CN115181429A - Biological oil modified rubber asphalt and phase separation evaluation method thereof - Google Patents
Biological oil modified rubber asphalt and phase separation evaluation method thereof Download PDFInfo
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- 229920001971 elastomer Polymers 0.000 title claims abstract description 153
- 239000010426 asphalt Substances 0.000 title claims abstract description 127
- 238000005191 phase separation Methods 0.000 title claims abstract description 76
- 238000011156 evaluation Methods 0.000 title claims abstract description 31
- 239000000843 powder Substances 0.000 claims abstract description 62
- 239000012075 bio-oil Substances 0.000 claims abstract description 51
- 239000003921 oil Substances 0.000 claims abstract description 39
- 238000002156 mixing Methods 0.000 claims abstract description 31
- 239000002699 waste material Substances 0.000 claims abstract description 30
- 238000012360 testing method Methods 0.000 claims abstract description 23
- 238000005227 gel permeation chromatography Methods 0.000 claims abstract description 14
- 239000003208 petroleum Substances 0.000 claims abstract description 10
- 238000012900 molecular simulation Methods 0.000 claims abstract description 5
- 238000000034 method Methods 0.000 claims description 11
- 238000010438 heat treatment Methods 0.000 claims description 8
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical group C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 claims description 6
- 238000010008 shearing Methods 0.000 claims description 6
- 230000002776 aggregation Effects 0.000 claims description 5
- 238000004220 aggregation Methods 0.000 claims description 5
- 230000008569 process Effects 0.000 claims description 4
- 238000004088 simulation Methods 0.000 claims description 4
- 238000009792 diffusion process Methods 0.000 claims description 3
- 238000002347 injection Methods 0.000 claims description 3
- 239000007924 injection Substances 0.000 claims description 3
- 239000000178 monomer Substances 0.000 claims description 3
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 claims description 3
- 239000006059 cover glass Substances 0.000 claims description 2
- 239000011521 glass Substances 0.000 claims description 2
- 238000000329 molecular dynamics simulation Methods 0.000 claims description 2
- 238000002360 preparation method Methods 0.000 claims description 2
- 238000003825 pressing Methods 0.000 claims description 2
- 238000000638 solvent extraction Methods 0.000 claims description 2
- 238000005457 optimization Methods 0.000 claims 1
- 238000005464 sample preparation method Methods 0.000 claims 1
- 238000012876 topography Methods 0.000 claims 1
- 239000010920 waste tyre Substances 0.000 abstract description 3
- 239000002028 Biomass Substances 0.000 abstract description 2
- 230000007613 environmental effect Effects 0.000 abstract description 2
- 229920002209 Crumb rubber Polymers 0.000 description 6
- 125000003118 aryl group Chemical group 0.000 description 5
- 239000000203 mixture Substances 0.000 description 5
- 229920006395 saturated elastomer Polymers 0.000 description 5
- 238000011160 research Methods 0.000 description 3
- 229920005549 butyl rubber Polymers 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 239000006185 dispersion Substances 0.000 description 2
- 230000002349 favourable effect Effects 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 125000000217 alkyl group Chemical group 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000004566 building material Substances 0.000 description 1
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- 230000000877 morphologic effect Effects 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
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- 238000005192 partition Methods 0.000 description 1
- 230000035515 penetration Effects 0.000 description 1
- 238000000197 pyrolysis Methods 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
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- 238000003860 storage Methods 0.000 description 1
- 230000001502 supplementing effect Effects 0.000 description 1
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- C08L95/00—Compositions of bituminous materials, e.g. asphalt, tar, pitch
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
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- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N33/00—Investigating or analysing materials by specific methods not covered by groups G01N1/00 - G01N31/00
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Abstract
The invention discloses biological oil modified rubber asphalt and a phase separation evaluation method thereof. The mixing amount of the rubber powder in the biological oil modified rubber asphalt is 20-45%, and the mixing amount of the biological oil is 5-30%. The evaluation method comprises three parts of microscopic morphology test evaluation phase separation, gel chromatography test evaluation phase separation and molecular simulation evaluation phase separation. The phase separation evaluation method of the bio-oil modified rubber asphalt has the characteristics of high test evaluation speed, simplicity in operation and environmental friendliness, fully utilizes waste tires (waste rubber powder), uses green renewable biomass resources (bio-oil), obviously reduces the use of petroleum asphalt, improves the use performance of rubber asphalt, and generates obvious economic, social and ecological benefits. The biological oil modified rubber asphalt meeting the index requirements is tested to meet the basic index of the road performance of the rubber asphalt according to the evaluation method.
Description
Technical Field
The invention belongs to the technical field of phase separation evaluation of bio-oil modified rubber asphalt, and particularly discloses bio-oil modified rubber asphalt and a phase separation evaluation method thereof.
Background
The rubber asphalt mixture pavement has the excellent characteristics of good flatness, skid resistance, noise reduction and the like. Among the modified asphalt, the rubber asphalt is a superior modified asphalt material for highway engineering, and is also a road building material with great popularization and application values currently and in the future. The high-doping-amount rubber asphalt further improves the doping amount of rubber powder, not only realizes the recycling of waste tires, but also greatly reduces the use of petroleum asphalt and the economic cost of road pavement. However, the rubber powder contains a large amount of nonpolar compounds and is inert on the surface, and the petroleum asphalt contains more polar compounds, so that the phase stability of the blend of the rubber powder and the asphalt is extremely poor and segregation is easy to occur. In the research and application of the high-doping-amount rubber asphalt mixture, the rubber powder doping amount is generally 0.85-1.27% of the mass of the mixture, and the high-doping-amount rubber asphalt cannot be broken through all the time, so that the application of the high-doping-amount rubber asphalt in highway engineering is limited to a certain extent. Researches find that the bio-oil produced by wood chip pyrolysis has good compatibility and excellent adhesion with asphalt, and can be used as a substitute material of the asphalt; however, the problems of high oxygen content, low temperature brittleness and the like of common bio-oil replacing/modifying asphalt exist, the low-temperature characteristic of the bio-asphalt can be obviously improved by adding the rubber powder into the bio-asphalt, and the solubility of the rubber powder and the asphalt can be promoted by adding the bio-oil, so that a synergistic effect is generated. However, the lack of deep research on the structure and compatibility mechanism of bio-oil modified rubber asphalt, especially high rubber powder content, is urgent. The phase separation evaluation method and the application method of the bio-oil modified rubber asphalt can further improve the utilization efficiency of rubber powder, improve the service performance of high-content rubber asphalt, quickly judge the phase separation of the bio-oil modified rubber asphalt and have important significance for popularization and application of the rubber asphalt.
Disclosure of Invention
In order to solve the problems in the background art, the invention provides biological oil modified rubber asphalt and a phase separation evaluation method thereof.
The preparation method of the biological oil modified rubber asphalt comprises the following steps: heating petroleum asphalt to a molten state, and then slowly adding biological oil, wherein the mixing amount of the biological oil is 5-30%; then adding 20-45% of waste rubber powder, slowly increasing the heating temperature to 170-190 ℃ to be in a molten state, finally shearing at high speed by using a high-speed shearing instrument, and storing for later use; wherein the waste rubber powder and the bio-oil are measured by adopting an external mixing method by taking the quality of the petroleum asphalt as a standard and adopting the mass fraction.
The phase separation evaluation method of the bio-oil modified rubber asphalt comprises the following steps: the method comprises three parts of microscopic morphology test evaluation phase separation, gel chromatography test evaluation phase separation and molecular simulation evaluation phase separation.
The rubber powder mixing amount of the biological oil modified rubber asphalt is 20-45%, and the biological oil mixing amount is 5-30%.
The specific operation of evaluating the phase separation by the microscopic morphology test is as follows: preparing a sample by adopting a tabletting method, namely heating the asphalt to a molten state, dripping the asphalt on a glass slide by using a dropper, and forcibly pressing by using a cover glass until the asphalt is yellow and transparent; performing micro-morphology test on the bio-oil modified rubber asphalt by using a fluorescence microscope, wherein the test multiple is 50-1000 times; obtaining the area of a phase separation area through testing, and dividing the area of the phase separation area by the total area of the appearance area of the test sample to obtain phase separation parameters; when the phase separation parameter is 5% or less, it indicates that no phase separation has occurred; when the phase separation parameter is greater than 5%, weak phase separation is indicated; when the phase separation parameter is 30% or more, it indicates that significant phase separation occurs.
The gel chromatography test evaluates the specific operation of phase separation as follows: carrying out component partition on the bio-oil modified rubber asphalt by using a gel chromatography, wherein the length of a chromatographic column is 300mm, the mobile phase is tetrahydrofuran, the flow rate is 1.0mL/min, the sample concentration is 2mg/mL, and the sample injection amount is 100 mu L; according to the area enclosed by a gel chromatography curve and a time axis, a part with a weight average molecular weight of more than 19000 is an agglomerate region, a region with a weight average molecular weight of more than 3000 and less than 19000 is an asphaltene region, and a region with a weight average molecular weight of less than 3000 is a soft asphalt (light component) region.
The molecular simulation evaluation phase separation comprises the following specific operations: molecular dynamics is utilized to draw molecular formulas of four components of biological oil, rubber powder (substituted by butyl rubber) and asphalt, an amophorus Cell Tools module is utilized to construct a molecular model of the biological oil modified rubber asphalt, a Forcite module is utilized to geometrically optimize the structure of the biological oil modified rubber asphalt to obtain the most stable configuration, and then a Mesociate module is utilized to simulate the aggregation state structure in the phase separation process of the biological oil modified rubber asphalt, wherein the total step number is 100, the total simulation time is 5 mu s, the time step length is 50ns, and the monomer diffusion coefficient is 1.0 x 10 -7 cm 2 S, temperature 298k.
The invention has the beneficial effects that:
the phase separation evaluation method of the bio-oil modified rubber asphalt has the characteristics of high test evaluation speed, simplicity in operation and environmental friendliness, fully utilizes waste tires (waste rubber powder), uses green renewable biomass resources (bio-oil), obviously reduces the use of petroleum asphalt, improves the use performance of the rubber asphalt and generates obvious economic, social and ecological benefits. The biological oil modified rubber asphalt meeting the index requirements is tested according to the evaluation method of the invention to meet the basic index of the road performance of the rubber asphalt.
Drawings
FIG. 1 shows molecular models of bio-oil modified rubber asphalt prepared in example 1, wherein (a) the rubber powder content is 20%, (b) the rubber powder content is 25%, (c) the rubber powder content is 30%, (d) the rubber powder content is 35%, (e) the rubber powder content is 40%, (f) the rubber powder content is 45%.
FIG. 2 shows fluorescence microscopic morphologies of the bio-oil modified rubber asphalt prepared in example 1, wherein (a) the rubber powder content is 20%, (b) the rubber powder content is 25%, (c) the rubber powder content is 30%, (d) the rubber powder content is 35%, (e) the rubber powder content is 40%, (f) the rubber powder content is 45%.
FIG. 3 phase separation parameters of bio-oil modified rubber asphalt prepared in example 1.
FIG. 4 is a gel chromatography curve of bio-oil modified rubber asphalt prepared in example 1.
FIG. 5 shows the aggregate structure of the bio-oil modified rubber asphalt prepared in example 1 during phase separation, wherein (a) the rubber powder content is 20%, (b) the rubber powder content is 25%, (c) the rubber powder content is 30%, (d) the rubber powder content is 35%, (e) the rubber powder content is 40%, (f) the rubber powder content is 45%.
Detailed Description
Example 1:
preparing the biological oil modified rubber asphalt: heating petroleum asphalt to a molten state, and then slowly adding biological oil, wherein the mixing amount of the biological oil is 10%; then adding 20%, 25%, 30%, 35%, 40% and 45% of waste rubber powder, slowly increasing the heating temperature to 170-190 ℃ to be in a molten state, finally shearing at high speed by using a high-speed shearing instrument, and storing for later use; wherein the waste rubber powder and the bio-oil are measured by adopting an external mixing method by taking the quality of the petroleum asphalt as a standard and adopting the mass fraction.
And (2) respectively carrying out micro-morphology test on the prepared bio-oil modified rubber asphalt by using an XSP-63X fluorescence microscope, wherein the test multiple is 100X, and preparing a sample by adopting a tabletting method. And solving the area of the phase separation region by using Image Pro Plus6.0 software, and dividing the solved area of the phase separation region by the total area of the morphological region of the test sample to obtain the phase separation Parameter (PD). When the PD of the system is less than or equal to 5 percent, the system does not generate phase separation; when the phase separation parameter of the system is more than 5 percent, the weak phase separation of the system is shown; when the phase separation parameter of the system is more than or equal to 30 percent, the system is shown to have obvious phase separation.
The micro-morphology of the bio-oil modified rubber asphalt is shown in fig. 2, and it can be seen from fig. 2 (a) - (c) that when the mixing amount of the crumb rubber is 20%, the common rubber asphalt has a partial yellow region, and the yellow region of the rubber bio-asphalt with higher mixing amount of the regional area (the mixing amount of the crumb rubber is 25-35%) is large; when the mixing amount of the waste rubber powder is 25-35%, no obvious phase separation is found in the bio-oil modified rubber asphalt; as shown in FIGS. 2 (d) to (e), when the amount of the crumb rubber exceeds 35%, the bio-oil-modified rubber asphalt undergoes a significant phase separation, and when the amount of the crumb rubber is 40% or 45%, the yellow region of the bio-oil-modified rubber asphalt occupies almost half of the entire visual field.
The phase separation process of the bio-oil modified rubber asphalt was evaluated by means of defined phase separation Parameters (PD). As can be seen from FIG. 3, in the high-doping-amount rubberized biological asphalt system, as the doping amount of the waste rubber powder increases, the PD of the biological oil modified rubber asphalt increases slowly, and when the doping amount of the waste rubber powder exceeds 35%, the PD of the biological oil modified rubber asphalt increases significantly, and an obvious phase separation phenomenon occurs. The optimal mixing amount of the waste rubber powder is 35 percent, and the waste rubber powder can ensure that the bio-oil modified rubber asphalt is stably stored without obvious phase separation phenomenon. Compared with the PD of the common rubber asphalt, the phase separation parameter of the biological oil modified rubber asphalt is found to be smaller than the PD of the common rubber asphalt, so that the biological oil can obviously reduce the phase separation parameter of the high-doped rubberized biological asphalt and increase the compatibility of the system. When the mixing amount of the waste rubber powder is 25-35%, the PD of the bio-oil modified rubber asphalt is 0-3%, and the system is not subjected to phase separation; when the mixing amount of the waste rubber powder exceeds 35%, the PD of 40% of the bio-oil modified rubber asphalt is 38%, and the PD of 45% of the bio-oil modified rubber asphalt is 50%, and then the bio-oil modified rubber asphalt is obviously separated.
The biological oil modified rubber asphalt is subjected to component partitioning by using America Agilent gel chromatography (GPC), the length of a chromatographic column is 300mm, the mobile phase is tetrahydrofuran, the flow rate is 1.0mL/min, the sample concentration is 2mg/mL, and the sample injection amount is 100 mu L. According to the area enclosed by a GPC curve and a time axis, the part with the weight average molecular weight larger than 19000 is an aggregate area; the area with the weight-average molecular weight more than 3000 and less than 19000 is an asphaltene area; the region having a weight average molecular weight of less than 3000 is a soft asphalt (light component) region. As shown in FIG. 4, the gel chromatography results of the bio-oil modified rubber asphalt show that when the mixing amount of the crumb rubber is between 25 and 45%, the areas of aggregates and asphaltene areas are increased with the increase of the mixing amount of the crumb rubber. That is, the waste rubber powder can increase the number of aggregates and asphaltenes in the bio-oil modified rubber asphalt system and increase the possibility of phase separation of the system. Comparing the curves of the common rubber asphalt (when the mixing amount of the waste rubber powder is 20%), finding that the area of the aggregate and the asphaltene area of the common rubber asphalt accounts for 25% of the total area, and defining that the sum of the areas of the aggregate area and the asphaltene area accounts for 25% of the total area as the maximum ratio without phase separation, wherein the system is obviously separated when the sum exceeds 25%, and the system is in a stable state when the sum is less than or equal to 25%. As can be seen from the figure, when the mixing amount of the waste rubber powder is 35%, the area of the bio-oil modified rubber asphalt aggregate and the area of the asphaltene areas are approximately equal to the area of the common rubber asphalt aggregate and the area of the asphaltene areas, and the total area is 24%. When the mixing amount of the waste rubber powder is 40%, the sum of the areas of the bio-oil modified rubber asphalt aggregate and the asphaltene area accounts for 30% of the total area, so that the bio-oil modified rubber asphalt system is subjected to a phase separation phenomenon when the mixing amount of the waste rubber powder exceeds 35%. When the mixing amount of the waste rubber powder is less than or equal to 35%, the area of an aggregate area in a gel chromatographic curve is smaller than the area of an asphaltene area, and when the mixing amount of the waste rubber powder exceeds 35%, the area of the aggregate area in the gel chromatographic curve is larger than the area of the asphaltene area, and at the moment, the system is subjected to phase separation, so that the ratio of the area of the aggregate area to the area of the asphaltene area in the gel chromatographic curve in the total area and the ratio of the area of the aggregate area to the area of the asphaltene area (larger than 1) are key judgment indexes for phase separation of the bio-oil modified rubber asphalt.
Molecular dynamics software is used for drawing molecular formulas of four components of biological oil, rubber powder (substituted by butyl rubber) and asphalt, an Amorphous Cell Tools module is used for constructing a molecular model of the biological oil modified rubber asphalt, a Forcite module is used for geometrically optimizing the structure of the biological oil modified rubber asphalt to obtain the most stable configuration, and then a Mesocite module is used for simulating an aggregation state structure in the phase separation process of the biological oil modified rubber asphalt, wherein the total step number is 100, the total simulation time is 5 mu s, the time step length is 50ns, and the monomer diffusion coefficient is 1.0 x 10 -7 cm 2 S, temperature 298k.
As shown in fig. 5, the aggregation structure simulation structure of the bio-oil modified rubber asphalt shows that when the mixing amount of the waste rubber powder is 25%, 30% or 35%, the bio-oil modified rubber asphalt is in a sol state, does not undergo large-scale aggregation, generates an aggregate state structure, and has a high overall dispersion degree. Therefore, when the mixing amount of the waste rubber powder is not more than 35%, the bio-oil modified rubber asphalt system has better intersolubility and good storage stability, and the phase separation phenomenon does not occur. When the mixing amount of the waste rubber powder is 40% and 45%, the bio-oil modified rubber asphalt system is in a gel state, the molecular structure shows a network shape of tight linkage and spatial interconnection, and the molecular dispersion degree is extremely low. The structure reflects that the mutual solubility of the waste rubber powder and the asphalt is very poor, the phase separation phenomenon is easy to occur, and coagulation is generated. The molecular structure of asphaltene is not favorable for mutual solubility of the system, and alkyl side chain molecules (saturated components and aromatic components) with proper length are favorable for mutual solubility of the system. Therefore, the content of asphaltene in the bio-oil modified rubber asphalt system can be increased along with the increase of the mixing amount of the waste rubber powder, and the content of saturated components and aromatic components can be reduced; when the mixing amount of the waste rubber powder is 25-35%, the biological oil has good effect of supplementing saturated components and aromatic components, so that the biological oil modified rubber asphalt does not have obvious phase separation phenomenon; when the mixing amount of the waste rubber powder exceeds 35 percent, saturated components and aromatic components in the bio-oil are not enough to adjust the saturated components and the aromatic components lost in the rubber asphalt, so that a phase separation phenomenon of a bio-oil modified rubber asphalt (40 percent and 45 percent of the waste rubber powder) system is caused.
The biological oil modified rubber asphalt is tested for penetration at 25 ℃, softening point and ductility at 5 ℃ according to JTGE20-2019 highway engineering asphalt and asphalt mixture test procedures, and the results are shown in Table 1, and the biological oil modified rubber asphalt in example 1 meets the basic performance of rubber asphalt roads according to CJJ/T273-2019 related parameters.
TABLE 1 basic Properties of Bio-oil modified rubber asphalt
Claims (6)
1. The preparation method of the biological oil modified rubber asphalt is characterized by comprising the following specific steps: heating petroleum asphalt to a molten state, and slowly adding biological oil, wherein the mixing amount of the biological oil is 5-30%; then adding 20-45% of waste rubber powder, slowly increasing the heating temperature to 170-190 ℃ to be in a molten state, finally shearing at high speed by using a high-speed shearing instrument, and storing for later use; wherein the waste rubber powder and the bio-oil are measured by adopting an external mixing method by taking the quality of the petroleum asphalt as a standard and adopting the mass fraction.
2. The phase separation evaluation method of the bio-oil modified rubber asphalt is characterized by comprising three parts of micro-morphology test evaluation phase separation, gel chromatography test evaluation phase separation and molecular simulation evaluation phase separation.
3. The evaluation method according to claim 2, wherein the rubber powder content in the bio-oil modified rubber asphalt is 20% -45%, and the bio-oil content is 5% -30%.
4. The evaluation method according to claim 2, wherein the micro-topography test evaluates the phase separation by: the sample preparation method comprises the steps of heating asphalt to a molten state, dripping the asphalt on a glass slide by a dropper, and forcibly pressing by a cover glass until the asphalt is yellow and transparent; performing micro-morphology test on the bio-oil modified rubber asphalt by using a fluorescence microscope, wherein the test multiple is 50-1000 times; obtaining the area of a phase separation area through testing, and dividing the area of the phase separation area by the total area of the appearance area of the test sample to obtain phase separation parameters; when the phase separation parameter is 5% or less, it indicates that no phase separation has occurred; when the phase separation parameter is greater than 5%, weak phase separation is indicated; when the phase separation parameter is 30% or more, it indicates that significant phase separation occurs.
5. The evaluation method according to claim 2, wherein the gel chromatography test evaluates the specific operation of phase separation as: carrying out component partitioning on the bio-oil modified rubber asphalt by using gel chromatography, wherein the length of a chromatographic column is 300mm, the mobile phase is tetrahydrofuran, the flow rate is 1.0mL/min, the sample concentration is 2mg/mL, and the sample injection amount is 100 mu L; according to the area enclosed by a gel chromatography curve and a time axis, the part with the weight average molecular weight of more than 19000 is an aggregate area, the area with the weight average molecular weight of more than 3000 and less than 19000 is an asphaltene area, and the area with the weight average molecular weight of less than 3000 is a soft asphalt area.
6. The evaluation method according to claim 2, wherein the molecular simulation evaluation phase separation is performed by: molecular dynamics is utilized to draw molecular formulas of four components of biological oil, rubber powder and asphalt, an Amorphous Cell Tools module is utilized to construct a molecular model of the biological oil modified rubber asphalt, a Forcite module is utilized to carry out geometric optimization on the structure of the biological oil modified rubber asphalt to obtain the most stable configuration, and then a Mesocite module is utilized to simulate an aggregation state structure in the phase separation process of the biological oil modified rubber asphalt, wherein the total step number is 100, the total simulation time is 5 mu s, the time step length is 50ns, the monomer diffusion coefficient is 1.0 x 10-7cm2/s, and the temperature is 298k.
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