CN110082256B - Method for distinguishing high modulus agent and anti-rutting agent - Google Patents
Method for distinguishing high modulus agent and anti-rutting agent Download PDFInfo
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- CN110082256B CN110082256B CN201910415064.0A CN201910415064A CN110082256B CN 110082256 B CN110082256 B CN 110082256B CN 201910415064 A CN201910415064 A CN 201910415064A CN 110082256 B CN110082256 B CN 110082256B
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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
- G01N1/286—Preparing 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
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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
- G01N1/36—Embedding or analogous mounting of 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
- G01N1/44—Sample treatment involving radiation, e.g. heat
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- G—PHYSICS
- G01—MEASURING; TESTING
- 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
- G01—MEASURING; TESTING
- 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
- G01N11/02—Investigating flow properties of materials, e.g. viscosity, plasticity; Analysing materials by determining flow properties by measuring flow of the material
- G01N11/04—Investigating 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
- G01N11/06—Investigating 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
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- G—PHYSICS
- G01—MEASURING; TESTING
- 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
- G01N11/10—Investigating flow properties of materials, e.g. viscosity, plasticity; Analysing materials by determining flow properties by moving a body within the material
- G01N11/12—Investigating 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
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N3/00—Investigating strength properties of solid materials by application of mechanical stress
- G01N3/28—Investigating ductility, e.g. suitability of sheet metal for deep-drawing or spinning
Abstract
The present invention provides a method for distinguishing between high modulus agents and anti-rutting agents. The method comprises the following steps: taking a sample to be measured, and measuring the melt mass flow rate of the sample to be measured at 190 ℃ under the load of 2.16kg of counter weight; if the mass flow rate of the melt is less than 2g/10min, judging that the sample to be detected is an anti-rutting agent; if the melt mass flow rate is more than or equal to 2g/10min, taking a matrix asphalt sample, and preparing an asphalt binder doped with the sample to be detected; determining ductility before and after aging of the asphalt binder, and/or penetration after aging at a temperature of 25 ℃; if the penetration degree of the asphalt binder after aging is more than 100; and/or judging that the sample to be detected is the anti-rutting agent if the ductility of the asphalt binder after aging is greater than that before aging; if the penetration degree of the asphalt binder after aging is less than or equal to 100; and if the ductility of the asphalt binder after aging is less than or equal to the ductility before aging, determining that the sample to be tested is the high modulus agent. The method is simple and easy to implement, and can effectively and quickly distinguish the high modulus agent from the anti-rutting agent.
Description
Technical Field
The invention relates to a method for distinguishing a high modulus agent and an anti-rutting agent, and belongs to the field of road material performance testing.
Background
The high-modulus asphalt mixture is suitable for high-temperature, large-traffic, heavy-load, overload and high-grade highways, the mixture design gives consideration to the high modulus, fatigue resistance, high temperature resistance and water loss resistance of the binder, the requirement of long-life asphalt pavement is met, and the technology of the high-modulus asphalt mixture is successfully applied at home and abroad.
At present, the research believes that there are three technical approaches for realizing high modulus asphalt mixture: (1) hard asphalt (low-grade asphalt with the penetration degree of less than 25 at 25 ℃) is adopted; (2) adding a high modulus modifier; (3) composite modified asphalt, such as natural asphalt modified asphalt, is adopted. According to the domestic current petrochemical production process level and market condition, in the aspect of low-grade asphalt, because the current demand is limited, large-scale production is not carried out in China, and trial production and use are only carried out in a small range; against this background, a variety of high modulus agent products have appeared in the popularization of high modulus asphalt concrete, including domestic self-developed products and some imported products.
In a broad sense, the additive capable of obviously improving the stiffness modulus and the fatigue resistance of the asphalt mixture is called a high modulus agent, also called a high modulus modifier, a high modulus additive and the like; all relevant asphalt modifiers applied for the purpose of anti-rutting can be called anti-rutting agents, also called anti-rutting modifiers, anti-rutting additives and the like. The high modulus agent and the anti-rutting agent are two common additives in asphalt, but some manufacturers directly adopt the anti-rutting agent to replace the high modulus agent due to similar appearance of the high modulus agent and the anti-rutting agent so as to meet the requirement of high modulus asphalt concrete. And the anti-rutting agent is used for replacing a high modulus agent, so that the technical requirement of the high modulus asphalt mixture cannot be met at all.
Along with the large-area popularization and application of high-modulus asphalt concrete, the requirement of a high modulus agent is very large, an effective test method for discriminating the high modulus agent and an anti-rutting agent is sought, and great benefit is brought to the development of high-modulus concrete technology. In the prior art, two additives are screened, chemical component analysis is required, including Vicat softening temperature, shrinkage rate and the like, the process is complicated, the requirement on the specialty is high, and the method is not easy to master generally.
Therefore, the research on a method for rapidly distinguishing the high modulus agent from the anti-rutting agent is a technical problem to be solved urgently.
Disclosure of Invention
Problems to be solved by the invention
In view of the technical problems in the prior art, for example: distinguishing between high modulus agents and anti-rutting agents requires chemical composition analysis and multiple performance measurements, such as: including vicat softening temperature, shrinkage, etc.; the detection process is complicated, the requirement on the specialty is high, and the detection method is not easy to master generally and the like. The invention provides a method for distinguishing a high modulus agent from an anti-rutting agent. The method is simple and easy to implement, can effectively and quickly distinguish the high modulus agent and the anti-rutting agent, and is strong in reliability and accurate in detection result.
Means for solving the problems
The invention provides a method for distinguishing a high modulus agent from an anti-rutting agent, comprising:
taking a sample to be tested, and measuring the melt mass flow rate of the sample to be tested at 190 ℃ under the load of 2.16kg of counter weight;
if the melt mass flow rate is less than 2g/10min, judging that the sample to be detected is an anti-rutting agent;
if the melt mass flow rate is more than or equal to 2g/10min, taking a matrix asphalt sample, and preparing an asphalt binder doped with the sample to be detected;
determining ductility before and after aging, and/or penetration after aging of the asphalt binder at a temperature of 25 ℃;
if the penetration degree of the asphalt binder after aging is more than 100; and/or judging that the sample to be detected is the anti-rutting agent if the ductility of the asphalt binder after aging is greater than that before aging;
if the penetration degree of the asphalt binder after aging is less than or equal to 100; and if the ductility of the asphalt binder after aging is less than or equal to the ductility of the asphalt binder before aging, determining that the sample to be tested is the high modulus agent.
The method for distinguishing the high modulus agent from the anti-rutting agent, provided by the invention, comprises the step of measuring the apparent viscosity of the sample to be measured before measuring the melt mass flow rate of the sample to be measured.
The method for distinguishing the high modulus agent from the anti-rutting agent comprises the step of adding the sample to be detected in an amount of 5-9% by mass of the total mass of the matrix asphalt sample.
The method for distinguishing the high modulus agent from the anti-rutting agent according to the present invention, wherein the preparation method of the asphalt binder comprises the following steps:
step 1), taking a matrix asphalt sample, heating, and then adding the sample to be tested to obtain a premix;
and 2) shearing the premix, and then casting a mold to obtain the asphalt binder.
The method for distinguishing the high modulus agent from the anti-rutting agent according to the invention is characterized in that in the step 1), the heating temperature is 160-180 ℃.
The method for distinguishing the high modulus agent from the anti-rutting agent according to the present invention, wherein the shearing treatment in the step 2) comprises:
pre-shearing, namely performing primary shearing treatment on the premix at the rotating speed of 4000-5000 r/min to obtain a pre-sheared object;
and (4) shearing and developing treatment, namely shearing the pre-sheared object at the rotating speed of 800 r/min-1500 r/min to obtain a sheared product.
The method for distinguishing the high modulus agent from the anti-rutting agent according to the invention, wherein the temperature of the pre-shearing step is 160-180 ℃; the time of the pre-shearing treatment is more than 30min, preferably 30 min-120 min.
The method for distinguishing the high modulus agent from the anti-rutting agent, provided by the invention, is characterized in that the temperature of the shearing development treatment is 160-180 ℃; the time of the shearing development treatment is 0.5 h-1.0 h.
The method of distinguishing between a high modulus agent and an anti-rutting agent according to the present invention, wherein the aging step comprises: and carrying out a rotary film heating test on the asphalt binder to obtain the aged asphalt binder.
The method for distinguishing the high modulus agent from the anti-rutting agent is characterized in that in the rotating film heating test, the heating temperature is 160-180 ℃, and the heating time is not less than 75min, preferably 75-85 min.
ADVANTAGEOUS EFFECTS OF INVENTION
The method for distinguishing the high modulus agent and the anti-rutting agent is simple and easy to implement, can effectively and quickly distinguish the high modulus agent and the anti-rutting agent, and is strong in reliability and accurate in detection result.
Furthermore, the method for distinguishing the high modulus agent from the anti-rutting agent does not need to add extra detection equipment, and the used raw materials are easy to obtain and sample preparation is easy, so that the test cost can be reduced.
Detailed Description
Various exemplary embodiments, features and aspects of the invention will be described in detail below. The word "exemplary" is used exclusively herein to mean "serving as an example, embodiment, or illustration. Any embodiment described herein as "exemplary" is not necessarily to be construed as preferred or advantageous over other embodiments.
Furthermore, in the following detailed description, numerous specific details are set forth in order to provide a better understanding of the present invention. It will be understood by those skilled in the art that the present invention may be practiced without some of these specific details. In other instances, methods, means, devices and steps which are well known to those skilled in the art have not been described in detail so as not to obscure the invention.
All units used in the present invention are international standard units unless otherwise stated, and numerical values and numerical ranges appearing in the present invention should be understood to include systematic errors inevitable in industrial production.
Considering the actual engineering characteristics of the additive, the inventor of the invention finds that the high modulus agent can give consideration to the high and low temperature performances of the asphalt mixture, and has the characteristics of excellent processing characteristics and the like, while the anti-rutting agent obviously improves the high temperature performance and loses the low temperature and medium temperature performances. Therefore, by utilizing the characteristic, the rut resistant agent and the high modulus agent can be discriminated by adopting a method of combining the melt mass flow rate of the sample to be tested with the penetration and/or ductility indexes before and after specific aging of the asphalt binder. Specifically, a melt index test is carried out on a sample to be tested, a part of the anti-track agent can be screened out, and then the penetration degree after aging and/or the ductility index and the apparent viscosity index before and after aging can be adopted to respectively evaluate the low-temperature performance and the construction characteristic of modified addition, so as to distinguish the anti-track agent from the high modulus agent. In particular, the method of manufacturing a semiconductor device,
the present invention provides a method for distinguishing between high modulus agents and anti-rutting agents. The method comprises the following steps:
taking a sample to be tested, and measuring the melt mass flow rate of the sample to be tested at 190 ℃ under the load of 2.16kg of counter weight;
and if the melt mass flow rate is less than 2g/10min, judging that the sample to be detected is an anti-rutting agent instead of a high modulus agent.
Further, in order to further distinguish the high modulus agent from the anti-rutting agent, after the determination of the melt mass flow rate of the sample to be tested, for the high modulus agent and the anti-rutting agent which are not distinguished, if the melt mass flow rate is greater than or equal to 2g/10min, the method further comprises the following steps:
taking a matrix asphalt sample, and preparing an asphalt binder doped with the sample to be detected;
determining ductility before and after aging, and/or penetration after aging of the asphalt binder at a temperature of 25 ℃;
if the penetration degree of the asphalt binder after aging is more than 100; and/or judging that the sample to be detected is the anti-rutting agent if the ductility of the asphalt binder after aging is greater than that before aging;
if the penetration degree of the asphalt binder after aging is less than or equal to 100; and if the ductility of the asphalt binder after aging is less than or equal to the ductility of the asphalt binder before aging, determining that the sample to be tested is the high modulus agent.
The method for distinguishing the high modulus agent and the anti-rutting agent is simple and easy to implement, can effectively and quickly distinguish the high modulus agent and the anti-rutting agent, and is strong in reliability and accurate in detection result.
Furthermore, the method for distinguishing the high modulus agent from the anti-rutting agent does not need to add extra detection equipment, and the used raw materials are easy to obtain and sample preparation is easy, so that the test cost can be reduced.
Melt mass flow rate
Melt Mass Flow Rate (MFR), also known as Melt flow rate, is the Melt Index (MI), which is the gram of Melt flowing through a standard capillary over a certain period of time (typically 10min) in a standardized Melt index apparatus at a certain temperature and pressure, and is given in g/10 min. The inventors of the present invention have found that the use of melt mass flow rate allows an initial distinction between anti-rutting agents and non-high modulus agents.
The melt mass flow rate of the sample to be tested can be measured according to the mass measurement method of the melt flow rate of the thermoplastic plastics in GB/T3682.1-2018 determination of melt mass flow rate and melt volume flow rate of the thermoplastic plastics. According to the invention, by measuring the melt mass flow rate of the sample to be detected and according to whether the melt mass flow rate is more than 2g/10min or not, a part of anti-rutting agent and high modulus agent can be distinguished. Namely: and if the melt mass flow rate is less than 2g/10min, judging that the sample to be detected is an anti-rutting agent instead of a high modulus agent. If the melt mass flow rate is greater than or equal to 2g/10min, further determination is required.
Matrix asphalt samples
In the present invention, when the melt mass flow rate is greater than 2g/10min, further determination is made by formulating an asphalt binder. When preparing the asphalt binder, a proper matrix asphalt sample can be selected for preparation. The matrix asphalt sample is not particularly limited in the present invention as long as the embodiment of the present invention can be achieved.
Preferably, the matrix asphalt sample may be road petroleum asphalt. Further, the road petroleum asphalt comprises one or more of low-grade road petroleum asphalt, 70# to 200# road petroleum asphalt and the like.
Further, the present invention preferably uses low-grade road petroleum asphalt, i.e., 50# road petroleum asphalt and road petroleum asphalt smaller than 50# road petroleum asphalt, such as 25# road petroleum asphalt, 35# road petroleum asphalt, 50# road petroleum asphalt, and the like.
Asphalt binder
The asphalt binder is asphalt binder doped with a sample to be detected. For more accurate distinction between the anti-rutting agent and the high modulus agent, the amount of the sample to be tested is 5-9% of the total mass of the matrix asphalt sample, for example: the addition amount of the sample to be detected can be 5.5%, 6%, 6.5%, 7%, 7.5%, 8%, 8.5% and the like. In the invention, when the adding amount of the sample to be measured is between 5% and 9%, the penetration degree and the ductility of the asphalt binder are both excellent, and the measurement result is stable. The adding amount of the sample to be detected is too small, and the modification effect of the sample to be detected is not obvious; when the amount of the asphalt is too large, the storage stability of the asphalt is deteriorated, segregation is liable to occur, and the viscosity of the asphalt is increased, which is disadvantageous for pumping. Therefore, too much or too little sample is not suitable for distinguishing the anti-rut agent from the high modulus agent.
Further, the preparation method of the asphalt binder comprises the following steps:
step 1), taking a matrix asphalt sample, heating, and then adding the sample to be tested to obtain a premix;
and 2) shearing the premix, and then casting a mold to obtain the asphalt binder.
Preferably, in step 1), the temperature for heating may be 160 to 180 ℃, for example, 165 ℃, 170 ℃, 175 ℃ or the like, in order to make the sample to be measured more soluble in the matrix asphalt sample.
In the step 2), in order to prepare the asphalt binder with excellent and stable performance, the shearing treatment comprises the following steps: a pre-cutting step and a cutting development step. Specifically, the method comprises the following steps:
the pre-shearing step comprises: performing primary shearing treatment on the premix at the rotating speed of 4000 r/min-5000 r/min to obtain a pre-shearing object; through the primary shearing treatment, the matrix asphalt sample and the sample to be detected can be subjected to primary premixing.
In the invention, when the rotating speed is 4000 r/min-5000 r/min, on one hand, the sample to be detected and the matrix asphalt sample can be fully and uniformly mixed, the sample to be detected can not agglomerate, and a stable system can be formed; on the other hand, the sample to be detected does not swell in the matrix asphalt sample, can be tightly combined with the light component and the waxy component in the asphalt, achieves the shrinkage balance of adsorption swelling on the interface between the sample to be detected and the matrix asphalt sample, forms a more stable interface layer, improves the compatibility between the sample to be detected and the matrix asphalt sample, and improves the performance of the asphalt. Therefore, when the rotating speed is 4000r/min to 5000r/min, for example: 4200r/min, 4500r/min, 4800r/min and the like, and can improve the penetration degree and ductility of the asphalt binder, so that the measurement result is more accurate.
Preferably, the temperature of the pre-shearing step is 160-180 ℃; when the temperature of the pre-shearing step is between 160 ℃ and 180 ℃, for example: the ductility of the asphalt binder can be improved at 165 ℃, 170 ℃ and 175 ℃, and the penetration degree is relatively stable. The time of the pre-shearing treatment is more than 30min, preferably 30 min-120 min. Generally speaking, the penetration and ductility of the asphalt binder are improved to different degrees along with the increase of time, so that the measurement result is more accurate and reliable.
The shearing development treatment comprises shearing the pre-sheared object at the rotating speed of 800 r/min-1500 r/min to obtain a sheared product; through the shearing development treatment, the sample to be measured can be stably dispersed in the matrix asphalt, the development condition is good, generally speaking, the dispersion degree of the sample to be measured in the asphalt is high, the performance of the asphalt binder is better, and the measurement result is more accurate and reliable. The rotating speed during the shearing development treatment can be 1000r/min, 1200r/min, 1400r/min and the like.
Preferably, the temperature of the shear development treatment is 160 ℃ to 180 ℃, for example: 165 ℃, 170 ℃, 175 ℃; the time of the shearing development treatment is 0.5h to 1.0h, for example: 0.6h, 0.7h, 0.8h, 0.9h and the like. The shearing development treatment is based on the fact that a sample is uniform and has no obvious sample particles to be detected, and specifically, the sample can be dipped by a glass rod and scraped on a piece of clean test paper, and the mixed state of the sample is visually observed.
Specifically, the preparation method of the asphalt binder comprises the following steps:
(1) taking a matrix asphalt sample, placing the sample in a sample container, and heating the sample to 160-180 ℃ in an oven.
(2) Taking 5-9% of a sample to be measured according to the total mass of the matrix asphalt sample, and slowly adding the sample to be measured into the heated matrix asphalt sample in several times to obtain a premix;
(3) shearing the pre-mixture by using a shearing machine at the speed of 4000-5000 r/min for not less than 30min +/-1 min, preferably 30-120 min, and keeping the temperature at 160-180 ℃ in the shearing process based on the uniform sample and no obvious sample particles to be detected.
(4) Sealing and slowly shearing at the rotation speed of 800-1500 r/min for 0.5-1.0 h in the environment of 160-180 ℃.
(5) And immediately pouring the mold after the shearing development is finished to obtain the asphalt binder for later use.
Aging of asphalt binders
The aged asphalt binder can be obtained by performing a rotary film heating test on the asphalt binder. The rotating film heating test is suitable for measuring the quality change of road petroleum asphalt and polymer modified asphalt after being heated by a rotating film oven (RTFOT for short). The present invention utilizes a rotary film heat test to obtain an aged asphalt binder. The spinning thin film heating experiment is preferably performed using a spinning thin film oven following the method of T0610 in JTG E20.
Preferably, in the rotating film heating test, the heating temperature is 160 ℃ to 180 ℃, for example: 165 ℃, 170 ℃, 175 ℃ and the like, and the heating time is not less than 75min, preferably 75min to 85 min. Specifically, according to the T0610 method in JTG E20, the rotary film oven should be raised back to 160-180 ℃ in 10min so that the sample is heated at this temperature for not less than 75min, and the total duration is not less than 85 min.
Penetration degree
Penetration is one of the main quality indicators of bitumen. Is an index which represents the degree and consistency of the softness and hardness of the asphalt, the ability to resist shear failure and reflects the relative viscosity of the asphalt under certain conditions. The inventor of the invention finds that by measuring the penetration degree of the asphalt binder before and after aging (only the penetration degree after aging can be measured), whether the sample to be measured is the high modulus agent or the anti-rutting agent can be judged according to the penetration degree.
Specifically, the penetration degree of the aged asphalt binder is measured at the temperature of 25 ℃, and if the penetration degree of the aged asphalt binder is greater than 100, the sample to be detected is determined to be the anti-rutting agent. However, if the penetration after aging is 100 or less, the extension needs to be further detected for determination in order to make the detection result more accurate.
The penetration of the present invention can be tested by the method in T0604 of JTG E20 to determine penetration before and after aging at 25 ℃.
Degree of extension
Asphalt ductility refers to the ductility of asphalt. The greater the ductility, the better the plasticity of the bitumen. Ductility is an important index for evaluating the plasticity of asphalt. The inventor of the invention finds that whether the sample to be tested is the high modulus agent or the anti-rutting agent can be judged according to the ductility by measuring the ductility of the asphalt binder before and after ageing.
Specifically, the ductility of the asphalt binder before and after aging is measured at the temperature of 25 ℃, and if the ductility of the asphalt binder after aging is greater than the ductility of the asphalt binder before aging, the sample to be measured is determined to be the anti-rutting agent. However, if the ductility of the asphalt binder after aging is equal to or less than the ductility before aging, it is necessary to further determine the ductility by measuring the penetration in order to obtain more accurate detection results.
The ductility of the present invention can be tested according to the method in T0605 of JTG E20 to determine the ductility before and after aging at 25 ℃.
If the penetration degree of the asphalt binder after aging is less than or equal to 100; and if the ductility of the asphalt binder after aging is less than or equal to the ductility of the asphalt binder before aging, determining that the sample to be tested is the high modulus agent.
Apparent viscosity
The method can also comprise the step of measuring the apparent viscosity of the sample to be measured before the step of measuring the melt mass flow rate of the sample to be measured. The apparent viscosity, i.e., the rotational viscosity, can be measured by the Brookfield viscometer method.
Specifically, the apparent viscosity is an index of pumping characteristics (construction characteristics) of asphalt binder construction, when the apparent viscosity is less than 3Pa · s, it indicates that the added sample to be tested does not influence the construction characteristics of the asphalt binder too much, but if the apparent viscosity is lower than that of a matrix asphalt sample, the modulus of the final asphalt mixture may be disadvantageously improved; if the average molecular weight is more than 3 pas, the needle penetration and ductility indexes after aging are further detected.
According to the method, the high modulus agent and the anti-rutting agent can be quickly and effectively discriminated on the basis of not increasing additional equipment. Wherein a portion of poor quality anti-rutting agents can be screened from a check of the melt mass flow rate indicator. And then, doping the sample to be detected into a matrix asphalt sample to prepare the asphalt binder, and further judging whether the sample to be detected is the high modulus agent or the anti-rutting agent by testing the performance indexes of the prepared asphalt binder before and after aging.
Examples
Embodiments of the present invention will be described in detail below with reference to examples, but those skilled in the art will appreciate that the following examples are only illustrative of the present invention and should not be construed as limiting the scope of the present invention. The examples, in which specific conditions are not specified, were conducted under conventional conditions or conditions recommended by the manufacturer. The reagents or instruments used are not indicated by the manufacturer, and are all conventional products commercially available.
Testing instrument
(1) An electronic balance: the sensory quantity is not more than 0.1 g;
(2) oven: the temperature can be adjusted between 50 ℃ and 200 ℃, and the temperature control precision is 0.5 ℃;
(3) asphalt sample containers such as metal pots and the like;
(4) a high-speed shearing machine: the rotating speed of 3000 r/min-5000 r/min is adjustable;
(5) a melt index meter;
(6) and others: for example: glass rods, and the like.
Testing a sample to be tested: sample No. 1, produced domestically, is a high modulus agent;
sample No. 2, produced domestically, is a high modulus agent;
the No. 3 sample is produced abroad and is an anti-rutting agent;
the sample No. 4, produced abroad, is an anti-rut agent.
Example 1
Melt mass flow rate determination
Taking a sample No. 1 as a sample to be detected. Weighing 5g of the No. 1 sample by using an analytical balance;
the melt mass flow rate was determined according to the method for measuring the mass of the melt flow rate of thermoplastics in GB/T3682.1-2018 "determination of melt mass flow rate and melt volume flow rate of thermoplastics". The specific measurement conditions are as follows: temperature 190 ℃ and weight 2.16 kg.
The sample was loaded into a measuring cylinder, and the test was performed according to the measurement method of section 9.5, and the measurement results of MFR test on a display screen were read and are shown in table 1 below.
Preparation of asphalt Binder
(1) Taking 500g of 35# road petroleum asphalt; heating to 170 deg.C in oven;
(2) weighing 35g of No. 1 sample (calculated by 7% of the mass of the No. 35 road petroleum asphalt), and slowly adding the sample into the heated No. 35 road petroleum asphalt in batches;
(3) and shearing the 35# road petroleum asphalt added with the 1# sample for not less than 30min by using a shearing machine at a speed of 5000r/min, and keeping the temperature at 175 ℃ in the shearing process based on the uniform sample and no obvious sample particles to be detected.
(4) Sealing and slowly shearing at 175 deg.C at 1200r/min for 0.5 h.
(5) And immediately pouring the die after the shearing is finished, and performing related tests.
Apparent viscosity measurement
The apparent viscosity (no aging treatment) was measured by the method of T0625 in JTG E20-2011.
Aging treatment
And aging the asphalt binder according to the method of T0610 in JTG E20-2011.
Determination of penetration and spread
Penetration before aging and penetration after aging, ductility index tests before aging and ductility index tests after aging were performed according to methods T0604 and T0605 in JTG E20-2011, and the test results are shown in Table 2.
Example 2
In example 2, the measurement was performed in the same manner as in example 1 except that the sample # 1 was replaced with the sample # 2, and the measurement results are shown in tables 1 and 2.
Example 3
In example 3, the measurement was performed in the same manner as in example 1 except that the sample # 1 was replaced with the sample # 3, and the measurement results are shown in tables 1 and 2.
Example 4
In example 4, the measurement was performed in the same manner as in example 1 except that the sample # 1 was replaced with the sample # 4, and the measurement results are shown in tables 1 and 2.
Measurement results
Table 1 shows the results of measuring the melt mass flow rate of the sample to be measured, and table 2 shows the results of measuring the apparent viscosity, penetration and ductility of the asphalt binder.
TABLE 1
As can be seen from Table 1, the melt mass flow rates of examples 1 to 3 were all 2g/10min or more, and further measurements were possible. Whereas the melt mass flow rate of example 4 was 1.78, less than 2g/10min, thus, the sample of example 4 was judged to be an anti-rutting agent.
TABLE 2
As can be seen from Table 2, the apparent viscosity of the asphalt binders blended with the sample No. 3 and the sample No. 4 is high, and the workability may be affected.
The penetration degree of the asphalt binder doped with the sample No. 1 and the sample No. 2 after aging is less than 100 at 25 ℃; and, the ductility of the asphalt binder after aging is less than that before aging, and it can be judged that the sample No. 1 and the sample No. 2 are both high modulus agents.
The penetration degree of the asphalt binder doped with the No. 3 sample after aging is more than 100 at 25 ℃; in addition, the ductility of the asphalt binder after aging is also greater than that before aging, and the No. 3 sample can be judged to be the anti-rutting agent.
For the sample No. 4, the sample can be judged as the anti-rutting agent by measuring the mass flow rate of the melt at 25 ℃, and the penetration degree of the asphalt binder doped with the sample No. 4 after aging is more than 100 by further measuring the anti-rutting agent; in addition, the ductility of the asphalt binder after aging is greater than that before aging, so that the No. 4 sample can be further judged to be an anti-rutting agent and is consistent with the measurement result of the melt mass flow rate.
Detection method verification
Carrying out uniaxial compression dynamic modulus test under the conditions of 20 ℃ and 10Hz according to a T0738 method in road engineering asphalt and asphalt mixture test specification (JTG E20); and performing a four-point bending fatigue life test under the conditions of 15 ℃ and 10Hz by a T0739 method, determining a fatigue equation according to 3 strain levels in a test room, and calculating a fatigue failure strain value epsilon corresponding to 100 ten thousand times10^6。
Taking 5 parts of EME2(0/20) graded asphalt mixture, respectively doping four samples to be tested in 4 parts of EME2(0/20) graded asphalt mixture, and carrying out the above two tests under the condition of the same doping amount (0.6% of the mass of the asphalt mixture). The results are shown in table 3 below:
TABLE 3
From the above table 3, it can be seen that under the same grading condition, for the high modulus agents of # 1 and # 2, the fatigue performance is obviously better than that of the anti-rutting agents of # 3 and # 4 under the same blending amount. This is because the anti-rutting agent acts mainly to increase the strength of the asphalt mixture, cannot ensure the durability of the asphalt mixture, and also reduces the fatigue failure strain. The high modulus agent can improve the strength of the asphalt mixture and simultaneously can not influence the durability of the asphalt mixture. Therefore, the method can effectively and quickly distinguish the high modulus agent and the anti-rutting agent, and is high in reliability and accurate in detection result.
The above examples of the present invention are merely examples for clearly illustrating the present invention and are not intended to limit the embodiments of the present invention. Other variations and modifications will be apparent to persons skilled in the art in light of the above description. And are neither required nor exhaustive of all embodiments. Any modification, equivalent replacement, and improvement made within the spirit and principle of the present invention should be included in the protection scope of the claims of the present invention.
Claims (12)
1. A method of distinguishing between a high modulus agent and an anti-rutting agent comprising:
taking a sample to be tested, and measuring the melt mass flow rate of the sample to be tested at 190 ℃ under the load of 2.16kg of counter weight;
if the melt mass flow rate is less than 2g/10min, judging that the sample to be detected is an anti-rutting agent;
if the melt mass flow rate is more than or equal to 2g/10min, taking a matrix asphalt sample, and preparing an asphalt binder doped with the sample to be detected;
determining ductility before and after aging, and/or penetration after aging, of the asphalt binder at a temperature of 25 ℃;
if the penetration degree of the asphalt binder after aging is more than 100; and/or judging that the sample to be detected is the anti-rutting agent if the ductility of the asphalt binder after aging is greater than that before aging;
if the penetration degree of the asphalt binder after aging is less than or equal to 100; and if the ductility of the asphalt binder after aging is less than or equal to the ductility of the asphalt binder before aging, determining that the sample to be tested is the high modulus agent.
2. The method of distinguishing between a high modulus agent and an anti-rutting agent according to claim 1, further comprising the step of determining the apparent viscosity of said sample to be tested prior to said step of determining the melt mass flow rate of said sample to be tested.
3. The method of distinguishing between a high modulus agent and an anti-rutting agent according to claim 1, wherein the sample to be tested is added in an amount of 5% to 9% based on the total mass of the matrix asphalt sample.
4. The method of distinguishing between a high modulus agent and an anti-rutting agent according to any of claims 1-3, wherein the asphalt binder is prepared by a process comprising the steps of:
step 1), taking a matrix asphalt sample, heating, and then adding the sample to be tested to obtain a premix;
and 2) shearing the premix, and then casting a mold to obtain the asphalt binder.
5. The method of distinguishing between a high modulus agent and an anti-rutting agent according to claim 4, wherein the temperature of heating in step 1) is 160 ℃ to 180 ℃.
6. The method of distinguishing between a high modulus agent and an anti-rutting agent according to claim 4, wherein in step 2) the shearing treatment comprises:
pre-shearing, namely performing primary shearing treatment on the premix at the rotating speed of 4000-5000 r/min to obtain a pre-sheared object;
and (4) shearing and developing treatment, namely shearing the pre-sheared object at the rotating speed of 800 r/min-1500 r/min to obtain a sheared product.
7. The method of distinguishing between a high modulus agent and an anti-rutting agent according to claim 6, wherein the temperature of the pre-shearing step is 160 ℃ to 180 ℃; the time of the pre-shearing step is more than 30 min.
8. The method of distinguishing between a high modulus agent and an anti-rutting agent according to claim 7, wherein the time of the pre-shearing step is between 30min and 120 min.
9. The method of distinguishing between a high modulus agent and an anti-rutting agent according to any of claims 6-8, wherein the temperature of the shear development treatment is 160 ℃ to 180 ℃; the time of the shearing development treatment is 0.5 h-1.0 h.
10. The method of distinguishing between a high modulus agent and an anti-rutting agent according to any of claims 1-3, wherein said aging step comprises: and carrying out a rotary film heating test on the asphalt binder to obtain the aged asphalt binder.
11. The method of distinguishing between a high modulus agent and an anti-rutting agent according to claim 10, wherein said heating is performed at a temperature of 160 ℃ to 180 ℃ for a time of not less than 75min in said rotating film heating test.
12. The method of distinguishing between a high modulus agent and an anti-rutting agent according to claim 11 wherein the heating is for a period of from 75min to 85 min.
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