CN112198082A - Quantitative determination method for content of SBS modifier in SBS modified asphalt - Google Patents
Quantitative determination method for content of SBS modifier in SBS modified asphalt Download PDFInfo
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Abstract
A quantitative detection method for the content of SBS modifier in SBS modified asphalt comprises the following steps: (1) at mass m1Adding a solvent A into SBS modified asphalt, heating for dissolving, and quickly filtering; (2) heating and refluxing filter paper containing filter residues with a filtrate containing a solvent A, and washing the filter residues to obtain an SBS solution containing the solvent A; (3) distilling SBS solution containing solvent A, recovering solvent A, adding organic solvent B, stirring for dissolving, separating, and collecting residue; (4) adding filter paper containing filter residue after centrifugation into the solvent C, heating and refluxing, and cleaning SBS in the filter residue to obtain SBS solution containing the solvent C; (5) adding solvent D into SBS solution containing solvent C to separate out SBS with mass m2Collecting SBS modifier with quantitative filter paper, drying to constant weight, cooling, and weighing to obtain m3And calculating the content of the SBS modifier. The method has the advantages of simple operation, low cost and accurate and reliable measuring result.
Description
Technical Field
The invention relates to the application field of SBS modified asphalt, in particular to a quantitative determination method for the content of SBS modifier in SBS modified asphalt.
Background
Asphalt is used as one of the oldest engineering materials, and the two main purposes are to be used as a cementing material of mineral aggregate and a roof waterproof coiled material in road engineering. Asphalt pavement is a common form of road pavement, and although the content of asphalt in asphalt mixture is small, its properties greatly affect the use performance of asphalt pavement. SBS is polystyrene thermoplastic elastomer, and has rubber-like polybutadiene chain segment (PB segment) and glass-like polystyrene chain segment (PS segment), so that it has the solubility and thermoplasticity of thermoplastic plastics, the flexibility and resilience of rubber, and the advantages of good elasticity, high tensile strength and good low-temperature deformation performance. The SBS is used as the asphalt modifier, so that the high-temperature stability and the low-temperature crack resistance of the asphalt can be improved, the service performance of the asphalt pavement is improved, and the asphalt pavement can be more suitable for increasingly heavy traffic loads.
There are many factors that affect the properties of SBS modified asphalt (SBSMA). For example, the configuration, the block ratio, the type of the base asphalt and the preparation method of the SBS modified asphalt all have great influence on the road performance of SBS modification, but the content of the modifier is a decisive factor influencing the performance of the modified asphalt, and the performance of the SBS modified asphalt increases with the increase of the mixing amount of the SBS modifier within a certain range. However, the cost of the modified asphalt is increased along with the increase of the content of the SBS modifier due to the high price of the SBS modifier. In order to prevent the phenomenon that the SBS modified asphalt does not reach the preset service performance and the pavement is damaged due to the fact that modified asphalt manufacturers save cost and reduce the using amount of the modifier, it is necessary to research a method for conveniently, quickly and efficiently detecting the content of the SBS modifier. Currently, the existing methods for detecting the content of the SBS modifier comprise an infrared spectroscopy method, a fluorescence microscopy analysis method, a gel permeation chromatography method, a thermogravimetric analysis method and a chemical and potentiometric titration method. In the infrared spectroscopy, due to the determination of the base line, the influence of atmospheric interference and the influence of the smoothing process on the calculated area of the target peak, a large error is generated in the actual use process. Both the fluorescence microscopy and the gel permeation chromatography have the phenomenon of fuzzy two phases of an asphalt phase and a modifier phase, and a large error exists in area calculation. The thermogravimetric analysis method is accurate only when the mixing amount of the SBS modified asphalt is 3-5%, and is generally only suitable for qualitative analysis. Both the chemical titration method and the potentiometric titration method are only suitable for the SBS modifier with the known structure, and the application range is limited. In summary, the existing methods for determining the content of the modifier in the SBS modified asphalt either lack accuracy or have great limitations on the type and configuration of the modifier. Therefore, it is very necessary to develop a convenient and fast measuring method with high precision for application in road engineering.
Disclosure of Invention
The invention aims to solve the technical problem of providing a method for quantitatively determining the content of SBS modifier in SBS modified asphalt, which is convenient and rapid, high in precision, simple to operate and low in cost.
The invention adopts the technical scheme that the quantitative determination method for the content of the SBS modifier in the SBS modified asphalt comprises the following steps:
(1) at mass m1Adding a solvent A into SBS modified asphalt, heating for dissolving, and quickly filtering;
(2) heating and refluxing filter paper containing filter residues with a filtrate containing a solvent A, and washing the filter residues to obtain an SBS solution containing the solvent A;
(3) distilling SBS solution containing solvent A, recovering solvent A, adding organic solvent B, stirring for dissolving, separating, and collecting residue;
(4) adding filter paper containing filter residue after centrifugation into the solvent C, heating and refluxing, and cleaning SBS in the filter residue to obtain SBS solution containing the solvent C;
(5) adding solvent D into SBS solution containing solvent C to separate out SBS with mass m2Collecting SBS modifier by quantitative filter paper, drying to constant weight, cooling, weighing to obtain mass m of filter paper and SBS3Calculating the content of the SBS modifier as follows: (m)3-m2）/m1×100%。
In the invention, the SBS modifier is obtained mainly through the solubility separation of the solvents A, B, C and D, namely the solvent A completely dissolves SBS but not asphaltene completely in a heating state so as to separate SBS from asphaltene, the solvent B completely does not dissolve SBS but can dissolve part of the asphaltene (the asphaltene A) so as to separate SBS from the asphaltene A, and the solvent C can completely dissolve SBS but does not dissolve the rest of the asphaltene B so as to separate SBS from the asphaltene B. The polarity of the solvent C can be adjusted by the solvent D, so that SBS is separated out from the solvent C, and the content of SBS modifier is quantitatively determined.
In the present invention, the solvent A is selected so that SBS and the saturated components, aromatic components and colloidal components (called as soft asphaltene) are sufficiently dissolved, but completely insoluble asphaltene.
Further, in the step (1), the solvent A is n-heptane or petroleum ether, which can better fully dissolve SBS, saturated components, aromatic components and colloid.
Further, in the step (2), the heating reflux conditions include: the heating temperature is 110-120 ℃, the heating time is 30-40 min, residual SBS, saturated components, aromatic components and colloid in the filter residue can be removed well, and SBS and asphaltene are separated thoroughly.
In the present invention, the solvent B is selected so as to separate SBS from a portion of the maltenes (maltenes A).
Further, in the step (3), the solvent B is n-hexane or 120# gasoline, so that SBS can be well separated from the maltene A.
In the present invention, the solvent C is selected so as to separate SBS from a portion of the soft asphaltene (soft asphaltene B).
Further, in the step (4), the solvent C is diethyl ether, so that SBS can be well separated from the soft asphaltene B.
Further, in the step (4), the heating reflux conditions include: the heating temperature is 70-80 ℃, the heating time is 60-90 min, SBS in the filter residue can be completely dissolved, and SBS and the soft asphalt B are thoroughly separated.
In the present invention, the solvent D is selected so as to change the polarity of the solvent C and separate SBS from the solvent C.
Further, in the step (5), the solvent D is at least one of acetone, water, formaldehyde and absolute ethyl alcohol, and the polarity of ethyl ether can be preferably changed, so that SBS is separated from the ethyl ether.
Compared with the prior art, the invention has the following beneficial effects:
1. the invention has lower requirements on experimental instruments and fields, can automatically detect according to the mode of the invention only by simple instruments and chemical reagents, and can obviously reduce the detection cost.
2. The invention has no limit to the structure, the block ratio, the molecular weight and the type of the matrix asphalt of the SBS, can carry out extraction experiments, and has accurate and reliable experimental results.
3. The determination method is suitable for SBS modified asphalt with any mixing amount.
Detailed Description
The present invention will be described in detail below by way of examples. In the following examples, the experimental apparatus: an electric heating jacket, a spherical condenser, a ground flask, a Soxhlet extractor, a rotary evaporator, a vacuum drying oven, an ultrasonic cleaning instrument, a centrifuge, filter paper, an analytical balance, a measuring cylinder and a glass funnel. Experimental reagent: n-heptane (analytical grade), petroleum ether (analytical grade), diethyl ether (analytical grade), n-hexane (analytical grade), 120# gasoline (industrial grade), acetone (analytical grade), formaldehyde (analytical grade), ethanol (analytical grade), distilled water.
Unless otherwise specified, commercially available instruments were used for the above-mentioned apparatuses, and commercially available products were used for the above-mentioned raw materials.
Example 1
A quantitative determination method for the content of SBS modifier in SBS modified asphalt comprises the following steps: (1) preparing SBS modified asphalt: adding SBS modifier with 2% of mixing amount, shearing at 175 deg.C for 40min with high speed shearing apparatus, and stirring with paddle stirrer for 2 h;
(2) weighing SBS modified asphalt with mass of 1 (+ -0.1) g, and recording the mass as mass m1Accurate to 0.1mg, placed in a flask (named No. 1), added with 60ml of organic solvent A (n-heptane), heated for 0.5h to dissolve, filtered quickly with filter paper, and rinsed with 30ml of hot n-heptane solution in flask 1;
(3) taking down and folding the filter paper, putting the filter paper into a Soxhlet extractor, connecting a No. 1 flask and the Soxhlet extractor with a condenser pipe, heating the flask and the Soxhlet extractor at 110 ℃ for 1 hour, heating and refluxing the n-heptane solution, and repeatedly washing the filter paper until the solution in the extractor is colorless, thereby obtaining a solution of the soft asphalt and SBS;
(4) removing n-heptane in the No. 1 flask by using a rotary evaporator, and putting the flask in a vacuum drying oven to volatilize the n-heptane until the weight of the flask is constant, wherein the solid in the flask is soft asphaltene (saturated component, aromatic component and colloid) and SBS; adding 60ml of solvent B (n-hexane) into a No. 1 flask, oscillating for 10min by using an ultrasonic cleaning instrument to promote the soluble components in the soft asphalt to be completely dissolved, separating by using a centrifugal machine until the centrifugal liquid is colorless, and collecting the filter residue after centrifugation to obtain SBS and the insoluble matter of the soft asphalt;
(5) taking down filter paper containing SBS and soft asphaltene indissolvable substances, folding and placing the filter paper into a Soxhlet extractor, placing 60ml of solvent C (ether) into a No. 2 flask, connecting the No. 2 flask with the Soxhlet extractor and a condenser tube, heating to heat and reflux the ether, and repeatedly washing the filter paper for 1h to obtain ether solution containing SBS;
(6) adding solvent D (acetone) into the ether solution containing SBS until no precipitate is separated out, wherein the precipitate is SBS with known mass m2After the SBS modifier is collected by the filter paper, the filter paper is dried to constant weight and weighed, and the mass m of the filter paper and the SBS is obtained3. Calculating the content of the SBS modifier in the SBS modified asphalt as follows: (m)3-m2）/m1X 100%, wherein m1M is the SBS modified asphalt mass2Mass of filter paper, m3The mass sum of the filter paper and the SBS modifier;
and (4) carrying out three parallel experiments according to the steps (2) to (6), and taking an average value of the obtained results.
Example 2
A quantitative determination method for the content of SBS modifier in SBS modified asphalt comprises the following steps:
(1) preparing SBS modified asphalt: adding SBS modifier with 2% of mixing amount, shearing at 180 deg.C for 40min with high speed shearing apparatus, and stirring with paddle stirrer for 2 h;
(2) weighing SBS modified asphalt with mass of 1 (+ -0.1) g, and recording the mass as mass m1Accurate to 0.1mg, placing into a flask (named as No. 1), adding 60ml of organic solvent A (petroleum ether), heating for 0.5h to dissolve, filtering with filter paper rapidly, and washing No. 1 flask with 30ml of hot petroleum ether solution for filtering;
(3) taking down and folding the filter paper, putting the filter paper into a Soxhlet extractor, connecting a No. 1 flask and the Soxhlet extractor with a condenser pipe, heating the flask and the Soxhlet extractor at 110 ℃ for 1 hour, heating and refluxing the petroleum ether solution, and repeatedly washing the filter paper until the solution in the extractor is colorless, thereby obtaining a solution of the soft asphalt and SBS;
(4) removing petroleum ether in the No. 1 flask by using a rotary evaporator, and putting the flask in a vacuum drying box to volatilize the petroleum ether until the weight of the flask is constant, wherein the solid in the flask is soft asphaltene and SBS; adding 60ml of solvent B (120 # gasoline) into a No. 1 flask, oscillating for 10min by using an ultrasonic cleaning instrument to promote the soluble components in the soft asphalt to be completely dissolved, separating by using a centrifugal machine until the centrifugal liquid is colorless, and collecting filter residues after centrifugation to obtain SBS and the insoluble matter of the soft asphalt;
(5) taking down filter paper containing SBS and soft asphaltene indissolvable substances, folding and placing the filter paper into a Soxhlet extractor, placing 60ml of solvent C (ether) into a No. 2 flask, connecting the No. 2 flask with the extractor and a condenser pipe, heating to heat and reflux the ether, and repeatedly washing the filter paper for 1h to obtain ether solution containing SBS;
(6) adding solvent D (absolute ethyl alcohol) into the ether solution containing SBS until no precipitate is separated out, wherein the precipitate is SBS with the known mass m2After the SBS modifier is collected by the filter paper, the filter paper is dried to constant weight and weighed, and the mass m of the filter paper and the SBS is obtained3. Calculating the content of the SBS modifier in the SBS modified asphalt as follows: (m)3-m2）/m1X 100%, wherein m1M is the SBS modified asphalt mass2Mass of filter paper, m3The mass sum of the filter paper and the SBS modifier;
(7) and (4) carrying out three parallel experiments according to the steps (2) to (6), and taking an average value of the obtained results.
Example 3
A quantitative determination method for the content of SBS modifier in SBS modified asphalt comprises the following steps:
(1) preparing SBS modified asphalt: adding 2% SBS modifier, shearing at 177 deg.C for 40min with high-speed shear apparatus, and stirring with paddle stirrer for 2 hr;
(2) weighing SBS modified asphalt with mass of 1 (+ -0.1) g, and recording the mass as mass m1Accurate to 0.1mg, placed in a flask (named No. 1), added with 60ml of organic solvent A (n-heptane), heated for 0.5h to dissolve it, filtered quickly with filter paper, and filtered by rinsing No. 1 flask with 30ml of hot n-heptane solution;
(3) taking down and folding the filter paper, putting the filter paper into a Soxhlet extractor, connecting a No. 1 flask and the Soxhlet extractor with a condenser pipe, heating the flask and the Soxhlet extractor at 110 ℃ for 1 hour, heating and refluxing the n-heptane solution, and repeatedly washing the filter paper until the solution in the extractor is colorless, thereby obtaining a solution of the soft asphalt and SBS;
(4) removing n-heptane in the No. 1 flask by using a rotary evaporator, and putting the flask in a vacuum drying box to volatilize the n-heptane until the weight of the flask is constant, wherein the solid in the flask is the soft asphaltene and SBS; adding 60ml of solvent B (120 # gasoline) into a No. 1 flask, oscillating for 10min by using an ultrasonic cleaning instrument to promote the soluble components in the soft asphalt to be completely dissolved, separating by using a centrifugal machine until the centrifugal liquid is colorless, and collecting filter residues after centrifugation to obtain SBS and the insoluble matter of the soft asphalt;
(5) taking down filter paper containing SBS and soft asphaltene indissolvable substances, folding and placing the filter paper into a Soxhlet extractor, placing 60ml of solvent C (ether) into a No. 2 flask, connecting the No. 2 flask with the extractor and a condenser pipe, heating to heat and reflux the ether, and repeatedly washing the filter paper for 1h to obtain ether solution containing SBS;
(6) adding into ethyl ether solution containing SBSSolvent D (formaldehyde) until no precipitate is precipitated, the precipitate being SBS, passing through a known mass m2After the SBS modifier is collected by the filter paper, the filter paper is dried to constant weight and weighed, and the mass m of the filter paper and the SBS is obtained3. Calculating the content of the SBS modifier in the SBS modified asphalt as follows: (m)3-m2）/m1X 100%, wherein m1M is the SBS modified asphalt mass2Mass of filter paper, m3The mass sum of the filter paper and the SBS modifier;
(7) and (4) carrying out three parallel experiments according to the steps (2) to (6), and taking an average value of the obtained results.
TABLE 1 SBS modified asphalt sample test results with 2% blend
Example 4
A quantitative determination method for the content of SBS modifier in SBS modified asphalt comprises the following steps: (1) preparing SBS modified asphalt: adding SBS modifier with the mixing amount of 4%, shearing for 40min at 175 ℃ by using a high-speed shearing instrument, and stirring for 2h by using a paddle stirrer;
(2) weighing SBS modified asphalt with mass of 1 (+ -0.1) g, and recording the mass as mass m1Accurate to 0.1mg, placing into a flask (named as No. 1), adding 60ml of organic solvent A (petroleum ether), heating for 0.5h to dissolve, filtering with filter paper rapidly, and washing No. 1 flask with 30ml of hot petroleum ether solution for filtering;
(3) taking down and folding the filter paper, putting the filter paper into a Soxhlet extractor, connecting a No. 1 flask and the Soxhlet extractor with a condenser pipe, heating the flask and the Soxhlet extractor at 110 ℃ for 1 hour, heating and refluxing the petroleum ether solution, and repeatedly washing the filter paper until the solution in the extractor is colorless, thereby obtaining a solution of the soft asphalt and SBS;
(4) removing petroleum ether in the No. 1 flask by using a rotary evaporator, and putting the flask in a vacuum drying box to volatilize the petroleum ether until the weight of the flask is constant, wherein the solid in the flask is soft asphaltene and SBS; adding 60ml of solvent B (n-hexane) into a No. 1 flask, oscillating for 10min by using an ultrasonic cleaning instrument to promote the soluble components in the soft asphalt to be completely dissolved, separating by using a centrifugal machine until the centrifugal liquid is colorless, and collecting the filter residue after centrifugation to obtain SBS and the insoluble matter of the soft asphalt;
(5) taking down filter paper containing SBS and soft asphaltene indissolvable substances, folding and placing the filter paper into a Soxhlet extractor, placing 60ml of solvent C (ether) into a No. 2 flask, connecting the No. 2 flask with the extractor and a condenser pipe, heating to heat and reflux the ether, and repeatedly washing the filter paper for 1h to obtain ether solution containing SBS;
(6) adding solvent D (water) into the ether solution containing SBS until no precipitate is separated out, wherein the precipitate is SBS with known mass m2After the SBS modifier is collected by the filter paper, the filter paper is dried to constant weight and weighed, and the mass m of the filter paper and the SBS is obtained3. Calculating the content of the SBS modifier in the SBS modified asphalt as follows: (m)3-m2）/m1X 100%, wherein m1M is the SBS modified asphalt mass2Mass of filter paper, m3The mass sum of the filter paper and the SBS modifier;
(7) and (4) carrying out three parallel experiments according to the steps (2) to (6), and taking an average value of the obtained results.
Example 5
A quantitative determination method for the content of SBS modifier in SBS modified asphalt comprises the following steps: (1) preparing SBS modified asphalt: adding SBS modifier with the mixing amount of 4%, shearing for 40min at the temperature of 180 ℃ by using a high-speed shearing instrument, and stirring for 2h by using a paddle stirrer;
(2) weighing SBS modified asphalt with mass of 1 (+ -0.1) g, and recording the mass as mass m1Accurate to 0.1mg, placing into a flask (named as No. 1), adding 60ml of organic solvent A (petroleum ether), heating for 0.5h to dissolve, rapidly filtering with filter paper, and flushing No. 1 flask with 30ml of hot petroleum ether solution for filtering;
(3) taking down and folding the filter paper, putting the filter paper into a Soxhlet extractor, connecting a No. 1 flask and the Soxhlet extractor with a condenser pipe, heating the flask and the Soxhlet extractor at 110 ℃ for 1 hour, heating and refluxing the petroleum ether solution, and repeatedly washing the filter paper until the solution in the extractor is colorless, thereby obtaining a solution of the soft asphalt and SBS;
(4) removing petroleum ether in the No. 1 flask by using a rotary evaporator, and putting the flask in a vacuum drying box to volatilize the petroleum ether until the weight of the flask is constant, wherein the solid in the flask is soft asphaltene and SBS; adding 60ml of solvent B (120 # gasoline) into a No. 1 flask, oscillating for 10min by using an ultrasonic cleaning instrument to promote the soluble components in the soft asphalt to be completely dissolved, separating by using a centrifugal machine until the centrifugal liquid is colorless, and collecting filter residues after centrifugation to obtain SBS and the insoluble matter of the soft asphalt;
(5) taking down filter paper containing SBS and soft asphaltene indissolvable substances, folding and placing the filter paper into a Soxhlet extractor, placing 60ml of solvent C (ether) into a No. 2 flask, connecting the No. 2 flask with the Soxhlet extractor and a condenser tube, heating and refluxing the ether, and repeatedly washing the filter paper for 1h to obtain ether solution containing SBS;
(6) adding solvent D (formaldehyde) into the ether solution containing SBS until no precipitate is separated out, wherein the precipitate is SBS with known mass m2After the SBS modifier is collected by the filter paper, the filter paper is dried to constant weight and weighed, and the mass m of the filter paper and the SBS is obtained3. Calculating the content of the SBS modifier in the SBS modified asphalt as follows: (m)3-m2）/m1X 100%, wherein m1M is the SBS modified asphalt mass2Mass of filter paper, m3The mass sum of the filter paper and the SBS modifier;
(7) and (4) carrying out three parallel experiments according to the steps (2) to (6), and taking an average value of the obtained results.
Example 6
A quantitative determination method for the content of SBS modifier in SBS modified asphalt comprises the following steps: (1) preparing SBS modified asphalt: adding SBS modifier with the mixing amount of 4%, shearing for 40min at 178 ℃ by using a high-speed shearing instrument, and stirring for 2h by using a paddle stirrer;
(2) weighing SBS modified asphalt with mass of 1 (+ -0.1) g, and recording the mass as mass m1To an accuracy of 0.1mg, placed in a flask (named No. 1), added with 60ml of organic solvent A (n-heptane), heated for 0.5h to dissolve it, and quickly filtered using filter paperFiltering, and flushing the flask No. 1 with 30ml of hot n-heptane solution for filtering;
(3) taking down and folding the filter paper, putting the filter paper into a Soxhlet extractor, connecting a No. 1 flask and the Soxhlet extractor with a condenser pipe, heating the flask and the Soxhlet extractor at 110 ℃ for 1 hour, heating and refluxing the n-heptane solution, and repeatedly washing the filter paper until the solution in the extractor is colorless, thereby obtaining a solution of the soft asphalt and SBS;
(4) removing n-heptane in the No. 1 flask by using a rotary evaporator, and putting the flask in a vacuum drying box to volatilize the n-heptane until the weight of the flask is constant, wherein the solid in the flask is the soft asphaltene and SBS; adding 60ml of solvent B (n-hexane) into a No. 1 flask, oscillating for 10min by using an ultrasonic cleaning instrument to promote the soluble components in the soft asphalt to be completely dissolved, separating by using a centrifugal machine until the centrifugal liquid is colorless, and collecting the filter residue after centrifugation to obtain SBS and the insoluble matter of the soft asphalt;
(5) taking down filter paper containing SBS and soft asphaltene indissolvable substances, folding and placing the filter paper into a Soxhlet extractor, placing 60ml of solvent C (ether) into a No. 2 flask, connecting the No. 2 flask with the Soxhlet extractor and a condenser tube, heating and refluxing the ether, and repeatedly washing the filter paper for 1h to obtain ether solution containing SBS;
(6) adding solvent D-formaldehyde into ethyl ether solution containing SBS until no precipitate is separated out, wherein the precipitate is SBS with known mass m2After the SBS modifier is collected by the filter paper, the filter paper is dried to constant weight and weighed, and the mass m of the filter paper and the SBS is obtained3. Calculating the content of the SBS modifier in the SBS modified asphalt as follows: (m)3-m2）/m1X 100%, wherein m1M is the SBS modified asphalt mass2Mass of filter paper, m3The mass sum of the filter paper and the SBS modifier;
(7) and (4) carrying out three parallel experiments according to the steps (2) to (6), and taking an average value of the obtained results.
TABLE 2 SBS modified asphalt sample test results with 4% blend
Example 7
A quantitative determination method for the content of SBS modifier in SBS modified asphalt comprises the following steps: (1) preparing SBS modified asphalt: adding SBS modifier with 6% of mixing amount, shearing at 175 deg.C for 40min with high speed shearing apparatus, and stirring with paddle stirrer for 2 h;
(2) weighing SBS modified asphalt with mass of 1 (+ -0.1) g, and recording the mass as mass m1Accurate to 0.1mg, placing into a flask (named as No. 1), adding 60ml of organic solvent A (petroleum ether), heating for 0.5h to dissolve, filtering with filter paper rapidly, and washing No. 1 flask with 30ml of hot petroleum ether solution for filtering;
(3) taking down and folding the filter paper, putting the filter paper into a Soxhlet extractor, connecting a No. 1 flask and the Soxhlet extractor with a condenser pipe, heating the flask and the Soxhlet extractor at 110 ℃ for 1 hour, heating and refluxing the petroleum ether solution, and repeatedly washing the filter paper until the solution in the extractor is colorless, thereby obtaining a solution of the soft asphalt and SBS;
(4) removing petroleum ether in the No. 1 flask by using a rotary evaporator, and putting the flask in a vacuum drying box to volatilize the petroleum ether until the weight of the flask is constant, wherein the solid in the flask is soft asphaltene and SBS; adding 60ml of solvent B (120 # gasoline) into a No. 1 flask, oscillating for 10min by using an ultrasonic cleaning instrument to promote the soluble components in the soft asphalt to be completely dissolved, separating by using a centrifugal machine until the centrifugal liquid is colorless, and collecting filter residues after centrifugation to obtain SBS and the insoluble matter of the soft asphalt;
(5) taking down filter paper containing SBS and soft asphaltene indissolvable substances, folding and placing the filter paper into a Soxhlet extractor, placing 60ml of solvent C (ether) into a No. 2 flask, connecting the No. 2 flask with the Soxhlet extractor and a condenser tube, heating and refluxing the ether, and repeatedly washing the filter paper for 1h to obtain ether solution containing SBS;
(6) adding solvent D (acetone) into the ether solution containing SBS until no precipitate is separated out, wherein the precipitate is SBS with known mass m2After the SBS modifier is collected by the filter paper, the filter paper is dried to constant weight and weighed, and the mass m of the filter paper and the SBS is obtained3. Calculating the content of the SBS modifier in the SBS modified asphalt as follows: (m)3-m2）/m1X 100%, wherein m1M is the SBS modified asphalt mass2Mass of filter paper, m3The mass sum of the filter paper and the SBS modifier;
(7) and (4) carrying out three parallel experiments according to the steps (2) to (6), and taking an average value of the obtained results.
Example 8
A quantitative determination method for the content of SBS modifier in SBS modified asphalt comprises the following steps: (1) preparing SBS modified asphalt: adding SBS modifier with 6% of mixing amount, shearing at 180 deg.C for 40min with high speed shearing apparatus, and stirring with paddle stirrer for 2 h;
(2) weighing SBS modified asphalt with mass of 1 (+ -0.1) g, and recording the mass as mass m1Accurate to 0.1mg, placing into a flask (named as No. 1), adding 60ml of organic solvent A (petroleum ether), heating for 0.5h to dissolve, filtering with filter paper rapidly, and washing No. 1 flask with 30ml of hot petroleum ether solution for filtering;
(3) taking down and folding the filter paper, putting the filter paper into a Soxhlet extractor, connecting a No. 1 flask and the Soxhlet extractor with a condenser pipe, heating the flask and the Soxhlet extractor at 110 ℃ for 1 hour, heating and refluxing the petroleum ether solution, and repeatedly washing the filter paper until the solution in the extractor is colorless, thereby obtaining a solution of the soft asphalt and SBS;
(4) removing petroleum ether in the No. 1 flask by using a rotary evaporator, and putting the flask in a vacuum drying box to volatilize the petroleum ether until the weight of the flask is constant, wherein the solid in the flask is soft asphaltene and SBS; adding 60ml of solvent B (n-hexane) into a No. 1 flask, oscillating for 10min by using an ultrasonic cleaning instrument to promote the soluble components in the soft asphalt to be completely dissolved, separating by using a centrifugal machine until the centrifugal liquid is colorless, and collecting the filter residue after centrifugation to obtain SBS and the insoluble matter of the soft asphalt;
(5) taking down filter paper containing SBS and soft asphaltene indissolvable substances, folding and placing the filter paper into a Soxhlet extractor, placing 60ml of solvent C (ether) into a No. 2 flask, connecting the No. 2 flask with the Soxhlet extractor and a condenser tube, heating and refluxing the ether, and repeatedly washing the filter paper for 1h to obtain ether solution containing SBS;
(6) adding solvent D (absolute ethyl alcohol) into the ether solution containing SBS until no precipitate is separated out, wherein the precipitate is SBS with the known mass m2After the SBS modifier is collected by the filter paper, the filter paper is dried to constant weight and weighed, and the mass m of the filter paper and the SBS is obtained3. Calculating the content of the SBS modifier in the SBS modified asphalt as follows: (m)3-m2）/m1X 100%, wherein m1M is the SBS modified asphalt mass2Mass of filter paper, m3The mass sum of the filter paper and the SBS modifier;
(7) and (4) carrying out three parallel experiments according to the steps (2) to (6), and taking an average value of the obtained results.
Example 9
A quantitative determination method for the content of SBS modifier in SBS modified asphalt comprises the following steps: (1) preparing SBS modified asphalt: adding SBS modifier with 6% of mixing amount, shearing at 176 deg.C for 40min with high speed shearing apparatus, and stirring with paddle stirrer for 2 h;
(2) weighing SBS modified asphalt with mass of 1 (+ -0.1) g, and recording the mass as mass m1Accurate to 0.1mg, placing into a flask (named as No. 1), adding 60ml of organic solvent A (petroleum ether), heating for 0.5h to dissolve, filtering with filter paper rapidly, and washing No. 1 flask with 30ml of hot petroleum ether solution for filtering;
(3) taking down and folding the filter paper, putting the filter paper into a Soxhlet extractor, connecting a No. 1 flask and the Soxhlet extractor with a condenser pipe, heating the flask and the Soxhlet extractor at 110 ℃ for 1 hour, heating and refluxing the petroleum ether solution, and repeatedly washing the filter paper until the solution in the extractor is colorless, thereby obtaining a solution of the soft asphalt and SBS;
(4) removing petroleum ether in the No. 1 flask by using a rotary evaporator, and putting the flask in a vacuum drying box to volatilize the petroleum ether until the weight of the flask is constant, wherein the solid in the flask is soft asphaltene and SBS; adding 60ml of solvent B (n-hexane) into a No. 1 flask, shaking for 10min by using an ultrasonic cleaning instrument to promote the soluble components in the soft asphalt to be completely dissolved, separating by using a centrifugal machine until the centrifugal liquid is colorless, and collecting filter residues after centrifugation to obtain SBS and the insoluble matter of the soft asphalt;
(5) taking down filter paper containing SBS and soft asphaltene indissolvable substances, folding and placing the filter paper into a Soxhlet extractor, placing 60ml of solvent C (ether) into a No. 2 flask, connecting the No. 2 flask with the Soxhlet extractor and a condenser tube, heating and refluxing the ether, and repeatedly washing the filter paper for 1h to obtain ether solution containing SBS;
(6) adding solvent D (distilled water) into the ether solution containing SBS until no precipitate is separated out, wherein the precipitate is SBS with known mass m2After the SBS modifier is collected by the filter paper, the filter paper is dried to constant weight and weighed, and the mass m of the filter paper and the SBS is obtained3. Calculating the content of the SBS modifier in the SBS modified asphalt as follows: (m)3-m2）/m1X 100%, wherein m1M is the SBS modified asphalt mass2Mass of filter paper, m3The mass sum of the filter paper and the SBS modifier;
(7) and (4) carrying out three parallel experiments according to the steps (2) to (6), and taking an average value of the obtained results.
TABLE 3 SBS modified asphalt sample test results with 6% blend
The preferred embodiments of the present invention have been described above in detail, but the present invention is not limited thereto. Within the scope of the technical idea of the invention, many simple modifications can be made to the technical solution of the invention, including combinations of various technical features in any other suitable way, and these simple modifications and combinations should also be regarded as the disclosure of the invention, and all fall within the scope of the invention.
Claims (7)
1. A quantitative determination method for the content of SBS modifier in SBS modified asphalt is characterized by comprising the following steps:
(1) at mass m1Adding a solvent A into SBS modified asphalt, heating for dissolving, and quickly filtering;
(2) heating and refluxing filter paper containing filter residues with a filtrate containing a solvent A, and washing the filter residues to obtain an SBS solution containing the solvent A;
(3) distilling SBS solution containing solvent A, recovering solvent A, adding organic solvent B, stirring for dissolving, separating, and collecting residue;
(4) adding filter paper containing filter residues into the solvent C, heating and refluxing, and cleaning SBS in the filter residues to obtain SBS solution containing the solvent C;
(5) adding solvent D into SBS solution containing solvent C to separate out SBS with mass m2Collecting SBS modifier by quantitative filter paper, drying to constant weight, cooling, weighing to obtain mass m of filter paper and SBS3Calculating the content of the SBS modifier as follows: (m)3-m2）/m1×100%。
2. The quantitative determination method according to claim 1, wherein in step (1), the solvent A is n-heptane or petroleum ether.
3. The quantitative determination method according to claim 1, wherein in the step (2), the conditions of the heating reflux include: the heating temperature is 110-120 ℃, and the heating time is 30-40 min.
4. The quantitative determination method according to claim 1, wherein in the step (3), the solvent B is n-hexane or 120# gasoline.
5. The quantitative determination method according to claim 1, wherein in step (4), the solvent C is diethyl ether.
6. The quantitative determination method according to claim 1, wherein in the step (4), the conditions of the heating reflux include: the heating temperature is 70-80 ℃, and the heating time is 60-90 min.
7. The quantitative determination method according to claim 1, wherein in the step (5), the solvent D is at least one of acetone, water, formaldehyde and absolute ethanol.
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