CN106290066B - A kind of determination method of asphalt mastic filler critical volume fraction - Google Patents
A kind of determination method of asphalt mastic filler critical volume fraction Download PDFInfo
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- CN106290066B CN106290066B CN201610634655.3A CN201610634655A CN106290066B CN 106290066 B CN106290066 B CN 106290066B CN 201610634655 A CN201610634655 A CN 201610634655A CN 106290066 B CN106290066 B CN 106290066B
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N11/00—Investigating flow properties of materials, e.g. viscosity, plasticity; Analysing materials by determining flow properties
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- G—PHYSICS
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
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- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/38—Diluting, dispersing or mixing samples
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
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Abstract
The present invention relates to a kind of determination methods of asphalt mastic filler critical volume fraction, it prepares Series of Asphalt rubber cement sample by (1), and (2) distinguish the complex modulus G of each asphalt mastic sample obtained by determination step (1) with dynamic shear rheometer*, (3) are using Origin software according to the packing volume mark of Series of Asphalt rubber cement sample and corresponding complex modulus G*It is fitted packing volume mark and complex modulus G*Between nonlinear function, to can determine the filler critical volume fraction Φ of the asphalt masticm；Pass through the determination of filler critical volume fraction, packing volume mark can be specified in the range of a certain determination, the enhancing of asphalt mastic complex modulus is that asphalt/filler reciprocation plays a leading role or filler particles interaction plays a leading role, positive effect is played to the research of asphalt mastic performance, simultaneously, the calculation formula of filler critical volume fraction of the invention is simple, and fit procedure is consistent with truth, as a result accurate reliable.
Description
Technical field
The invention belongs to the performance study technical fields of asphalt mastic, and in particular to a kind of asphalt mastic filler critical size
The determination method of score.
Background technique
According to composite theory, asphalt mastic can be considered a kind of particulate reinforced composite, including pitch (matrix phase),
Filler particles (reinforced phase) and the interface phase formed by reciprocation.Existing research shows that asphalt mastic compound system
Interior effect is complex, interact there are asphalt/filler reciprocation and filler particles etc., and all have with packing volume mark
It closes.The present invention proposes the determination method of filler critical volume fraction and filler critical volume fraction, evaluates packing volume mark
With the relationship between filler particles interaction, asphalt/filler reciprocation, when to evaluate asphalt/filler reciprocation, filler
Determining for volume fraction range provides theoretical foundation.
At present when analyzing asphalt/filler reciprocation, the selection for packing volume mark is empirical, no spy
Fixed theoretical foundation.Carried out under packing volume mark and the not yet specific situation of the interactive relationship of asphalt/filler
Interaction capacity evaluation, accuracy and reliability need further to be verified.Current research is only very wide in range to be shown to drip
The particle enhancing of green rubber cement be the reciprocation joint effect between Interaction between particles and pitch and filler by filler as a result,
But there is no packing volume mark is specifically distinguished in the range of a certain determination, the enhancing of asphalt mastic complex modulus is drip
Blueness/filler reciprocation plays a leading role or filler particles enhancement effect plays a leading role.
Summary of the invention
For deficiency existing for existing method, the invention proposes this concepts of filler critical volume fraction, and provide
The determination method of asphalt mastic filler critical volume fraction, this method can analyze out packing volume mark and asphalt/filler is handed over
Relationship between interaction and filler particles interaction, in packing volume mark and asphalt/filler reciprocation and particle
In the specific situation of relationship between interaction, carries out the interactive evaluation of asphalt/filler, can be further improved evaluation
Accuracy and reliability.
The technical scheme adopted by the invention is that being realized by following steps:
(1) surface of aggregate impurity is removed, milling makes uniform powdered granule, at 0.075mm square hole screen sieving
Reason obtains filler, dries in the baking oven that temperature is 100~130 DEG C, later will in the baking oven that temperature is 110 DEG C~140 DEG C
Pitch is heated to flow regime, with packing volume mark be respectively 0 by the pitch of heating and filler, 15%, 25%, 40%,
50%, 65% ratio is mixed to get campaign, and each sample is put into baking oven, supports at a temperature of 110 DEG C~140 DEG C
Life continuously stirs, so that pitch and filler particles sufficiently react, synthetic time series asphalt mastic sample；
It (2) is 0.5% in strain level with dynamic shear rheometer, loading frequency 10Hz, the item that 70 DEG C of test temperature
The complex modulus G of each asphalt mastic sample obtained by determination step (1) is distinguished under part*, test period 120s；
(3) using Origin software according to the packing volume mark of Series of Asphalt rubber cement sample and corresponding complex modulus G*
It is fitted packing volume mark and complex modulus G*Between nonlinear function, be expressed as follows:
In formula: G*- asphalt mastic complex modulus/KPa；
Φ-packing volume mark/%；
Φm- filler critical volume fraction/%；
β-asphalt/filler interaction capacity related coefficient, is the fitting parameter of Origin software；
It can determine the filler critical volume fraction Φ of the asphalt mastic according to the deformation of formula (1)m。
The determination method of asphalt mastic filler critical volume fraction of the invention, propose filler critical volume fraction this
Concept and the determination method for proposing filler critical volume fraction, using Origin software to the different fillers of asphalt mastic sample
Volume fraction and corresponding complex modulus are fitted analysis, so that it is determined that packing volume mark, filler critical volume fraction out
Relationship between complex modulus, and then the filler critical volume fraction of asphalt mastic can be calculated, pass through the critical body of filler
The determination of fraction, can specify packing volume mark in the range of a certain determination, and the enhancing of asphalt mastic complex modulus is
Asphalt/filler reciprocation plays a leading role or filler particles interaction plays a leading role, and grinds to asphalt mastic performance
Study carefully and plays positive effect, meanwhile, the calculation formula of filler critical volume fraction of the invention is simple, fit procedure and truth
It is consistent, it is as a result accurate reliable.
Detailed description of the invention
Fig. 1 is filler critical volume fraction schematic diagram.
Fig. 2 is 70# matrix pitch rubber cement complex modulus G* with packing volume mark change curve.
Fig. 3 is 90# matrix pitch rubber cement complex modulus G* with packing volume mark change curve.
Specific embodiment
Technical solution of the present invention is further described now in conjunction with drawings and examples.
Asphalt mastic complex modulus is respectively defined as " dilution rank with two stages that packing volume mark changes by the present invention
Section " and " aggregation stage ", and the corresponding packing volume mark of two stage turning point is defined as filler critical volume fraction
Φm, as shown in Figure 1.
Smaller in the volume fraction of dilution stage, filler, the content of pitch is enough compared with filler and can be by filler with list
The form of a particle is wrapped up, and forms " structure pitch " in filler surface, " structure pitch " viscosity is larger；Remaining pitch is by filler
Particle spreads out with formation " free pitch ", apart from each other between particle and do not contact with each other, therefore filler particles phase interaction
With not yet occurring.Therefore in the stage asphalt mastic compound system modulus enhancing be occupied by asphalt/filler reciprocation it is leading.With
Increasing for filer content, " free pitch " be gradually converted into " structure pitch ", when packing volume mark reaches critical size point
When number, " free pitch " is completely reformed into " structure pitch " just, and filler is wrapped up still in the form of individual particle, but filler particles
Between be in contact with each other, Interaction between particles start to occur.
It has been more than the aggregation stage then to be entered, in the rank after critical volume fraction with further increasing for filer content
In section, since filler is excessive, pitch is not enough to individually wrap up filler particles, if again by pitch after there is dry filler particles reunion
The phenomenon that package, leads to filler particles Interaction enhanced, and the influence to the enhancing of asphalt mastic compound system modulus is much larger than
Asphalt/filler reciprocation, thus it is interior at this stage, and filler particles interaction plays leading work to the enhancing of asphalt mastic modulus
With.Thus we are it can be found that in different packing volume mark sections, the enhancing of asphalt mastic modulus by different effects Lai
It is leading, as long as filler critical volume fraction has been determined, so that it may clearly only exist filling body when asphalt/filler reciprocation
Fraction range.
Determine that the specific method of filler critical volume fraction is realized by following steps:
(1) preparation process of asphalt mastic
1. making filler
Surface of aggregate impurity is removed, milling makes to gather materials as uniform powdered granule, at the square hole screen sieving of 0.075mm
Reason obtains filler, dries in the baking oven that temperature is 100~130 DEG C.
2. pitch heats
Pitch is heated to flow regime in the baking oven that temperature is 110 DEG C~140 DEG C, so that filler can be fully mixed.
3. mixing
By the pitch of heating and filler particles respectively with packing volume mark for 0,15%, 25%, 40%, 50%, 65%
Ratio mixing, obtain Series of Asphalt and filler mixture, be respectively put into baking oven, at a temperature of 110 DEG C~140 DEG C support
Life continuously stirs, so as to sufficiently react between pitch and filler particles, synthetic time series asphalt mastic sample.
(2) measurement of the asphalt mastic rheological equationm of state
It is measured respectively using Series of Asphalt rubber cement sample of the dynamic shear rheometer to step (1):
1. the working condition of dynamic shear rheometer is tuned into oscillation mode, use diameter for the parallel plate fixtures of 25mm,
Using strain controlling, strain level 0.5%, loading frequency 10Hz, 70 DEG C of test temperature.
2. device returns to zero
3. adjusting upper flat plate, make 1050 ± 10 μm of gap between upper flat plate and lower plate, scrapes off plate up and down with hot knife
Between the rubber cement that is extruded, the constant temperature health 15min at 70 DEG C presses the rheological equationm of state of start key acquisition rubber cement, and test period is
120s takes a value at interval of 10s, measures the complex modulus G of Series of Asphalt rubber cement sample*。
(3) the determination method of filler critical volume fraction
Using Origin software according to the packing volume mark of Series of Asphalt rubber cement sample and corresponding complex modulus G*It is quasi-
Close packing volume mark and complex modulus G*Between nonlinear function, expression formula is as follows:
In formula: G*- asphalt mastic complex modulus/KPa；
Φ-packing volume mark/%；Φm- filler critical volume fraction/%；
β-asphalt/filler interaction capacity related coefficient, is the fitting parameter of Origin software；
It can determine the filler critical volume fraction Φ for locating the Series of Asphalt rubber cement sample according to the deformation of formula (1)m。
With the aforedescribed process to two kinds of matrix pitches of 70#, 90# and three kinds of limestone, diabase and granite fillers
Be prepared into 6 kinds of asphalt mastic samples respectively, it be successively taken as according to packing volume mark: 0,15%, 25%, 40%, 50%,
65%, determine the filler critical volume fraction of each asphalt mastic sample, the results are shown in Table 1 for correlation analysis.
1 filler critical volume fraction of table
No matter which kind of matrix pitch as can be seen from Table 1, the filler critical volume fraction Φ of asphalt masticmSubstantially divide
It is distributed in 30% or so.
In order to analyze the relationship between packing volume mark and asphalt/filler reciprocation and filler particles enhancement effect,
The present invention prepares asphalt adhesive using two kinds of matrix pitches of 70#, 90# and three kinds of limestone, diabase and granite fillers respectively
Starch sample.Packing volume mark is successively taken as: 0,15%, 25%, 40%, 50%, 65%.Using dynamic shear rheometer to base
Matter pitch and rubber cement sample carry out rheological test (being specifically shown in second part test process), obtain the complex modulus of asphalt mastic with
The change curve of packing volume mark, as shown in Figures 2 and 3.
It can be observed how from Fig. 2 and 3, the complex modulus G of asphalt mastic*As the increase of packing volume mark substantially divides
For two stages.When packing volume mark is smaller, the complex modulus G of asphalt mastic*As the increase of packing volume mark is in
The trend of linear increase, complex modulus are increased more slowly；When packing volume mark is more than 30% or so, asphalt mastic
The trend that complex modulus is exponentially increased with the increase of packing volume mark, modulus increase more rapid, this and the meter in table 1
It calculates result more to coincide, also illustrates the filler critical volume fraction Φ that function of the invention obtainsmReliability with higher.
Claims (1)
1. a kind of determination method of asphalt mastic filler critical volume fraction, it is characterised in that realized by following steps:
(1) surface of aggregate impurity is removed, milling makes uniform powdered granule, handled with 0.075mm square hole screen sieving
It to filler, is dried in the baking oven that temperature is 100~130 DEG C, later by pitch in the baking oven that temperature is 110 DEG C~140 DEG C
Be heated to flow regime, by the pitch of heating and filler with packing volume mark be respectively 0,15%, 25%, 40%, 50%,
65% ratio is mixed to get Series of Asphalt and filler mixture sample, and each sample is put into baking oven, 110 DEG C~140
Health at a temperature of DEG C continuously stirs, so that pitch and filler particles sufficiently react, synthetic time series asphalt mastic sample；
It (2) is 0.5%, loading frequency 10Hz in strain level with dynamic shear rheometer, under conditions of 70 DEG C of test temperature
The complex modulus G of each asphalt mastic sample obtained by determination step (1) respectively*, test period 120s；
(3) using Origin software according to the packing volume mark of Series of Asphalt rubber cement sample and corresponding complex modulus G*Fitting
Packing volume mark and complex modulus G*Between nonlinear function, be expressed as follows:
In formula: G*Asphalt mastic complex modulus/KPa；
Φ-packing volume mark/%；
ΦmFiller critical volume fraction/%；
β-asphalt/filler interaction capacity related coefficient, is the fitting parameter of Origin software；
It can determine the filler critical volume fraction Φ of the asphalt mastic according to the deformation of formula (1)m。
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| CN107817174B (en) * | 2017-11-20 | 2019-12-03 | 哈尔滨工业大学 | A kind of interactive body asphalt phase rubber cement dynamic shearing complex modulus test method of consideration substrate-rubber cement |
| CN113607608B (en) * | 2021-09-02 | 2023-05-12 | 交通运输部公路科学研究所 | Method for evaluating interfacial interaction capability of cement emulsified asphalt cement and old asphalt |
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