CN110082256A - A method of distinguishing high-modulus agent and anti-rut agent - Google Patents

A method of distinguishing high-modulus agent and anti-rut agent Download PDF

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Publication number
CN110082256A
CN110082256A CN201910415064.0A CN201910415064A CN110082256A CN 110082256 A CN110082256 A CN 110082256A CN 201910415064 A CN201910415064 A CN 201910415064A CN 110082256 A CN110082256 A CN 110082256A
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sample
agent
aging
tested
modulus
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CN201910415064.0A
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CN110082256B (en
Inventor
周合宽
王国晓
严二虎
李明杰
李�昊
郝玮
谢琳
李青
魏东
周震宇
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Henan No2 Highway Engineering Co Ltd
Research Institute of Highway Ministry of Transport
Henan Highway Engineering Group Co Ltd
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Henan No2 Highway Engineering Co Ltd
Research Institute of Highway Ministry of Transport
Henan Highway Engineering Group Co Ltd
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    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00Sampling; Preparing specimens for investigation
    • G01N1/28Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
    • G01N1/286Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q involving mechanical work, e.g. chopping, disintegrating, compacting, homogenising
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00Sampling; Preparing specimens for investigation
    • G01N1/28Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
    • G01N1/36Embedding or analogous mounting of samples
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00Sampling; Preparing specimens for investigation
    • G01N1/28Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
    • G01N1/44Sample treatment involving radiation, e.g. heat
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N11/00Investigating flow properties of materials, e.g. viscosity, plasticity; Analysing materials by determining flow properties
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N11/00Investigating flow properties of materials, e.g. viscosity, plasticity; Analysing materials by determining flow properties
    • G01N11/02Investigating flow properties of materials, e.g. viscosity, plasticity; Analysing materials by determining flow properties by measuring flow of the material
    • G01N11/04Investigating flow properties of materials, e.g. viscosity, plasticity; Analysing materials by determining flow properties by measuring flow of the material through a restricted passage, e.g. tube, aperture
    • G01N11/06Investigating flow properties of materials, e.g. viscosity, plasticity; Analysing materials by determining flow properties by measuring flow of the material through a restricted passage, e.g. tube, aperture by timing the outflow of a known quantity
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N11/00Investigating flow properties of materials, e.g. viscosity, plasticity; Analysing materials by determining flow properties
    • G01N11/10Investigating flow properties of materials, e.g. viscosity, plasticity; Analysing materials by determining flow properties by moving a body within the material
    • G01N11/12Investigating flow properties of materials, e.g. viscosity, plasticity; Analysing materials by determining flow properties by moving a body within the material by measuring rising or falling speed of the body; by measuring penetration of wedged gauges
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N3/00Investigating strength properties of solid materials by application of mechanical stress
    • G01N3/28Investigating ductility, e.g. suitability of sheet metal for deep-drawing or spinning

Abstract

The present invention provides a kind of method for distinguishing high-modulus agent and anti-rut agent.The described method includes: taking sample to be tested, under 190 DEG C, the load of counterweight 2.16kg, the melt mass flow rate of sample to be tested is measured;If melt mass flow rate is less than 2g/10min, determine sample to be tested for anti-rut agent;If melt mass flow rate >=2g/10min, matrix pitch sample is taken, preparation adds the asphalt binder of sample to be tested;25 DEG C at a temperature of, measure asphalt binder aging before and aging after ductility and/or aging after needle penetration;If the needle penetration after asphalt binder aging is greater than 100;And/or the ductility after asphalt binder aging is greater than the ductility before aging, then determines sample to be tested for anti-rut agent;If needle penetration≤100 after asphalt binder aging;Also, the ductility before ductility≤aging after asphalt binder aging then determines sample to be tested for high-modulus agent.This method is simple and easy, effectively can quickly distinguish high-modulus agent and anti-rut agent.

Description

A method of distinguishing high-modulus agent and anti-rut agent
Technical field
The present invention relates to a kind of methods for distinguishing high-modulus agent and anti-rut agent, belong to pavement material performance test field.
Background technique
High Modulus Asphalt Mixture is suitable for high temperature, heavy traffic, heavy duty, overload high-grade highway, and asphalt mixture design is simultaneous It cares for binder high-modulus, anti-fatigue performance, resistant to high temperatures and water resistant and damages performance, meet Long Life Asphalt Pavement requirement, technology exists It has largely been applied successfully both at home and abroad.
Existing research is thought at present, and realizing High Modulus Asphalt Mixture, there are three types of technological approaches: (1) using hard grades of bitumen (the low grade pitch of 25 DEG C of needle penetration < 25);(2) high-modulus modifier is added;(3) composite modified asphalt, such as natural drip are used Green modified pitch.According to domestic existing petrochemical iy produced technological level and market situation at present, low grade pitch aspect, due to current Demand is limited, domestic there is no being mass produced, and is only in the tentative production of small range and use;Exactly in this context, Occur various high-modulus agent products in the popularization of high-modulus asphalt concrete, including domestic independent research product With some imported products.
It is known as height from the additive that asphalt stiffness modulus and anti-fatigue performance broadly, can be significantly improved Modulus agent, also known as high-modulus modifier, high-modulus additive etc.;And all related asphalt modifications applied for the purpose of Rut resistance Agent all can be described as anti-rut agent, also known as tracking-resisting modifier, anti-rutting additive etc..And high-modulus agent and anti-rut agent are pitch In two kinds of common additives, but because the two appearance is similar, some manufacturers directly adopt anti-rut agent substitution high-modulus agent It uses, it is expected to reach the requirement of high-modulus asphalt concrete.And anti-rut agent is substantially replaced into high-modulus agent, at all can not Reach the technical requirements of High Modulus Asphalt Mixture.
With the large scale application of high-modulus asphalt concrete, the demand of high-modulus agent is very big, seeks a kind of Zhen The efficiency test method of other high-modulus agent and anti-rut agent, it is of great advantage for the development of high-modulus concrete technology.Existing In technology, two kinds of additives are screened, need to carry out chemical composition analysis, including vicat softening temperature, shrinking percentage etc., process is more It is cumbersome, it is high for professional requirement, generally it is not easy to grasp.
Therefore, a kind of method for quickly distinguishing high-modulus agent and anti-rut agent is studied, technical problem urgently to be resolved is become.
Summary of the invention
Problems to be solved by the invention
In view of the technical problems existing in the prior art, such as: it distinguishes high-modulus agent and anti-rut agent needs to carry out chemistry Constituent analysis and multinomial performance measurement, such as: including vicat softening temperature, shrinking percentage etc.;Detection process is relatively complicated, for special Industry requires height, is generally not easy grasp etc..The present invention provides a kind of methods for distinguishing high-modulus agent and anti-rut agent.The party Method is simple and easy, effectively can quickly distinguish high-modulus agent and anti-rut agent, and highly reliable, testing result is accurate.
The solution to the problem
The present invention provides a kind of method for distinguishing high-modulus agent and anti-rut agent comprising:
Sample to be tested is taken, under 190 DEG C, the load of counterweight 2.16kg, measures the melt mass flow of the sample to be tested Rate;
If the melt mass flow rate is less than 2g/10min, determine the sample to be tested for anti-rut agent;
If the melt mass flow rate is more than or equal to 2g/10min, matrix pitch sample is taken, is prepared described in adding The asphalt binder of sample to be tested;
25 DEG C at a temperature of, needle after measuring the ductility and/or aging before the asphalt binder aging and after aging In-degree;
If the needle penetration after the asphalt binder aging is greater than 100;And/or prolonging after the asphalt binder aging Degree is greater than the ductility before aging, then determines the sample to be tested for anti-rut agent;
If the needle penetration after the asphalt binder aging is less than or equal to 100;Also, after the asphalt binder aging Ductility is less than or equal to the ductility before aging, then determines the sample to be tested for high-modulus agent.
The method according to the present invention for distinguishing high-modulus agent and anti-rut agent, wherein to test sample described in the measurement Before the melt mass flow rate of product, further include the steps that the apparent viscosity for measuring the sample to be tested.
The method according to the present invention for distinguishing high-modulus agent and anti-rut agent, wherein with the matrix pitch sample Gross mass meter, the additional amount of the sample to be tested is 5%~9%.
The method according to the present invention for distinguishing high-modulus agent and anti-rut agent, wherein the system of the asphalt binder Preparation Method the following steps are included:
Step 1) takes matrix pitch sample and heats, the sample to be tested is then added, obtains premix;
Step 2) obtains asphalt binder to moulding after premix progress shear treatment.
The method according to the present invention for distinguishing high-modulus agent and anti-rut agent, wherein in the step 1), heating Temperature is 160 DEG C~180 DEG C.
The method according to the present invention for distinguishing high-modulus agent and anti-rut agent, wherein described to cut in the step 2) Cutting processing includes:
Pre- shearing step tentatively shears the premix under the revolving speed of 4000r/min~5000r/min Processing, obtains pre- cutting object;
Development processing is sheared, under the revolving speed of 800r/min~1500r/min, the pre- cutting object is carried out at shearing Reason obtains shearing product.
The method according to the present invention for distinguishing high-modulus agent and anti-rut agent, wherein the temperature of the pre- shearing step Degree is 160 DEG C~180 DEG C;The time of the pre- shear treatment is 30min or more, preferably 30min~120min.
The method according to the present invention for distinguishing high-modulus agent and anti-rut agent, wherein the shearing development processing Temperature is 160 DEG C~180 DEG C;The time of the shearing development processing is 0.5h~1.0h.
The method according to the present invention for distinguishing high-modulus agent and anti-rut agent, wherein the step of aging includes: Rotating thin film heat run is carried out to the asphalt binder, obtains the asphalt binder of aging.
The method according to the present invention for distinguishing high-modulus agent and anti-rut agent, wherein the rotating thin film heating examination In testing, the temperature of the heating is 160 DEG C~180 DEG C, and the time of the heating is to be no less than 75min, preferably 75min~ 85min。
The effect of invention
The method of differentiation high-modulus agent and anti-rut agent of the invention is simple and easy, effectively can quickly distinguish high-modulus agent And anti-rut agent, and it is highly reliable, testing result is accurate.
Further, the method for differentiation high-modulus agent of the invention and anti-rut agent can not increase additional detection and set It is standby, and used raw material is easily obtained, sample preparation is easy, and can reduce experimentation cost.
Specific embodiment
It will be detailed below various exemplary embodiments, feature and aspect of the invention.Dedicated word " example herein Property " mean " being used as example, embodiment or illustrative ".Here as any embodiment illustrated by " exemplary " should not necessarily be construed as Preferred or advantageous over other embodiments.
In addition, in order to better illustrate the present invention, numerous details is given in specific embodiment below. It will be appreciated by those skilled in the art that without certain details, the present invention equally be can be implemented.In other example, Method well known to those skilled in the art, means, equipment and step are not described in detail, in order to highlight master of the invention Purport.
Such as without Special Statement, unit used in the present invention is SI units, and the number occurred in the present invention Value, numberical range should all be interpreted as containing the inevitable Systematic Errors of institute in industrial production.
The Practical Project feature of additive is considered, it was found by the inventors of the present invention that high-modulus agent can take into account pitch mixing The high temperature performance of material, while having the characteristics that processing characteristics are excellent, and anti-rut agent improves obviously high-temperature behavior, and it is right It is then lost in low temperature and medium temperature performance.So using this feature, it can be by using the melt matter for examining sample to be tested The method that needle penetration and/or stretch indexe of the flow rate before and after the specific aging of asphalt binder combine is measured to screen Anti-rut agent and high-modulus agent.Specifically, carrying out melt index test to sample to be tested, a part of anti-vehicle can be filtered out and removed Agent, so can again using before and after the needle penetration and/or aging after aging stretch indexe and apparent viscosity index evaluate respectively The cryogenic property and construction property of modified addition, and then distinguish anti-rut agent and high-modulus agent.Specifically,
The present invention provides a kind of method for distinguishing high-modulus agent and anti-rut agent.The described method includes:
Sample to be tested is taken, under 190 DEG C, the load of counterweight 2.16kg, measures the melt mass flow of the sample to be tested Rate;
If the melt mass flow rate be less than 2g/10min, determine the sample to be tested for anti-rut agent, rather than High-modulus agent.
Further, in order to further discriminate between high-modulus agent and anti-rut agent, in the molten of the measurement sample to be tested After weight flow rate, to the high-modulus agent not differentiated between out and anti-rut agent, if the melt mass flow rate is greater than Equal to 2g/10min, then the method also includes following steps:
Matrix pitch sample is taken, preparation adds the asphalt binder of the sample to be tested;
25 DEG C at a temperature of, needle after measuring the ductility and/or aging before the asphalt binder aging and after aging In-degree;
If the needle penetration after the asphalt binder aging is greater than 100;And/or prolonging after the asphalt binder aging Degree is greater than the ductility before aging, then determines the sample to be tested for anti-rut agent;
If the needle penetration after the asphalt binder aging is less than or equal to 100;Also, after the asphalt binder aging Ductility is less than or equal to the ductility before aging, then determines the sample to be tested for high-modulus agent.
The method of differentiation high-modulus agent and anti-rut agent of the invention is simple and easy, effectively can quickly distinguish high-modulus agent And anti-rut agent, and it is highly reliable, testing result is accurate.
Further, the method for differentiation high-modulus agent of the invention and anti-rut agent can not increase additional detection and set It is standby, and used raw material is easily obtained, sample preparation is easy, and can reduce experimentation cost.
Melt mass flow rate
Melt mass flow rate (Melt mass-flow rate, abbreviation MFR, also known as melt flow rate (MFR)), also refers to molten Melt index (melt index, MI), is in standardization fusion index instrument under certain temperature and pressure, resin melt passes through The melt grams that standard capillary flows out in (general 10min) within a certain period of time, unit g/10min.Invention of the invention People's discovery, can tentatively distinguish anti-rut agent and non-high-modulus agent using melt mass flow rate.
The melt mass flow rate of the sample to be tested can be according to GB/T 3682.1-2018 " thermoplastic melt Mass flow rate and melt volume-flow rate measurement " in thermoplastic melt flow rate (MFR) mass measuring method into Row.Whether the present invention is greater than by the melt mass flow rate of the measurement sample to be tested according to melt mass flow rate 2g/10min can distinguish the anti-rut agent and high-modulus agent of a part.That is: if the described melt mass flow rate is less than 2g/10min, then determine the sample to be tested for anti-rut agent, rather than high-modulus agent.If the melt mass flow rate is greater than Equal to 2g/10min, then need to further determine.
Matrix pitch sample
In the present invention, when the melt mass flow rate is greater than 2g/10min, need to prepare asphalt binder progress It is further to determine.When preparing asphalt binder, suitable matrix pitch sample can be selected to be prepared.The present invention is to base Matter asphalt sample is not particularly limited, as long as can be realized the solution of the present invention.
Preferably, the matrix pitch sample can be bi tumenf orr oad.Further, the bi tumenf orr oad Combination including one or more of low grade bi tumenf orr oad, 70#~200# bi tumenf orr oad etc..
Further, present invention preferably uses low grade bi tumenf orr oad, i.e., 50# bi tumenf orr oad and it is less than 50# The bi tumenf orr oad of bi tumenf orr oad, such as 25# bi tumenf orr oad, 35# bi tumenf orr oad and 50# road petroleum Pitch etc..
Asphalt binder
The asphalt binder of the invention refers to the asphalt binder for adding sample to be tested.In order to more accurately distinguish Anti-rut agent and high-modulus agent, in terms of the gross mass of the matrix pitch sample, the additional amount of the sample to be tested is 5%~ 9%, such as: the additional amount of the sample to be tested can be 5.5%, 6%, 6.5%, 7%, 7.5%, 8%, 8.5% etc..At this In invention, when the additional amount of sample to be tested is between 5%~9%, needle penetration, the ductility of asphalt binder are excellent, measurement As a result stable.The additional amount of sample to be tested is very few, and the modified effect of sample to be tested is unobvious;Additional amount is excessive, the storage of pitch Bad stability is easy to produce isolation, and increases the viscosity of pitch, is unfavorable for pumping.Therefore, sample to be tested additional amount is excessive Or very few all it is unsuitable for distinguishing anti-rut agent and high-modulus agent.
Further, the asphalt binder of the invention preparation method the following steps are included:
Step 1) takes matrix pitch sample and heats, the sample to be tested is then added, obtains premix;
Step 2) obtains asphalt binder to moulding after premix progress shear treatment.
Preferably, in the step 1), in order to be dissolved in sample to be tested preferably in matrix pitch sample, the temperature of heating Degree can be 160 DEG C~180 DEG C, for example, 165 DEG C, 170 DEG C, 175 DEG C etc..
In the step 2), it is had excellent performance stable asphalt binder in order to be prepared, the shear treatment includes: pre- Shear step and shearing development step.Specifically:
The pre- shearing step includes: to carry out under the revolving speed of 4000r/min~5000r/min to the premix Preliminary shear treatment obtains pre- cutting object;By preliminary shear treatment, matrix pitch sample and sample to be tested can be carried out just Step premix.
In the present invention, when revolving speed is 4000r/min~5000r/min, on the one hand, sample to be tested and matrix pitch sample Product can be sufficiently mixed uniformly, and sample to be tested will not reunite, and can form stable system;On the other hand, sample to be tested is in base Will not be swollen in matter asphalt sample, can in pitch light components and waxy component combine closely, to test sample The contraction for reaching absorption swelling on the interface of product and matrix pitch sample balances, and forms relatively stable boundary layer, makes to test sample The compatibility of product and matrix pitch sample is improved, so that the performance of pitch be made to be improved.Therefore, when revolving speed is in 4000r/ When min~5000r/min, such as: 4200r/min, 4500r/min, 4800r/min etc. can be improved the needle of asphalt binder In-degree and ductility, to keep measurement result more accurate.
Preferably, the temperature of the pre- shearing step is 160 DEG C~180 DEG C;When the temperature of pre- shearing step is at 160 DEG C Between~180 DEG C, such as: at 165 DEG C, 170 DEG C, 175 DEG C, it can be improved the ductility of asphalt binder, and needle penetration also phase To stabilization.The time of the pre- shear treatment is 30min or more, preferably 30min~120min.In general, with the time Extension, needle penetration, the ductility of asphalt binder have different degrees of raising, to keep measurement result more accurate and reliable.
The shearing development processing includes, and under the revolving speed of 800r/min~1500r/min, carries out to the pre- cutting object Shear treatment obtains shearing product;Shearing development processing through the invention, can be such that sample to be tested stablizes in matrix pitch Dispersion, developmental state are good, it is however generally that, degree of scatter of the sample to be tested in pitch is high, and the performance of asphalt binder is better, Measurement result is more accurate and reliable.Revolving speed when shearing development processing can be 1000r/min, 1200r/min, 1400r/min Deng.
Preferably, the temperature of shearing development processing is 160 DEG C~180 DEG C, and such as: 165 DEG C, 170 DEG C, 175 DEG C;It is described The time of shearing development processing is 0.5h~1.0h, such as: 0.6h, 0.7h, 0.8h, 0.9h etc..Shearing development processing is with sample Uniformly, subject to without obvious sample to be tested particle, specifically sample can be dipped using glass bar, scrapes and smears on a clean test paper, Estimate its mixing state.
Specifically, asphalt binder of the invention preparation method the following steps are included:
(1) it takes matrix pitch sample specimens to be put in sample holder ware, is heated to 160 DEG C~180 DEG C in an oven.
(2) in terms of the gross mass of matrix pitch sample, 5%~9% sample to be tested is taken, is slowly added to the base of heating by several times In matter asphalt sample, premix is obtained;
(3) shearing is carried out not less than 30min to premix by 4000r/min~5000r/min rate using cutter ± 1min, preferably 30min~120min, sample of being subject to uniformly, without obvious sample to be tested particle, temperature is protected in shear history Hold 160 DEG C~180 DEG C.
(4) in the environment of 160 DEG C~180 DEG C, under the revolving speed of 800r/min~1500r/min, sealing is sheared at a slow speed Develop 0.5h~1.0h.
(5) after the completion of shearing development should moulding immediately, obtain asphalt binder, it is spare.
The aging of asphalt binder
The present invention can be by carrying out rotating thin film heat run to the asphalt binder, and the pitch for obtaining aging combines Material.Rotating thin film heat run is suitable for measurement bi tumenf orr oad, the heating of polymer modified asphalt rotary thin film in drying oven (referred to as RTFOT the mass change after).The present invention is to obtain the asphalt binder of aging using the purpose of rotating thin film heat run. It is preferable to use rotary thin film in drying oven to carry out rotating thin film Heating Experiment according to the method for the T0610 in JTG E20.
Preferably, the temperature of the heating is 160 DEG C~180 DEG C in the rotating thin film heat run, and such as: 165 DEG C, 170 DEG C, 175 DEG C etc., the time of heating is no less than 75min, preferably 75min~85min.Specifically, according to JTG 0610 method of T in E20, rotary thin film in drying oven should go up in 10min to 160 DEG C~180 DEG C, make sample in this temperature condition Lower heated time is no less than 75min, and total duration is no less than 85min.
Needle penetration
Needle penetration is one of primary quality measure of pitch.It is to indicate the soft or hard degree of pitch and consistency, resist failure by shear Ability, the index of the reflection relative viscosity of pitch under certain condition.It was found by the inventors of the present invention that passing through measurement pitch knot The needle penetration (can only measure the needle penetration after aging) before expecting aging and after aging is closed, according to the size of needle penetration, can be sentenced Determining sample to be tested is high-modulus agent or anti-rut agent.
Specifically, 25 DEG C at a temperature of, needle penetration after measuring the asphalt binder aging, if the pitch combines Needle penetration after expecting aging is greater than 100, then determines the sample to be tested for anti-rut agent.If but the needle penetration after aging is less than Equal to 100, in order to keep testing result more accurate, need further to detect ductility to be determined.
Needle penetration of the invention can be tested according to the method in T 0604 in JTG E20, when measuring 25 DEG C, aging Needle penetration after preceding and aging.
Ductility
Bitumen ductility just refers to the extensibility of pitch.Ductility is bigger, shows that the plasticity of pitch is better.Ductility is evaluation pitch The important indicator of plasticity.It was found by the inventors of the present invention that by the ductility before measurement asphalt binder aging and after aging, according to The size of ductility, it is possible to determine that sample to be tested is high-modulus agent or anti-rut agent.
Specifically, 25 DEG C at a temperature of, measure the ductility before and after the asphalt binder aging, if the pitch combine Ductility after expecting aging is greater than the ductility before aging, then determines the sample to be tested for anti-rut agent.If but the pitch knot The ductility that ductility after closing material aging is less than or equal to before aging needs further to pass through survey to keep testing result more accurate Determine needle penetration to be determined.
Ductility of the invention can be tested according to the method in T 0605 in JTG E20, when measuring 25 DEG C, before aging With the ductility after aging.
If the needle penetration after the asphalt binder aging is less than or equal to 100;Also, after the asphalt binder aging Ductility is less than or equal to the ductility before aging, then determines the sample to be tested for high-modulus agent.
Apparent viscosity
The present invention can also include described in measurement before the melt mass flow rate of the measurement sample to be tested The step of apparent viscosity of sample to be tested.Apparent viscosity, that is, rotary viscosity can be carried out using Bu Luoke Philid viscometer method Measurement.
Specifically, apparent viscosity is that asphalt binder is constructed pumping performance index (construction property), as < 3Pas, The construction property for illustrating the not excessive influence asphalt binder of the sample to be tested being added, if but than the table of matrix pitch sample It is also low to see viscosity, it would be possible that unfavorable for the raising of the modulus of final asphalt;If > 3Pas, then more Ying Jinyi Needle penetration and stretch indexe after step detection aging.
According to the method for the present invention, high-modulus agent can be fast and effeciently screened on the basis of not increasing extras and is resisted Rut agent.It wherein can a part of second-rate anti-rut agent of screening from the inspection of melt mass flow rate index.Then Asphalt binder will be prepared in sample to be tested doped matrix asphalt sample, before and after the asphalt binder aging by examining preparation Performance indicator can further determine that sample to be tested is high-modulus agent or anti-rut agent.
Embodiment
Embodiment of the present invention is described in detail below in conjunction with embodiment, but those skilled in the art will Understand, the following example is merely to illustrate the present invention, and should not be taken as limiting the scope of the invention.It is not specified in embodiment specific Condition person carries out according to conventional conditions or manufacturer's recommended conditions.Reagents or instruments used without specified manufacturer is It can be with conventional products that are commercially available.
Test apparatus
(1) electronic balance: sensibility reciprocal is not more than 0.1g;
(2) baking oven: 50 DEG C -200 DEG C adjustable, and temperature control precision is 0.5 DEG C;
(3) pitches such as metal pan sample holder ware;
(4) high-speed shearing machine: 3000r/min~5000r/min revolving speed is adjustable;
(5) fusion index instrument;
(6) other: for example: glass bar etc..
Sample to be tested: 1# sample is tested, domestic production is high-modulus agent;
2# sample, domestic production are high-modulus agent;
3# sample, foreign countries' production are anti-rut agent;
4# sample, foreign countries' production are anti-rut agent.
Embodiment 1
Melt mass flow rate measurement
1# sample is taken, as sample to be tested.1# sample 5g is weighed using assay balance;
According to GB/T 3682.1-2018, " thermoplastic melt mass flow rate and melt volume-flow rate are surveyed The mass measuring method of thermoplastic melt flow rate (MFR) in calmly " measures melt mass flow rate.Specific determination condition Are as follows: 190 DEG C of temperature, under the load of counterweight 2.16kg.
Sample is packed into graduated cylinder, is tested according to the measurement method of 9.5 sections, MFR test result on display screen is read, is surveyed It is as shown in table 1 below to determine result.
The preparation of asphalt binder
(1) 35# bi tumenf orr oad 500g is taken;Be heated in an oven 170 DEG C it is spare;
(2) 1# sample 35g (based on the 7% of 35# bi tumenf orr oad quality) is weighed, is slowly added into heating by several times In 35# bi tumenf orr oad;
(3) the 35# bi tumenf orr oad shearing that 1# sample is added is not less than by 5000r/min rate using cutter 30min, sample of being subject to uniformly, without obvious sample to be tested particle, temperature is kept for 175 DEG C in shear history.
(4) under 175 DEG C of environment, shearing development 0.5h at a slow speed is sealed under the revolving speed of 1200r/min.
(5) after the completion of shearing should moulding immediately, carry out correlation test.
Apparent viscosity measurement
The measurement of apparent viscosity (not aging process) is carried out according to the method for T0625 in JTG E20-2011.
Aging process
Aging process is carried out to asphalt binder according to the method for T0610 in JTG E20-2011.
The measurement of needle penetration and ductility
Needle penetration before aging and after aging, old is carried out respectively according to the method for T0604, T0605 in JTG E20-2011 Stretch indexe before changing and after aging is examined, and inspection result is as shown in table 2.
Embodiment 2
In example 2, it other than 1# sample is replaced with 2# sample, is surveyed in the same manner as example 1 Fixed, measurement result is as shown in Table 1 and Table 2.
Embodiment 3
In embodiment 3, it other than 1# sample is replaced with 3# sample, is surveyed in the same manner as example 1 Fixed, measurement result is as shown in Table 1 and Table 2.
Embodiment 4
In example 4, it other than 1# sample is replaced with 4# sample, is surveyed in the same manner as example 1 Fixed, measurement result is as shown in Table 1 and Table 2.
Measurement result
Table 1 is the melt mass flow rate measurement result of sample to be tested, and table 2 is the apparent viscosity of asphalt binder, needle In-degree and ductilometers result.
Table 1
As can be seen from Table 1, the melt mass flow rate of embodiment 1-3 is in 2g/10min or more, can carry out into The measurement of one step.And the melt mass flow rate of embodiment 4 is 1.78, is less than 2g/10min, therefore, it is possible to determine that embodiment 4 sample is anti-rut agent.
Table 2
As can be seen from Table 2, higher mixed with the apparent viscosity of 3# sample and the asphalt binder of 4# sample, it may will affect Construction property.
At 25 DEG C, mixed with the needle penetration after the asphalt binder aging of 1# sample and 2# sample less than 100;Also, it should Ductility after asphalt binder aging is less than the ductility before aging, then can be determined that 1# sample and 2# sample is high-modulus agent.
At 25 DEG C, it is greater than 100 mixed with the needle penetration after the asphalt binder aging of 3# sample;In addition, the pitch combines Ductility after expecting aging then can be determined that 3# sample is anti-rut agent also greater than the ductility before aging.
For 4# sample, at 25 DEG C, can be determined that by melt mass flow rate measurement as anti-rut agent, by right It is further measured, it can be seen that is greater than 100 mixed with the needle penetration after the asphalt binder aging of 4# sample;In addition, Ductility after the asphalt binder aging is greater than the ductility before aging, can further determine that 4# sample is anti-rut agent, and molten Weight flow rate measurement result is consistent.
Detection method verifying
20 DEG C are carried out according to 0738 method of T in " highway engineering pitch and Asphalt Mixture Experiment regulation " (JTG E20), Uniaxial compression dynamic modulus test under the conditions of 10Hz;And 0739 method of T carries out 15 DEG C, the four-point bending under the conditions of 10Hz Fatigue life test, laboratory determine fatigue equation according to 3 strain levels, calculate 1,000,000 corresponding fatigue rupture strains Value ε10^6
5 parts of EME2 (0/20) gradation asphalts are taken, wherein in 4 parts of EME2 (0/20) gradation asphalts respectively Four kinds of samples to be tested are added, both the above test is carried out under the conditions of same volume (by the 0.6% of quality of asphalt mixtures).Knot Fruit is as shown in table 3 below:
Table 3
As can be seen from Table 3, under the conditions of same gradation, high-modulus agent for 1# and 2#, in identical volume item Under part, fatigue behaviour is substantially better than 3# and 4# anti-rut agent.This is because the effect of anti-rut agent is mainly so that pitch mixes The intensity of material increases, and does not ensure that the durability of asphalt, and fatigue rupture strain can also decline.And high-modulus agent Not only the intensity of asphalt can be improved, but also the durability of asphalt will not be made to be affected.Therefore, this Shen Method please effectively can quickly distinguish high-modulus agent and anti-rut agent, and highly reliable, and testing result is accurate.
The above embodiment of the present invention be only to clearly illustrate example of the present invention, and not be to the present invention Embodiment restriction.For those of ordinary skill in the art, it can also make on the basis of the above description Other various forms of variations or variation.There is no necessity and possibility to exhaust all the enbodiments.It is all of the invention Made any modifications, equivalent replacements, and improvements etc., should be included in the protection of the claims in the present invention within spirit and principle Within the scope of.

Claims (10)

1. a kind of method for distinguishing high-modulus agent and anti-rut agent characterized by comprising
Sample to be tested is taken, under 190 DEG C, the load of counterweight 2.16kg, measures the melt mass flow rate of the sample to be tested;
If the melt mass flow rate is less than 2g/10min, determine the sample to be tested for anti-rut agent;
If the melt mass flow rate is more than or equal to 2g/10min, matrix pitch sample is taken, preparation adds described to be measured The asphalt binder of sample;
25 DEG C at a temperature of, measure needle penetration after the ductility and/or aging before the asphalt binder aging and after aging;
If the needle penetration after the asphalt binder aging is greater than 100;And/or the ductility after the asphalt binder aging is big Ductility before aging then determines the sample to be tested for anti-rut agent;
If the needle penetration after the asphalt binder aging is less than or equal to 100;Also, the ductility after the asphalt binder aging Less than or equal to the ductility before aging, then determine the sample to be tested for high-modulus agent.
2. the method according to claim 1 for distinguishing high-modulus agent and anti-rut agent, which is characterized in that described in the measurement Before the melt mass flow rate of sample to be tested, further include the steps that the apparent viscosity for measuring the sample to be tested.
3. the method according to claim 1 or 2 for distinguishing high-modulus agent and anti-rut agent, which is characterized in that with the base The gross mass meter of matter asphalt sample, the additional amount of the sample to be tested are 5%~9%.
4. the method according to claim 1-3 for distinguishing high-modulus agent and anti-rut agent, which is characterized in that described The preparation method of asphalt binder the following steps are included:
Step 1) takes matrix pitch sample and heats, the sample to be tested is then added, obtains premix;
Step 2) obtains asphalt binder to moulding after premix progress shear treatment.
5. the method according to claim 4 for distinguishing high-modulus agent and anti-rut agent, which is characterized in that the step 1) In, the temperature of heating is 160 DEG C~180 DEG C.
6. the method according to claim 4 or 5 for distinguishing high-modulus agent and anti-rut agent, which is characterized in that the step 2) in, the shear treatment includes:
Pre- shearing step carries out preliminary shear treatment to the premix under the revolving speed of 4000r/min~5000r/min, Obtain pre- cutting object;
Development processing is sheared, under the revolving speed of 800r/min~1500r/min, shear treatment is carried out to the pre- cutting object, is obtained Product must be sheared.
7. the method according to claim 6 for distinguishing high-modulus agent and anti-rut agent, which is characterized in that the pre- shearing step Rapid temperature is 160 DEG C~180 DEG C;The time of the pre- shear treatment is 30min or more, preferably 30min~120min.
8. the method for differentiation the high-modulus agent and anti-rut agent according to claim 6 or 7, which is characterized in that institute The temperature for stating shearing development processing is 160 DEG C~180 DEG C;The time of the shearing development processing is 0.5h~1.0h.
9. the method according to claim 1-8 for distinguishing high-modulus agent and anti-rut agent, which is characterized in that described The step of aging includes: to carry out rotating thin film heat run to the asphalt binder, obtains the asphalt binder of aging.
10. the method according to claim 9 for distinguishing high-modulus agent and anti-rut agent, which is characterized in that the Rotational Thin In film heat run, the temperature of the heating is 160 DEG C~180 DEG C, and the time of the heating is no less than 75min, preferably 75min~85min.
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