CN114686011A - Preparation method of hydrothermal carbon modified asphalt - Google Patents
Preparation method of hydrothermal carbon modified asphalt Download PDFInfo
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- CN114686011A CN114686011A CN202210218918.8A CN202210218918A CN114686011A CN 114686011 A CN114686011 A CN 114686011A CN 202210218918 A CN202210218918 A CN 202210218918A CN 114686011 A CN114686011 A CN 114686011A
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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Abstract
The invention discloses a preparation method of hydrothermal carbon modified asphalt, relates to a preparation method of modified asphalt, and aims to solve the technical problems of poor dispersibility of a hydrothermal carbon material in asphalt and poor modification effect of the hydrothermal carbon material in the existing method for modifying asphalt by using the hydrothermal carbon material. The method comprises the following steps: the waste biomass is used as a carbon source, and a hydrothermal carbon method is adopted for carbonization to obtain bulk and granular hydrothermal carbon; immersing hydrothermal carbon in liquid nitrogen for soaking treatment, and grinding until the particle size reaches 1-100 mu m to obtain hydrothermal carbon powder; then adding the hydrothermal carbon powder into the asphalt, and shearing and stirring by adopting a high-speed shearing stirrer; and naturally cooling to obtain the hydrothermal carbon modified asphalt. The invention has good high-temperature anti-rutting and medium-temperature anti-fatigue performance, the fatigue life of the hydrothermal carbon modified asphalt is respectively prolonged by 212.6 percent and 271.8 percent compared with that of the matrix asphalt at 19 ℃ and 25 ℃, and the asphalt can be used in high-temperature and high-load areas.
Description
Technical Field
The invention relates to a preparation method of modified asphalt, belonging to the field of road building materials.
Background
The flexible pavement, namely the asphalt pavement, has the advantages of good road performance, short construction period, easy maintenance, low running noise and the like, and is widely applied worldwide, especially on high-grade roads. Large scale pavement construction has begun to progress since the 21 st century, particularly in developing countries, and the demand for petroleum asphalt has also increased at an incredible rate. The petroleum asphalt is mainly extracted from crude oil, the reserve is limited, and the energy consumption in the extraction process is huge. Therefore, finding alternatives to petroleum asphalt has become a common focus in the field of road engineering.
In recent years, hydrothermal carbonization of waste biomass has attracted increasing attention from researchers. However, the effect of the hydrothermal carbon obtained by hydrothermal carbonization directly used for asphalt modification is not good. Firstly, the aggregation phenomenon of the hydrothermal carbon material in the asphalt is always a problem that the hydrothermal carbon material is difficult to ignore as an asphalt modifier, and the storage stability of the modified asphalt is easily greatly influenced; secondly, the hydrothermal carbon forms a three-dimensional space network structure in the asphalt to further enhance the high-low temperature performance of the asphalt, the particle size of the hydrothermal carbon directly influences the quality of the modification effect, and a better space network structure cannot be formed due to too large particle size; and thirdly, abundant nano-pore structures and fibrous structures are distributed on the surface of the hydrothermal carbon, if the hydrothermal carbon is directly milled and refined, due to the characteristics of anisotropy, low hardness and the like of the hydrothermal carbon material, the material is easy to damage in processing, such as defects of outlet tearing, burr damage, pits on a hole wall and the like, and even nano-pores and chemical bonds on the surface of the hydrothermal carbon are damaged, so that the bonding force between the hydrothermal carbon material and an asphalt matrix is deteriorated, and the modification effect is further influenced.
Disclosure of Invention
The invention provides a preparation method of hydrothermal carbon modified asphalt, aiming at solving the technical problems of poor dispersibility and poor modification effect of a hydrothermal carbon material in the asphalt in the existing method for modifying the asphalt by using the hydrothermal carbon material.
The preparation method of the hydrothermal carbon modified asphalt comprises the following steps:
firstly, taking waste biomass as a carbon source, and carbonizing by adopting a hydrothermal carbon method to obtain bulk and granular hydrothermal carbon;
secondly, immersing the hydrothermal charcoal in liquid nitrogen for 3-5 min;
thirdly, adding the hydrothermal carbon treated by the liquid nitrogen into a grinder to grind the hydrothermal carbon powder until the particle size of the hydrothermal carbon powder reaches 1-100 mu m, so as to obtain the hydrothermal carbon powder;
fourthly, putting the petroleum asphalt with the penetration degree of 50-120 (0.01 mm) into an oven with the temperature of 160-170 ℃ for heating for 1-1.5 hours to ensure that the asphalt flows fully; adding the hydrothermal carbon powder obtained in the third step into the asphalt, and shearing and stirring by adopting a high-speed shearing stirrer; and naturally cooling to obtain the hydrothermal carbon modified asphalt.
Furthermore, in the first step, the biomass is wood or crop straws;
further, the hydrothermal carbonization in the first step is specifically performed as follows:
(1) crushing waste wood or crop straws to obtain biomass powder;
(2) mixing biomass powder and deionized water, and then placing the mixture in a hydrothermal reaction kettle, wherein the mass ratio of the biomass powder to the deionized water is 1 (10-20); then heating the hydrothermal reaction kettle to 200-300 ℃ and keeping the temperature for 1-6 h; cooling to room temperature;
(3) and (3) filtering and separating substances in the hydrothermal reaction kettle, and drying the solid-phase substance at the temperature of 80-100 ℃ for 10-12 h to obtain the bulk and granular hydrothermal carbon.
Furthermore, the adding amount of the hydrothermal carbon powder in the fourth step is 2-15% of the mass of the asphalt;
furthermore, the shear rate in the fourth step is 4500-4800 rpm,
furthermore, in the fourth step, the stirring temperature is 165-170 ℃, and the stirring time is 45-50 min.
According to the method, the hydrothermal carbon liquid obtained after biomass hydrothermal carbonization is subjected to nitrogen treatment and ground to 1-100 mu m, and then the hydrothermal carbon liquid is subjected to composite modification with asphalt, so that in the whole process of immersing the hydrothermal carbon material into liquid nitrogen for treatment, the temperature of the whole hydrothermal carbon material and a processing area can be effectively reduced due to liquid nitrogen cooling, the phenomenon that the hydrothermal carbon material is stuck on a grinding disc during grinding is greatly reduced, and the sharpness of the grinding disc is kept. In addition, the liquid nitrogen acts as a cold lubricant added to the whole grinding process, and meanwhile, as the thermal expansion coefficient difference between the grinding disc and the hydrothermal carbon material is very large, once the temperature changes, the temperature interacts with each other to generate compressive stress, so that the internal bonding force of the hydrothermal carbon material is strengthened, and the damage degree of an interface is remarkably reduced. The hydrothermal carbon modified asphalt obtained by the invention has good high-temperature anti-rutting and medium-temperature fatigue resistance performances, and the increase ranges of rutting factors at four test temperatures of 52 ℃, 58 ℃, 64 ℃ and 70 ℃ are 287%, 298%, 293% and 280% respectively; the fatigue life of the hydrothermal carbon modified asphalt is respectively prolonged by 212.6 percent and 271.8 percent compared with that of the matrix asphalt at the temperature of 19 ℃ and 25 ℃. The pavement performance of the matrix asphalt is improved, the use of petroleum asphalt is reduced, the pollution of waste biomass to the environment is reduced, and a green solution is provided for the treatment of the waste biomass. The hydrothermal carbon modified asphalt is suitable for high-temperature and high-load areas.
Drawings
FIG. 1 is a scanning electron micrograph of the hydrothermal carbon powder obtained in step three of example 1;
FIG. 2 is a scanning electron micrograph at low magnification of a hydrothermal carbon-modified asphalt prepared in example 1;
FIG. 3 is a high magnification scanning electron micrograph of the hydrothermal carbon-modified asphalt prepared in example 1;
FIG. 4 is a complex modulus master curve for the hydrothermal carbon modified asphalt prepared in example 1;
FIG. 5 is a main graph of the phase angle of the hydrothermal carbon-modified asphalt prepared in example 1;
FIG. 6 is a graph of rutting factor results for hydrothermal carbon-modified asphalt prepared in example 1;
FIG. 7 is a graph of the fatigue life results of a linear amplitude sweep test of the hydrothermal carbon-modified asphalt prepared in example 1;
FIG. 8 is a graph of creep stiffness results from flexural beam rheology tests for the hydrothermal carbon modified asphalt prepared in example 1;
FIG. 9 is the m-value results of the flexural Beam rheology test for the hydrothermal carbon-modified asphalt prepared in example 1.
Detailed Description
The following examples are used to demonstrate the beneficial effects of the present invention.
Example 1: the preparation method of the hydrothermal carbon modified asphalt provided by the embodiment comprises the following steps:
the method comprises the following steps of taking waste corn straws as a carbon source, and carbonizing by adopting a hydrothermal carbon method, wherein the specific hydrothermal carbon method carbonization operation comprises the following steps: crushing waste corn straws, putting the crushed waste corn straws into a hydrothermal reaction kettle, adding plasma water with the mass 15 times that of the corn straw powder, sealing the hydrothermal reaction kettle, putting the reaction kettle into a heating furnace, heating to 250 ℃ and keeping the temperature for 3 hours, cooling the hydrothermal reaction kettle to room temperature, filtering and separating a reaction product by using filter paper, and finally keeping the obtained solid product in an oven with the temperature of 80 ℃ for 12 hours to obtain bulk and granular hydrothermal carbon;
secondly, immersing the hydrothermal charcoal in liquid nitrogen for 3 min;
adding the hydrothermal carbon treated by the liquid nitrogen into a grinder for grinding, analyzing the particle size of the ground hydrothermal carbon powder by a laser particle size analyzer, and finishing grinding when the particle size of the hydrothermal carbon powder reaches the range of 1-100 mu m to obtain the hydrothermal carbon powder;
fourthly, putting the petroleum asphalt with the penetration degree of 100 (0.01 mm) into a baking oven at the temperature of 170 ℃ for heating for 1 hour to ensure that the asphalt flows fully; adding the hydrothermal carbon powder obtained in the third step into asphalt according to 14% of the mass of the asphalt, stirring for 45min by adopting a high-speed shearing stirrer under the conditions that the stirring temperature is 170 ℃ and the shearing rate is 4500rpm, and shearing and stirring; and naturally cooling to obtain the hydrothermal carbon modified asphalt.
The prepared hydrothermal carbon modified asphalt is stored in a sealed manner.
In this example, a scanning electron micrograph of the hydrothermal carbon powder obtained through the third step is shown in fig. 1, and it can be seen from fig. 1 that the hydrothermal carbon powder is in a micron order, and it can be clearly observed that the hydrothermal carbon powder has a nanoporous and fibrous structure. This shows that this example basically realizes high-efficiency low-damage grinding of the hydrothermal carbon material, and retains the nanopores and fibrous structure of the hydrothermal carbon material to the maximum extent. The hydrothermal carbon powder is composed of irregular fibrous particles with a porous structure, and the surface texture is extremely complex. The porous and fibrous structure of the hydrothermal carbon powder is helpful for constructing a strong carbon cementing material matrix, thereby improving the performance of the cementing material.
In the embodiment, scanning electron micrographs of the hydrothermal carbon modified asphalt obtained through the fourth step are shown in fig. 2 and fig. 3, and it can be seen from fig. 3 that the hydrothermal carbon and the asphalt are effectively mixed, and a sheet structure and an increased specific surface area are presented. Scanning electron microscope results show that the hydrothermal carbon is in a uniform dispersion state and is tightly fixed by an asphalt matrix. From fig. 3, it can be observed that the bituminous material is excellent in compatibility with the hydrothermal carbon composed of irregular fibrous particles having a porous structure and uniformly dispersed. This is because the liquid nitrogen treatment is adopted in this embodiment, and the nanopores and fibrous structures of the hydrothermal carbon material are retained to a great extent. Due to the porous layered structure and large specific surface area of the hydrothermal carbon, the pitch effectively penetrates into the free space and forms a strong interfacial bond. In addition, the fibrous structure of the hydrothermal carbon acts as a bridge between the asphalt matrices, further enhancing the interfacial bonding. The porous layered structure and fibrous structure of the hydrothermal carbon are the key for improving the rheological and mechanical behaviors of the modified asphalt material.
The complex modulus main curve of the hydrothermal carbon modified asphalt obtained in the fourth step of the present embodiment is shown in fig. 4, and as can be seen from fig. 4, the addition of the hydrothermal carbon enables the complex modulus main curve of the asphalt to significantly move upwards in the low frequency region, and the maximum modulus increase in the low frequency region can reach one order of magnitude, which corresponds to the significant improvement of the high temperature rutting resistance; the low-temperature performance is basically not influenced when the low-temperature performance is basically unchanged in a high-frequency region.
The main curve diagram of the phase angle of the hydrothermal carbon modified asphalt obtained in the fourth step of the present embodiment is shown in fig. 5, and it can be seen from fig. 5 that the phase angle of the hydrothermal carbon modified asphalt is much smaller than that of the matrix asphalt, and the maximum difference between the phase angles of the matrix asphalt and the hydrothermal carbon modified asphalt can reach 10 °, which indicates that the addition of the hydrothermal carbon improves the elastic recovery performance of the asphalt and reduces the formation and development of fatigue cracking of a road surface, which is attributed to the high elasticity of the porous layered structure and the fibrous structure of the hydrothermal carbon.
The rutting factor result chart of the hydrothermal carbon modified asphalt obtained in the fourth step of this example is shown in fig. 6. The higher the rut factor, the better the high temperature rut resistance of the asphalt. As can be seen from FIG. 6, the addition of the hydrothermal charcoal significantly improves the high temperature performance of the asphalt, and the rutting factors at the four test temperatures of 52 ℃, 58 ℃, 64 ℃ and 70 ℃ increase by 287%, 298%, 293% and 280%, respectively.
Fig. 7 shows the fatigue life results of the hydrothermal carbon-modified asphalt obtained in the example through the step four in the linear amplitude sweep test. The longer the fatigue life, the better the fatigue cracking resistance of the asphalt. As can be seen from fig. 7, the addition of hydrothermal charcoal significantly improved the fatigue properties of the asphalt. When the test temperature is 19 ℃ and 25 ℃, the fatigue life of the hydrothermal carbon modified asphalt is respectively prolonged by 212.6 percent and 271.8 percent.
The creep stiffness and m value results of the bending beam rheological test of the hydrothermal carbon modified asphalt obtained in the fourth step of this example are shown in fig. 8 and fig. 9, respectively, where the lower the creep stiffness, the higher the m value, and the better the low temperature crack resistance of the asphalt. As can be seen from fig. 8 and 9, the addition of the hydrothermal charcoal had no significant effect on the low temperature performance of the asphalt.
Example 2: the preparation method of the hydrothermal carbon modified asphalt provided by the embodiment comprises the following steps:
firstly, taking waste wood as a carbon source, and carbonizing by adopting a hydrothermal carbon method; the specific hydrothermal carbon method carbonization operation is as follows: crushing waste wood into powder, putting the powder into a hydrothermal reaction kettle, adding plasma water with the mass 20 times that of the wood powder, sealing the hydrothermal reaction kettle, heating the hydrothermal reaction kettle to 300 ℃ for 1h, cooling the hydrothermal reaction kettle to room temperature, filtering and separating a reaction product by using filter paper, and finally putting the obtained solid product into an oven with the temperature of 100 ℃ for 12 hours to obtain bulk and granular hydrothermal carbon;
secondly, immersing the hydrothermal charcoal in liquid nitrogen for 5 min;
adding the hydrothermal carbon treated by the liquid nitrogen into a grinder for grinding, analyzing the particle size of the ground hydrothermal carbon powder by a laser particle size analyzer, and finishing grinding when the particle size of the hydrothermal carbon powder reaches the range of 1-100 mu m to obtain the hydrothermal carbon powder;
fourthly, putting the petroleum asphalt with the penetration degree of 100 (0.01 mm) into an oven with the temperature of 170 ℃ for heating for 1 hour to ensure that the asphalt flows fully; adding the hydrothermal carbon powder obtained in the third step into asphalt according to 5% of the mass of the asphalt, stirring for 50min by adopting a high-speed shearing stirrer under the conditions that the stirring temperature is 165 ℃ and the shearing rate is 4500rpm, and shearing and stirring; and naturally cooling to obtain the hydrothermal carbon modified asphalt.
The high-temperature performance and the medium-temperature performance of the hydrothermal carbon modified asphalt obtained by the embodiment are obviously improved relative to those of matrix asphalt, and by taking the rutting factor and the fatigue life as evaluation indexes, the improvement degrees of the two indexes reach 280% and 212% respectively.
Claims (7)
1. A preparation method of hydrothermal carbon modified asphalt is characterized by comprising the following steps:
firstly, taking waste biomass as a carbon source, and carbonizing by adopting a hydrothermal carbon method to obtain bulk and granular hydrothermal carbon;
secondly, immersing the hydrothermal charcoal in liquid nitrogen for 3-5 min;
thirdly, adding the hydrothermal carbon treated by the liquid nitrogen into a grinder to grind the hydrothermal carbon powder until the particle size of the hydrothermal carbon powder reaches 1-100 mu m, so as to obtain the hydrothermal carbon powder;
fourthly, putting the petroleum asphalt with the penetration degree of 50-120 (0.01 mm) into an oven with the temperature of 160-170 ℃ for heating for 1-1.5 hours to ensure that the asphalt flows fully; adding the hydrothermal carbon powder obtained in the third step into the asphalt, and shearing and stirring by adopting a high-speed shearing stirrer; and naturally cooling to obtain the hydrothermal carbon modified asphalt.
2. The method for preparing the hydrothermal carbon modified asphalt according to claim 1, wherein the biomass in the first step is wood or crop straw.
3. The preparation method of the hydrothermal carbon modified asphalt according to claim 1 or 2, characterized in that the hydrothermal carbon carbonization in the step one is specifically performed as follows:
(1) crushing waste wood or crop straws to obtain biomass powder;
(2) mixing biomass powder and deionized water, and then placing the mixture in a hydrothermal reaction kettle, wherein the mass ratio of the biomass powder to the deionized water is 1 (10-20); then heating the hydrothermal reaction kettle to 200-300 ℃ and keeping the temperature for 1-6 h; cooling to room temperature;
(3) and (3) filtering and separating substances in the hydrothermal reaction kettle, and drying the solid-phase substance at the temperature of 80-100 ℃ for 10-12 h to obtain the bulk and granular hydrothermal carbon.
4. The preparation method of the hydrothermal carbon modified asphalt as claimed in claim 1 or 2, wherein the addition amount of the hydrothermal carbon powder in the fourth step is 2-15% of the mass of the asphalt.
5. The preparation method of the hydrothermal carbon modified asphalt according to claim 1 or 2, wherein the shear rate in the fourth step is 4500-4800 rpm.
6. The method for preparing the hydrothermal carbon modified asphalt according to claim 1 or 2, wherein the temperature during stirring in the fourth step is 165-170 ℃.
7. The preparation method of the hydrothermal carbon modified asphalt according to claim 1 or 2, characterized in that the mixing time in the fourth step is 45-50 min.
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Patent Citations (5)
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| US20150128829A1 (en) * | 2013-11-08 | 2015-05-14 | University Of Tennessee Research Foundation | Development of a renewable carbon-based bio-modifier for asphalt cement |
| CN105017788A (en) * | 2015-07-16 | 2015-11-04 | 长安大学 | Methods for modifying asphalt and mixture thereof by using biochar |
| US20190330443A1 (en) * | 2018-04-27 | 2019-10-31 | Thomas Jefferson University | Nanocomposite hemp |
| CN110615441A (en) * | 2019-09-10 | 2019-12-27 | 崔建中 | Highland barley peel-based silicon dioxide refining process |
| CN111019365A (en) * | 2019-11-29 | 2020-04-17 | 复旦大学 | Method for preparing biological asphalt from lignocellulose biomass hydrothermal carbon |
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