CN114395263A - Infiltration type emulsifiable asphalt and preparation method thereof - Google Patents
Infiltration type emulsifiable asphalt and preparation method thereof Download PDFInfo
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Abstract
The invention discloses infiltration type emulsifiable asphalt and a preparation method thereof, and relates to the technical field of asphalt. The invention firstly reacts nano-silica, di (triisopropyl silicon-based) amine and glycidoxypropyl trimethoxy silane to prepare amphiphilic bi-spherical modified silica sol which can emulsify asphalt and simultaneously drive the asphalt to enter tiny pores on the surface of stone material to ensure that the asphalt has adhesiveness; secondly, performing secondary modification, introducing chitosan and dodecane primary amine, reducing the surface tension of the asphalt emulsion, and improving the adhesion of asphalt; then stripping the expanded graphite by microwave ultrasonic to prepare mesoporous nanosheets, and depositing magnetic iron by pulsed current assisted plasma sputtering to obtain magnetic nanosheets; and then, stirring the magnetic nanosheet and the modified asphalt emulsion in a magnetic field, and shearing to form a three-dimensional network structure, so that the modified asphalt emulsion has a low-temperature resistant effect. The prepared infiltration type emulsifiable asphalt has the effects of high adhesion and low temperature resistance.
Description
Technical Field
The invention relates to the technical field of asphalt, in particular to infiltration type emulsifiable asphalt and a preparation method thereof.
Background
Asphalt pavement refers to various types of pavement that are made by incorporating into mineral materials a road asphalt material. The asphalt binder improves the capability of the paving aggregate to resist damage of traveling vehicles and natural factors to the pavement, and enables the pavement to be smooth, less in dust, impermeable and durable. Accordingly, asphalt pavement is one of the most widely used high-grade pavements in road construction.
At present, the bonding effect of asphalt and stone is poor, the adhesion is usually 2-3 grades, and the standard requirement cannot be met, at the moment, the adhesion of the asphalt and the stone is improved by adding an anti-stripping agent, cement or slaked lime and other additives in a common treatment method, but the prepared asphalt has higher viscosity compared with the common asphalt, and can meet the national industry standard requirement without adding additives even if being bonded with the stone.
In addition, with the development of Chinese highway traffic, the construction of Chinese highways enters a period of high-speed development, and new conditions such as high speed, heavy load, complex stress bearing and the like all put higher requirements on high-grade pavements, but the problems of poor temperature stability and easy brittle fracture in winter of asphalt materials on the market generally exist, and the use of the asphalt pavements is severely restricted. Therefore, the invention improves the low-temperature cracking resistance of the asphalt while increasing the adhesiveness of the asphalt.
Disclosure of Invention
The invention aims to provide infiltration type emulsifiable asphalt and a preparation method thereof, which are used for solving the problems in the prior art.
In order to solve the technical problems, the invention provides the following technical scheme: the infiltration type emulsifiable asphalt is characterized by mainly comprising, by weight, 100-200 parts of matrix asphalt, 30-40 parts of magnetic nanosheets, 16-22 parts of modified silica sol, 0.6-2 parts of rubber operating oil and 0.09-0.2 part of sulfur.
Further, the matrix asphalt is one or a mixture of more of natural asphalt, coal tar asphalt or petroleum asphalt.
Further, the modified silica sol is prepared by reacting nano-silica, bis (triisopropylsilyl) amine and glycidoxypropyltrimethoxysilane to obtain an amphiphilic microspherical sol.
Furthermore, the magnetic nanosheet is prepared by the following method, namely firstly stripping expanded graphite by microwave ultrasonic to prepare a mesoporous nanosheet, and then depositing magnetic iron by pulse current assisted plasma sputtering.
Further, the preparation method of the infiltration type emulsifiable asphalt is characterized by mainly comprising the following preparation steps:
(1) placing the modified silica sol into a container, adding 5% by mass of hydrochloric acid until the pH of the solution is 5-6, adding 2.1-2.8 by mass of sodium chloride of the modified silica sol, heating to 75-80 ℃, and stirring at 100-200 rpm for 2-3 min to obtain an emulsifier; adding an emulsifier and matrix asphalt into a colloid mill preheated to 70-80 ℃ according to the mass ratio of 4: 100-6: 100, and shearing at 3000-3600 rpm for 10-14 min to obtain asphalt emulsion;
(2) adding chitosan, acetic acid and deionized water into a container according to the mass ratio of 1:0.9: 70-1: 1.1:70, stirring and dissolving, adding an asphalt emulsion with the mass of 0.8-0.9 times that of the chitosan, placing the mixture into an oil bath kettle at the temperature of 100-110 ℃, stirring at 50-100 rpm for 20-24 hours, cooling to 50-60 ℃, and distilling at the temperature of 115-120 ℃ and the pressure of 0.1-0.3 MPa for 4-5 hours to obtain a glycosyl asphalt emulsion;
(3) putting the glycosyl asphalt emulsion, the dodecane primary amine and the methanol into a container according to the mass ratio of 1:0.6: 8-1: 0.7:9, stirring for 20-24 hours at 200-300 rpm, putting into an ice water bath, adding sodium borohydride with the mass of 0.2-0.3 time of that of the glycosyl asphalt emulsion, stirring at the same speed until no bubbles are generated, then adding hydrochloric acid with the mass fraction of 10% until the pH value of the solution is 1-2, and performing suction filtration to obtain a filter cake; washing the filter cake with ice water and acetic acid for 3-5 times in sequence, drying at 70-80 ℃ and 0.01-0.03 MPa for 3-4 h, adding a methanol/sodium methoxide solution with the mass of 4-6 times of that of the glycosyl asphalt emulsion, stirring at 100-200 rpm for 20-24 h with the mass ratio of methanol to sodium methoxide being 2.2: 1-2.6: 1, heating to 85-90 ℃, reacting for 1-2 h, cooling to room temperature, and performing suction filtration to obtain a modified emulsion;
(4) expanding the flake graphite, performing microwave ultrasonic stripping to obtain a nanosheet, and performing magnetic modification to obtain a magnetic nanosheet;
(5) placing the magnetic nanosheets and the modified emulsion in a magnetic field with a mass ratio of 1: 5-1: 8 at 25-35 Hz, uniformly stirring, shearing at 170-180 ℃ for 30-45 min, adding sulfur with a mass of 0.003-0.005 times that of the magnetic nanosheets and rubber operating oil with a mass of 0.02-0.05 times that of the magnetic nanosheets, and stirring and developing at 150-180 ℃ for 1-2 h to obtain the infiltration type emulsifiable asphalt.
Further, the preparation method of the modified silica sol in the step (1) comprises the following steps:
a. adding tetraethoxysilane, absolute ethyl alcohol, deionized water and 25-28% ammonia water in a mass ratio of 1:8.2:0.2: 0.05-1: 8.7:0.3:0.06 into a beaker, stirring for 2-3 hours at 30 ℃ and 100-200 rpm, and aging for 6-7 days at room temperature to obtain nano-silica sol;
b. adding the nano-silica sol into a container, adding bis (triisopropylsilyl) amine with the mass of 0.25-0.33 times that of the nano-silica sol, stirring at 30-40 ℃ and 200-300 rpm for 2-3 h, and aging at room temperature for 6-7 d to obtain lipophilic nano-silica sol;
c. adding the nano-silica sol into a container, adding glycidoxypropyltrimethoxysilane of which the mass is 0.5-0.6 times that of the nano-silica sol, stirring at 30-40 ℃ and 200-300 rpm for 1-2 h, and aging at room temperature for 6-7 d to obtain hydrophilic nano-silica sol;
d. adding lipophilic nano-silica sol into a container, adding aminopropyltriethoxysilane which is 0.0009-0.001 time of the mass of the lipophilic nano-silica sol, stirring at 30-40 ℃ and 100-200 rpm for 5-7 h, adding hydrophilic nano-silica sol which is 1-1.5 times of the mass of the lipophilic nano-silica sol, stirring at the same temperature and speed for 30-45 min, and aging at room temperature for 6-7 d to obtain the modified silica sol.
Further, the specific preparation steps of the magnetic nanosheet in the step (4) are as follows:
A. uniformly stirring and mixing the flake graphite and potassium permanganate according to the mass ratio of 10:1, adding concentrated sulfuric acid with the mass fraction of 85% and the mass fraction of 2-3 times of the flake graphite, placing the mixture into a water bath kettle at 35-40 ℃, stirring the mixture for 80-90 min at 100-200 rpm, sequentially washing the mixture with hydrochloric acid and deionized water with the mass fraction of 10% until the pH of the solution is 6-7, filtering the mixture, drying the mixture for 1-2 h at 60-70 ℃, placing the dried mixture into a microwave oven, pretreating for 15-20 s, adding a methyl formamide/water mixed solution with the mass fraction of 2-3 times of the flake graphite, ultrasonically stripping the methyl formamide/water mixed solution for 4-5 h at 40-50 ℃ to prepare a graphene nanosheet;
B. placing the graphene nanosheets in a plasma sputtering instrument, treating for 3-5 min, and placing at a current density of
And (3) in a 14-15A/mm & lt-2 & gt pulse current auxiliary sintering furnace, heating to 400-500 ℃ at a speed of 10-15 ℃/min, pressurizing to 40-50 MPa, keeping the temperature and pressure for 3-5 min, and cooling to room temperature to obtain the magnetic nanosheets.
Further, the power of the microwave oven in the step A is 10-20 kW, and the heating temperature is 900-950 ℃; the frequency of ultrasonic stripping is 30-35 kHz.
Further, the vacuum degree of the plasma sputtering instrument in the step B is 1 multiplied by 10-4～4×10-4And Pa, introducing oxygen mixed gas, wherein the volume ratio of oxygen to argon in the oxygen mixed gas is 10:16, the sputtering pressure is 2-5 Pa, the sputtering power is 120-200W, and the target material is a pure iron target.
Further, the shearing rotating speed in the step (5) is 5000-8000 rpm; the stirring speed is 600-800 rpm.
Compared with the prior art, the invention has the following beneficial effects:
the asphalt is prepared through the steps of asphalt emulsion preparation, magnetic nanosheet preparation, shearing treatment and the like in sequence, so that the effects of good adhesion and low-temperature cracking resistance are achieved.
Firstly, reacting hydroxyl on the surface of nano silicon dioxide with silyl of bis (triisopropylsilyl) amine to prepare lipophilic nano silicon dioxide sol; taking another part of nano silicon dioxide, reacting with silane group of glycidoxypropyltrimethoxysilane, and aging to obtain hydrophilic nano silicon dioxide sol, wherein part of epoxy groups are changed into hydroxyl groups; the amido on the surface of the lipophilic nano-silica sol reacts with the residual epoxy group of the hydrophilic nano-silica sol to prepare the bi-spherical modified silica sol which has hydrophilicity and lipophilicity and can be used as an asphalt emulsifier to form asphalt emulsion, the oleophilic end wraps the surface of the asphalt, and the hydrophilic end drives the asphalt to enter tiny pores on the surface of stone materials to ensure that the asphalt has adhesiveness; and then introducing chitosan and dodecane primary amine to modify the modified chitosan, reacting the amino group of the chitosan with the hydroxyl group of the hydrophilic nano silica sol, and simultaneously reacting the hydroxyl group of the chitosan with the amino group of the dodecane primary amine to graft the chitosan and the dodecane primary amine into the molecular chain of the asphalt emulsion, so that the surface tension of the asphalt emulsion is reduced, and the adhesion of asphalt is further improved.
Secondly, ultrasonically stripping expanded graphite by using microwaves, wherein under the action of microwaves, oxygen-containing groups in the graphite are thermally decomposed to release gas, and pores are formed on the surface, so that mesoporous nano sheets are ultrasonically stripped; then carrying out magnetic modification treatment on the nanosheets, depositing magnetic iron by pulse current assisted plasma sputtering, ionizing gas molecules by the plasma sputtering through direct-current voltage between two electrodes in a vacuum state, generating glow discharge, bombarding a metal iron target and knocking out atoms of the metal iron target to form high-current metal iron plasma ion beams, depositing the high-current metal iron plasma ion beams on the surface layers of the nanosheets, and simultaneously giving higher energy to the metal iron by the pulse current to further grow the metal iron to form nanowires; then adding the magnetic nano-sheets into the asphalt emulsion, applying an electric field to rapidly disperse the magnetic nano-sheets in the asphalt emulsion, adhering the magnetic nano-sheets to the medium holes of the magnetic nano-sheets by utilizing the adhesiveness of the asphalt emulsion, wrapping part of nano-wires with the asphalt emulsion, and fixing the nano-wires on the magnetic nano-sheets, wherein when the asphalt shrinks at low temperature, the nano-wires on the surface fill the shrinkage holes among the asphalt, so that the asphalt is prevented from cracking at low temperature, and the asphalt has better low-temperature resistance; and finally, carrying out shearing treatment, and winding and connecting the residual nanowires under the action of high-speed shearing force, so that the asphalt is crosslinked to form a three-dimensional network structure, the asphalt has stability and elasticity, the low-temperature cracking phenomenon of the asphalt is prevented, and the low-temperature resistance effect of the asphalt is improved.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
In order to more clearly illustrate the method of the present invention, the following examples are given, and the method for testing each index of the wet type emulsified asphalt prepared in the following examples is as follows:
adhesion: the adhesion effect test is carried out on the embodiment and the comparative example which have the same mass according to JTJ 052 test procedure of asphalt and asphalt mixture for highway engineering.
Low temperature resistance: the low temperature resistance effect test is carried out on the embodiment and the comparative example with the same mass, and the JTGE 20 test procedure for road engineering asphalt and asphalt mixture is referred.
Example 1
The infiltration type emulsifiable asphalt mainly comprises the following components in parts by weight: 100 parts of petroleum asphalt, 30 parts of magnetic nanosheets, 16 parts of modified silica sol, 0.6 part of rubber operating oil and 0.09 part of sulfur.
A preparation method of infiltration type emulsifiable asphalt mainly comprises the following preparation steps:
(1) adding tetraethoxysilane, absolute ethyl alcohol, deionized water and 25% ammonia water in a mass ratio of 1:8.2:0.2:0.05 into a beaker, stirring for 3 hours at 30 ℃ and 100rpm, and aging for 6 days at room temperature to obtain nano-silica sol;
(2) adding the nano-silica sol into a container, adding di (triisopropylsilyl) amine with the mass of 0.25 time of that of the nano-silica sol, stirring at 30 ℃ and 200rpm for 3 hours, and aging at room temperature for 6 days to obtain lipophilic nano-silica sol;
(3) adding the nano-silica sol into a container, adding glycidoxypropyltrimethoxysilane of which the mass is 0.5 time that of the nano-silica sol, stirring at 30 ℃ and 200rpm for 2h, and aging at room temperature for 6d to obtain hydrophilic nano-silica sol;
(4) adding lipophilic nano-silica sol into a container, adding aminopropyltriethoxysilane which is 0.0009 time of the mass of the lipophilic nano-silica sol, stirring at 30 ℃ and 100rpm for 7 hours, adding hydrophilic nano-silica sol which is 1 time of the mass of the lipophilic nano-silica sol, stirring at the same temperature and speed for 45 minutes, and aging at room temperature for 6 days to obtain modified silica sol;
(5) placing the modified silica sol in a container, adding hydrochloric acid with the mass fraction of 5% until the pH of the solution is 5, adding sodium chloride with the mass of 2.1 of the modified silica sol, heating to 75 ℃, and stirring at 100rpm for 3min to obtain an emulsifier; adding an emulsifier and petroleum asphalt into a colloid mill preheated to 70 ℃ according to the mass ratio of 4:100, and shearing at 3000rpm for 14min to obtain asphalt emulsion;
(6) adding chitosan, acetic acid and deionized water into a container according to the mass ratio of 1:0.9:70, stirring and dissolving, adding asphalt emulsion with the mass of 0.8 time that of the chitosan, placing the mixture into an oil bath kettle at 100 ℃, stirring at 50rpm for 24 hours, cooling to 50 ℃, and distilling at 115 ℃ and 0.1MPa for 4 hours to obtain glycosyl asphalt emulsion;
(7) placing the glycosyl asphalt emulsion, the dodecane primary amine and the methanol in a mass ratio of 1:0.6:8 in a container, stirring at 200rpm for 24 hours, placing in an ice water bath, adding sodium borohydride which is 0.2 times of the mass of the glycosyl asphalt emulsion, stirring at the same speed until no bubbles are generated, then adding hydrochloric acid with the mass fraction of 10% until the pH value of the solution is 1, and performing suction filtration to obtain a filter cake; washing the filter cake with ice water and acetic acid for 3 times, drying at 70 ℃ under 0.01MPa for 3h, adding methanol/sodium methoxide solution with the mass ratio of 4 times that of the glycosyl asphalt emulsion, wherein the mass ratio of methanol to sodium methoxide in the methanol/sodium methoxide solution is 2.2:1, stirring at 100rpm for 24h, heating to 85 ℃, reacting for 2h, cooling to room temperature, and performing suction filtration to obtain modified emulsion;
(8) uniformly stirring and mixing the flake graphite and potassium permanganate according to the mass ratio of 10:1, adding concentrated sulfuric acid with the mass fraction of 85% and the mass fraction of 2 times of the flake graphite, placing the mixture in a 35 ℃ water bath kettle, stirring the mixture at 100rpm for 90min, sequentially washing the mixture by using hydrochloric acid with the mass fraction of 10% and deionized water until the pH of the solution is 6, filtering the mixture, drying the mixture at 60 ℃ for 2h, placing the dried mixture in a microwave oven with the power of 10kW, heating the dried mixture to 900 ℃, pretreating the dried mixture for 20s, adding a methyl formamide/water mixed solution with the mass fraction of 2 times of the flake graphite, and ultrasonically stripping the methyl formamide/water mixed solution for 5h at the mass ratio of 8.73:1, 40 ℃ and 30kHz to prepare a graphene nanosheet;
(9) placing graphene nanosheets in a plasma sputtering instrument, treating for 3min, and placing at a current density of 14A/mm-2The pulse current auxiliary sintering furnace is heated to 400 ℃ at the speed of 10 ℃/min, pressurized to 40MPa, kept at the temperature and pressure for 3min, and cooled to room temperature to obtain magnetic nano sheets; the vacuum degree of the plasma sputtering instrument is 1 multiplied by 10-4Pa, introducing oxygen mixed gas, wherein the volume ratio of oxygen to argon in the oxygen mixed gas is 10:16, the sputtering pressure is 2Pa, the sputtering power is 120W, and the target material is a pure iron target;
(10) and (2) placing the magnetic nanosheets and the modified emulsion in a magnetic field with the mass ratio of 1:5 at 25Hz, uniformly stirring, shearing at 170 ℃ and 5000rpm for 45min, adding sulfur with the mass of 0.003 time of that of the magnetic nanosheets and rubber operating oil with the mass of 0.02 time of that of the magnetic nanosheets, and stirring and developing at 150 ℃ and 600rpm for 2h to obtain the infiltration type emulsifiable asphalt.
Example 2
The infiltration type emulsifiable asphalt mainly comprises the following components in parts by weight: 160 parts of petroleum asphalt, 35 parts of magnetic nanosheets, 19 parts of modified silica sol, 1.05 parts of rubber process oil and 0.14 part of sulfur.
A preparation method of infiltration type emulsifiable asphalt mainly comprises the following preparation steps:
(1) adding tetraethoxysilane, absolute ethyl alcohol, deionized water and ammonia water with the mass fraction of 26% into a beaker according to the mass ratio of 1:8.41:0.24:0.057, stirring for 2.5 hours at 30 ℃ and 160rpm, and aging for 7 days at room temperature to obtain nano silicon dioxide sol;
(2) adding the nano-silica sol into a container, adding di (triisopropylsilyl) amine with the mass of 0.29 time of that of the nano-silica sol, stirring at 35 ℃ and 250rpm for 2.5 hours, and aging at room temperature for 6 days to obtain lipophilic nano-silica sol;
(3) adding the nano-silica sol into a container, adding glycidoxypropyltrimethoxysilane of which the mass is 0.56 times that of the nano-silica sol, stirring at 34 ℃ and 270rpm for 1.5h, and aging at room temperature for 7d to obtain hydrophilic nano-silica sol;
(4) adding lipophilic nano-silica sol into a container, adding aminopropyltriethoxysilane which is 0.001 time of the mass of the lipophilic nano-silica sol, stirring at 33 ℃ and 140rpm for 6 hours, adding hydrophilic nano-silica sol which is 1.41 times of the mass of the lipophilic nano-silica sol, stirring at the same temperature and speed for 42 minutes, and aging at room temperature for 7 days to obtain modified silica sol;
(5) placing the modified silica sol in a container, adding 5% by mass of hydrochloric acid until the pH of the solution is 5.5, adding 2.5% by mass of sodium chloride of the modified silica sol, heating to 78 ℃, and stirring at 180rpm for 3min to obtain an emulsifier; adding an emulsifier and petroleum asphalt into a colloid mill preheated to 77 ℃ according to the mass ratio of 5:100, and shearing at 3400rpm for 13min to obtain asphalt emulsion;
(6) adding chitosan, acetic acid and deionized water into a container according to the mass ratio of 1:1.07:70, stirring and dissolving, adding asphalt emulsion with the mass of 0.84 time that of the chitosan, placing the mixture into an oil bath kettle at 145 ℃, stirring at 70rpm for 22 hours, cooling to 57 ℃, and distilling at 118 ℃ and 0.2MPa for 4.5 hours to obtain glycosyl asphalt emulsion;
(7) placing the glycosyl asphalt emulsion, the dodecane primary amine and the methanol into a container according to the mass ratio of 1:0.66:8.19, stirring at 255rpm for 22 hours, placing into an ice water bath, adding sodium borohydride which is 0.27 times of the mass of the glycosyl asphalt emulsion, stirring at the same speed until no bubbles are generated, then adding hydrochloric acid with the mass fraction of 10% until the pH value of the solution is 1.5, and performing suction filtration to obtain a filter cake; washing the filter cake with ice water and acetic acid sequentially for 4 times, drying at 74 ℃ and 0.02MPa for 3.5h, adding methanol/sodium methoxide solution with the mass ratio of methanol to sodium methoxide being 2.4:1, the mass ratio of methanol to sodium methoxide in the methanol/sodium methoxide solution being 5 times of that of the glycosyl asphalt emulsion, stirring at 180rpm for 23h, heating to 89 ℃, reacting for 1.5h, cooling to room temperature, and performing suction filtration to obtain modified emulsion;
(8) uniformly stirring and mixing the flake graphite and potassium permanganate according to the mass ratio of 10:1, adding concentrated sulfuric acid with the mass fraction of 85% and the mass fraction of 2.78 times of the mass of the flake graphite, placing the flake graphite in a 38 ℃ water bath, stirring the mixture at 150rpm for 88min, sequentially washing the flake graphite with hydrochloric acid with the mass fraction of 10% and deionized water until the pH of the solution is 6.5, filtering the solution, drying the flake graphite at 68 ℃ for 1.5h, placing the flake graphite in a microwave oven with the power of 16kW, heating the flake graphite to 944 ℃ for pretreatment for 18s, adding a methyl formamide/water mixed solution with the mass fraction of 2.71 times of the mass of the flake graphite, ultrasonically stripping the flake graphite for 4.5h at the mass ratio of 8.73:1, 43 ℃ and 32kHz to prepare a graphene nanosheet;
(9) placing graphene nanosheets in a plasma sputtering instrument, treating for 4min, and placing at a current density of 15A/mm-2The temperature is raised to 456 ℃ at the speed of 12 ℃/min in the pulse current auxiliary sintering furnace, the pressure is increased to 48MPa, the temperature and the pressure are kept for 4min, and then the magnetic nano-sheet is obtained after cooling to room temperature; the vacuum degree of the plasma sputtering instrument is 2 multiplied by 10-4Pa, introducing oxygen mixed gas, wherein the volume ratio of oxygen to argon in the oxygen mixed gas is 10:16, the sputtering pressure is 4Pa, the sputtering power is 170W, and the target material is a pure iron target;
(10) and (2) placing the magnetic nanosheets and the modified emulsion in a magnetic field with the mass ratio of 1:7 at 30Hz, uniformly stirring, shearing at 177 ℃ and 6000rpm for 41min, adding sulfur with the mass of 0.004 time of that of the magnetic nanosheets and rubber operating oil with the mass of 0.03 time of that of the magnetic nanosheets, and stirring and developing at 169 ℃ and 700rpm for 1.5h to obtain the infiltration type emulsifiable asphalt.
Example 3
The infiltration type emulsifiable asphalt mainly comprises the following components in parts by weight: 200 parts of petroleum asphalt, 40 parts of magnetic nanosheets, 22 parts of modified silica sol, 2 parts of rubber operating oil and 0.2 part of sulfur.
A preparation method of infiltration type emulsifiable asphalt mainly comprises the following preparation steps:
(1) adding tetraethoxysilane, absolute ethyl alcohol, deionized water and 28% ammonia water into a beaker according to the mass ratio of 1:8.7:0.3:0.06, stirring for 2 hours at 30 ℃ and 200rpm, and aging for 7 days at room temperature to obtain nano silicon dioxide sol;
(2) adding the nano-silica sol into a container, adding di (triisopropylsilyl) amine with the mass of 0.33 time of that of the nano-silica sol, stirring at 40 ℃ and 300rpm for 2 hours, and aging at room temperature for 7 days to obtain lipophilic nano-silica sol;
(3) adding the nano-silica sol into a container, adding glycidoxypropyltrimethoxysilane with the mass of 0.6 time that of the nano-silica sol, stirring at 40 ℃ and 300rpm for 1h, and aging at room temperature for 7d to obtain hydrophilic nano-silica sol;
(4) adding lipophilic nano-silica sol into a container, adding aminopropyltriethoxysilane which is 0.001 time of the mass of the lipophilic nano-silica sol, stirring at 40 ℃ and 200rpm for 5 hours, adding hydrophilic nano-silica sol which is 1.5 times of the mass of the lipophilic nano-silica sol, stirring at the same temperature and speed for 30 minutes, and aging at room temperature for 7 days to obtain modified silica sol;
(5) placing the modified silica sol in a container, adding 5% by mass of hydrochloric acid until the pH of the solution is 6, adding 2.8% by mass of sodium chloride of the modified silica sol, heating to 80 ℃, and stirring at 200rpm for 2min to obtain an emulsifier; adding the emulsifier and the asphalt into a colloid mill preheated to 80 ℃ according to the mass ratio of 6:100, and shearing at 3600rpm for 10min to obtain asphalt emulsion;
(6) adding chitosan, acetic acid and deionized water into a container according to the mass ratio of 1:0.1:70, stirring and dissolving, adding asphalt emulsion with the mass of 0.9 time that of the chitosan, placing the mixture into an oil bath kettle at 110 ℃, stirring at 100rpm for 20 hours, cooling to 60 ℃, and distilling at 120 ℃ and 0.3MPa for 5 hours to obtain glycosyl asphalt emulsion;
(7) placing the glycosyl asphalt emulsion, the dodecane primary amine and the methanol into a container according to the mass ratio of 1:0.7:9, stirring for 20 hours at 300rpm, placing into an ice water bath, adding sodium borohydride which is 0.3 times of the mass of the glycosyl asphalt emulsion, stirring at the same speed until no bubbles are generated, then adding hydrochloric acid with the mass fraction of 10% until the pH value of the solution is 2, and performing suction filtration to obtain a filter cake; washing the filter cake with ice water and acetic acid for 5 times, drying at 80 ℃ and 0.03MPa for 4 hours, adding methanol/sodium methoxide solution with the mass ratio of methanol to sodium methoxide being 2.6:1, the mass ratio of methanol to sodium methoxide in the methanol/sodium methoxide solution being 6 times of that of the glycosyl asphalt emulsion, stirring at 200rpm for 20 hours, heating to 90 ℃, reacting for 2 hours, cooling to room temperature, and performing suction filtration to obtain modified emulsion;
(8) uniformly stirring and mixing the flake graphite and potassium permanganate according to the mass ratio of 10:1, adding concentrated sulfuric acid with the mass fraction of 85% and the mass fraction of 3 times of the flake graphite, placing the mixture in a 40 ℃ water bath, stirring the mixture for 80min at 200rpm, sequentially washing the mixture by using hydrochloric acid with the mass fraction of 10% and deionized water until the pH of the solution is 7, filtering the mixture, drying the mixture for 2h at 70 ℃, placing the dried mixture in a microwave oven with the power of 20kW, heating the mixture to 950 ℃, pretreating the mixture for 15s, adding a methyl formamide/water mixed solution with the mass fraction of 3 times of the flake graphite, and ultrasonically stripping the methyl formamide/water mixed solution for 4h at the mass ratio of 8.73:1, 50 ℃ and 35kHz to prepare a graphene nanosheet;
(9) placing graphene nanosheets in a plasma sputtering instrument, treating for 5min, and placing at a current density of 15A/mm-2The pulse current auxiliary sintering furnace is heated to 500 ℃ at the speed of 15 ℃/min, pressurized to 50MPa, kept at the temperature and pressure for 5min, and cooled to room temperature to obtain magnetic nano sheets; the vacuum degree of the plasma sputtering instrument is 4 multiplied by 10-4Pa, introducing oxygen mixed gas, wherein the volume ratio of oxygen to argon in the oxygen mixed gas is 10:16, the sputtering pressure is 5Pa, the sputtering power is 200W, and the target material is a pure iron target;
(10) and (2) placing the magnetic nano sheet and the modified emulsion in a 35Hz magnetic field according to the mass ratio of 1:8, uniformly stirring, shearing at 180 ℃ and 8000rpm for 30min, adding sulfur with the mass of 0.005 time of the magnetic nano sheet and rubber operating oil with the mass of 0.05 time of the magnetic nano sheet, and stirring and developing at 180 ℃ and 800rpm for 1h to obtain the infiltration type emulsifiable asphalt.
Comparative example 1
The infiltration type emulsifiable asphalt mainly comprises the following components in parts by weight: 160 parts of petroleum asphalt, 35 parts of magnetic nanosheets, 1.05 parts of rubber operating oil and 0.14 part of sulfur.
A preparation method of infiltration type emulsifiable asphalt mainly comprises the following preparation steps:
(1) uniformly stirring and mixing the flake graphite and potassium permanganate according to the mass ratio of 10:1, adding concentrated sulfuric acid with the mass fraction of 85% and the mass fraction of 2.78 times of the mass of the flake graphite, placing the flake graphite in a 38 ℃ water bath, stirring the mixture at 150rpm for 88min, sequentially washing the flake graphite with hydrochloric acid with the mass fraction of 10% and deionized water until the pH of the solution is 6.5, filtering the solution, drying the flake graphite at 68 ℃ for 1.5h, placing the flake graphite in a microwave oven with the power of 16kW, heating the flake graphite to 944 ℃ for pretreatment for 18s, adding a methyl formamide/water mixed solution with the mass fraction of 2.71 times of the mass of the flake graphite, ultrasonically stripping the flake graphite for 4.5h at the mass ratio of 8.73:1, 43 ℃ and 32kHz to prepare a graphene nanosheet;
(2) placing graphene nanosheets in a plasma sputtering instrument, treating for 4min, and placing at a current density of 15A/mm-2The temperature is raised to 456 ℃ at the speed of 12 ℃/min in the pulse current auxiliary sintering furnace, the pressure is increased to 48MPa, the temperature and the pressure are kept for 4min, and then the magnetic nano-sheet is obtained after cooling to room temperature; the vacuum degree of the plasma sputtering instrument is 2 multiplied by 10-4Pa, introducing oxygen mixed gas, wherein the volume ratio of oxygen to argon in the oxygen mixed gas is 10:16, the sputtering pressure is 4Pa, the sputtering power is 170W, and the target material is a pure iron target;
(3) and (2) placing the magnetic nanosheets and the modified emulsion in a magnetic field with the mass ratio of 1:7 at 30Hz, uniformly stirring, shearing at 177 ℃ and 6000rpm for 41min, adding sulfur with the mass of 0.004 time of that of the magnetic nanosheets and rubber operating oil with the mass of 0.03 time of that of the magnetic nanosheets, and stirring and developing at 169 ℃ and 700rpm for 1.5h to obtain the infiltration type emulsifiable asphalt.
Comparative example 2
Comparative example 2 was formulated in the same manner as in example 2. The preparation method of the wet type emulsifiable asphalt is different from that of example 2 only in that the steps (6) and (7) are not included. The rest of the preparation steps are the same as example 2.
Comparative example 3
The formulation of comparative example 3 was the same as that of example 2. The preparation method of the infiltration type emulsified asphalt is different from that of the embodiment 2 only in the step (9), and the step (9) is changed into the following steps: and (3) placing the graphene nanosheets in a plasma sputtering instrument, treating for 4min, and cooling to room temperature to obtain the magnetic nanosheets. The rest of the preparation steps are the same as example 1
Comparative example 4
The infiltration type emulsifiable asphalt mainly comprises the following components in parts by weight: 160 parts of petroleum asphalt, 35 parts of magnetic nanosheets, 1.05 parts of rubber operating oil and 0.14 part of sulfur.
A preparation method of infiltration type emulsifiable asphalt mainly comprises the following preparation steps:
(1) uniformly stirring and mixing the flake graphite and potassium permanganate according to the mass ratio of 10:1, adding concentrated sulfuric acid with the mass fraction of 85% and the mass fraction of 2.78 times of the mass of the flake graphite, placing the flake graphite in a 38 ℃ water bath, stirring the mixture at 150rpm for 88min, sequentially washing the flake graphite with hydrochloric acid with the mass fraction of 10% and deionized water until the pH of the solution is 6.5, filtering the solution, drying the flake graphite at 68 ℃ for 1.5h, placing the flake graphite in a microwave oven with the power of 16kW, heating the flake graphite to 944 ℃ for pretreatment for 18s, adding a methyl formamide/water mixed solution with the mass fraction of 2.71 times of the mass of the flake graphite, ultrasonically stripping the flake graphite for 4.5h at the mass ratio of 8.73:1, 43 ℃ and 32kHz to prepare a graphene nanosheet;
(2) placing graphene nanosheets in a plasma sputtering instrument, treating for 4min, and placing at a current density of 15A/mm-2The temperature is raised to 456 ℃ at the speed of 12 ℃/min in the pulse current auxiliary sintering furnace, the pressure is increased to 48MPa, the temperature and the pressure are kept for 4min, and then the magnetic nano-sheet is obtained after cooling to room temperature; the vacuum degree of the plasma sputtering instrument is 2 multiplied by 10-4Pa, introducing oxygen mixed gas, wherein the volume ratio of oxygen to argon in the oxygen mixed gas is 10:16, the sputtering pressure is 4Pa, the sputtering power is 170W, and the target material is a pure iron target;
(3) and (2) placing the magnetic nanosheets and the asphalt in a magnetic field with a mass ratio of 1:7 at 30Hz, uniformly stirring, shearing at 177 ℃ and 6000rpm for 41min, adding sulfur with the mass of 0.004 time of that of the magnetic nanosheets and rubber operating oil with the mass of 0.03 time of that of the magnetic nanosheets, and stirring and developing at 169 ℃ and 700rpm for 1.5h to obtain the infiltration type emulsifiable asphalt.
Examples of effects
Table 1 below shows the results of performance analysis of the wet type emulsifiable asphalts using examples 1 to 3 of the present invention and comparative examples 1 to 4.
TABLE 1
Compared with the experimental data of the examples 1, 2 and 3 and the comparative example 4, the modified silicon dioxide is used as the emulsifier to drive the asphalt to adhere to the stone surface, so that the adhesion of the asphalt is improved, and simultaneously, chitosan and dodecane primary amine are introduced to further modify, so that the surface free energy is reduced, and the adhesion of the asphalt is improved; magnetic iron is deposited on the surface of the mesoporous nanosheet by using pulse current assisted vacuum arc plasma discharge, the mesoporous nanosheet is modified, asphalt is adhered by using mesopores, the asphalt is uniformly dispersed, and meanwhile, the magnetic nanowires on the surface of the nanosheet are mutually wound and connected in the shearing treatment process, so that the asphalt is in a three-dimensional network structure and has low-temperature resistance; from the comparison of experimental data of examples 1, 2 and 3 and comparative examples 1 and 2, it can be found that the nano-silica respectively reacts with di (triisopropylsilyl) amine and glycidoxypropyltrimethoxysilane to prepare lipophilic and hydrophilic sols, and the sols are assembled into a double-sphere shape, one end of the sols is wrapped on the surface of the asphalt, and the other end of the sols drives the asphalt to enter the stone gap, so that the asphalt has better adhesiveness; in addition, after the nano silicon dioxide is subjected to primary modification, chitosan and dodecane primary amine are introduced for secondary modification, so that the surface free energy of the asphalt is reduced, and the adhesion of the asphalt is improved; from the comparison of the experimental data of the examples 1, 2 and 3 and the comparative example 3, it can be found that if the magnetic nanosheets are prepared without the assistance of the pulse current, the pulse current cannot endow the metallic iron with high energy, so that the iron deposited on the surfaces of the nanosheets cannot further grow to grow nanowires, and in the subsequent shearing process, the nanosheets cannot be cross-linked with each other, so that a three-dimensional network structure cannot be formed among asphalt molecules, and the low-temperature resistance of the asphalt is poor.
It will be evident to those skilled in the art that the invention is not limited to the details of the foregoing illustrative embodiments, and that the present invention may be embodied in other specific forms without departing from the spirit or essential attributes thereof. The present embodiments are therefore to be considered in all respects as illustrative and not restrictive, the scope of the invention being indicated by the appended claims rather than by the foregoing description, and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein. Any reference sign in a claim should not be construed as limiting the claim concerned.
Claims (10)
1. The infiltration type emulsifiable asphalt is characterized by mainly comprising, by weight, 100-200 parts of matrix asphalt, 30-40 parts of magnetic nanosheets, 16-22 parts of modified silica sol, 0.6-2 parts of rubber operating oil and 0.09-0.2 part of sulfur.
2. The asphalt of claim 1, wherein the base asphalt is one or more of natural asphalt, coal tar asphalt, and petroleum asphalt.
3. The asphalt of claim 2, wherein the modified silica sol is an amphiphilic bi-spherical sol prepared by reacting nano-silica, bis (triisopropylsilyl) amine and glycidoxypropyltrimethoxysilane.
4. The infiltration type emulsifiable asphalt of claim 3, wherein the magnetic nanosheets are prepared by microwave ultrasonic exfoliation of expanded graphite to prepare mesoporous nanosheets, and pulsed current assisted plasma sputtering to deposit magnetic iron.
5. The preparation method of the infiltration type emulsifiable asphalt is characterized by mainly comprising the following preparation steps:
(1) placing the modified silica sol into a container, adding 5% by mass of hydrochloric acid until the pH of the solution is 5-6, adding 2.1-2.8 times of sodium chloride by mass of the modified silica sol, heating to 75-80 ℃, and stirring at 100-200 rpm for 2-3 min to obtain an emulsifier; adding an emulsifier and matrix asphalt into a colloid mill preheated to 70-80 ℃ according to the mass ratio of 4: 100-6: 100, and shearing at 3000-3600 rpm for 10-14 min to obtain asphalt emulsion;
(2) adding chitosan, acetic acid and deionized water into a container according to the mass ratio of 1:0.9: 70-1: 1.1:70, stirring and dissolving, adding an asphalt emulsion with the mass of 0.8-0.9 times that of the chitosan, placing the mixture into an oil bath kettle at the temperature of 100-110 ℃, stirring at 50-100 rpm for 20-24 hours, cooling to 50-60 ℃, and distilling at the temperature of 115-120 ℃ and the pressure of 0.1-0.3 MPa for 4-5 hours to obtain a glycosyl asphalt emulsion;
(3) putting the glycosyl asphalt emulsion, the dodecane primary amine and the methanol into a container according to the mass ratio of 1:0.6: 8-1: 0.7:9, stirring for 20-24 hours at 200-300 rpm, putting into an ice water bath, adding sodium borohydride with the mass of 0.2-0.3 time of that of the glycosyl asphalt emulsion, stirring at the same speed until no bubbles are generated, then adding hydrochloric acid with the mass fraction of 10% until the pH value of the solution is 1-2, and performing suction filtration to obtain a filter cake; washing the filter cake with ice water and acetic acid for 3-5 times in sequence, drying at 70-80 ℃ and 0.01-0.03 MPa for 3-4 h, adding a methanol/sodium methoxide solution with the mass of 4-6 times of that of the glycosyl asphalt emulsion, stirring at 100-200 rpm for 20-24 h with the mass ratio of methanol to sodium methoxide being 2.2: 1-2.6: 1, heating to 85-90 ℃, reacting for 1-2 h, cooling to room temperature, and performing suction filtration to obtain a modified emulsion;
(4) expanding the flake graphite, performing microwave ultrasonic stripping to obtain a nanosheet, and performing magnetic modification to obtain a magnetic nanosheet;
(5) the magnetic nanosheet and the modified emulsion are placed in a magnetic field with the mass ratio of 1: 5-1: 8 at 25-35 Hz, are uniformly stirred, are sheared for 30-45 min at 170-180 ℃, are added with sulfur with the mass of 0.003-0.005 time of that of the magnetic nanosheet and rubber operating oil with the mass of 0.02-0.05 time of that of the magnetic nanosheet, and are stirred and developed for 1-2 h at 150-180 ℃ to obtain the infiltration type emulsifiable asphalt.
6. The method for preparing the infiltrated emulsified asphalt as claimed in claim 5, wherein the modified silica sol prepared in step (1) is prepared by:
a. adding tetraethoxysilane, absolute ethyl alcohol, deionized water and 25-28% ammonia water in a mass ratio of 1:8.2:0.2: 0.05-1: 8.7:0.3:0.06 into a beaker, stirring for 2-3 hours at 30 ℃ and 100-200 rpm, and aging for 6-7 days at room temperature to obtain nano-silica sol;
b. adding the nano-silica sol into a container, adding bis (triisopropylsilyl) amine with the mass of 0.25-0.33 times that of the nano-silica sol, stirring at 30-40 ℃ and 200-300 rpm for 2-3 h, and aging at room temperature for 6-7 d to obtain lipophilic nano-silica sol;
c. adding the nano-silica sol into a container, adding glycidoxypropyltrimethoxysilane of which the mass is 0.5-0.6 times that of the nano-silica sol, stirring at 30-40 ℃ and 200-300 rpm for 1-2 h, and aging at room temperature for 6-7 d to obtain hydrophilic nano-silica sol;
d. adding lipophilic nano-silica sol into a container, adding aminopropyltriethoxysilane which is 0.0009-0.001 time of the mass of the lipophilic nano-silica sol, stirring at 30-40 ℃ and 100-200 rpm for 5-7 h, adding hydrophilic nano-silica sol which is 1-1.5 times of the mass of the lipophilic nano-silica sol, stirring at the same temperature and speed for 30-45 min, and aging at room temperature for 6-7 d to obtain the modified silica sol.
7. The preparation method of infiltration-type emulsified asphalt according to claim 5, wherein the specific preparation steps of the magnetic nanosheets in step (4) are as follows:
A. uniformly stirring and mixing the flake graphite and potassium permanganate according to the mass ratio of 10:1, adding concentrated sulfuric acid with the mass fraction of 85% and the mass fraction of 2-3 times of the flake graphite, placing the mixture into a water bath kettle at 35-40 ℃, stirring the mixture for 80-90 min at 100-200 rpm, sequentially washing the mixture with hydrochloric acid and deionized water with the mass fraction of 10% until the pH of the solution is 6-7, filtering the mixture, drying the mixture for 1-2 h at 60-70 ℃, placing the dried mixture into a microwave oven, pretreating for 15-20 s, adding a methyl formamide/water mixed solution with the mass fraction of 2-3 times of the flake graphite, ultrasonically stripping the methyl formamide/water mixed solution for 4-5 h at 40-50 ℃ to prepare a graphene nanosheet;
B. placing the graphene nanosheets in a plasma sputtering instrument, treating for 3-5 min, and placing at a current density of 14-15A/mm-2Pulse current auxiliary sintering furnaceAnd heating to 400-500 ℃ at a speed of 10-15 ℃/min, pressurizing to 40-50 MPa, keeping the temperature and pressure for 3-5 min, and cooling to room temperature to obtain the magnetic nanosheet.
8. The method for preparing the infiltrated emulsified asphalt as claimed in claim 7, wherein the microwave oven in step A has a power of 10-20 kW and a heating temperature of 900-950 ℃; the frequency of ultrasonic stripping is 30-35 kHz.
9. The method of claim 7, wherein the vacuum degree of the plasma sputtering apparatus in step B is 1X 10-4～4×10-4And Pa, introducing oxygen mixed gas, wherein the volume ratio of oxygen to argon in the oxygen mixed gas is 10:16, the sputtering pressure is 2-5 Pa, the sputtering power is 120-200W, and the target material is a pure iron target.
10. The method for preparing the infiltrated emulsified asphalt as claimed in claim 5, wherein the shear rate in step (5) is 5000-8000 rpm; the stirring speed is 600-800 rpm.
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| CN108250774A (en) * | 2017-12-21 | 2018-07-06 | 天津城建道桥工程有限公司 | Cold-application chromatic bitumen mixture and preparation method thereof |
| CN108948754A (en) * | 2017-05-17 | 2018-12-07 | 交通运输部公路科学研究所 | A kind of special asphalt, its mixture and application for heavily loaded porous pavement making |
| CN111234540A (en) * | 2020-01-19 | 2020-06-05 | 长安大学 | Low-temperature-resistant nano modified asphalt and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108948754A (en) * | 2017-05-17 | 2018-12-07 | 交通运输部公路科学研究所 | A kind of special asphalt, its mixture and application for heavily loaded porous pavement making |
| CN108250774A (en) * | 2017-12-21 | 2018-07-06 | 天津城建道桥工程有限公司 | Cold-application chromatic bitumen mixture and preparation method thereof |
| CN111234540A (en) * | 2020-01-19 | 2020-06-05 | 长安大学 | Low-temperature-resistant nano modified asphalt and preparation method thereof |
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