CN113899651B - Method for detecting content of effective rubber powder in rubber asphalt - Google Patents

Method for detecting content of effective rubber powder in rubber asphalt Download PDF

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CN113899651B
CN113899651B CN202111156801.3A CN202111156801A CN113899651B CN 113899651 B CN113899651 B CN 113899651B CN 202111156801 A CN202111156801 A CN 202111156801A CN 113899651 B CN113899651 B CN 113899651B
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rubber
rubber powder
asphalt
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CN113899651A (en
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谭继宗
袁海涛
王秋敏
熊保林
王勇
张红波
张洪刚
尹业豪
王晓磊
刘平
潘治琼
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Guangxi Jiaoke New Materials Technology Co ltd
Guangxi Jiaoke Group Co Ltd
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    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N5/00Analysing materials by weighing, e.g. weighing small particles separated from a gas or liquid
    • G01N5/04Analysing materials by weighing, e.g. weighing small particles separated from a gas or liquid by removing a component, e.g. by evaporation, and weighing the remainder
    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02WCLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
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    • Y02W30/62Plastics recycling; Rubber recycling

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Abstract

The invention provides a method for detecting the content of effective rubber powder in rubber asphalt, belonging to the technical field of component detection. Mixing rubber asphalt to be detected with a solvent, and sequentially oscillating, centrifuging, filtering and drying; the solvent is one or more of trichloroethylene, kerosene and n-heptane; the content of the available rubber powder in the rubber asphalt is calculated according to the formula 1. The invention utilizes the property that the rubber powder in the rubber asphalt is hardly dissolved in trichloroethylene, kerosene and n-heptane solvents, and the property that the asphalt is dissolved in the trichloroethylene, the kerosene and the n-heptane solvents, and can simply, conveniently and quickly obtain the content of the effective rubber powder in the rubber asphalt by calculating the mass percentage of the insoluble rubber powder in the asphalt and complementing the loss of the dissolving quality of the rubber powder in the solvents, thereby providing a basis for evaluating the quality of the rubber asphalt. The difference value between the effective rubber powder content obtained by the method and the rubber powder content in the rubber asphalt standard product is within-0.3 percent, which shows that the detection method provided by the invention has good accuracy.

Description

Method for detecting content of effective rubber powder in rubber asphalt
Technical Field
The invention relates to the technical field of component detection, in particular to a method for detecting the content of effective rubber powder in rubber asphalt.
Background
The rubber asphalt is a modified asphalt material formed by mixing rubber powder and asphalt and reacting at high temperature. The rubber asphalt can not only greatly improve the road performance of asphalt road surfaces, prolong the service life of road surfaces and reduce the construction cost of highways, but also play a role in controlling pollution, saving resources and comprehensively utilizing a large amount of waste and old materials because the used rubber powder is waste tire rubber powder, and meet the requirements of national environmental protection policies and development of circular economy and the construction of conservation-oriented society.
When rubber asphalt is produced, rubber powder is contacted with asphalt, obvious matter exchange can occur between the rubber powder and the asphalt, the rubber powder is partially cracked, and the crosslinking agent sulfur and acetone extracts in the rubber powder, the oily filler, the anti-aging agent, the zinc compound and other additives and part of active ingredients such as carbon black enter the asphalt through interface exchange, so that the effects of improving the high-temperature performance and the anti-aging performance of the asphalt and improving the bonding condition between the asphalt and mineral materials can be achieved, and the high-temperature performance and the low-temperature performance of the asphalt can be greatly improved. However, in the existing rubber asphalt, the addition amount of rubber powder in some rubber asphalt is lower than the normal level, or some rubber powder substitutes (such as organic matters such as cheap resin and the like) are used for replacing the rubber powder, so that the content of the effective rubber powder in the rubber asphalt does not reach the standard, and the performance of the rubber asphalt is reduced.
The rubber powder content in the rubber asphalt is an important index for evaluating the quality of the rubber asphalt, but no research on a detection method of the effective rubber powder content in the rubber asphalt exists in the prior art.
Disclosure of Invention
In view of the above, the present invention aims to provide a method for detecting the content of effective rubber powder in rubber asphalt. The method provided by the invention can simply, conveniently and quickly detect the content of the effective rubber powder in the rubber asphalt.
In order to achieve the above object, the present invention provides the following technical solutions:
the invention provides a method for detecting the content of effective rubber powder in rubber asphalt, which comprises the following steps:
mixing the rubber asphalt to be detected with a solvent, and sequentially oscillating, centrifuging, filtering and drying; the solvent is one or more of trichloroethylene, kerosene and n-heptane;
calculating the content of the effective rubber powder in the rubber asphalt according to the formula 1:
Figure BDA0003286633140000021
in the formula 1,. omega. is the content of the effective rubber powder in the rubber asphalt%
m 1 G, drying mass of residual centrifugal insoluble substances after centrifugation;
m 2 g is the total mass of the filtering equipment used for filtering;
m 3 g, filtering equipment after filtering and drying mass of residues;
m 0 g, measuring the mass of the rubber asphalt;
R 0 is the solubility of the rubber powder in a solvent.
Preferably, the method for testing the solubility of the rubber powder in the solvent comprises the following steps:
mixing rubber powder with a solvent, and sequentially oscillating, centrifuging, filtering and drying, wherein the solvent is one or more of trichloroethylene, kerosene and n-heptane;
the solubility of the crumb rubber in the rubber asphalt was calculated according to formula 2:
Figure BDA0003286633140000022
in the formula 2, R 0 Is the solubility of the rubber powder in a solvent,%;
M 0 the mass of the rubber powder raw material is g;
M 1 g, drying mass of centrifugal residual insoluble substances after centrifugation;
M 2 g is the total mass of the filtering equipment used for filtering;
M 3 g is the filtration equipment after filtration and the drying mass of the residue.
Preferably, the solubility of the rubber powder in trichloroethylene is 4.87%;
the solubility of the rubber powder in kerosene is 3.22%;
the solubility of the rubber powder in n-heptane is 4.02%.
Preferably, the mass ratio of the rubber asphalt to be detected to the solvent is 1: 50-100.
Preferably, the mixing is carried out under the condition of micro-heating, the mixing temperature is 40-50 ℃, and the mixing time is 0.5-1 h.
Preferably, the oscillation speed is 200-500 r/min; the oscillation time is 20-30 min.
Preferably, the rotation speed of the centrifugation is 500-2000 rpm.
Preferably, the method further comprises, after the centrifugation: repeatedly centrifuging the liquid phase part obtained by centrifuging; the repeated centrifugation is performed for 1-2 times, and the time of single centrifugation is 10-20 min.
Preferably, the drying temperature is 100-110 ℃, and the drying time is 2-3 h.
Preferably, the particle size of the rubber powder is 30-80 meshes.
The invention provides a method for detecting the content of effective rubber powder in rubber asphalt, which comprises the following steps: mixing the rubber asphalt to be detected with a solvent, and sequentially oscillating, centrifuging, filtering and drying; the solvent is one or more of trichloroethylene, kerosene and n-heptane; the content of the available rubber powder in the rubber asphalt is calculated according to the formula 1. According to the invention, by utilizing the property that the rubber powder in the rubber asphalt is hardly dissolved in the trichloroethylene, the kerosene and the n-heptane solvent, and the property that the asphalt is dissolved in the trichloroethylene, the kerosene and the n-heptane solvent, the content of the effective rubber powder in the rubber asphalt can be simply, conveniently and quickly obtained by calculating the mass percentage of the insoluble rubber powder in the asphalt and complementing the loss of the dissolving quality of the rubber powder in the solvent, thereby providing a basis for evaluating the quality of the rubber asphalt. The results of the examples show that the difference between the effective rubber powder content calculated by the detection method of the invention and the rubber powder content in the rubber asphalt standard is within-0.3%, which indicates that the detection method provided by the invention has good accuracy.
Detailed Description
The invention provides a method for detecting the content of effective rubber powder in rubber asphalt, which comprises the following steps:
mixing the rubber asphalt to be detected with a solvent, and sequentially oscillating, centrifuging, filtering and drying; the solvent is one or more of trichloroethylene, kerosene and n-heptane;
calculating the content of the effective rubber powder in the rubber asphalt according to the formula 1:
Figure BDA0003286633140000031
in the formula 1, omega is the content of the effective rubber powder in the rubber asphalt%
m 1 G, drying mass of centrifugal residual insoluble substances after centrifugation;
m 2 g is the total mass of the filtering equipment used for filtering;
m 3 g, filtering equipment after filtering and drying mass of residues;
m 0 g, measuring the mass of the rubber asphalt;
R 0 is the solubility of the rubber powder in a solvent.
In the invention, the content of the effective rubber powder in the rubber asphalt is the content by an internal mixing method.
In the invention, the rubber asphalt to be detected comprises asphalt and rubber powder. The invention does not require any particular kind of bitumen, and it is sufficient to use a bitumen of a kind well known to the person skilled in the art. In the invention, the rubber powder is preferably one or more of rubber powder of tires of large-sized vehicles and rubber powder of tires of small vehicles. In the invention, the content of the rubber powder in the rubber asphalt to be detected by an internal mixing method is preferably 13-20%, and more preferably 14-18%.
In the invention, the mass ratio of the rubber asphalt to be detected to the solvent is preferably 1: 50-100, and more preferably 1: 60-80.
In the present invention, the mixing is preferably performed under a condition of slight heating. In the invention, the mixing temperature is preferably 40-50 ℃, and more preferably 42-48 ℃; the time is preferably 0.5 to 1 hour, and more preferably 0.6 to 0.8 hour.
In the invention, the oscillation speed is preferably 200-500 r/min, more preferably 300-400 r/min, and the time is preferably 20-30 min, more preferably 20-25 min.
In the invention, the rotation speed of the centrifugation is preferably 500-2000 rpm, and more preferably 1000-1500 rpm.
In the present invention, the centrifugation further comprises: repeatedly centrifuging the liquid phase part obtained by centrifuging; the repeated centrifugation is performed for 1-2 times, and the time of single centrifugation is preferably 10-20 min, and more preferably 15 min.
In the present invention, when the number of the centrifugation is plural, the present invention combines the solids obtained after each centrifugation.
The invention has no special requirements on the drying mode, and the drying mode known by the technicians in the field can be used; in the invention, the drying temperature is preferably 100-110 ℃, and more preferably 105 ℃; the time is preferably 1 to 2 hours, and more preferably 1.5 hours.
In the present invention, the method for testing the solubility of the rubber powder in the solvent preferably comprises the following steps:
mixing rubber powder with a solvent, and sequentially oscillating, centrifuging, filtering and drying, wherein the solvent is one or more of trichloroethylene, kerosene and n-heptane;
the solubility of the rubber powder in the rubber asphalt is calculated according to the formula 2:
Figure BDA0003286633140000051
in the formula 2, R 0 Is the solubility of the rubber powder in a solvent,%;
M 0 g is the mass of the rubber powder raw material;
M 1 drying the residual insoluble substances after centrifugationDry mass, g;
M 2 g is the total mass of the filtering equipment used for filtering;
M 3 g is the filtration equipment after filtration and the drying mass of the residue.
In the invention, the rubber powder is preferably one or more of rubber powder for large vehicle tires and rubber powder for small vehicle tires. In the invention, the particle size of the rubber powder is preferably 30-80 meshes, and more preferably 40-70 meshes.
In the invention, the mass ratio of the rubber powder to the solvent is preferably 1: 50-100, and more preferably 1: 60-80.
In the present invention, the mixing is preferably performed under heating. In the invention, the mixing temperature is preferably 40-50 ℃, and more preferably 42-48 ℃; the time is preferably 0.5 to 1 hour, and more preferably 0.6 to 0.8 hour.
In the invention, the oscillation speed is preferably 200-500 r/min, more preferably 300-400 r/min, and the time is preferably 15-30 min, more preferably 20-25 min.
In the invention, the rotation speed of the centrifugation is preferably 500-2000 rpm, and more preferably 1000-1500 rpm.
In the present invention, the centrifugation further comprises: repeatedly centrifuging the liquid phase part obtained by centrifuging; the repeated centrifugation is performed for 1-2 times, and the time of single centrifugation is preferably 10-20 min, and more preferably 15 min.
In the present invention, when the number of times of centrifugation is plural, the present invention combines the solids obtained after each centrifugation.
The invention has no special requirements on the drying mode, and the drying mode known by the technicians in the field can be used; in the invention, the drying temperature is preferably 100-110 ℃, and more preferably 105 ℃; the time is preferably 2-3 h, and more preferably 2.5 h.
In the invention, the solubility of the rubber powder in trichloroethylene is preferably 4.87%; the solubility of the rubber powder in kerosene is preferably 3.22%; the solubility of the rubber powder in n-heptane is preferably 4.02%.
The following examples are provided to illustrate the method for detecting the content of the rubber powder in the rubber asphalt of the present invention in detail, but they should not be construed as limiting the scope of the present invention.
Example 1
3 solvents (kerosene, trichloroethylene and n-heptane) are selected to respectively dissolve rubber powder R (large vehicle tire rubber powder) and rubber asphalt AR. Wherein, the dissolving glue powder R comprises the following steps:
mass is M 0 The rubber powder and the solvent are mixed at the temperature of 45 ℃, the mass ratio of the rubber powder to the solvent is 1:50, the mixture is oscillated at the speed of 400r/min, and the insoluble substances are primarily separated and precipitated by a centrifuge (at the speed of 1500rpm) to obtain the drying mass M of the insoluble substances 1 Then filtering the mixture by using precise filtering equipment to respectively obtain the total mass M of the filtering equipment 2 Filtration equipment after filtration and residue drying quality M 3 Insoluble matter is considered as undissolved gum powder.
The solubility of the crumb rubber in the rubber asphalt was calculated according to equation 2.
Figure BDA0003286633140000061
The solubility of the gum powder in three different solvents is shown in table 1.
TABLE 1 solubility of the rubber powders in three different solvents
Figure BDA0003286633140000062
Figure BDA0003286633140000071
The rubber asphalt used in this example was 20% rubber powder as an external blend, and was 16.67% as an internal blend in terms of 20/(100+ 20).
The dissolving of the rubber asphalt AR comprises the following steps:
mass m 0 The rubber asphalt is mixed with a solvent at 45 ℃,the mass ratio of the rubber powder to the solvent is 1:50, the mixture is oscillated at the oscillating speed of 400r/min, and insoluble substances are obtained by preliminary separation and precipitation through a centrifuge (at the speed of 1500rpm) 1 And then obtaining the total mass m of the filtering equipment through the precise filtering equipment 2 Filtration equipment after filtration and residue drying mass m 3 Insoluble matter is considered as undissolved gum powder.
Calculating the content of the effective rubber powder in the rubber asphalt according to the formula 1:
Figure BDA0003286633140000072
the effective rubber powder content of the rubber asphalt internally doped with 16.67 wt% after being dissolved in three solvents is shown in Table 2.
TABLE 2 effective rubber powder content of rubber asphalt after dissolution in three solvents
Figure BDA0003286633140000073
Figure BDA0003286633140000081
After being dissolved by three solvents, the rubber powder has different dissolution degrees R in different solvents 0 (ii) a As can be seen from Table 2, when a certain amount of rubber asphalt is dissolved in different solvents, the calculated rubber powder mixing amounts are similar.
The mixing amount of the rubber powder dissolved in the solvent is definitely smaller than the standard mixing amount in the rubber asphalt, and the content of the residual rubber powder after direct dissolution is the content of the residual rubber powder after the rubber asphalt finished product is dissolved by the solvent. The effective rubber powder content is obtained by adding the residual rubber powder content and the dissolution loss of the rubber powder in a solvent, and the effective rubber powder content represents the rubber powder content which is actually contained in a rubber asphalt finished product and plays a role in forming a skeleton, and directly influences the performance of the rubber asphalt.
After the three solvents are dissolved, the content of the residual rubber powder of the obtained rubber asphalt is in the range of-1% of the designed doping amount, the content of the effective rubber powder obtained by further calculation is about-0.3% of the designed doping amount, and the dissipation of impurities such as water in the rubber powder in the rubber asphalt processing process is considered and is basically in the normal loss range.
Example 2
Selecting trichloroethylene as a solvent, and respectively taking 2 groups of rubber asphalt samples with different items to carry out rubber powder mixing amount detection. The calculation steps are the same as example 1, wherein the solubility of the rubber powder in trichloroethylene is 4.87%, and the test results are respectively obtained by carrying out parallel tests as follows:
Figure BDA0003286633140000082
the results of three groups of parallel tests have almost the same difference, and the average value is taken as the final effective rubber powder content within the test error range. The test method can quickly and quantitatively detect the mixing amount of the main modifier rubber powder in the rubber asphalt on site, thereby evaluating the performance of the asphalt to a certain extent. The low effective crumb content of sample B in example 2 suggests the user to be aware of the performance of this asphalt. Because the rubber powder is in the process of gradual dissolution reaction in the high-temperature storage of the rubber asphalt, when the effective rubber powder content is sampled and detected at different time, the overall change condition of the rubber asphalt can be pre-judged, and a user is guided to reasonably use the asphalt or judge the quality of the asphalt in an entrance so as to reduce the construction risk caused by the reduction of the asphalt performance.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.

Claims (2)

1. A method for detecting the content of effective rubber powder in rubber asphalt comprises the following steps:
mixing the rubber asphalt to be detected with a solvent, and sequentially oscillating, centrifuging, filtering and drying; the solvent is one or more of trichloroethylene, kerosene and n-heptane;
the mass ratio of the rubber asphalt to be detected to the solvent is 1: 50-100;
the mixing is carried out under the condition of micro-heating, the temperature of the mixing is 40-50 ℃, and the time is 0.5-1 h;
the oscillation speed is 200-500 r/min; the oscillation time is 20-30 min;
the rotating speed of the centrifugation is 500-2000 rpm;
after the centrifugation, the method further comprises: repeatedly centrifuging the liquid phase part obtained by centrifuging; the repeated centrifugation is performed for 1-2 times, and the time of single centrifugation is 10-20 min;
the drying temperature is 100-110 ℃, and the drying time is 2-3 h;
calculating the content of the effective rubber powder in the rubber asphalt according to the formula 1:
Figure FDA0003749433780000011
in the formula 1, omega is the content of the effective rubber powder in the rubber asphalt%
m 1 G, drying mass of residual centrifugal insoluble substances after centrifugation;
m 2 mass of the filtration equipment used for filtration, g;
m 3 g, filtering equipment after filtering and drying mass of residues;
m 0 g, measuring the mass of the rubber asphalt;
R 0 the solubility of the rubber powder in a solvent is percent;
the method for testing the solubility of the rubber powder in the solvent comprises the following steps:
mixing rubber powder with a solvent, and sequentially oscillating, centrifuging, filtering and drying, wherein the solvent is one or more of trichloroethylene, kerosene and n-heptane;
the particle size of the rubber powder is 30-80 meshes;
the solubility of the crumb rubber in the rubber asphalt was calculated according to formula 2:
Figure FDA0003749433780000012
in the formula 2, R 0 The solubility of the rubber powder in a solvent is percent;
M 0 the mass of the rubber powder raw material is g;
M 1 g, drying mass of centrifugal residual insoluble substances after centrifugation;
M 2 mass of the filtration equipment used for filtration, g;
M 3 g is the filtration equipment after filtration and the drying mass of the residue.
2. The detection method according to claim 1, wherein the rubber powder has a solubility of 4.87% in trichloroethylene;
the solubility of the rubber powder in kerosene is 3.22%;
the rubber powder has a solubility of 4.02% in n-heptane.
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CN103645106B (en) * 2013-11-18 2016-03-23 江苏省交通科学研究院股份有限公司 A kind of quality detecting method of SBS modified bitumen
CN107389494B (en) * 2017-06-28 2019-09-03 西安公路研究院 The measuring method of SBS content in SBS modified pitch
CN107389496B (en) * 2017-07-26 2020-08-14 河北省交通规划设计院 Method for rapidly determining effective rubber powder content of rubber powder modified asphalt
CN109346133A (en) * 2018-10-18 2019-02-15 长安大学 The method for determining the best rubber type of rubber modified asphalt and best rubber volume
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