CN112666115A - Method for testing dispersity of SBS (styrene butadiene styrene) modifier in asphalt mixture - Google Patents
Method for testing dispersity of SBS (styrene butadiene styrene) modifier in asphalt mixture Download PDFInfo
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Abstract
The invention relates to the technical field of road engineering material detection, in particular to a method for testing the dispersibility of an SBS modifier in an asphalt mixture. The method for testing the dispersibility of the SBS modifier in the asphalt mixture comprises the following steps: (1) dispersedly sampling the asphalt mixture to be detected, dissolving the sample and filtering to obtain a solution; (2) performing infrared test on the solution by using a calcium fluoride or potassium bromide slide transmission method; (3) carrying out quantitative analysis on the obtained infrared image, integrating the infrared spectrogram, and calculating the areas of two single peaks in the characteristic peaks of the asphalt and the SBS respectively; (4) the area ratio of the two peaks is recorded as Z, and the average value is calculated
Analysis of all samples ZiValue, calculating the discreteness; when the dispersion coefficient is less than 10%, the dispersibility meets the requirement. The testing method can characterize the dispersibility of the SBS modifier in the asphalt mixture in various aspectsAnd the dispersibility evaluation is carried out on the mixing and paving processes of different SBS modified asphalt, so that a basis is provided for the improvement of the construction process.
Description
Technical Field
The invention relates to the technical field of road engineering material detection, in particular to a method for testing the dispersibility of an SBS modifier in an asphalt mixture.
Background
With the development of modern transportation, the traditional asphalt is gradually difficult to meet the technical requirements of road pavements. Styrene-butadiene-styrene block copolymer (SBS) is an important asphalt modifier, and can effectively improve the high and low temperature performance, the anti-rutting capability and the like of asphalt. The SBS modifier used in the industry at present is mainly modified by a wet method, namely SBS is ground and then is uniformly mixed with asphalt by means of high-speed shearing and the like to prepare SBS modified asphalt, and then the SBS modified asphalt is used in construction. However, the wet process has very obvious limitations, needs special modification equipment and has complex process; the asphalt is high in heating temperature and easy to age; the SBS modifier has poor compatibility with asphalt and is easy to separate; in addition, the mixing amount of the SBS modifier and the quality of the base asphalt are difficult to control, and the factors directly cause the SBS wet modified asphalt to have a plurality of problems, thereby seriously influencing the service life of the asphalt pavement. The dry direct-vat-set process is to prepare the SBS modifier into appropriate solid particles in advance through a certain processing technology, and directly mix the solid particles with the asphalt mixture to realize crosslinking and dispersion in the mixing process. The dry method effectively solves various problems in the wet method process and ensures the quality of the asphalt mixture.
By adopting a dry-process direct-vat set process, the modification influence of SBS modifier particles on asphalt greatly depends on the mixing amount and the dispersion state, particularly the uniformity of the SBS modifier particles in the asphalt mixture. However, for the dry-process direct vat set process, the SBS modifier particles are directly mixed into a mixing pan to be mixed into a mixture, so that the dispersion state of the SBS modifier in the mixture is difficult to characterize specifically. However, this method is often very variable, inaccurate, unspecific and lacks scientificity and stringency. In addition, the traditional visualization-mathematical calculation method (V-C method) for measuring SBS content/distribution is limited by its measurement principle, and most of the data collection methods are estimation methods, even though the result is close to an accurate value through mathematical processing, the actual value cannot be measured by this method.
Therefore, for the dry process, no good analysis means exists for ensuring that the dry SBS modifier is uniformly dispersed in the asphalt mixture in the process of blending with the aggregate. Aiming at the characteristic of short mixing time of the asphalt mixture in the dry construction process, how to quickly analyze and identify the dispersion uniformity of SBS modifier particles becomes a key factor influencing the quality of the asphalt mixture in the dry SBS direct vat set process. A scientific and accurate method is found for representing the dispersion state of SBS in the asphalt mixture, and the method has great significance for improving the dry SBS mixing process and the construction process and further ensuring the quality of the asphalt mixture.
Disclosure of Invention
The invention provides a method for testing the dispersibility of SBS modifier in asphalt mixture, which can accurately represent the dispersibility of SBS modifier in asphalt mixture in many aspects, is convenient for carrying out dispersibility evaluation on different SBS modified asphalt mixing and paving processes, and provides basis for improvement of construction process; has good practical and popularization value and solves the problems in the prior art.
The technical scheme adopted by the invention is as follows:
a method for testing the dispersibility of an SBS modifier in an asphalt mixture comprises the following operation steps:
(1) performing dispersed sampling on the modified asphalt mixture to be detected, dissolving the sample and filtering to obtain a solution for later use;
(2) using calcium fluoride (CaF)2) Or carrying out infrared test on the solution in the step (1) by a potassium bromide slide transmission method;
(3) carrying out quantitative analysis on the obtained infrared image, integrating the infrared spectrogram by using OPUS software, and calculating the areas of two single peaks in the characteristic peaks of the asphalt and the SBS respectively;
(4) the area ratio of the two peaks is recorded as Z, and the average value is calculated
Analyzing Zi values of all samples, and obtaining the discreteness of the Zi values according to the following formula; the specific calculation formula is as follows:
variance (variance)
Coefficient of dispersion
When the dispersion coefficient is less than 10%, the dispersibility meets the requirement, and the SBS modifier is uniformly dispersed in the asphalt mixture; on the contrary, the dispersibility is not satisfactory, and the SBS modifier is not uniformly dispersed in the asphalt mixture.
Further, in the step (1), 3-5 points are selected at different positions of the modified asphalt mixture to be detected by means of dispersed sampling; using a proper amount of carbon tetrachloride (CCl) for the sample in the step (1)4) Dissolving to obtain a solution.
Further, in the step (1), 4-5 points are selected at different positions of the modified asphalt mixture to be detected by means of dispersed sampling.
Further, in the step (1), 4 points are selected at different positions of the modified asphalt mixture to be detected by means of dispersed sampling.
Further, the infrared test in the step (2) takes a blank slide as a background, the background scanning time is 64 times, the sample scanning time is 64 times, the scanning speed is 7.5KHz, and the 4000-one 600cm sample is reserved－1Data in interval with resolution of 4cm－1。
Further, the characteristic peaks of the asphalt and SBS in the step (3) are 1356cm respectively－1And 955cm－1(ii) a The integration limits were set to 1425-1329.5 cm, respectively－1And 985.5-952.5 cm－1；
The method for testing the dispersibility of the SBS modifier in the asphalt mixture further comprises the following steps:
(5) selecting asphalt and SBS modifier with the same type as the tested object to prepare a series of SBS modified asphalt, performing infrared test by using the methods of the synchronous steps (2) and (3), and drawing a standard curve of absorbance-SBS content by using the Z value and the ratio as coordinates respectively;
(6) and comparing the Z value of the actual sampling point with the standard curve, wherein the corresponding proportioning value is the absolute concentration of the SBS at the sampling position.
The SBS absolute concentration obtained by the method is a true value of SBS content, and the method is an accurate measuring method constructed based on the Lambert beer law. The actual value-based discrete analysis is undoubtedly more accurate and reliable than the existing traditional method of analyzing by using the estimated value.
The invention has the beneficial effects that:
the invention discloses a method for testing the dispersibility of an SBS modifier in an asphalt mixture, which is an innovation for solving the problem that no scientific and accurate analysis method for the dispersibility of the existing dry-process SBS modifier in the asphalt mixture exists. Specifically, the interference of various components in the asphalt mixture is eliminated by carrying out scientific sampling design, dissolution, separation and other treatments on a sample, so that the analysis environment is simplified, and the real content of the dispersion coefficient and the absolute concentration of SBS in the asphalt mixture is obtained by adopting Fourier transform infrared spectrum representation. The testing method can accurately represent the dispersibility of the SBS modifier in the asphalt mixture in many aspects, is convenient for carrying out dispersibility evaluation on different SBS modified asphalt mixing and paving processes, and provides basis and guidance for improvement of the construction process; has good practical and popularization value.
From a microscopic view point, the SBS modification effect on the asphalt mixture is mainly realized by dispersing in the asphalt mixture and mutually crosslinking to form a stable network dispersion system, and the process is more physical dispersion than chemical combination. Therefore, for the SBS modified asphalt, the performance is good and bad, and the mixing amount and the distribution uniformity of the SBS modifier are closely related. The existing conventional methods such as a fluorescence microscope method, a gel permeation chromatography method, a thermogravimetric analysis method, a total reflection infrared spectroscopy (ATR) method and the like are used for analyzing the SBS mixing amount in the modified asphalt, are not accurate, only can analyze the modified asphalt, cannot analyze complex modified asphalt mixture and are interfered by other components. The method for analyzing the distribution uniformity of SBS in the modified asphalt mixture can be well used for measuring the dispersibility of SBS in the asphalt mixture, the dispersibility of SBS in the asphalt mixture is normalized by introducing the dispersion coefficient and taking the dispersion coefficient as the standard, and the absolute concentration of SBS in the asphalt mixture is measured at the same time, so that the quantitative SBS dispersibility test is realized, and the method has obvious effect on actual production.
The invention establishes an analysis method for the distribution uniformity of SBS in the modified asphalt mixture by infrared spectroscopy, takes SMA-13 gradation as an example, and analyzes the distribution uniformity of SBS modifier in the mixture under different mixing time and the corresponding mixture performance by using the method. By using the method, the dispersion uniformity of the SBS in the modified asphalt mixture can be accurately judged, and the absolute content of the SBS at a certain position can be obtained through conversion. More importantly, the analysis result can guide the construction process of the dry SBS to make targeted adjustment, which is undoubtedly significant for the practical application of the dry SBS.
Drawings
FIG. 1 is a graph of the present invention showing the sampling points determining the dispersion coefficient deviation for different sampling times in an experiment;
FIG. 2 is a dry SBS absorbance-concentration standard curve;
FIG. 3 shows the IR spectrum of SBS modified asphalt and the corresponding characteristic peak integrals.
Wherein, the fitting formula in fig. 2 is: Y-123.58X +13.3131, i.e. Z-123.58 c +13.3131, R2＝0.9868。
Detailed Description
In order to clearly explain the technical features of the present invention, the following detailed description of the present invention is provided with reference to the accompanying drawings.
Example 1
A method for testing the dispersibility of SBS modifier in asphalt comprises the following steps:
(1) performing dispersed sampling on the modified asphalt mixture to be detected, wherein the sampling position has obvious distinction degree and comprises an edge, a center, a bottom layer and a surface layer; adding proper amount of carbon tetrachloride (CCl)4) Dissolving the sample to obtain a solution for later use;
(2) performing infrared test on the solution in the step (1) by using a calcium fluoride or potassium bromide slide transmission method; using blank slide as background, background scanning time is 64 times, sample scanning time is 64 times, scanning speed is 7.5KHz, and 4000-one 600cm is reserved－1Data in interval with resolution of 4cm－1；
(3) Carrying out quantitative analysis on the obtained infrared image, integrating the infrared spectrogram by using OPUS software, integrating the infrared spectrogram, and calculating the areas of two single peaks in the characteristic peaks of the asphalt and the SBS respectively;
(4) the area ratio of the two peaks is recorded as Z, and the average value is calculated
Analysis of all samples for ZiA value whose discreteness is calculated; the specific calculation formula is as follows:
variance (variance)
Coefficient of dispersion
When the dispersion coefficient is less than 10%, the dispersibility meets the requirement, and the SBS modifier is uniformly dispersed in the asphalt mixture; on the contrary, the dispersibility is not satisfactory, and the SBS modifier is not uniformly dispersed in the asphalt mixture.
The detection method also comprises the step of measuring the content of the SBS modifier in the asphalt mixture.
The method of the invention comprises the following steps:
selecting 10 points from different positions of the modified asphalt mixture to be detected, respectively taking a small number of small mixture samples, wherein the sampled positions have obvious distinction degree and comprise representative positions such as edges, centers, bottom layers, surface layers and the like, and each position is respectively taken with at least one sample. Using appropriate carbon tetrachloride (CCl)4) Dissolving the sample, simply filtering to remove interference of solid impurities, or placing the sample on a filter paper, and adding the same portion of CCl4And (5) repeatedly flushing. The filtrate was collected and an appropriate amount of the filtrate was dropped onto a potassium bromide (KBr) window using a dropper for infrared testing.
Carrying out quantitative analysis on the obtained infrared image, integrating the infrared spectrogram by using OPUS software, and calculating the areas of two single peaks in the characteristic peaks of the asphalt and the SBS respectively, wherein the integration limit selected in the text is 1347-－1And 946 ion 986cm－1. And (4) recording the area ratio of the two peaks as Z, analyzing Zi values of all samples, and calculating the dispersion coefficient of the Zi values.
For infrared spectroscopy, theoretically, the more the number of sampling points, the more comprehensive the analysis result is. However, the number of samplings follows a marginal effect, taking a limited number of samples to be measured, in terms of cost and ease of operation, so that the results obtained are not far from a large number of measurements. Taking SBS modified asphalt with the mass percent of 4% as an example, the same object to be tested is sampled for 10 times, the Z value obtained by each sampling test is recorded, and the average value is calculated
Taking the final dispersion coefficient CV10 obtained by 10 tests as a standard value, and then calculating the sampling times to be i in sequence
And the difference of CVi from the standard value. As can be seen from fig. 1, when the number of samples is greater than or equal to 3, the change of Δ CV tends to be smooth, and the optimal number of samples is determined to be 3-5 by comprehensively considering the accuracy of the experiment and the test cost. To ensure the accuracy of the experiment, samples were taken uniformly 4 times during the subsequent experiments.
The results of the experiment are shown in table 1 below:
TABLE 1 number of optimal sampling points for infrared spectroscopy
Example 2
In this example, a pre-configured series of concentration gradients of SBS modified asphalt is used to plot an absorbance-concentration standard curve. The infrared acquisition and data processing both use the OPUS software, and other data processing software with an integral function can also be used. Area ratio Z after integrationiThe discrete computation of (2) may use any data processing software.
Establishment of absorbance-dry SBS mixing amount standard curve
Weighing a certain amount of dry-process SBS modifier particles and No. 70 matrix asphalt by using an analytical balance, dissolving by using carbon tetrachloride to prepare an SBS modified asphalt solution with specified concentration, setting the concentration gradient to be 4-6%, setting 5 groups in total, and setting 5 parallel samples in each group. When infrared measurement is carried out, if the data of the test is not abnormal, the slide glass can be moved, and positions with different shade distributions on the slide glass are selected for carrying out infrared measurement again. The results of the experiment are shown in table 2 below. The SBS absorbance-concentration standard curve is shown in FIG. 2.
TABLE 2 Standard Curve plotting Table
Wherein m1 is the mass of the matrix asphalt, and m2 is the mass of the dry SBS modifier.
Example 3
This example illustrates the SMA-13 grade and determines the optimum mixing time for dry SBS at the SMA-13 grade. A dry SBS modifier with the content of 7% is doped into No. 70 asphalt, basalt coarse aggregates and limestone fine aggregates are selected as stone materials, and three groups of different mixing time are set.
The method provided by the invention is used for carrying out SBS dispersibility analysis on the prepared three groups of mixtures, Marshall stability experiments, freeze-thaw splitting experiments, rutting experiments and the like, and analyzing the influence of the mixing time on SBS dispersibility and the influence of the dispersibility of a dry SBS modifier in the asphalt mixture on the macroscopic performance of a test piece.
Firstly, preparing a dry SBS modified asphalt mixture:
(1) dry mixing 60/90/120s of the dry SBS modifier and the hot aggregate so as to uniformly disperse the dry SBS modifier in the mineral aggregate;
(2) adding asphalt according to a preset dosage, and stirring for 60/90/120 s; adding the mineral powder and mixing for 60/90/120 s;
(3) and (3) placing the mixed mixture into a heat-insulating barrel or an enamel tray, placing the mixture into an oven with the temperature of 170 and 180 ℃ for constant-temperature development for 2h (simulating the heat-insulating working condition of a transport vehicle before paving), then taking out the mixture, sampling and cooling the mixture for later use according to the requirements provided by the invention, and forming asphalt mixture test pieces by using the rest of the mixture. The temperature control was performed as in table 3 below.
TABLE 3 test temperature of SMA-13-graded mixes
Second, SBS Dispersion test
The mixtures with different mixing times are respectively numbered 1-3, the dispersibility of the SBS modifier in the mixtures is tested by the same method by using the good samples, and the formed test pieces are respectively subjected to a Marshall stability test, a freeze-thaw splitting test, a rutting test and the like. The experimental results are shown in table 4 below.
TABLE 4 SBS blending analysis of three sets of blends
It can be seen from table 4 above that, when the two stirring times are set to 60s, the calculated dispersion coefficient is 10.16%, which is slightly higher than the range of dispersion coefficient less than 10% required by the testing method of the present invention, indicating that the uniformity of the dispersion effect of the SBS modifier is general, and further adjustment of the process is required. Comparing the groups 2 and 3, it can be seen that the dispersion of SBS tends to be uniform slowly with increasing stirring time. And the dispersion effect of the group 3 is better and more uniform than that of the group 2, but the advantages are not obvious, and the experiment shows that the two-time stirring time is about 90s when dry SBS construction is carried out in consideration of construction cost and operation difficulty. Particularly, the standard curve of the embodiment 2 is adopted to calculate the SBS content, and calculated values of the SBS content obtained by three groups of tests are better in accordance with actual values, so that the reliability of the measuring method is further illustrated. Therefore, the testing method provided by the invention is used for detecting the dispersity and the content of SBS in the asphalt mixture, and the construction process can be guided and improved according to the dispersion coefficient determined by the dispersity, so that the method is favorable for providing a basis for the improvement of the construction process and making targeted adjustment.
Third, testing the mixture performance
The performance test of the mixture is carried out according to the technical requirements of the technical Specification of the asphalt pavement for roads, and the test results are shown in the following table 5:
TABLE 5 Performance analysis of the three-component mixtures
The experimental results in table 5 show that the degree of uniformity of the SBS dispersion is positively correlated to the properties of the corresponding modified asphalt mixture, so that the control of the uniformity index of SBS in the modified asphalt mixture is good, and undoubtedly, the control of the overall properties of the mixture has an important guiding function. The method and the standard of the invention can be used for continuously improving and monitoring the dry SBS construction process and continuously exploring the construction conditions capable of obtaining the optimal uniformity.
The above-described embodiments should not be construed as limiting the scope of the invention, and any alternative modifications or alterations to the embodiments of the present invention will be apparent to those skilled in the art.
The present invention is not described in detail, but is known to those skilled in the art.
Claims (6)
1. A method for testing the dispersibility of an SBS modifier in an asphalt mixture is characterized by comprising the following operation steps:
(1) performing dispersed sampling on the modified asphalt mixture to be detected, dissolving the sample and filtering to obtain a solution for later use;
(2) performing infrared test on the solution in the step (1) by using a calcium fluoride or potassium bromide slide transmission method;
(3) carrying out quantitative analysis on the obtained infrared image, integrating the infrared spectrogram, and calculating the areas of two single peaks in the characteristic peaks of the asphalt and the SBS respectively;
(4) the area ratio of the two peaks is recorded as Z, and the average value is calculated
Analysis of all samples for ZiThe value, whose discreteness is obtained according to the following formula; the specific calculation formula is as follows:
variance (variance)
Coefficient of dispersion
When the dispersion coefficient is less than 10%, the dispersibility meets the requirement, and the SBS modifier is uniformly dispersed in the asphalt mixture; on the contrary, the dispersibility is not satisfactory, and the SBS modifier is not uniformly dispersed in the asphalt mixture.
2. The method for testing the dispersibility of the SBS modifier in the asphalt mixture according to claim 1, wherein in the step (1), the dispersing sampling is performed by selecting 3 to 5 points at different positions of the modified asphalt mixture to be tested; using a proper amount of carbon tetrachloride (CCl) for the sample in the step (1)4) Dissolving to obtain a solution.
3. The method for testing the dispersibility of the SBS modifier in the asphalt mixture according to claim 2, wherein the step (1) of sampling the dispersion is performed by selecting 3 to 5 points at different positions of the modified asphalt mixture to be tested.
4. The method for testing the dispersibility of SBS modifier in asphalt mixture as claimed in claim 1, wherein the infrared test in step (2) uses blank slide as background, the background scanning time is 64 times, the sample scanning time is 64 times, the scanning speed is 7.5KHz, and the 4000-cm retention time is 600cm－1Data in interval with resolution of 4cm－1。
5. The method for testing the dispersibility of the SBS modifier in the asphalt mixture as claimed in claim 1, wherein the characteristic peaks of the asphalt and the SBS in the step (3) are 1356cm respectively－1And 955cm－1(ii) a The integration limits were set to 1425-1329.5 cm, respectively－1And 985.5-952.5 cm－1。
6. The method for testing the dispersibility of SBS modifiers in asphalt of claim 1, further comprising:
(5) selecting asphalt and SBS modifier with the same type as the tested object to prepare a series of SBS modified asphalt, performing infrared test by using the methods of the synchronous steps (2) and (3), and drawing a standard curve of absorbance-SBS content by using the Z value and the ratio as coordinates respectively;
(6) and comparing the Z value of the actual sampling point with the standard curve, wherein the corresponding proportioning value is the SBS content value of the sampled position.
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| CN114047098A (en) * | 2021-11-11 | 2022-02-15 | 山东高速工程检测有限公司 | Method for quantitatively determining dissolution degree of dry-process modifier in asphalt mixture |
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