CN115266403A - Quantitative and qualitative combined rubber asphalt phase structure evaluation method - Google Patents
Quantitative and qualitative combined rubber asphalt phase structure evaluation method Download PDFInfo
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Abstract
The invention provides a quantitative and qualitative combined evaluation method for a rubber asphalt phase structure, which comprises the following steps: heating the asphalt to be measured to a molten state, and then pouring a 25mm flat round sample; dividing the samples into two groups, and respectively applying a temperature scanning and frequency scanning dynamic shear rheological test; carrying out temperature scanning rheological test and frequency scanning rheological test on a poured rubber asphalt sample to obtain rheological property test data, establishing Han theoretical curve relation of a multiphase dispersion polymer system under temperature scanning and frequency scanning, and respectively calculating curve slope k; quantitatively judging the phase structure characteristics and the compatibility characteristics of the rubber composite modified asphalt under temperature scanning and frequency scanning by using the obtained curve slope k; establishing a Black relation curve of a multiphase dispersion polymer system; obtaining linear fitting characteristics of the obtained relation curve, and qualitatively judging the phase structure characteristics and compatibility characteristics of the rubber composite modified asphalt by using Black curve fitting characteristics; the rubber asphalt phase structure evaluation method combining quantification and qualification provided by the invention has the advantages of simple preliminary preparation work, short testing time, clear physical mechanics theory, simpler data processing and good reproducibility.
Description
Technical Field
The invention belongs to the technical field of highway engineering, and particularly relates to a quantitative and qualitative evaluation method for a phase structure of rubber asphalt.
Background
With the proposal of the concept of building green roads, the rubber asphalt market demand in China has unprecedented great situation. For many years, domestic researchers make a lot of researches on aspects such as rubber asphalt modification, mix proportion design, production process, construction key technology and the like, and achieve great achievements. However, the rubber asphalt products in the current market are not good and have the problems of selectivity obstacle and the like for engineering application. The rubber asphalt is used as a mixed system, the polymer is swelled in the asphalt, so that the performance of the polymer is transferred to the asphalt, and the mechanical properties of the modified asphalt can be effectively evaluated by researching the distribution form, the structure and the phase state of the polymer in the asphalt. Therefore, it is important to control the formation and evolution of the phase structure of a multi-component polymer system to obtain better polymer properties.
Quantitative analysis of the phase structure of the composite modified rubber asphalt can explain the reasons of performance difference of different composite modified asphalt, and the quantitative analysis can be used as a macro performance index of an asphalt microstructure to establish the correlation between the microstructure and a macro mechanical performance index, so that the comprehensive use performance of the composite modified rubber asphalt can be evaluated more intuitively and in real time through the micro phase structure. The phase structure of the composite modified rubber asphalt is approximately a multi-phase miscible structure with an asphalt continuous phase and a modifier or rubber powder polymer as a disperse phase. The traditional method for analyzing the phase structure of the modified asphalt usually adopts a fluorescence microscope photography technology or a fluorescence digital image technology to obtain the relationship between the rheological property and the microstructure of the polymer modified asphalt, and most scholars adopt the area percentage of the microstructure of the polymer as a microscopic parameter representative value for qualitatively or semi-quantitatively revealing the macroscopic performance index of the asphalt, but cannot completely quantify the correlation index of the phase structure and the macroscopic performance of the modified asphalt. The rheological response of the modified asphalt can accurately reflect the change of the morphological structure of the modified asphalt, and how to realize the microscopic quantitative characterization of the macroscopic performance of the composite modified asphalt by the viscoelastic analysis of the rheological property of the modified asphalt and the assistance of reasonable evaluation parameters of the phase structure. The dynamic rheology analysis method reflects the phase behavior of the multi-component polymer under the three-dimensional condition, and the multi-component polymer shows linear viscoelastic response under the small-strain oscillatory shear condition, has strong sensitivity to the formation and evolution of the phase structure of the multi-component polymer, and can accurately sense the change of the phase behavior. The composite modified rubber asphalt has larger difference with the traditional modified asphalt in thermodynamic property, belongs to a typical heterogeneous phase polymerization blending system, a Han curve can directly distinguish the phase state change of a multiphase polymer and a homogeneous polymer according to a relation curve of lgG & lt- & gt', the Han curve slope in an online viscoelasticity interval of the multiphase polymer is given to quantitatively represent the compatibility effect of the multiphase polymer blending system, and the Han curve slope k value can be used as an evaluation index for quantifying the composite modified rubber asphalt and a mucilage system thereof in deep discussion.
The rheological mechanical property of different modifiers for the composite modification of the rubber asphalt is researched, the phase separation temperature of different composite modified rubber asphalt is analyzed through the Han curve temperature dependence characteristic of different composite modified rubber asphalt, and the phase structure modification effect of the composite modified rubber asphalt is quantitatively evaluated according to the fitting slope k value of the lgG 'to lgG' relation curve; the invention provides a new method for further optimizing modification of rubber asphalt, researching a filling mechanism of a mucilage system, reasonably upgrading and transforming products and selecting functional products, and can be directly used as a quantitative evaluation index for composite modification and optimization improvement of rubber asphalt.
Disclosure of Invention
The invention aims to provide a rubber asphalt phase structure evaluation method combining quantification and qualification, which selects the phase structures of matrix asphalt, modified asphalt, different types of composite modified rubber asphalt, rubber asphalt mucilage systems and the like to study, obtains the phase structure behavior characteristics of the matrix asphalt, the modified asphalt, the composite modified rubber asphalt and the mucilage systems thereof under different loading conditions according to a dynamic shear rheometer test, and provides theoretical guidance for rubber asphalt composite modification.
In order to achieve the technical purpose and achieve the technical effect, the invention is realized by the following technical scheme:
the invention provides a quantitative and qualitative combined rubber asphalt phase structure evaluation method, which comprises the following steps:
step 1: heating the asphalt to be measured to a molten state, and then pouring a 25mm flat round sample;
step 2: dividing 25mm flat round samples into two groups, and respectively applying a temperature scanning and frequency scanning dynamic shear rheological test;
and step 3: under a constant value stress-strain level and with fixed frequency, carrying out a temperature scanning rheological test on a group of 25mm rubber asphalt samples which are cast, and obtaining rheological property test data, wherein the rheological property test data comprises the following steps: storage modulus G' and loss modulus G ";
and 4, step 4: deriving the storage modulus G 'and the loss modulus G' of the rheological property test data obtained in the step 3, drawing relationship curves of lgG '(omega) -lgG' (omega), establishing a Han theoretical curve relationship of the multiphase dispersed polymer system under temperature scanning, and calculating the slope k of the relationship curves of lgG '(omega) -lgG' (omega);
and 5: another set of 25mm rubber asphalt samples was cast at a constant stress-strain level and fixed temperatureFrequency sweep rheology test, obtaining rheology performance test data comprising: storage modulus G', loss modulus G ", composite shear modulus G*And a phase angle δ;
step 6: deriving the storage modulus G 'and the loss modulus G' obtained in the step 5, drawing relation curves of lgG '(omega) -lgG' (omega), establishing a Han theoretical curve relation of the multiphase dispersion polymer system under frequency scanning, and calculating the slope k of the relation curves of lgG '(omega) -lgG' (omega);
and 7: quantitatively judging the phase structure characteristics and the compatibility characteristics of the rubber composite modified asphalt under temperature scanning and frequency scanning by utilizing the slope k of the relationship curve from lgG '(omega) to lgG' (omega) obtained in the step 4 and the step 6;
and 8: and (3) the rheological property test data obtained in the step (5) comprises the following steps: composite shear modulus G*And phase angle delta, plot G*The delta relation curve is obtained, and a Black relation curve of the multiphase dispersion polymer system is established;
and step 9: obtaining G obtained in step 8*And (3) linear fitting characteristics of the delta relation curve, and qualitative judgment of phase structure characteristics and compatibility characteristics of the rubber composite modified asphalt by using Black curve fitting characteristics.
As a further improvement of the invention, the heating temperature of the asphalt in the step 1 is not more than 160 ℃, and before a flat round sample of 25mm is poured, the molten asphalt to be measured is fully and uniformly stirred, and bubbles are removed.
As a further improvement of the invention, the temperature scanning test in step 3 is an analysis test of a matrix asphalt, a modified asphalt, a composite modified rubber asphalt and a rubber asphalt mortar system thereof by using a dynamic shear rheometer; a rotor of the dynamic shear rheometer is 25mm in size and 1mm in gap, and a temperature scanning test is carried out by adopting a strain control mode; the experimental parameters were set as follows: the fixed loading frequency is 1.59Hz, and the temperature interval is 58-80 ℃.
As a further improvement of the present invention, in the frequency sweep test in step 5, a dynamic shear rheometer is used to analyze a matrix asphalt, a modified asphalt, a composite modified rubber asphalt and a rubber asphalt mortar system thereof, a rotor is selected to be 25mm, a gap is 1mm, a strain control mode is adopted to perform the frequency sweep test, and the test parameters are set as follows: the fixed loading temperature is 60 ℃, and the frequency interval is controlled to be 0.1-10 Hz.
As a further development of the invention, the Han theoretical curve of the multiphase dispersion polymer systems described in steps 4 and 6 is as follows:
wherein k is the slope of the relationship of lgG '(omega) to lgG' (omega);
is the plateau modulus.
The invention has the advantages that:
the method for evaluating the phase structure of the rubber asphalt by combining the quantification and the qualification has the advantages of simple preliminary preparation work, short testing time, clear physical and mechanical theory, simpler data processing and good reproducibility, and combines Han curve chart and Black curve chart theories to carry out quantitative evaluation and qualitative analysis on the phase structure of the rubber asphalt and a rubber cement system thereof so as to promote factory application of the rubber asphalt and product upgrading iteration.
Drawings
FIG. 1 is a flow chart of the method for evaluating the phase structure of the quantitative and qualitative rubber asphalt.
FIG. 2 is a Han plot under temperature sweeps for two test samples (SampleI: eastern sea base asphalt; sampleII: a brand of modified asphalt) in example 1;
FIG. 3 is a Han plot under a frequency sweep of two test samples (SampleI: east China sea base asphalt; sampleII: a brand of modified asphalt) in example 1;
FIG. 4 is a Black plot under frequency sweep of two test samples (SampleI: east China sea base asphalt; sampleII: a brand of modified asphalt) in example 1;
FIG. 5 is a Han plot under temperature scanning of nine test samples (rubber asphalt SampleI to rubber asphalt SampleIX) in example 2;
FIG. 6 is a histogram of Han curve slope k under temperature scanning for nine test samples (rubber asphalt SampleI to rubber asphalt SampleIX) in example 2;
FIG. 7 is a Han plot under frequency scanning of nine test samples (rubber asphalt SampleI to rubber asphalt SampleIX) in example 2;
FIG. 8 is a histogram of the slope k of the Han curve under frequency scanning of the nine test samples (rubber asphalt SampleI to rubber asphalt SampleIX) in example 2;
FIG. 9 is a Black plot under frequency sweep of nine test samples (rubber asphalt SampleI to rubber asphalt SampleIX) in example 2;
FIG. 10 is a Han plot of temperature sweeps for six test samples (rubber asphalt mastic system I through rubber asphalt mastic system VI) in example 3;
FIG. 11 is a histogram of Han curve slope k under temperature scanning for six test samples (rubber asphalt cement system I to rubber asphalt cement system VI) in example 3;
FIG. 12 is a Han plot under frequency sweep of six test samples (rubber asphalt mastic system I to rubber asphalt mastic system VI) in example 3;
FIG. 13 is a histogram of Han curve slope k under frequency scanning for six test samples (rubber asphalt cement system I to rubber asphalt cement system VI) in example 3;
FIG. 14 is a Black plot of frequency sweep for six test samples (rubberized asphalt mastic system I through rubberized asphalt mastic system VI) from example 3.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail by embodiments with reference to the accompanying drawings. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
Example 1
The embodiment of the invention provides a quantitative and qualitative combined evaluation method for a rubber asphalt phase structure, which specifically comprises the following steps:
step 1: heating the asphalt to be measured to a molten state, and then pouring a 25mm flat round sample;
selecting a common base asphalt and a modified asphalt for testing, namely east China sea base asphalt (marked as SampleI) and a certain brand of modified asphalt (SampleII); and (3) placing the two test sample asphalts indoors into a 160 ℃ oven for 1 hour, fully stirring the asphalts by using a glass rod after the asphalts are completely melted, removing bubbles in the asphalts, and then pouring a 25mm flat round sample.
Step 2: dividing 25mm flat round samples into two groups, and respectively carrying out a temperature scanning test and a frequency scanning test by adopting a dynamic shear rheometer;
and step 3: the fixed loading frequency is 1.59Hz, the temperature interval is selected to be 58-80 ℃, a strain control mode is adopted, and a set of 25mm asphalt samples of two poured test samples, namely SampleI and SampleII, are subjected to temperature scanning rheological test respectively to obtain the storage modulus G 'and the loss modulus G' of rheological property test data under the action of cyclic loading;
and 4, step 4: deriving the storage modulus G 'and the loss modulus G' of the rheological property test data obtained in the step 3, drawing relationship curves of lgG '(omega) -lgG' (omega) of two test samples by adopting Origin data processing software, establishing a Han theoretical curve relationship of the multiphase dispersed polymer system under temperature scanning, and calculating the slope k of the relationship curves of lgG '(omega) -lgG' (omega);
in this example, the logarithmic value of the loss modulus G ' and the storage modulus G ″ is calculated based on 10, the logarithmic value of the corresponding loss modulus G ' is used as the first coordinate value, the logarithmic value of the corresponding storage modulus G ″ is used as the second coordinate value, a graph is drawn in a planar rectangular coordinate system, and a Han rheological property index test curve under the working condition is formed by connecting points (lgG ', lgG ") under different coordinates;
the measured Han rheological curve is subjected to linear fitting and regression to obtain the slope k of the curve, which is used as a quantitative evaluation index of the phase structure performance characteristics of the sample SampleI and the sample SampleII, and is shown in Table 1.
TABLE 1 Han rheological Curve Linear regression results of base asphalt and modified asphalt under temperature scanning conditions
FIG. 2 is a Han plot of test sample I and test sample II under temperature sweep conditions, the slope of which is sized to quantitatively evaluate the phase structure characteristics of the bituminous polymer, and FIG. 2 shows that the phase separation temperature does not occur in lgG' (ω) -lgG "(ω) of the homogeneous polymer, i.e., that there is no temperature dependence.
And 5: the fixed loading temperature is 60 ℃, the frequency interval is controlled to be 0.1-10 Hz, and a strain control mode is adopted to respectively carry out a frequency scanning rheological test on the other 25mm asphalt sample of the two poured test samples SampleI and SampleII so as to obtain stress strain data under the action of cyclic loading;
step 6: deriving the storage modulus G 'and the loss modulus G' obtained in the step 5, drawing relationship curves of lgG '(omega) -lgG' (omega) of two groups of samples by adopting Origin data processing software, establishing Han theoretical curve relationship of the multiphase dispersed polymer system under frequency scanning, and calculating the slope k of the relationship curves of lgG '(omega) -lgG' (omega);
in this example, the log values of the loss modulus G ' and the storage modulus G ″ are calculated by taking 10 as a base number, the corresponding log value of the loss modulus G ' is used as a first coordinate value, the corresponding log value of the storage modulus G ″ is used as a second coordinate value, a graph is drawn in a planar rectangular coordinate system, and a Han rheological property index test curve under the working condition is formed by connecting points (lgG ', lgG ") under different coordinates;
the measured Han rheological curve is subjected to linear fitting and regression to obtain the slope k of the curve, which is used as a quantitative evaluation index of the phase structure performance characteristics of the sample SampleI and the sample SampleII, and is shown in Table 2.
TABLE 2 Han rheological Curve Linear regression results of base asphalt and modified asphalt under frequency scanning conditions
And 7: fig. 3 is a Han plot of test sample I and test sample II under frequency sweep conditions, the slope magnitudes of which allow quantitative assessment of the phase structure characteristics of the bituminous polymer. FIG. 3 shows that the phase separation frequencies of lgG' (ω) to lgG "(ω) of the homogeneous polymers do not occur, i.e., that there is no frequency dependence.
And 8: and (3) the rheological property test data obtained in the step (5) comprises the following steps: composite shear modulus G*And phase angle delta is derived, and G of two groups of samples is drawn by adopting Origin data processing software*A delta relation curve, and establishing a Black relation curve of the multiphase dispersion polymer system;
it should be noted that, in the present example, the corresponding complex modulus G is used*As a first coordinate value, the corresponding phase angle δ as a second coordinate value, and drawing a graph in a planar rectangular coordinate system, under different coordinates (G)*Delta) to form a Black rheological property index test curve under the working condition;
and step 9: obtaining G obtained in step 8*The linear fitting characteristic of the delta relation curve is utilized to qualitatively judge the phase structure characteristic and the compatibility characteristic of the rubber composite modified asphalt, FIG. 4 is a Black curve graph of a test sample I and a sample II under a frequency scanning rheological test, table 3 is the Black curve fitting characteristic, the phase structure change of the asphalt can be visually observed by utilizing the Black curve, and a smooth and coherent Black curve can be formed due to the good compatibility of the polymer and the asphalt; from FIG. 4, it can be seen that the fitted curves of the two test samples are smooth and coherent, and the characteristic correlation coefficient R of the curve fitting2Respectively reaches 0.9828 and 0.9631, can be qualitatively used as a judgment standard of the phase structure change of the polymer modified asphalt and used as a supplementary verification condition in the steps.
TABLE 3 Black curve fitting characteristics of base asphalt and modified asphalt under frequency sweep conditions
Example 2
Step 1: heating the asphalt to be measured to a molten state, and then pouring a 25mm flat round sample;
nine test samples such as rubber asphalt with different rubber powder mixing amounts and different composite modifiers for compounding rubber asphalt are selected for testing, namely rubber asphalt SampleI to rubber asphalt SampleIX. Nine test sample asphalts are placed in a 160 ℃ oven for 1 hour indoors, after the asphalts are completely melted, the asphalts are fully stirred by a glass rod, bubbles in the asphalts are removed, and then 25mm flat round samples are cast.
And 2, step: dividing 25mm flat round samples into two groups, and respectively carrying out a temperature scanning test and a frequency scanning test by adopting a dynamic shear rheometer;
and step 3: the fixed loading frequency is 1.59Hz, the temperature interval is selected to be 58-80 ℃, and a strain control mode is adopted to respectively carry out temperature scanning rheological tests on a group of 25mm asphalt samples of nine kinds of poured rubber asphalt SampleI-rubber asphalt SampleIX so as to obtain stress strain data under the action of cyclic loading;
and 4, step 4: deriving the storage modulus G 'and the loss modulus G' of the rheological property test data obtained in the step 3, drawing relation curves of lgG '(omega) -lgG' (omega) of nine test samples by adopting Origin data processing software, establishing a Han theoretical curve relation of the multiphase dispersed polymer system under temperature scanning, and calculating the slope k of the relation curves of lgG '(omega) -lgG' (omega);
in this example, the logarithmic value of the loss modulus G ' and the storage modulus G ″ is calculated based on 10, the logarithmic value of the corresponding loss modulus G ' is used as the first coordinate value, the logarithmic value of the corresponding storage modulus G ″ is used as the second coordinate value, a graph is drawn in a planar rectangular coordinate system, and a Han rheological property index test curve under the working condition is formed by connecting points (lgG ', lgG ") under different coordinates;
the measured Han rheological curve was subjected to linear fitting and regression to obtain a slope k of the curve as a quantitative evaluation index of the phase structure performance characteristics of the rubber asphalt SampleI to rubber asphalt SampleIX, as shown in table 4.
TABLE 4 Han rheological Curve linear regression results of rubber asphalt under temperature scanning conditions
FIG. 5 is a Han curve diagram of a rubber asphalt sample I to a rubber asphalt sample IX under temperature scanning conditions, and the slope magnitude of the Han curve diagram can quantitatively evaluate the phase structure characteristics of asphalt polymers, as shown in FIG. 6. Fig. 5 shows that the phase separation temperatures of lgG' (ω) to lgG "(ω) of the heterophasic polymers do not occur, i.e. they do not have a temperature dependence.
And 5: the fixed loading temperature is 60 ℃, the frequency interval is controlled to be 0.1-10 Hz, and a strain control mode is adopted to respectively carry out frequency scanning rheological tests on another 25mm asphalt sample of nine poured test sample rubber asphalt samples I-IX so as to obtain stress strain data under the action of cyclic loading;
step 6: deriving the storage modulus G 'and the loss modulus G' obtained in the step 5, drawing relation curves of lgG '(omega) -lgG' (omega) of nine test samples by adopting Origin data processing software, establishing Han theoretical curve relation of the multiphase dispersed polymer system under frequency scanning, and calculating slope k of the relation curves of lgG '(omega) -lgG' (omega);
in this example, the log values of the loss modulus G ' and the storage modulus G ″ are calculated by taking 10 as a base number, the corresponding log value of the loss modulus G ' is used as a first coordinate value, the corresponding log value of the storage modulus G ″ is used as a second coordinate value, a graph is drawn in a planar rectangular coordinate system, and a Han rheological property index test curve under the working condition is formed by connecting points (lgG ', lgG ") under different coordinates;
the measured Han rheological curve was subjected to linear fitting and regression to obtain a curve slope k as a quantitative evaluation index of the phase structure performance characteristics of the rubber asphalt samples I to IX, as shown in table 5.
TABLE 5 Han rheological Curve linear regression results of rubber asphalt under frequency sweep conditions
And 7: fig. 7 is a Han plot of the frequency sweep conditions of test sample I and test sample II with slope magnitudes that allow quantitative assessment of the phase structure characteristics of the bituminous polymer, as shown in fig. 8. FIG. 7 shows that the phase separation frequencies of lgG' (ω) to lgG "(ω) of the homogeneous polymers do not occur, i.e., that there is no frequency dependence.
And 8: and (3) the rheological property test data obtained in the step (5) comprises the following steps: composite shear modulus G*And phase angle delta, and drawing G of nine test samples by using Origin data processing software*A delta relation curve, and establishing a Black relation curve of the multiphase dispersion polymer system;
it should be noted that, in the present example, the corresponding complex modulus G is used*As a first coordinate value, the corresponding phase angle δ as a second coordinate value, and drawing a graph in a planar rectangular coordinate system, under different coordinates (G)*Delta) to form a Black rheological property index test curve under the working condition;
and step 9: obtaining G obtained in step 8*And (3) linear fitting characteristics of a delta relation curve, qualitatively judging phase structure characteristics and compatibility characteristics of the rubber composite modified asphalt by using Black curve fitting characteristics, wherein FIG. 9 is a Black curve graph of a rubber asphalt sample I-a rubber asphalt sample IX under a frequency scanning rheological test, and Table 6 is the Black curve fitting characteristics, phase structure changes of the asphalt can be visually observed by using the Black curve, and a smooth consistent curve can be formed by using the good compatibility of the polymer and the asphalt. From FIG. 9, the phase junction of the two test samples can be seenGood structural uniformity and curve fitting characteristic correlation coefficient R2The phase structure of the polymer modified asphalt can be qualitatively judged as the standard for judging the phase structure change of the polymer modified asphalt and can be used as a supplementary verification condition in the steps.
TABLE 6 Black curve fitting characteristics of base asphalt and modified asphalt under frequency sweep conditions
Example 3
Step 1: heating the asphalt to be measured to a molten state, and then pouring a 25mm flat round sample;
in order to further analyze the applicability of the theory to the rubber asphalt cement system, in this embodiment, two kinds of rubber powders (activated rubber powder and non-activated rubber powder) are selected and respectively mixed with one kind of mineral powder to prepare rubber asphalt cement systems with different rubber powder ratios (0.8, 1.0 and 1.2), and six kinds of test samples are prepared, namely a rubber asphalt cement system I (activated rubber powder and rubber powder ratio 0.8), a rubber asphalt cement system II (activated rubber powder and rubber powder ratio 1.0), a rubber asphalt cement system III (activated rubber powder and rubber powder ratio 1.2), a rubber asphalt cement system IV (non-activated rubber powder and rubber powder ratio 0.8), a rubber asphalt cement system V (non-activated rubber powder and rubber powder ratio 1.0) and a rubber asphalt cement system VI (non-activated rubber powder and rubber powder ratio 1.2). The six test samples are placed in an oven at 160 ℃ for 1 hour indoors, after the asphalt is completely melted, the asphalt is fully stirred by a glass rod, bubbles in the asphalt are removed, and then a flat round sample of 25mm is cast.
And 2, step: dividing 25mm flat round samples into two groups, and respectively carrying out a temperature scanning test and a frequency scanning test by adopting a dynamic shear rheometer;
and step 3: the fixed loading frequency is 1.59Hz, the temperature interval is selected to be 58-80 ℃, and a strain control mode is adopted to respectively carry out temperature scanning rheological tests on a group of 25mm asphalt samples of six poured rubber asphalt mortar systems I-VI to obtain stress strain data under the action of cyclic loading;
and 4, step 4: deriving the storage modulus G 'and the loss modulus G' of the rheological property test data obtained in the step 3, drawing relationship curves of lgG '(omega) -lgG' (omega) of six test samples by adopting Origin data processing software, establishing a Han theoretical curve relationship of the multiphase dispersed polymer system under temperature scanning, and calculating the relationship curve slope k of lgG '(omega) -lgG' (omega);
in this example, the log values of the loss modulus G ' and the storage modulus G ″ are calculated by taking 10 as a base number, the corresponding log value of the loss modulus G ' is used as a first coordinate value, the corresponding log value of the storage modulus G ″ is used as a second coordinate value, a graph is drawn in a planar rectangular coordinate system, and a Han rheological property index test curve under the working condition is formed by connecting points (lgG ', lgG ") under different coordinates;
the measured Han rheological curve is subjected to linear fitting and regression to obtain a curve slope k as a quantitative evaluation index of the phase structure performance characteristics of the rubber asphalt cement system I to the rubber asphalt cement system VI, which is shown in Table 7.
TABLE 7 Han rheological curve linear regression results of rubber asphalt mortar system under temperature scanning conditions
FIG. 10 is a Han curve diagram of rubber asphalt cement system I to rubber asphalt cement system VI under temperature scanning conditions, and the slope magnitude of the Han curve diagram can quantitatively evaluate the phase structure characteristics of asphalt polymers, as shown in FIG. 11. Fig. 10 shows that the phase separation temperatures of lgG' (ω) to lgG "(ω) of the heterophasic polymers do not occur, i.e. they do not have a temperature dependence.
And 5: the fixed loading temperature is 60 ℃, the frequency interval is controlled to be 0.1-10 Hz, and a strain control mode is adopted to respectively carry out frequency scanning rheological tests on another 25mm asphalt sample of six poured test samples, namely a rubber asphalt mastic system I to a rubber asphalt mastic system VI, so as to obtain stress strain data under the action of cyclic loading;
step 6: deriving the storage modulus G 'and the loss modulus G' obtained in the step 5, drawing relation curves of lgG '(omega) -lgG' (omega) of six test samples by adopting Origin data processing software, establishing Han theoretical curve relation of the multiphase dispersed polymer system under frequency scanning, and calculating slope k of the relation curves of lgG '(omega) -lgG' (omega);
in this example, the logarithmic value of the loss modulus G ' and the storage modulus G ″ is calculated based on 10, the logarithmic value of the corresponding loss modulus G ' is used as the first coordinate value, the logarithmic value of the corresponding storage modulus G ″ is used as the second coordinate value, a graph is drawn in a planar rectangular coordinate system, and a Han rheological property index test curve under the working condition is formed by connecting points (lgG ', lgG ") under different coordinates;
the measured Han rheological curve is subjected to linear fitting and regression to obtain a curve slope k as a quantitative evaluation index of the phase structure performance characteristics of the rubber asphalt cement system I to the rubber asphalt cement system VI, which is shown in Table 8.
TABLE 8 Han rheological curve linear regression results of rubber asphalt under frequency scanning conditions
And 7: fig. 12 is a Han plot of the frequency sweep conditions for test sample I and test sample II with slope magnitudes that allow quantitative assessment of the phase structure characteristics of the bituminous polymer, as shown in fig. 13. FIG. 12 shows that the phase separation frequencies of lgG' (ω) to lgG "(ω) of the homogeneous polymers do not occur, i.e., that there is no frequency dependence.
And step 8: and (3) the rheological property test data obtained in the step (5) comprises the following steps: composite shear modulusG*And phase angle delta, and drawing G of six test samples by using Origin data processing software*A delta relation curve, and establishing a Black relation curve of the multiphase dispersion polymer system;
it should be noted that, in the present example, the corresponding complex modulus G is used*As a first coordinate value, the corresponding phase angle δ as a second coordinate value, and drawing a graph in a planar rectangular coordinate system, under different coordinates (G)*Delta) to form a Black rheological property index test curve under the working condition;
and step 9: obtaining G obtained in step 8*And (3) linear fitting characteristics of a delta relation curve, qualitatively judging phase structure characteristics and compatibility characteristics of the rubber composite modified asphalt by using Black curve fitting characteristics, and obtaining a Black curve graph of a rubber asphalt mortar system I-a rubber asphalt mortar system VI under a frequency scanning rheological test in FIG. 14. Table 9 shows the fitting characteristics of the Black curve, the phase structure change of the asphalt can be visually observed by using the Black curve, and the smooth coherent curve can be formed by good compatibility of the polymer and the asphalt. From fig. 14, it can be seen that the phase structure uniformity of the six test samples is good, and the correlation coefficient R of the curve fitting characteristic is good2The phase change of the polymer modified asphalt cement system can be qualitatively used as a judgment standard for the phase structure change of the polymer modified asphalt cement system, and can be used as a supplementary verification condition in the steps.
TABLE 9 Black curve fitting characteristics of base asphalt and modified asphalt under frequency sweep conditions
In conclusion, the rubber asphalt phase structure evaluation method combining quantification and qualification provided by the invention obtains the rheological property index loss modulus G ', the storage modulus G' and the composite modulus G by performing dynamic shear rheological tests on test samples at different temperatures and frequencies*And a phase angle δ. Based on the rheological property index, the lgG '(omega) -lgG' (omega) Han graphs and G of the rheological property index are drawn*Delta Black plot, buildHan theoretical curve equation of the vertical multi-phase dispersion polymer system, thereby quantitatively calculating the slope k of the Han curve. For a multiphase polymer in a linear visco-elastic interval, the closer the slope of a Han curve is to 2, the closer the slope is to a homogeneous polymer, the better the compatibility of a rubber asphalt cement system is, and the evaluation and judgment method for quantitatively evaluating the phase structure of the rubber asphalt and the rubber cement system thereof can be provided; in order to effectively avoid the unicity of an evaluation means, the method is combined with the Black curve block diagram theory, the phase structure change of the rubber modified asphalt can be visually seen through the Black curve, a continuous curve can be drawn from rheological data at different temperatures, and the continuous smooth characteristic of the curve reflects the good compatibility of the polymer and the asphalt to a certain extent. The quantitative and quantitative combined evaluation method avoids the fuzziness of the traditional evaluation rubber modification mechanism and the phase structure, has high test speed, can collect a large amount of analysis data, ensures the objectivity and scientificity of test evaluation to a certain extent, and ensures the accuracy and the effectiveness of the performance evaluation of the rubber asphalt in the actual engineering application.
Reference in the specification to "some embodiments," "one embodiment," or "an embodiment," etc., means that a particular feature, structure, or characteristic described in connection with the embodiment is included in at least one embodiment. Thus, appearances of the phrases "in some embodiments," "in one embodiment," or "in an embodiment," etc., in various places throughout this specification are not necessarily referring to the same embodiment. Furthermore, the particular features, structures, or characteristics may be combined in any suitable manner in one or more embodiments. Additionally, the various elements of the drawings of the present application are merely schematic illustrations and are not drawn to scale.
Having thus described several aspects of at least one embodiment of this invention, it is to be appreciated various alterations, modifications, and improvements will readily occur to those skilled in the art. Such alterations, modifications, and improvements are intended to be within the spirit and scope of the invention.
Claims (5)
1. A method for evaluating the phase structure of rubber asphalt by combining quantification and qualification is characterized by comprising the following steps:
step 1: heating the asphalt to be measured to a molten state, and then pouring a 25mm flat round sample;
step 2: dividing 25mm flat round samples into two groups, and respectively applying temperature scanning and frequency scanning dynamic shear rheological tests;
and 3, step 3: under a constant value stress-strain level and with fixed frequency, carrying out a temperature scanning rheological test on a group of 25mm rubber asphalt samples which are cast, and obtaining rheological property test data, wherein the rheological property test data comprises the following steps: storage modulus G' and loss modulus G ";
and 4, step 4: deriving the storage modulus G 'and the loss modulus G' of the rheological property test data obtained in the step 3, drawing a relationship curve of lgG '(omega) -lgG' (omega), establishing a Han theoretical curve relationship of the multiphase dispersed polymer system under temperature scanning, and calculating the slope k of the relationship curve of lgG '(omega) -lgG' (omega);
and 5: under a constant value stress-strain level and at a fixed temperature, performing a frequency scanning rheological test on another group of poured 25mm rubber asphalt samples to obtain rheological property test data, wherein the rheological property test data comprises the following steps: storage modulus G', loss modulus G ", composite shear modulus G*And a phase angle δ;
step 6: deriving the storage modulus G 'and the loss modulus G' obtained in the step 5, drawing relation curves of lgG '(omega) -lgG' (omega), establishing a Han theoretical curve relation of the multiphase dispersion polymer system under frequency scanning, and calculating the slope k of the relation curves of lgG '(omega) -lgG' (omega);
and 7: quantitatively judging the phase structure characteristics and the compatibility characteristics of the rubber composite modified asphalt under temperature scanning and frequency scanning by utilizing the slope k of the relationship curve from lgG '(omega) to lgG' (omega) obtained in the step 4 and the step 6;
and 8: and (3) the rheological property test data obtained in the step (5) comprises the following steps: composite shear modulus G*And phase angle delta, plot G*The delta relation curve is obtained, and a Black relation curve of the multiphase dispersion polymer system is established;
and step 9: obtaining G obtained in step 8*Linear fitting characteristic of delta relation curve, and qualitative judgment of rubber compounding by using Black curve fitting characteristicThe phase structure characteristic and the compatibility characteristic of the modified asphalt.
2. The method for quantitatively and qualitatively evaluating the phase structure of rubberized asphalt according to claim 1, wherein the asphalt is heated at a temperature not higher than 160 ℃ in step 1, and molten asphalt to be measured is sufficiently and uniformly stirred to remove air bubbles before casting a flat round sample of 25 mm.
3. The method for quantitatively and qualitatively evaluating the phase structure of rubber asphalt as claimed in claim 1, wherein the temperature sweep test in step 3 is an analytical test using a dynamic shear rheometer for base asphalt, modified asphalt, composite modified rubber asphalt and rubber asphalt cement systems thereof; a rotor of the dynamic shear rheometer is 25mm in size and 1mm in gap, and a temperature scanning test is carried out by adopting a strain control mode; the experimental parameters were set as follows: the fixed loading frequency is 1.59Hz, and the temperature interval is 58-80 ℃.
4. The method for quantitatively and qualitatively evaluating the phase structure of rubber asphalt as claimed in claim 1, wherein the frequency sweep test in step 5 is performed by using a dynamic shear rheometer to analyze the matrix asphalt, the modified asphalt, the composite modified rubber asphalt and the rubber asphalt cement system thereof, the rotor is 25mm and the gap is 1mm, and the frequency sweep test is performed by using a strain control mode, and the test parameters are set as follows: the fixed loading temperature is 60 ℃, and the frequency interval is controlled to be 0.1-10 Hz.
5. The method for quantitatively and qualitatively evaluating the phase structure of rubber asphalt as claimed in claim 1, wherein the Han theoretical curve of the multi-phase dispersion polymer system in steps 4 and 6 is as follows:
wherein k is lgThe slope of the G' (ω) -lgG "(ω) relationship;
is the plateau modulus.
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| CN117408090B (en) * | 2023-12-14 | 2024-03-08 | 华南理工大学 | Rubber modified asphalt main curve characterization method based on combined model |
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