sodium borohydride is added in batches under ice bath at 0-5°C, then the temperature is raised to room temperature and reacted for 2-3h; after the reaction solution is acidified to neutral, it is extracted with 300-400 parts of ethyl acetate, and the organic phase is washed and dried to obtain tris(2-mercaptoethyl) cyanurate;

[0014] (5) dissolve the tris (2-mercaptoethyl) cyanurate in 200 parts of THF, add 140 parts of glycerol triglycidyl ether and 8 parts of catalyst, continuously pass 0.5-1L / min oxygen, react at 60-80℃ for 4-6h, after the reaction is completed, evaporate to remove the solvent, to prepare the self-repairing gel master batch; add the matrix asphalt to mix to prepare the self-repairing gel modified asphalt material;

[0015] (6) take 90-95 parts of modified basalt porous ceramic hybrid aggregate, 6-10 parts of self-repairing gel modified asphalt material, and then add an anti-stripping agent, mix, heat to 100-120℃, and stir for 1-3h to prepare the asphalt mixture.

[0016] Further, the foaming agent in the step (1) refers to one of calcium carbonate, dolomite and manganese dioxide; the cosolvent refers to one of potassium feldspar, calcium feldspar and spodumene.

[0017] Further, the dilute hydrochloric acid in the step (2) is 6-10 times the volume of the ceramic particles.

[0018] Further, the coupling agent in the step (3) refers to one of KH-550, KH-560 and KH-835.

[0019] Further, the gradient curing in the step (3) refers to first curing at 60-100℃ for 1h, and then heating to 80-120℃ for 2h.

[0020] Further, the fine aggregate and the filler in the step (3) refer to machine-made basalt sand and lime powder, respectively.

[0021] Further, the 2-(acetylmercapto) ethyl dichlorophosphate in the step (4) is prepared by dissolving 100 parts of 2-mercaptoethanol in 200 parts of anhydrous THF, cooling to 0-5℃ in an ice bath, adding a mixture of 85 parts of acetyl chloride and 95 parts of pyridine dropwise, after titration, heating to 25℃ and stirring for 2h, evaporating the solvent under reduced pressure, adding 100 parts of anhydrous THF, adding 140 parts of phosphorus oxychloride dropwise in an ice bath, stirring at 25℃ for 1h, filtering, and evaporating and concentrating to prepare 2-(acetylmercapto) ethyl dichlorophosphate.

[0022] Further, the matrix asphalt in the step (5) is 8-10 times the mass of the gel master batch.

[0023] Further, the anti-stripping agent in the step (6) is AD-here LOF65-00, and the addition amount is 0.2-0.6% of the total mass of the self-repairing gel modified asphalt.

[0024] Compared with the prior art, the present application has the following beneficial effects:

[0025] The asphalt mixture prepared by the present application comprises modified basalt porous ceramic aggregate and self-repairing gel modified asphalt material, so as to realize the effects of low noise, water damage resistance and heat insulation.

[0026] Firstly, basalt ore is used as raw material, and after being crushed, ground, granulated and formed, the basalt is mixed with a dissolving aid and a foaming agent to perform segmented sintering: vacuum sintering is performed in the early stage, and after sintering is completed, carbon dioxide gas is introduced to continue heat preservation sintering, and the pore structure is optimized through gas phase regulation; temporary carbonates are formed through gas-solid reaction with calcium oxide, magnesium oxide and other components, and the porosity of the material is increased by subsequent temperature rise; after the sintered product is cooled and sieved to obtain porous basalt ceramic particles, surface activation treatment is performed, the particles are soaked in a coupling agent, and then a polyurethane solution is filled into the ceramic pores through a vacuum assisted impregnation process, and after drying and crosslinking, a continuous polymer film layer with a hydrophobic modified surface is formed to obtain hybrid aggregate to modify asphalt; the low noise effect of sound wave dissipation and noise reduction of the porous structure is achieved, and the surface hydrophobicity and water damage resistance are achieved.

[0027] Secondly, under the protection of nitrogen, trichloro cyanuric acid is prepared by the reaction of phosphorus oxychloride and cyanuric acid and through vacuum distillation, and then a nucleophilic substitution reaction is performed with 2-(acetylmercapto) ethyl dichlorophosphate: a nitrogen-carbon-oxygen bond is formed to construct tris(2-acetylmercaptoethyl) cyanurate, and tris(2-mercaptoethyl) cyanurate is obtained by reducing the acetylmercapto group; appropriate oxygen is introduced and glycerol triglycidyl ether is introduced to perform epoxy-mercapto reaction to generate a thioether bond, and a gel master batch with a three-dimensional crosslinked network is formed under the action of a catalyst; the three-dimensional rigid structure of the cyanuric acid core provides mechanical support; the mercapto group is oxidized into a dynamic disulfide bond to give the material self-repairing characteristics; after the gel master batch is compounded with asphalt, the three-dimensional network structure not only enhances the water damage resistance of the material, but also forms a synergistic noise reduction effect with the modified basalt porous ceramic, and also has certain heat insulation capacity; and when the material is subjected to external force or microcracks due to temperature change, the dynamic disulfide bond can be broken and rearranged to realize self-repairing of the damaged area, thereby significantly prolonging the service life of the asphalt. DETAILED DESCRIPTION

[0028] The technical solutions in the embodiments of the present application will be clearly and completely described below in combination with the embodiments of the present application. Obviously, the described embodiments are only a part of the embodiments of the present application, rather than all the embodiments. Based on the embodiments in the present application, all other embodiments obtained by those skilled in the art without creative labor fall within the scope of protection of the present application.

[0029] In order to more clearly illustrate the method provided by the present application, the following embodiments are used for detailed description, and the test methods of various indexes of a low noise water damage resistant asphalt mixture prepared in the following embodiments are as follows:

[0030] Low noise: The low noise of the asphalt mixtures prepared in the examples and the comparative examples was determined according to the provisions of GB / T 21396-2008 Road Traffic Noise Measurement Method.

[0031] Water damage resistance: The water damage resistance of the asphalt mixtures prepared in the examples and the comparative examples was determined according to the provisions of JTG / F40-2004 Highway Asphalt Pavement Construction Technical Specification. Example 1

[0032] (1) Take 100 parts of basalt ore as the base body, crush to 100 mesh, add 3 parts of calcium carbonate foaming agent and 5 parts of potassium feldspar dissolving aid to mix evenly at a stirring speed of 300 rpm, sinter at 900°C for 1 h in a vacuum environment with a vacuum degree of 10 Pa, then increase the temperature to 1000°C and introduce 1 L / min of carbon dioxide to regenerate the oxides into carbonates, continue to heat for 2 h, then increase the temperature to 1100°C and react for 2 h, screen out 2 mm particles after cooling to prepare porous basalt ceramic; -1

[0033] (2) Soak the porous basalt ceramic particles in 10 wt% dilute hydrochloric acid for 30 min and stir at a low speed of 200 rpm to dissolve the surface metal oxides, the amount of dilute hydrochloric acid is 6 times the volume of the ceramic; then wash with deionized water until neutral, dry at 60°C for 2 h, expose the hydroxyl groups, and irradiate with plasma at a voltage of 5 Kv and a current of 12 mA for 1 min in an argon atmosphere to prepare pre-modified basalt porous ceramic;

[0034] (3) Prepare a polyurethane prepolymer by polymerizing 100 parts of polyether polyol and 25 parts of isocyanate at 60°C under moderate stirring at 300 rpm for 3 h; prepare a 1 wt% ethanol solution of 1 part of silane coupling agent KH-560, mix with 60 parts of pre-modified ceramic particles at a stirring speed of 200 rpm, and soak for 1 h; add 10 parts of polyurethane prepolymer and mix at a high speed of 500 rpm to degas, maintain vacuum at -0.1 MPa for 30 min, then gradiently solidify: first at 60°C for 1 h, then increase the temperature to 80°C for 2 h to prepare modified basalt porous ceramic; finally, add 20 parts of machine-made basalt sand and 8 parts of lime powder to the modified basalt porous ceramic to prepare modified basalt porous ceramic hybrid aggregate;

[0035] ​(4) The whole process is under nitrogen protection. 100 parts of cyanuric acid is stirred with 260 parts of phosphorus oxychloride at 80°C for 3h, the stirring speed is 100rpm, and the pressure is 3.5KPa. The excess phosphorus oxychloride is recovered by reduced pressure distillation to obtain material A. 400 parts of anhydrous THF is added to material A, and then 70 parts of material D is added in three batches with an interval of 15min. The stirring reaction is carried out at 60°C and 300rpm for 6h. After filtering to remove inorganic salts, the filtrate is evaporated and concentrated to 1 / 3 of the original volume to obtain material B. Then 300 parts of anhydrous methanol, 180 parts of potassium carbonate and 1 part of BHT are added. 20 parts of sodium borohydride is added in two batches with an interval of 15min under 0°C ice bath. After the reaction at room temperature and 300rpm for 2h, the reaction solution is acidified to neutral with anhydrous THF and extracted with 300 parts of ethyl acetate. The organic phase is washed with saturated brine, dried with anhydrous sodium sulfate, and then evaporated and concentrated to 1 / 3 of the original volume of the filtrate to obtain material C. Under nitrogen protection, 100 parts of 2-mercaptoethanol is dissolved in 200 parts of anhydrous THF. 85 parts of acetyl chloride and 95 parts of pyridine mixture is added dropwise under 0°C ice bath. After the titration is completed, the temperature is increased to 25°C, and the stirring is carried out at 300rpm for 2h. After removing the solvent by reduced pressure distillation at 1.5KPa, 100 parts of anhydrous THF is added. 140 parts of phosphorus oxychloride is added dropwise under 0°C ice bath. The stirring is carried out at 25°C and 300rpm for 1h. After filtration, the filtrate is evaporated and concentrated to 1 / 3 of the original volume to obtain material D;

[0036] (5) 100 parts of material C is dissolved in 200 parts of THF. 140 parts of glycerol triglycidyl ether and 8 parts of triethylamine are added. Oxygen is continuously introduced at a rate of 0.5L / min. The reaction is carried out at 60°C for 4h. After evaporation at 80°C for 4h, self-repairing gel master batch is obtained. 8 times the mass of the gel master batch of Shell No. 70 asphalt is added. The stirring is carried out at 120°C and 500rpm for 2h to obtain self-repairing gel modified asphalt material;

[0037] (6) 90 parts of modified basalt porous ceramic hybrid aggregate is mixed with 6 parts of self-repairing gel modified asphalt. 0.2% of AD-here LOF65-00 anti-stripping agent is added based on the total mass of the self-repairing gel modified asphalt. The temperature is increased to 100°C. The stirring is carried out at a speed of 500rpm for 1h to obtain asphalt mixture. Example 2

[0038] (1) 100 parts of basalt ore is used as the base body. After being crushed to 150 mesh, 5 parts of dolomite foaming agent and 8 parts of calcium feldspar dissolving aid are added and uniformly dry mixed at a stirring speed of 300rpm. In a vacuum environment with a vacuum degree of 10 -1 Pa, sintering is carried out at 950°C for 1.5h. Then the temperature is increased to 1050°C, 2L / min of carbon dioxide is introduced to regenerate oxides into carbonates, and the temperature is continuously maintained for 2.5h. Then the temperature is increased to 1150°C and reacted for 2.5h. After cooling, 2.5mm particles are screened to obtain porous basalt ceramic;

[0039] (2) The porous basalt ceramic particles are soaked in 15wt% dilute hydrochloric acid with a dosage of 8 times the ceramic volume for 45 min and stirred at a low speed of 200 rpm to dissolve the surface metal oxides, washed with deionized water until neutral, and dried at 60°C for 2h to expose the hydroxyl groups. The pre-modified porous basalt ceramic is prepared by plasma irradiation at a voltage of 5Kv and a current of 12mA for 2min in an argon atmosphere;

[0040] (3) The polyurethane prepolymer is prepared by polymerization of 100 parts of polyether polyol and 25 parts of isocyanate at 60°C under nitrogen protection and stirring at a medium speed of 300 rpm for 3h. 2 parts of silane coupling agent KH-550 are prepared into a 2wt% ethanol solution, mixed with 60 parts of pre-modified ceramic particles at a stirring speed of 200 rpm, and soaked for 1.5h. 20 parts of polyurethane prepolymer are added and mixed and degassed at a high speed of 500 rpm. Vacuum is maintained at -0.1MPa for 40min, and then gradient curing is performed: first at 80°C for 1h, and then at 100°C for 2h to prepare the modified porous basalt ceramic. Finally, 20 parts of machine-made basalt sand and 8 parts of lime powder are added to the modified porous basalt ceramic to prepare the modified porous basalt ceramic hybrid aggregate;

[0041] (4) In this step, the whole process is under nitrogen protection. 100 parts of cyanuric acid and 300 parts of phosphorus oxychloride are stirred at 90°C for 4h at a stirring speed of 100 rpm and a pressure of 3.5KPa. Excess phosphorus oxychloride is recovered by reduced pressure distillation to obtain material A. 400 parts of anhydrous THF are added to material A, and 70 parts of material D are added in three batches at intervals of 15min. Stirring is performed at 60°C at a medium speed of 300 rpm for 7h. After filtering to remove inorganic salts, evaporation and concentration are performed to 1 / 3 of the original filtrate volume to obtain material B. 300 parts of anhydrous methanol, 180 parts of potassium carbonate, and 1 part of BHT are added. Sodium borohydride is added in two batches at intervals of 15min at 0°C ice bath. The reaction is performed at room temperature at a medium speed of 300 rpm for 2.5h. The reaction liquid is acidified to neutral with anhydrous THF and extracted with 350 parts of ethyl acetate. The organic phase is washed with saturated brine, dried with anhydrous sodium sulfate, and then evaporated and concentrated to 1 / 3 of the original filtrate volume to obtain material C. Under nitrogen protection, 100 parts of 2-mercaptoethanol are dissolved in 200 parts of anhydrous THF. A mixed solution of 85 parts of acetyl chloride and 95 parts of pyridine is added dropwise at 0°C ice bath. After titration is completed, the temperature is increased to 25°C, and stirring is performed at a medium speed of 300 rpm for 2h. Solvent is removed by reduced pressure distillation at 1.5KPa. 100 parts of anhydrous THF are added. 140 parts of phosphorus oxychloride are added dropwise at 0°C ice bath. Stirring is performed at 25°C at a medium speed of 300 rpm for 1h. Filtration and evaporation and concentration are performed to 1 / 3 of the original filtrate volume to obtain material D;

[0042] (5) 100 parts of material C is dissolved in 200 parts of THF, 140 parts of glycerol triglycidyl ether and 8 parts of triethylamine are added, 0.8 L / min of oxygen is continuously introduced, and reaction is carried out at 70°C for 5 h; evaporation is carried out at 80°C for 4 h to prepare self-repairing gel master batch, then 9 times the mass of the self-repairing gel master batch of Shell No. 70 asphalt is added, stirring is carried out at 500 rpm and 120°C for 2 h to prepare self-repairing gel modified asphalt material;

[0043] (6) 93 parts of modified basalt porous ceramic hybrid aggregate is taken and mixed with 8 parts of self-repairing gel modified asphalt, 0.4% of AD-here LOF65-00 anti-stripping agent based on the total mass of the self-repairing gel modified asphalt is added, the temperature is raised to 110°C, and stirring is carried out at a speed of 500 rpm for 2 h to prepare asphalt mixture. Example 3

[0044] (1) 100 parts of basalt ore is taken as a base, is crushed to 200 mesh, 8 parts of manganese dioxide foaming agent and 12 parts of spodumene dissolving aid are added, and dry mixing is carried out at a stirring speed of 300 rpm, and then sintering is carried out at 1000°C for 2 h in a vacuum environment with a vacuum degree of 10 -1 Pa, then the temperature is raised to 1100°C, 3 L / min of carbon dioxide is introduced to regenerate oxides into carbonates, and then the temperature is continuously maintained at 1100°C for 3 h, then the temperature is raised to 1200°C and reaction is carried out for 3 h, and then 3 mm particles are screened to prepare porous basalt ceramic;

[0045] (2) The porous basalt ceramic particles are soaked in 20 wt% dilute hydrochloric acid for 60 min at a dosage of 10 times the volume of the ceramic and are stirred at a low speed of 200 rpm to dissolve the surface metal oxides, and then deionized water is used for washing until neutral, and then the ceramic is heated and dried at 60°C for 2 h to expose the hydroxyl groups, and then plasma irradiation is carried out under an argon atmosphere at a voltage of 5 Kv and a current of 12 mA for 3 min to prepare pre-modified basalt porous ceramic;

[0046] (3) Polyurethane prepolymer is prepared by polymerization of 100 parts of polyether polyol and 25 parts of isocyanate at 60°C under stirring at a medium speed of 300 rpm for 3 h; 2 parts of silane coupling agent KH-835 is prepared into a 3 wt% ethanol solution, and 60 parts of pre-modified ceramic particles are mixed and stirred at a speed of 200 rpm for 2 h; 30 parts of polyurethane prepolymer is added and mixed and degassed at a high speed of 500 rpm, and then vacuum is maintained at -0.1 MPa for 50 min, and then gradient curing is carried out: first, curing is carried out at 100°C for 1 h, then the temperature is raised to 120°C and curing is carried out for 2 h to prepare modified basalt porous ceramic; finally, 20 parts of machine-made basalt sand and 8 parts of lime powder are added to the modified basalt porous ceramic, and mixing is carried out to prepare modified basalt porous ceramic hybrid aggregate;

[0047] (4) The whole process is under nitrogen protection. 100 parts of cyanuric acid is stirred with 340 parts of phosphorus oxychloride at 100°C for 5h, the stirring speed is 100rpm, and the pressure is 3.5KPa. The excess phosphorus oxychloride is recovered by reduced pressure distillation to obtain material A. Then 400 parts of anhydrous THF is added to material A, and 70 parts of material D is added in three batches with an interval of 15min. The stirring reaction is carried out at 60°C and 300rpm for 7h. After filtering to remove inorganic salts, the filtrate is evaporated and concentrated to 1 / 3 of the original volume to obtain material B. Then 300 parts of anhydrous methanol, 180 parts of potassium carbonate and 1 part of BHT are added. 20 parts of sodium borohydride is added in two batches with an interval of 15min under 0°C ice bath. After reaction at room temperature and 300rpm for 3h, the reaction solution is neutralized with anhydrous THF and extracted with 400 parts of ethyl acetate. The organic phase is washed with saturated brine, dried with anhydrous sodium sulfate, and then evaporated and concentrated to 1 / 3 of the original volume to obtain material C. In the process, 100 parts of 2-mercaptoethanol is dissolved in 200 parts of anhydrous THF under nitrogen protection. 85 parts of acetyl chloride and 95 parts of pyridine mixture are added dropwise under 0°C ice bath. After titration, the temperature is increased to 25°C, and the stirring is carried out at 300rpm for 2h. After removing the solvent by reduced pressure distillation at 1.5KPa, 100 parts of anhydrous THF is added. 140 parts of phosphorus oxychloride is added dropwise under 0°C ice bath. After stirring at 25°C and 300rpm for 1h, the filtrate is evaporated and concentrated to 1 / 3 of the original volume to obtain material D.

[0048] (5) 100 parts of material C is dissolved in 200 parts of THF. 140 parts of glycerol triglycidyl ether and 8 parts of triethylamine are added. 1L / min of oxygen is continuously introduced. The reaction is carried out at 80°C for 6h. After evaporation at 80°C for 4h, self-repairing gel master batch is obtained. 10 times the mass of the gel master batch of Shell No. 70 asphalt is added. The stirring is carried out at 120°C and 500rpm for 2h to obtain self-repairing gel modified asphalt material.

[0049] (6) 95 parts of modified basalt porous ceramic hybrid aggregate is mixed with 10 parts of self-repairing gel modified asphalt. 0.6% of AD-here LOF65-00 anti-stripping agent is added to the total mass of the self-repairing gel modified asphalt. The temperature is increased to 120°C. The stirring is carried out at 500rpm for 3h to obtain asphalt mixture.

[0050] Comparative Example 1

[0051] The difference between Comparative Example 1 and Example 2 is that step (1) is different. Step (1) is changed to: 100 parts of basalt ore is used as the base material. After being crushed to 150 mesh, 5 parts of dolomite foaming agent and 8 parts of calcium feldspar dissolving aid are added and uniformly dry mixed at a stirring speed of 300rpm. The vacuum degree is 10 -1Pa was sintered in vacuum environment at 950℃ for 1h, then heated to 1050℃ for 2.5h, and then heated to 1150℃ for 2.5h. After cooling, the 2.5mm particles were sieved to obtain the porous basalt ceramic. The remaining steps were the same as in Example 2.

[0052] Comparative Example 2

[0053] Comparative Example 2 differs from Example 2 in that step (3) is changed to: under nitrogen protection, 100 parts of polyether polyol and 25 parts of isocyanate are stirred at 60℃ at a medium speed of 300rpm for 3h to obtain a polyurethane prepolymer; 2 parts of silane coupling agent KH-550 are prepared into a 2wt% ethanol solution, mixed with 60 parts of pre-modified ceramic particles at a stirring speed of 200rpm, and soaked for 1.5h to obtain modified basalt porous ceramic; finally, 20 parts of machine-made basalt sand and 8 parts of lime powder are added to the modified basalt porous ceramic to obtain modified basalt porous ceramic hybrid aggregate; the remaining steps are the same as in Example 2.

[0054] Comparative Example 3

[0055] Comparative Example 3 differs from Example 2 in that steps (4), (5), and (6) are changed to: (4) in this step, 100 parts of cyanuric acid and 300 parts of phosphorus oxychloride are stirred at 90℃ for 4h under nitrogen protection at a stirring speed of 100rpm and a pressure of 3.5KPa, excess phosphorus oxychloride is recovered by reduced pressure distillation to obtain material A; 400 parts of anhydrous THF are added to material A, and 70 parts of material D are added in three batches at intervals of 15min, stirred at 60℃ at a medium speed of 300rpm for 7h, filtered to remove inorganic salts, and evaporated and concentrated to 1 / 3 of the original filtrate volume to obtain material B; wherein, 100 parts of 2-mercaptoethanol are dissolved in 200 parts of anhydrous THF under nitrogen protection, and a mixture of 85 parts of acetyl chloride and 95 parts of pyridine is added dropwise at 0℃ with ice bath, the temperature is raised to 25℃ after titration is completed, and stirred at a medium speed of 300rpm for 2h; 100 parts of anhydrous THF are added after the solvent is removed by reduced pressure distillation at 1.5KPa, 140 parts of phosphorus oxychloride are added dropwise at 0℃ with ice bath, and stirred at 25℃ at a medium speed of 300rpm for 1h, filtered and evaporated and concentrated to 1 / 3 of the original filtrate volume to obtain material D;

[0056] 100 parts of material B are dissolved in 200 parts of THF, 140 parts of glycerol triglycidyl ether and 8 parts of triethylamine are added, and 0.8L / min of oxygen is continuously introduced, and reacted at 70℃ for 5h; after evaporation at 80℃ for 4h, 9 times the mass of the masterbatch of Shell No. 70 asphalt is added, and stirred at a high speed of 500rpm at 120℃ for 2h to obtain a modified asphalt material;

[0057] Take 93 modified basalt porous ceramic hybrid aggregate and 8 modified asphalt mixture, add 0.4% AD-here LOF65-00 anti-stripping agent of the total mass of modified asphalt, heated to 110°C, stirring at 500 rpm for 2h to prepare asphalt mixture; the rest of the steps are the same as example 2.

[0058] Comparative example 4

[0059] The difference between comparative example 4 and example 2 is that the steps (5) (6) are different, change steps (5) (6) to: (5) dissolve 100 parts of material C in 200 parts of THF, continuously pass in 0.8L / min oxygen, react at 70°C for 5h; after evaporating at 80°C for 4h to prepare masterbatch, add 9 times the mass of masterbatch of Shell No. 70 asphalt at 120°C and stir at 500 rpm for 2h to prepare modified asphalt material;

[0060] (6) take 93 modified basalt porous ceramic hybrid aggregate and 8 modified asphalt mixture, add 0.4% AD-here LOF65-00 anti-stripping agent of the total mass of modified asphalt, heated to 110°C, stirring at 500 rpm for 2h to prepare asphalt mixture; the rest of the steps are the same as example 2.

[0061] Effect example

[0062] The performance analysis results of a low-noise water damage resistant asphalt mixture using examples 1 to 3 and comparative examples 1 to 4 of the present application are given in Table 1 below.

[0063] Table 1

[0064]

[0065] From the comparison of the water immersion residual stability and noise decibel experimental data of the examples and the comparative examples, it can be found that the water damage resistance and noise reduction performance of the asphalt mixture are significantly improved by the combined action of the innovative treatment of the porous basalt ceramic matrix, the composite reinforcement of the aggregate and the self-repairing gel modified asphalt. Firstly, the basalt ore is crushed to a specific particle size, foaming agent / fluxing agent is added in a certain ratio and vacuum gradient sintering is performed, and carbon dioxide is introduced to regenerate oxides into carbonates, and this activation process optimizes the ceramic pore structure and surface activity. Secondly, after acid washing and plasma activation pretreatment, the porous ceramic is composite immersed and gradient cured with silane coupling agent and polyurethane prepolymer, and then is hybridized with machine-made sand and lime powder, which greatly enhances the interfacial bonding force, structural integrity and water damage resistance of the aggregate. Finally, tri(2-mercaptoethyl) cyanurate containing active mercapto groups is synthesized through multi-step reaction, and then a thiol-epoxy click chemistry reaction with glycerol triglycidyl ether occurs in an oxygen atmosphere to form a crosslinked network structure, and a gel master batch with self-repairing function is prepared, which is uniformly dispersed in the matrix asphalt. It can be seen that in the experimental scheme, the aggregate accounts for the majority, and if the carbon dioxide activation step is omitted, the ceramic performance will be degraded, the pore will be reduced, and the water immersion resistance and sound insulation effect will be reduced. If the polyurethane composite modification is omitted, the reinforcement effect of the aggregate will be seriously weakened, and the water immersion resistance and noise reduction performance will be seriously reduced. If the reduction of active mercapto groups is not completed or the gel network construction is omitted, the self-repairing function will be significantly ineffective, and the comprehensive performance of the mixture will be reduced. The asphalt mixture prepared according to the complete implementation of the scheme has the sound insulation and noise reduction effect of the activated ceramic, the skeleton support and anti-peeling property of the reinforced aggregate, and the crack self-healing ability of the gel network, and the water damage resistance and low noise performance are synergistically improved. Among them, the process parameter combination represented by Example 2 shows the best balance of comprehensive performance.

[0066] It should be apparent to those skilled in the art that the application is not limited to the details of the foregoing illustrative examples, and that the present application can be carried out in other embodiments that are within the scope and spirit of the application. Therefore, from any point of view, the examples should be regarded as exemplary and non-limiting, and the scope of the present application is defined by the appended claims rather than the above description, and it is intended to encompass all changes falling within the meaning and scope of the equivalent elements of the claims. Any mark in the claims should not be considered as limiting the involved claims.

Claims

1. A low-noise, water-damage-resistant asphalt mixture, comprising the following preparation steps: (1) Using 100 parts of basalt ore as the matrix, first crush it to 100-200 mesh, add 3-8 parts of foaming agent and 5-12 parts of fluxing agent and dry mix evenly, sinter at 900-1000℃ in a vacuum environment for 1-2 hours, after sintering, raise the temperature to 1000-1100℃ and introduce 1-3L / min of carbon dioxide to regenerate the oxide into carbonate, continue to keep warm for 2-3 hours; then raise the temperature to 1100-1200℃ and react for 2-3 hours; after cooling, sieve 2-3mm particles to make porous basalt ceramics; (2) Soak the porous basalt ceramic in a 10-20% dilute hydrochloric acid solution for 30-60 min to dissolve the surface metal oxides, wash with deionized water until neutral, then dry at 60℃ to expose the hydroxyl groups, and irradiate with argon atmosphere plasma for 1-3 min to obtain pre-modified porous basalt ceramic. (3) Polyurethane prepolymer was prepared by polymerization of polyether polyol and isocyanate under nitrogen protection; 1-3 parts of coupling agent were prepared into a solution and mixed with premodified basalt porous ceramic particles and soaked for 1-2 hours; 10-30 parts of polyurethane prepolymer were added to it and mixed and degassed under vacuum for 30-50 minutes; after degassed, it was cured at gradient temperature to obtain modified basalt porous ceramic; 20-30 parts of fine aggregate and 8-10 parts of filler were added to obtain modified basalt porous ceramic hybrid aggregate. (4) Under nitrogen protection, 100 parts of cyanuric acid and 260-340 parts of phosphorus oxychloride were mixed and reacted at 80-100℃ for 3-5h. After the reaction was completed, excess phosphorus oxychloride was recovered by vacuum distillation and trichlorocyanuric acid was obtained. 400 parts of anhydrous THF were added and then 210 parts of 2-(acetylmercapto)ethyl dichlorophosphate were added in sequence. The mixture was stirred at 60-80℃ for 6-8h. After the reaction was completed, inorganic salts were removed by filtration and the filtrate was concentrated and evaporated to obtain tri(2-acetylmercaptoethyl) cyanurate. 300 parts of anhydrous methanol, 180 parts of potassium carbonate and 1 part of BHT were added. 40 parts of sodium borohydride were added in batches under an ice bath at 0-5℃. The mixture was then raised to room temperature and reacted for 2-3h. The reaction solution was acidified to neutral and then extracted with 300-400 parts of ethyl acetate. The organic phase was washed and dried to obtain tri(2-mercaptoethyl) cyanurate. (5) Dissolve tris(2-mercaptoethyl) cyanurate in 200 parts THF, add 140 parts glycerol triglycidyl ether and 8 parts catalyst, continuously introduce oxygen at 0.5-1 L / min, react at 60-80℃ for 4-6 h, evaporate the solvent after the reaction is completed to obtain self-healing gel masterbatch; add to matrix asphalt and mix to obtain self-healing gel modified asphalt material; (6) Take 90-95 parts of modified basalt porous ceramic hybrid aggregate, 6-10 parts of self-healing gel modified asphalt material, add anti-stripping agent, mix and heat to 100-120℃ and stir for 1-3 hours to obtain asphalt mixture; In step (1), the foaming agent is one of calcium carbonate, dolomite, and manganese dioxide; the co-solvent is one of potassium feldspar, calcium feldspar, and spodumene. In step (2), the amount of dilute hydrochloric acid aqueous solution used is 6-10 times the volume of the ceramic particles; In step (3), the coupling agent is one of KH-550 and KH-560; In step (3), gradient temperature curing refers to curing at 60-100℃ for 1 hour first, and then raising the temperature to 80-120℃ for 2 hours. In step (3), the fine aggregate and filler refer to machine-made basalt sand and lime powder, respectively. In step (4), 2-(acetylmercapto)ethyl dichlorophosphate is prepared by dissolving 100 parts of 2-mercaptoethanol in 200 parts of anhydrous THF under nitrogen protection, cooling to 0-5°C in an ice bath, adding dropwise a mixture of 85 parts of acetyl chloride and 95 parts of pyridine, heating to 25°C and stirring for 2 hours after titration, removing the solvent by vacuum evaporation, adding 100 parts of anhydrous THF, adding dropwise 140 parts of phosphorus oxychloride in an ice bath, stirring at 25°C for 1 hour, filtering, and evaporating and concentrating to obtain 2-(acetylmercapto)ethyl dichlorophosphate. In step (5), the base asphalt is 8-10 times the mass of the gel masterbatch; In step (6), the anti-stripping agent is AD-here LOF65-00, and the amount added is 0.2-0.6% of the total mass of the self-healing gel modified asphalt.

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