CN101571427B - Transition temperature method for detecting aggregative state of asphalt with ultraviolet aging - Google Patents
Transition temperature method for detecting aggregative state of asphalt with ultraviolet aging Download PDFInfo
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- CN101571427B CN101571427B CN2009100723067A CN200910072306A CN101571427B CN 101571427 B CN101571427 B CN 101571427B CN 2009100723067 A CN2009100723067 A CN 2009100723067A CN 200910072306 A CN200910072306 A CN 200910072306A CN 101571427 B CN101571427 B CN 101571427B
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Abstract
The invention provides a transition temperature method for detecting the aggregative state of asphalt with ultraviolet aging, which relates to a transition temperature method for detecting the aggregative state of the asphalt with the ultraviolet aging. The invention overcomes the defects that the existing transition method for detecting the aggregative state of the asphalt with the ultraviolet aging has complicated operation, high cost and disagreement with time-temperature equivalence principle. The transition performance method for the aggregative state of the asphalt with the ultraviolet aging is proceeded as the following steps: 1. frequency scanning is carried out, and the frequency scanning is carried out again after temperature rise or temperature drop; 2. the principal curve of the frequency scanning is obtained; 3. the time-temperature equivalent invalidation temperature of the aging asphalt is found out, and the temperature is the aggregative state transition temperature of the asphalt with the ultraviolet aging. The method has simple operation, low cost and conformity with time-temperature equivalence principle.
Description
Technical field
The present invention relates to the method for state of aggregation conversion temperature after detection ageing of asphalt.
Background technology
The method of state of aggregation conversion temperature mainly has three kinds after existing detection asphalt with ultraviolet aging:First, dilatometry (DTA), this method is classical measuring method, and the correlation curve of quality volume and temperature in cooling is determined using appropriate technology, and the temperature when slope of curve is changed is taken as Tg, in practical operation, T on curvegThe intersection point of two sections of straight lines of below and above is taken as Tg, slope is relevant with thermal cubic expansion coefficient a, and it is in TgDiscontinuity is presented in place, the principle of the method is very simple, but do very complicated, commonly used is discharge method, the amount for the fluid that sealing process has been discharged by polymer is determined, thermal coefficient of expansion is obtained, it is whether appropriate whether this method successfully depends on selected sealing fluid, the sealing fluid can not be by Polymer absorption, and not to be undergone phase transition within the temperature range of studying;2nd, calorimetry, with the thermal history and the difference of programming rate of sample, in TgWhen be observed that discontinuity point or peak occurs in thermal capacity, differential thermal analysis and the latest development of differential scanning calorimetry improve thermodynamics assay method it is determined that TgThe importance of aspect, differential thermal analysis is easily affected by various factors, disk shape as samples, material, firing rate, and there is heat exchange between sample and reference substance, heating rate dT/dt and furnace temperature T is non-linear temperature increase, so that rectifying parameter K changes, it is difficult to carry out quantitative analysis exactly, differential scanning calorimetry (DSC) is under the conditions of programed temperature, measurement inputs to the difference power and a kind of heat analysis method of temperature relation of sample and reference substance, differential scanning calorimetry overcomes differential thermal analysis with the ripe effect of temperature difference indirect expression material, and differential thermal analysis curve influence factor is a lot, it is difficult to the defect of quantitative analysis, with high resolution, the advantages of sensitivity is high, but measurement equipment is complicated, cost is high, detection method is complicated, on-line checking can not be realized;3rd, the method (DMA) of dynamic mechanical, it is under the conditions of constant heatingrate, one constant force is applied to high polymer, the relation of the deformation of sample generation and temperature, that is, the curve that can obtain temperature deformation or title heat-machine curve within certain action time is observed;Also temperature-modulus curve can be measured, glass transition temperature, the T that this method is determined are obtained using tangential methodgThe T determined than calorimetry or dilatometrygIt is high, but can clearly characterize the direction of high polymer mechanical state conversion, existing dynamic mechanical method is that the compatible polymeric system that is judged with glass transition temperature of temperature in use spectral method does not meet time temperature equivalence principle, because DSC and DMA TEMPERATURE SPECTROSCOPYs can not detect the presence of microcell of the size less than 50nm.
The content of the invention
The present invention be in order to solve it is existing detection asphalt with ultraviolet aging after state of aggregation conversion performance method in dilatometry complex operation, differential thermal analysis measurement equipment is complicated, cost is high, detection method is complicated, can not realize on-line checking, and the method for differential thermal analysis and dynamic mechanical does not meet the defect of time temperature equivalence principle, and provide the method for detecting state of aggregation conversion temperature after asphalt with ultraviolet aging.
The method of state of aggregation conversion temperature is followed the steps below after present invention detection asphalt with ultraviolet aging:
One, pitch to be detected is heated into rubber cement shape to be placed on parallel-plate, thickness of the pitch on parallel-plate is 1000 μm~2000 μm, it is that initial temperature is scanned with 0.1~10Hz frequency to the pitch on parallel-plate with 5 DEG C, performed a scan again with 0.1~10Hz frequency on asphalt at interval of n DEG C, wherein 0 < n≤10, until the temperature of pitch reaches 63~67 DEG C of progress last time frequency scannings, the angular frequency and the corresponding relation of composite modulus obtained according to scanning draws composite modulus curve under different temperatures, composite modulus curve is wherein drawn using angular frequency as abscissa, using composite modulus as ordinate;2nd, the different composite modulus curve for drawing step one carries out time temperature equivalence conversion, and reference temperature is set as 25 DEG C, obtains the frequency scanning principal curve at 25 DEG C;3rd, the frequency of time temperature equivalence failure, the temperature that the temperature corresponding to the frequency of time temperature equivalence failure converts for state of aggregation after asphalt with ultraviolet aging are found out from the frequency scanning principal curve at 25 DEG C that step 2 is obtained;Detection pitch is heated to rubber cement shape wherein in step one, heating-up temperature is no more than 135 DEG C, and the heat time is no more than 75min;Dynamic shear rheometer is used to the frequency scanning of pitch in step one.
The method of state of aggregation conversion temperature is followed the steps below after another detection asphalt with ultraviolet aging of the present invention:First, pitch to be detected is heated into rubber cement shape to be placed on parallel-plate, thickness of the pitch on parallel-plate is 1000 μm~2000 μm, it is that initial temperature is scanned with 0.1~10Hz frequency to the pitch on parallel-plate with 65 DEG C, is performed a scan again with 0.1~10Hz frequency on asphalt at interval of n DEG C.Wherein 0 < n≤10, until the temperature of pitch reaches 3~7 DEG C of progress last time frequency scannings, the angular frequency and the corresponding relation of composite modulus obtained according to scanning draws composite modulus curve under different temperatures, composite modulus curve is wherein drawn using angular frequency as abscissa, using composite modulus as ordinate;2nd, the different composite modulus curve for drawing step one carries out time temperature equivalence conversion, and reference temperature is set as 25 DEG C, obtains the frequency scanning principal curve at 25 DEG C;3rd, the frequency of time temperature equivalence failure, the temperature that the temperature corresponding to the frequency of time temperature equivalence failure converts for state of aggregation after asphalt with ultraviolet aging are found out from the frequency scanning principal curve at 25 DEG C that step 2 is obtained;Detection pitch is heated to rubber cement shape wherein in step one, heating-up temperature is no more than 135 DEG C, and the heat time is no more than 75min;Dynamic shear rheometer is used to the frequency scanning of pitch in step one.
The method of state of aggregation conversion performance has advantages below after present invention detection asphalt with ultraviolet aging:The compatible polymeric system that is judged with DSC or DMA TEMPERATURE SPECTROSCOPYs with glass transition temperature does not simultaneously meet time temperature equivalence principle, because DSC and DMA TEMPERATURE SPECTROSCOPYs can not detect the presence of microcell of the size less than 50nm, and the phase separation of smaller yardstick can be detected with the method (method of DMA frequency spectrums) of the present invention, and meet time temperature equivalence principle.Single measurement cost of the present invention is lower than differential thermal analysis by 80%~90%, it is only necessary to which the instrument such as dynamic shear rheometer (DSR) can be detected, simple to operate.
The Method And Principle of state of aggregation conversion performance is after present invention detection asphalt with ultraviolet aging:Pitch belongs to polymer, polymer can be in one of glassy state, rubbery state and viscous state with temperature difference, each physical state concentrated expression physical characteristic of polymer, when by a certain physical state transformations into another state when, various characteristics just accordingly change.Under glassy state, because temperature is very low, the energy of molecular motion is very low, it is not enough to overcome the potential barrier of rotation in main chain, segment is in frozen state, only those less moving cells, such as side base, side chain is enough mobile with chainlet energy-conservation, when polymer is by external force, because sub-chain motion is frozen, can only be that the bond angle of main chain and bond distance have small change, as temperature is raised, the energy of molecular thermalmotion gradually increases, when reaching a certain temperature, the energy of molecular thermalmotion has been enough to overcome the potential barrier of interior rotation, at this moment segment can constantly change conformation by the interior rotation of singly-bound in main chain, moiety segments can be even made to produce sliding, polymer just enters elastomeric state, temperature continues to raise, not only the slack time of sub-chain motion shortens, and the slack time of whole strand movement also shortens to the time same order of magnitude with experimental observation, at this moment VISCOUS FLOW occurs in the presence of external force for polymer, polymer enters viscous state.Pitch issues biochemical reaction in action of ultraviolet radiation, causes asphalt component to change, and has broken original colloform texture balance, has been separated.Therefore, it can detect that state of aggregation is converted after asphalt with ultraviolet aging, characterizes the ultraviolet aging degree of pitch using the invalid temperature of time temperature equivalence principle.
But time temperature equivalence principle tends not to be applied to multiphase polymer co-mixing system (such as the pitch after ultraviolet ageing), this is due to that temperature changes the influence difference to out of phase slack time and caused.If homogeneous polymer co-mixing system is separated, special viscoelastic relaxation behavior just occurs in relaxation area in short-term or high frequency relaxation area, time temperature equivalence principle is just no longer applicable.Therefore, it there is a critical-temperature so that blend is when higher or lower than this temperature, and time temperature equivalence principle is no longer applicable, and the temperature is called the invalid temperature of time temperature equivalence principle.Many researchs confirm that the failure of time temperature equivalence principle and phase separation have close relationship, and invalid temperature is consistent with phase separation temperature, is not influenceed by Polydispersity.
Brief description of the drawings
Fig. 1 is pitch 1-9 aging 0h composite modulus curves, wherein " ■ " is principal curve, "○" is 15 DEG C of curves, and " △ " is 25 DEG C of curves,For 35 DEG C of curves,For 45 DEG C of curves,For 55 DEG C of curves,For 65 DEG C of curves;Fig. 2 is pitch 1-9 aging 110h composite modulus curves, wherein " ■ " is principal curve, "○" is 5 DEG C of curves, and " △ " is 15 DEG C of curves,For 25 DEG C of curves,For 35 DEG C of curves,For 45 DEG C of curves,For 55 DEG C of curves,For 65 DEG C of curves;Fig. 3 is pitch 1-9 aging 220h composite modulus curves, wherein " ■ " is principal curve, "○" is 5 DEG C of curves, and " △ " is 15 DEG C of curves,For 25 DEG C of curves,For 35 DEG C of curves,For 45 DEG C of curves,For 55 DEG C of curves,For 65 DEG C of curves;Fig. 4 is pitch 1-9 aging 440h composite modulus curves, wherein " ■ " is principal curve, "○" is 15 DEG C of curves, and " △ " is 25 DEG C of curves,For 35 DEG C of curves,For 45 DEG C of curves,For 55 DEG C of curves,For 65 DEG C of curves;Fig. 5 is pitch 2-9 aging 0h composite modulus curves, wherein " ■ " is principal curve, "○" is 5 DEG C of curves, and " △ " is 15 DEG C of curves,For 25 DEG C of curves,For 35 DEG C of curves,For 45 DEG C of curves,For 55 DEG C of curves,For 65 DEG C of curves;Fig. 6 is pitch 2-9 aging 110h composite modulus curves, wherein " ■ " is principal curve, "○" is 5 DEG C of curves, and " △ " is 15 DEG C of curves,For 25 DEG C of curves,For 35 DEG C of curves,For 45 DEG C of curves,For 55 DEG C of curves,For 65 DEG C of curves;Fig. 7 is pitch 2-9 aging 220h composite modulus curves, wherein " ■ " is principal curve, "○" is 5 DEG C of curves, and " △ " is 15 DEG C of curves,For 25 DEG C of curves,For 35 DEG C of curves,For 45 DEG C of curves,For 55 DEG C of curves,For 65 DEG C of curves;Fig. 8 is pitch 2-9 aging 440h composite modulus curves, wherein " ■ " is principal curve, "○" is 15 DEG C of curves, and " △ " is 25 DEG C of curves,For 35 DEG C of curves,For 45 DEG C of curves,For 55 DEG C of curves,For 65 DEG C of curves.
Embodiment
Technical solution of the present invention is not limited to act embodiment set forth below, in addition to any combination between each embodiment.
Embodiment one:The method of state of aggregation conversion temperature is followed the steps below after present embodiment detection asphalt with ultraviolet aging:One, pitch to be detected is heated into rubber cement shape to be placed on parallel-plate, thickness of the pitch on parallel-plate is 1000 μm~2000 μm, it is that initial temperature is scanned with 0.1~10Hz frequency to the pitch on parallel-plate with 5 DEG C, performed a scan again with 0.1~10Hz frequency on asphalt at interval of n DEG C, wherein 0 < n≤10, until the temperature of pitch reaches 63~67 DEG C of progress last time frequency scannings, the angular frequency and the corresponding relation of composite modulus obtained according to scanning draws composite modulus curve under different temperatures, composite modulus curve is wherein drawn using angular frequency as abscissa, using composite modulus as ordinate;2nd, the different composite modulus curve for drawing step one carries out time temperature equivalence conversion, and reference temperature is set as 25 DEG C, obtains the frequency scanning principal curve at 25 DEG C;3rd, time temperature equivalence invalid temperature is found out from the frequency scanning principal curve at 25 DEG C that step 2 is obtained, is the temperature that state of aggregation is converted after asphalt with ultraviolet aging;Detection pitch is heated to rubber cement shape wherein in step one, heating-up temperature is no more than 135 DEG C, and the heat time is no more than 75min;Dynamic shear rheometer is used to the frequency scanning of pitch in step one.
Gap of the thickness of pitch between about a pair parallel circular plates is determined in present embodiment step one.
The temperature that state of aggregation is converted after the asphalt with ultraviolet aging that present embodiment is detected is that the interval temperature n in a temperature range, step one is smaller, and the temperature principal curve error of fitting of gained is smaller, and state of aggregation conversion temperature is more accurate.
Conversion temperature is higher, and the probability that aggregation state change occurs at normal temperatures is bigger, illustrates that the degree of aging of pitch is bigger, the rheological property of pitch is poorer.
Embodiment two:The difference of present embodiment and embodiment one is:Pitch to be detected is heated into rubber cement shape in step one to be placed on parallel-plate, thickness of the pitch on parallel-plate is 1000 μm.Other steps and parameter are identical with embodiment one.
A diameter of 25mm of parallel circular plate in present embodiment.
Embodiment three:The difference of present embodiment and embodiment one is:Pitch to be detected is heated into rubber cement shape in step one to be placed on parallel-plate, thickness of the pitch on parallel-plate is 2000 μm.Other steps and parameter are identical with embodiment one.
A diameter of 8mm of parallel circular plate in present embodiment.
Embodiment four:The difference of present embodiment and embodiment one to three is:First time scanning is carried out to the pitch on parallel-plate with 2~8Hz frequency in step one.Other steps and parameter are identical with embodiment one to three.
Embodiment five:The difference of present embodiment and embodiment one to three is:First time scanning is carried out to the pitch on parallel-plate with 4~6Hz frequency in step one.Other steps and parameter are identical with embodiment one to three.
Embodiment six:The difference of present embodiment and embodiment one to three is:First time scanning is carried out to the pitch on parallel-plate with 5Hz frequency in step one.Other steps and parameter are identical with embodiment one to three.
Embodiment seven:The difference of present embodiment and embodiment one to six is:Performed a scan again with 2~8Hz frequency on asphalt at interval of n DEG C in step one, wherein 2≤n≤8.Other steps and parameter are identical with embodiment one to six.
Embodiment eight:The difference of present embodiment and embodiment one to six is:Performed a scan again with 5Hz frequency on asphalt at interval of 5 DEG C in step one.Other steps and parameter are identical with embodiment one to six.
Embodiment nine:The difference of present embodiment and embodiment one to eight is:Until the temperature of pitch reaches 64~66 DEG C of progress last time frequency scannings in step one.Other steps and parameter are identical with embodiment one to eight.
Embodiment ten:The difference of present embodiment and embodiment one to eight is:Until the temperature of pitch reaches 65 DEG C of progress last time frequency scannings in step one.Other steps and parameter are identical with embodiment one to eight.
Embodiment 11:The method of state of aggregation conversion temperature is followed the steps below after present embodiment detection asphalt with ultraviolet aging:First, pitch to be detected is heated into rubber cement shape to be placed on parallel-plate, thickness of the pitch on parallel-plate is 1000 μm, it is that initial temperature is scanned with 5Hz frequency to the pitch on parallel-plate with 5 DEG C, performed a scan again with 5Hz frequency on asphalt at interval of 10 DEG C, until the temperature of pitch reaches 65 DEG C of progress last time frequency scannings, the angular frequency and the corresponding relation of composite modulus obtained according to scanning draws composite modulus curve under different temperatures, composite modulus curve is wherein drawn using angular frequency as abscissa, using composite modulus as ordinate;2nd, the different composite modulus curve for drawing step one carries out time temperature equivalence conversion, and reference temperature is set as 25 DEG C, obtains the frequency scanning principal curve at 25 DEG C;3rd, the frequency of time temperature equivalence failure, the temperature that the temperature corresponding to the frequency of time temperature equivalence failure converts for state of aggregation after asphalt with ultraviolet aging are found out from the frequency scanning principal curve at 25 DEG C that step 2 is obtained;It will detect that the heating-up temperature that pitch is heated to rubber cement shape is 135 DEG C wherein in step one, the heat time is 75min;Dynamic shear rheometer is used to the frequency scanning of pitch in step one.
A diameter of 25mm of parallel circular plate in present embodiment.
Detect the pitch 1-9 (CNOOC pitch 36-1 brand 90#) without ultraviolet ageing respectively with the method for present embodiment, ultraviolet ageing 110h pitch 1-9, ultraviolet ageing 220h pitch 1-9, ultraviolet ageing 440h pitch 1-9, there is no the pitch 2-9 (Panjin pitch 90#) of ultraviolet ageing, ultraviolet ageing 110h pitch 2-9, ultraviolet ageing 220h pitch 2-9, ultraviolet ageing 440h pitch 2-9, testing result difference is as shown in Figures 1 to 8, show that measurement result is as shown in table 1 from Fig. 1 to Fig. 8, as can be seen from Table 1, ultraviolet aging degree of asphalt is bigger, the state of aggregation conversion temperature detected is higher, illustrate that the testing result of the method for present embodiment meets the scientific law of ageing of asphalt and state of aggregation conversion temperature, testing result is accurate.
The method single testing cost of present embodiment is substantially reduced, lower than the differential scanning calorimetry of prior art by 90%.
The mixed degree (DEG C) of state of aggregation conversion of the different ageing times of 12 kinds of pitches of table
Embodiment 12:The method of state of aggregation conversion temperature is followed the steps below after present embodiment detection asphalt with ultraviolet aging:One, pitch to be detected is heated into rubber cement shape to be placed on parallel-plate, thickness of the pitch on parallel-plate is 1000 μm~2000 μm, it is that initial temperature is scanned with 0.1~10Hz frequency to the pitch on parallel-plate with 65 DEG C, performed a scan again with 0.1~10Hz frequency on asphalt at interval of n DEG C, wherein 0 < n≤10, until the temperature of pitch reaches 3~7 DEG C of progress last time frequency scannings, the angular frequency and the corresponding relation of composite modulus obtained according to scanning draws composite modulus curve under different temperatures, composite modulus curve is wherein drawn using angular frequency as abscissa, using composite modulus as ordinate;2nd, the different composite modulus curve for drawing step one carries out time temperature equivalence conversion, and reference temperature is set as 25 DEG C, obtains the frequency scanning principal curve at 25 DEG C;3rd, time temperature equivalence invalid temperature is found out from the frequency scanning principal curve at 25 DEG C that step 2 is obtained, is the temperature that state of aggregation is converted after asphalt with ultraviolet aging;Detection pitch is heated to rubber cement shape wherein in step one, heating-up temperature is no more than 135 DEG C, and the heat time is no more than 75min;Dynamic shear rheometer is used to the frequency scanning of pitch in step one.
Gap of the thickness of pitch between about a pair parallel circular plates is determined in present embodiment step one.
The temperature that state of aggregation is converted after the asphalt with ultraviolet aging that present embodiment is detected is that the interval temperature n in a temperature range, step one is smaller, and the temperature principal curve error of fitting of gained is smaller, and state of aggregation conversion temperature is more accurate.
Conversion temperature is higher, and the probability that aggregation state change occurs at normal temperatures is bigger, illustrates that the degree of aging of pitch is bigger, the rheological property of pitch is poorer.
Embodiment 13:The difference of present embodiment and embodiment 12 is:Pitch to be detected is heated into rubber cement shape in step one to be placed on parallel-plate, thickness of the pitch on parallel-plate is 1000 μm.Other steps and parameter are identical with embodiment 12.
A diameter of 25mm of parallel circular plate in present embodiment.
Embodiment 14:The difference of present embodiment and embodiment 12 is:Pitch to be detected is heated into rubber cement shape in step one to be placed on parallel-plate, thickness of the pitch on parallel-plate is 2000 μm.Other steps and parameter are identical with embodiment 12.
A diameter of 8mm of parallel circular plate in present embodiment.
Embodiment 15:The difference of present embodiment and embodiment 12 to 14 is:First time scanning is carried out to the pitch on parallel-plate with 2~8Hz frequency in step one.Other steps and parameter are identical with embodiment 12 to 14.
Embodiment 16:The difference of present embodiment and embodiment 12 to 14 is:First time scanning is carried out to the pitch on parallel-plate with 4~6Hz frequency in step one.Other steps and parameter are identical with embodiment 12 to 14.
Embodiment 17:The difference of present embodiment and embodiment 12 to 14 is:First time scanning is carried out to the pitch on parallel-plate with 5Hz frequency in step one.Other steps and parameter are identical with embodiment 12 to 14.
Embodiment 18:The difference of present embodiment and embodiment 12 to 17 is:Performed a scan again with 2~8Hz frequency on asphalt at interval of n DEG C in step one, wherein 2≤n≤8.Other steps and parameter are identical with embodiment 12 to 17.
Embodiment 19:The difference of present embodiment and embodiment 12 to 17 is:Performed a scan again with 5Hz frequency on asphalt at interval of 5 DEG C in step one.Other steps and parameter are identical with embodiment one to six.
Embodiment 20:The difference of present embodiment and embodiment 12 to 19 is:Until the temperature of pitch reaches 4~6 DEG C of progress last time frequency scannings in step one.Other steps and parameter are identical with embodiment 12 to 19.
Embodiment 21:The difference of present embodiment and embodiment 12 to 19 is:Until the temperature of pitch reaches 5 DEG C of progress last time frequency scannings in step one.Other steps and parameter are identical with embodiment 12 to 19.
Claims (9)
1. detect the method for state of aggregation conversion temperature after asphalt with ultraviolet aging, it is characterised in that the method for state of aggregation conversion temperature is followed the steps below after detection asphalt with ultraviolet aging:One, pitch to be detected is heated into rubber cement shape to be placed on parallel-plate, thickness of the pitch on parallel-plate is 1000 μm~2000 μm, it is that initial temperature is scanned with 0.1~10Hz frequency to the pitch on parallel-plate with 5 DEG C, performed a scan again with 0.1~10Hz frequency on asphalt at interval of n DEG C, wherein 0 < n≤10, until the temperature of pitch reaches 63~67 DEG C of progress last time frequency scannings, the angular frequency and the corresponding relation of composite modulus obtained according to scanning draws composite modulus curve under different temperatures, composite modulus curve is wherein drawn using angular frequency as abscissa, using composite modulus as ordinate;2nd, the different composite modulus curve for drawing step one carries out time temperature equivalence conversion, and reference temperature is set as 25 DEG C, obtains the frequency scanning principal curve at 25 DEG C;3rd, the frequency of time temperature equivalence failure, the temperature that the temperature corresponding to the frequency of time temperature equivalence failure converts for state of aggregation after asphalt with ultraviolet aging are found out from the frequency scanning principal curve at 25 DEG C that step 2 is obtained;Detection pitch is heated to rubber cement shape wherein in step one, heating-up temperature is no more than 135 DEG C, and the heat time is no more than 75min;Dynamic shear rheometer is used to the frequency scanning of pitch in step one.
2. the method for state of aggregation conversion temperature after detection asphalt with ultraviolet aging according to claim 1, it is characterised in that first time scanning is carried out to the pitch on parallel-plate with 2~8Hz frequency in step one.
3. the method for state of aggregation conversion temperature after detection asphalt with ultraviolet aging according to claim 1 or 2, it is characterised in that first time scanning is carried out to the pitch on parallel-plate with 4~6Hz frequency in step one.
4. the method for state of aggregation conversion temperature after detection asphalt with ultraviolet aging according to claim 1 or 2, it is characterised in that performed a scan again with 2~8Hz frequency on asphalt at interval of n DEG C in step one, wherein 2≤n≤8.
5. a kind of method for detecting state of aggregation conversion temperature after asphalt with ultraviolet aging according to claim 3, it is characterised in that performed a scan again with 2~8Hz frequency on asphalt at interval of n DEG C in step one, wherein 2≤n≤8.
6. the method for state of aggregation conversion temperature after a kind of detection asphalt with ultraviolet aging according to claim 1,2 or 5, it is characterised in that performed a scan again with 5Hz frequency on asphalt at interval of 5 DEG C.
7. detect the method for state of aggregation conversion temperature after asphalt with ultraviolet aging, it is characterised in that the method for state of aggregation conversion temperature is followed the steps below after detection asphalt with ultraviolet aging:One, pitch to be detected is heated into rubber cement shape to be placed on parallel-plate, thickness of the pitch on parallel-plate is 1000 μm~2000 μm, it is that initial temperature is scanned with 0.1~10Hz frequency to the pitch on parallel-plate with 65 DEG C, performed a scan again with 0.1~10Hz frequency on asphalt at interval of n DEG C, wherein 0 < n≤10, until the temperature of pitch reaches 3~7 DEG C of progress last time frequency scannings, the angular frequency and the corresponding relation of composite modulus obtained according to scanning draws composite modulus curve under different temperatures, composite modulus curve is wherein drawn using angular frequency as abscissa, using composite modulus as ordinate;2nd, the different composite modulus curve for drawing step one carries out time temperature equivalence conversion, and reference temperature is set as 25 DEG C, obtains the frequency scanning principal curve at 25 DEG C;3rd, the frequency of time temperature equivalence failure, the temperature that the temperature corresponding to the frequency of time temperature equivalence failure converts for state of aggregation after asphalt with ultraviolet aging are found out from the frequency scanning principal curve at 25 DEG C that step 2 is obtained;Detection pitch is heated to rubber cement shape wherein in step one, heating-up temperature is no more than 135 DEG C, and the heat time is no more than 75min;Dynamic shear rheometer is used to the frequency scanning of pitch in step one.
8. a kind of method for detecting state of aggregation conversion temperature after asphalt with ultraviolet aging according to claim 7, it is characterised in that first time scanning is carried out to the pitch on parallel-plate with 4~6Hz frequency in step one.
9. a kind of method for detecting state of aggregation conversion temperature after asphalt with ultraviolet aging according to claim 7, it is characterised in that until the temperature of pitch reaches 4~6 DEG C of progress last time frequency scannings in step one.
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