Test analysis method for determining five components of coal-based modified asphalt

Abstract

The invention relates to a test analysis method for determining five components of coal-based modified asphalt. The method comprises the following steps: 1, pretreating a coal-based modified asphalt sample, and carrying out an n-heptane and toluene solvent separation process to obtain a toluene insoluble substance and asphaltene of the coal-based modified asphalt sample, and 2, wetting the obtained n-heptane with aluminum oxide; step 3, separating saturated components from the concentrated solution of the n-heptane solution in the step 1; step 4, separating aromatic components from the concentrated solution of the n-heptane solution in the step 1; step 5, separating colloid from the concentrated solution of the n-heptane solution in the step 1; step 6, removing the solvent from the toluene insoluble solution, the asphaltene solution, the colorless saturated solution, the yellow-dark brown aromatic solution and the dark brown-black colloid solution, and weighing until the weight is constant; and 7, calculating the contents of toluene insoluble, asphaltene, saturates, aromatics and colloids in the coal-based modified asphalt. The method can completely separate all components of the sample, and has the characteristics of simplicity and convenience in operation, good repeatability and wide adaptability.

Description

Technical Field

[0001] The invention relates to the technical field of material science analysis and detection, and in particular to an experimental analysis method for determining five components of coal-based modified asphalt. Background Art

[0002] In the modification research of coal-based asphalt, the four-component separation method is an important technical means, which mainly involves the chemical composition and microstructure theory of asphalt. Asphalt is usually divided into four basic components: saturated component (Sa), aromatic component (Ar), colloid (Re) and asphaltene (As). This classification helps to understand the physicochemical properties of asphalt and its performance in industrial applications. The four-component determination of coal-based modified asphalt not only helps to understand its chemical composition and physicochemical properties, but also has important significance for optimizing the performance and application of modified asphalt.

[0003] Coal-based modified asphalt is classified according to the group composition characteristics of the compounds: toluene insolubles, saturated fractions, aromatic fractions, colloids, and asphaltene. Toluene insolubles are composed of unreacted coal, catalysts, and inorganic minerals. There is no corresponding method for the four components of coal-based modified asphalt in the existing specifications and standards in my country. It is usually carried out according to the standard NB / SH / T 0509 heavy oil four-component determination method. 40g of activated alumina is filled in the glass adsorption column as an adsorbent, and a certain volume of solvent is added in turn to perform gradient elution on the sample. After separation and removal of the solvent, the corresponding components are obtained. This test process relies on natural gravity or artificial pressure to elute and separate components. The flow rate is not easy to control, and the elution end point of each component is visually observed, resulting in poor separation effect, low efficiency, and poor data stability and reliability. In addition, the test is time-consuming, the manual work intensity is high, and the artificial judgment of the separation point of each component is prone to component overlap. The end point of the solvent removal process is not uniform, which will increase the deviation of the repeatability of the data results of each component. Summary of the invention

[0004] In order to overcome the defects of the above-mentioned prior art, the purpose of the present invention is to provide an experimental analysis method for determining the five components of coal-based modified asphalt, which can completely separate the components of the sample, is easy to operate, has good repeatability and wide adaptability.

[0005] In order to achieve the above object, the technical solution adopted by the present invention is:

[0006] An experimental analysis method for determining five components of coal-based modified asphalt comprises the following steps:

[0007] Step 1: pretreating the coal-based modified asphalt sample;

[0008] Objective To make the coal-based modified asphalt sample uniform and reduce the sampling and weighing error.

[0009] Weigh the uniform coal-based modified asphalt sample and 0.1 μm nylon filter membrane after pretreatment, place the weighed sample in a clean centrifuge tube, add n-heptane, tighten the bottle cap and place it in an ultrasonic instrument for ultrasonic dispersion and dissolution, then place it in a high-speed centrifuge and centrifuge until the final n-heptane solution collected is colorless and transparent. At this time, the collected mixed n-heptane solution is a mixture of saturated fraction, aromatic fraction and colloid, which is concentrated to 10ml-15ml for standby use;

[0010] Add toluene to the residue in the centrifuge tube, disperse and dissolve it by ultrasonication, then put it into a high-speed centrifuge, centrifuge and filter, collect the toluene insoluble matter on the quantitative filter paper for later use;

[0011] Filtration process: Take the toluene insoluble matter collected by the quantitative filter paper and rinse it with toluene solvent in the glass filtration device, collect the toluene soluble solution in the centrifuge tube and the glass filtration device, this solution is the asphaltene solution;

[0012] The toluene insoluble content of the coal-based modified asphalt is calculated by weighing the filter membrane with toluene insoluble matter, drying and weighing.

[0013] Step 2, preparing the aluminum oxide adsorbent before analysis;

[0014] The purpose of this step and the effect it has on the final result is that the pore structure and specific surface area of ​​alumina are optimized, and the moisture of aluminum oxide is removed, thereby enhancing its adsorption performance and catalytic activity, which is crucial for the separation of the four components of coal-based modified asphalt samples.

[0015] Step 3: Separate the saturated fraction from the concentrated solution of the n-heptane solution (a mixture of saturated fraction, aromatic fraction and colloid) of step 1: Use the second flushing agent (n-heptane). The purpose of this step and the effect on the final result is to use the solubility characteristics of n-heptane to selectively elute the saturated fraction in the asphalt sample. n-heptane is a non-polar solvent that can dissolve saturated hydrocarbon compounds in asphalt, which are usually molecules with smaller molecular weight and lower polarity.

[0016] Step 4: Separate the aromatic component from the concentrated n-heptane solution of step 1 (a mixture of saturated component, aromatic component and colloid): use No. 3 flushing agent (n-heptane-dichloromethane); the purpose of this step and the effect on the final result are to effectively separate the aromatic component of coal-based modified asphalt. The mixed solvent can better adjust the solubility and selectivity, thereby improving the separation efficiency.

[0017] Step 5: Separate the colloid from the concentrated solution of the n-heptane solution (a mixture of saturated fraction, aromatic fraction and colloid) in step 1 by using No. 4 flushing agent (anhydrous ethanol-dichloromethane).

[0018] Step 6: Remove the solvent from the four ground-mouth Erlenmeyer flask solutions (asphaltene solution, saturated fraction solution, aromatic fraction solution, and colloid solution) that have been labeled after separation and weigh them to a constant weight.

[0019] Step 7: Calculate the toluene insoluble matter, asphaltenes, saturated fractions, aromatic fractions, and colloids of the coal-based modified asphalt.

[0020] The step 1 is specifically as follows:

[0021] 1) Heat the coal-based modified asphalt sample in an oven at 135°C-150°C to a fluid state and stir it thoroughly;

[0022] 2) Prepare n-heptane, toluene, dichloromethane, and anhydrous ethanol reagents (all reagents used are analytical grade) for use;

[0023] 3) Weighing samples: Weigh 0.9g-1.0g (accuracy: ±0.0001g) (marked as m1) and 0.1μm nylon filter membrane (accuracy: ±0.0001g) (marked as M0) of the uniform coal-based modified asphalt sample pretreated in step 1) respectively, place the weighed sample in a clean centrifuge tube, add 40ml-50ml of n-heptane at 65℃-70℃, tighten the bottle cap and place it in an ultrasonic instrument for ultrasonic dispersion and dissolution for 5min-10min; then place it in a high-speed centrifuge to The speed is 8000 rpm-10000 rpm, centrifuged for 5min-10min, and then taken out and allowed to stand for 5min-10min; the upper layer solution is collected in an ordinary conical flask, and this step is repeated 3-5 times until the final n-heptane solution collected is colorless and transparent. At this time, the mixed n-heptane solution collected is a mixture of saturated fraction, aromatic fraction, and colloid (marked m2), which is evaporated and concentrated to 10ml-15ml in a constant temperature water bath b with water circulation in a four-component separation device for standby use;

[0024] 4) Add 40ml-50ml of analytical pure toluene at a temperature of 60°C-70°C to the residue in the centrifuge tube of step 1) 3), and then ultrasonically oscillate for 5min-10min to disperse and dissolve it, and then put it into a high-speed centrifuge, centrifuge it at a speed of 8000 rpm-10000 rpm for 5min-10min, take it out and let it stand for 5min-10min; collect the upper toluene solution in a constant weight ground-mouth conical flask d; repeat this step until the collected toluene solution is colorless and transparent, pour the residue in the centrifuge tube into a funnel equipped with quantitative filter paper, place a constant weight ground-mouth conical flask d under the funnel, and after filtering, collect the toluene insoluble matter on the quantitative filter paper for standby use;

[0025] 5) Filtration: Take the toluene insoluble matter collected by the quantitative filter paper in step 1 (4) and rinse it with hot toluene solvent (No. 1 flushing agent) at a temperature of 60°C-70°C in a glass filtration device (using a 0.1μm nylon filter membrane) until the toluene solvent in the ground-mouth filtration bottle is colorless and clear after rinsing the sample (marked as m7). Collect the toluene soluble solution in the centrifuge tube and the glass filtration device in a constant weight ground-mouth conical flask d. This solution is an asphaltene solution, marked as m3;

[0026] 6) Remove the solvent: Place the filter membrane with toluene insoluble matter in a vacuum drying oven at a temperature of 105°C-110°C and a pressure of -0.1Mpa for 30 minutes. Weigh the filter membrane with toluene insoluble matter (marked M7) and calculate the toluene insoluble matter content of the coal-based modified asphalt.

[0027] The step 2 is specifically as follows:

[0028] 1) Activation of aluminum oxide: 100g-150g of neutral 100-200 mesh aluminum oxide for chromatography is activated in a muffle furnace at 450°C-500°C for 5.5h-6.5h, and after cooling, it is placed in a glass container, and 0.5%-1% of the mass of aluminum oxide is added in distilled water, shaken well, and allowed to stand for 24h-36h for use;

[0029] 2) Take 40g-45g of activated aluminum oxide and put it into the glass adsorption column a in the four-component separation device, use the sand core filter e as the aluminum oxide support, and gently tap the column with a leather hammer to make the aluminum oxide compact and uniform;

[0030] 3) Add 40ml-50ml of n-heptane to moisten the aluminum oxide in the glass adsorption column a to obtain n-heptane-soaked aluminum oxide, which is beneficial to improve the separation effect and reduce the operation time.

[0031] The step three is specifically as follows:

[0032] Transfer 10ml-15ml of the n-heptane concentrated solution obtained in step 3) to the glass adsorption column a, then add 80ml-100ml of analytical grade n-heptane to rinse the glass adsorption column a for 3-5 times, collect the rinsed concentrated solution in a conical flask, connect the constant weight ground-mouth conical flask d with a frosted mouth to the lower part of the frosted glass adsorption column, and then slowly pour the rinsed concentrated liquid into the glass adsorption column a; turn on the filtration device after 15min-30min, adjust the filtration speed to 1ml / min-2ml / min, stop filtration when the n-heptane in the glass adsorption column a is filtered until no liquid drips, and the constant weight ground-mouth conical flask d contains a colorless saturated solution, marked as m4.

[0033] The step 4 is specifically as follows:

[0034] Replace the constant weight ground-mouth conical flask d at the lower end of the glass adsorption column a, add 80ml-100ml of n-heptane-dichloromethane (1:1) into the glass adsorption column a, wait for 10min-20min, start the vacuum pump c with a pressure regulator for filtration, adjust the filtration speed to 2ml / min-3ml / min, and stop filtration when the toluene in the glass adsorption column a is filtered until no liquid drips. The constant weight ground-mouth conical flask d contains a yellow to dark brown aromatic solution, marked as m5.

[0035] The step five is specifically as follows:

[0036] Replace the constant weight ground-mouth conical flask d at the lower end of the glass adsorption column a, add 80ml-100ml of anhydrous ethanol-dichloromethane (1:1) into the glass adsorption column a, wait for 10min-20min, start the vacuum pump c with a pressure regulator for filtration, adjust the filtration speed to 2ml / min-3ml / min, and stop filtration when the toluene-ethanol in the glass adsorption column a is filtered until no liquid drips. The constant weight ground-mouth conical flask d contains a dark brown-black colloidal solution, marked as m6.

[0037] The step six is ​​specifically as follows:

[0038] Take the components of the solution in the ground-mouth conical flasks d marked as m3, m4, m5, and m6, and evaporate the solvent in a constant temperature water bath until the remaining solvent is 0.3ml-0.5ml. Put them into a vacuum drying oven at 105℃-110℃ and keep them at a negative pressure of 90Kpa-100Kpa for 1h-2h. After cooling in a desiccator for 20min-40min, weigh their masses respectively: M 3、 M 4、 M 5、 M6; then place it in a dryer and dry it for 20min-40min for constant weight check, until the difference between two consecutive weighings does not exceed 0.0005g, and the weighing accuracy is 0.0001g. The saturated content, aromatic content, gum and asphaltene are calculated by weighing.

[0039] The step seven is specifically as follows:

[0040] Calculate the specific content of each component based on the weighed sample mass:

[0041] Toluene insoluble matter: (M7-M0) / m1×100%; Asphaltene: M3 / m1×100%;

[0042] Saturated fraction: M4 / m1×100%; Aromatic fraction: M5 / m1×100%;

[0043] Colloid:M6 / m1×100%.

[0044] Beneficial effects of the present invention:

[0045] The four-component determination method for determining coal-based modified asphalt of the present invention can completely separate the components, is easy to operate, has good repeatability and wide adaptability.

[0046] 1) Through a coal-based modified asphalt sample analysis test, with the help of two experimental separation devices and four solvent flushing agents, the contents of five components of coal-based modified asphalt, including toluene insoluble matter, asphaltenes, saturated fractions, aromatic fractions, and colloids, can be obtained.

[0047] 2) The membrane used in the toluene insoluble device is a 0.1μm nylon filter membrane, which can effectively filter all aqueous solutions and most organic solvents, such as alcohols, hydrocarbons, ethers, lipids, ketones, etc. The organic solvents used in this experiment can be effectively filtered by a 0.1μm nylon filter membrane; literature data and experiments have shown that the use of a 0.1μm nylon filter membrane fully meets the requirements for intercepting the solid particle size of coal-based modified asphalt.

[0048] 3) In the four-component analysis experiment, the selection of a suitable mixed solvent is crucial to the success of the experiment. The experimenter needs to select a suitable solvent combination and ratio according to the properties of the substance to be tested and the analysis objectives to achieve the best separation effect. This paper uses mixed solvents No. 3 flushing agent (n-heptane-dichloromethane) and No. 4 flushing agent (anhydrous ethanol-dichloromethane) to separate aromatic components and colloids in coal-based modified asphalt. The experimental results show that the aromatic components and colloids are completely separated.

[0049] 4) By utilizing the polarity principle of the solvent and two sets of devices, the overlap between the components is completely blocked, ensuring that the five components are separated more thoroughly and without overlap. BRIEF DESCRIPTION OF THE DRAWINGS

[0050] Figure 1 Schematic diagram of the toluene insoluble separation device for coal-based modified asphalt.

[0051] Figure 2 Schematic diagram of the four-component separation device for coal-based modified asphalt. DETAILED DESCRIPTION

[0052] The present invention is further described in detail below in conjunction with embodiments.

[0053] Embodiment 1:

[0054] Step 1: Sample pretreatment:

[0055] 1) Heat the coal-based modified asphalt in an oven at 145°C to a fluid state and stir it thoroughly;

[0056] 2) Prepare n-heptane, toluene, dichloromethane, and anhydrous ethanol reagents (all reagents are analytical grade) for use; 10 ground-mouth conical flasks with constant weight;

[0057] 3) Weighing samples: Weigh 1.0075g and 0.9894g (marked m1) of the uniform coal-based modified asphalt sample treated in step 1 and a 0.1μm nylon filter membrane (accuracy of ±0.0001g) (marked M0), respectively, place the weighed sample in a clean centrifuge tube, add 50ml of n-heptane at 70°C, tighten the bottle cap and place it in an ultrasonic instrument for ultrasonic dispersion and dissolution for 5 minutes; then place it in a high-speed centrifuge, centrifuge at a speed of 10000 rpm for 10 minutes, take it out and let it stand for 5 minutes; collect the upper solution in an ordinary conical flask, repeat this step 5 times until the final n-heptane solution collected is colorless and transparent. At this time, the mixed n-heptane solution collected is a mixture of saturated fraction, aromatic fraction and colloid (marked m2), which is placed in a centrifuge tube. Figure 2 Evaporate and concentrate to 15 ml in a constant temperature water bath b with water circulation in a four-component separation device for later use;

[0058] 4) Add 50 ml of analytical pure toluene at 65°C to the residue in the centrifuge tube, then ultrasonically oscillate for 10 minutes to disperse and dissolve it, then put it into a high-speed centrifuge, centrifuge it at a speed of 10,000 rpm for 10 minutes, take it out and let it stand for 5 minutes; collect the upper toluene solution in a constant weight ground-mouth conical flask d; repeat this step until the collected toluene solution is colorless and transparent, pour the residue in the centrifuge tube into a funnel equipped with quantitative filter paper, place a constant weight ground-mouth conical flask d under the funnel, and after filtering, collect the toluene insoluble matter on the quantitative filter paper for standby use;

[0059] 5) Filtration: Take the toluene insoluble matter collected by the quantitative filter paper in step 1 (4) and Figure 1 The coal-based modified asphalt toluene insoluble separation device (using 0.1 μm nylon filter membrane) is flushed with hot toluene solvent (No. 1 flushing agent) at a temperature of 65°C until the toluene solvent flowing into the ground-mouth suction filtration bottle after the flushing sample is colorless and clear (marked as m7). The toluene soluble solution of the centrifuge tube and the glass suction filtration device is collected in a constant weight ground-mouth conical flask d. This solution is the asphaltene solution, marked as m3;

[0060] 6) Removal of solvent: Place the filter membrane with toluene insoluble matter in a vacuum drying oven at a temperature of 110°C and a pressure of -0.1Mpa for 30 minutes. Weigh the filter membrane with toluene insoluble matter (marked as M7) and calculate the toluene insoluble matter content of the coal-based modified asphalt.

[0061] Step 2: Preparation before analysis:

[0062] 1) Activation of aluminum oxide: 150 g of neutral 100-200 mesh aluminum oxide for chromatography was activated in a muffle furnace at 500°C for 6.5 h, and after cooling, it was placed in a glass container, and distilled water with a concentration of 1% by weight of aluminum oxide was added, and the mixture was shaken and allowed to stand for 24 h for use;

[0063] 2) Take 40g of activated aluminum oxide and put it into Figure 2 In the glass adsorption column a of the coal-based modified asphalt four-component separation device, the sand core filter e is used as the aluminum oxide support, and the column is gently tapped with a leather hammer to make the aluminum oxide compact and uniform;

[0064] 3) Add 50 ml of n-heptane to moisten the aluminum oxide in the glass adsorption column a and set aside for use.

[0065] Step 3: Separate the saturated fraction from the concentrated solution of the mixture of the saturated fraction, the aromatic fraction and the colloid (marked as m2): Use No. 2 flushing agent (n-heptane);

[0066] Transfer 15 ml of the n-heptane concentrate obtained in step 1) to Figure 2 The glass adsorption column a of the device was added with 100 ml of analytical pure n-heptane and rinsed into the glass adsorption column a for 5 times. The concentrated liquid after rinsing was collected in a conical flask. The constant weight ground-mouth conical flask d with a frosted mouth was connected to the lower part of the glass adsorption column with a frosted mouth, and then the concentrated liquid after rinsing was slowly poured into the glass adsorption column a. After 20 minutes, the filtration device was turned on and the filtration speed was adjusted to 1 ml / min. The n-heptane in the glass adsorption column a was filtered until no liquid was dripped and then the filtration was stopped. The constant weight ground-mouth conical flask d contained a colorless saturated solution, marked as m4.

[0067] Step 4: Separate the aromatic fraction from the concentrated solution of the mixture of saturated fraction, aromatic fraction and colloid (marked as m2) of the n-heptane solution: use No. 3 flushing agent (n-heptane-dichloromethane);

[0068] replace Figure 2 Add 80 ml of n-heptane-dichloromethane (1:1) into the constant weight ground-mouth flask d at the lower end of the glass adsorption column a of the device. After 10 minutes, start the vacuum pump c with a pressure regulator for filtration. Adjust the filtration speed to 2 ml / min. Stop filtration when the toluene in the glass adsorption column a is filtered until no liquid drips. The constant weight ground-mouth flask d contains a yellow-dark brown aromatic solution, marked as m5.

[0069] Step 5: Separate the colloid from the concentrated solution of the mixture of saturated fraction, aromatic fraction and colloid (marked as m2) of the n-heptane solution: use No. 4 flushing agent (anhydrous ethanol-dichloromethane);

[0070] replace Figure 2 Add 80 ml of anhydrous ethanol-dichloromethane (1:1) into the constant weight ground-mouth flask d at the lower end of the glass adsorption column a of the device. After 10 minutes, start the vacuum pump c with a pressure regulator for filtration. Adjust the filtration speed to 2 ml / min. Stop filtration when the toluene-ethanol in the glass adsorption column a is filtered until no liquid drips. The constant weight ground-mouth flask d contains a dark brown-black colloidal solution, marked as m6.

[0071] Step 6: Weigh to constant weight:

[0072] The components of the solution in the ground-mouth conical flasks d marked as m3, m4, m5, and m6 were evaporated in a constant temperature water bath until the solvent remained to 0.5 ml, and then placed in a vacuum drying oven at 110°C and a negative pressure of 90 KPa for 1 hour. After cooling in a desiccator for 30 minutes, their masses were weighed as follows: M 3、 M 4、 M 5、 M6; then place it in a dryer and dry it for 20 minutes for constant weight check, until the difference between two consecutive weighings does not exceed 0.0005g, and the weighing accuracy is 0.0001g. The saturated content, aromatic content, gum and asphaltene are calculated by weighing.

[0073] Step 7: Calculation:

[0074] Calculate the specific content of each component based on the weighed sample mass:

[0075] Toluene insoluble matter: (M7-M0) / m1×100%; Asphaltene: M3 / m1×100%;

[0076] Saturated fraction: M4 / m1×100%; Aromatic fraction: M5 / m1×100%;

[0077] Colloid:M6 / m1×100%.

[0078] Table 1. Content of five components of coal-based modified asphalt

[0079] Sample mass (g) 1#(1.0075) 2#(0.9894) average value Toluene insoluble content (% (wt)) 5.14 5.03 5.09 Asphaltene (% (wt)) 73.7 71.4 72.55 Saturated content (% (wt)) 0.76 0.89 1.21 Aromatic content (% (wt)) 4.01 4.15 4.08 Gel (% (wt)) 12.3 11.7 12.00

[0080] like Figure 1 As shown in FIG. 1 , the schematic diagram of the toluene insoluble separation device of coal-based modified asphalt consists of three parts: the first part (1-filter cup, 2-sand core filter head, 3-clamp, 4-filter bottle) is used as a filter sample unit; the second part (5-buffer bottle, 6-granular activated carbon, 7-vacuum regulating valve, 8-vacuum gauge) is used to absorb toluene solvent to prevent the solvent from entering the vacuum pump unit; the third part (9-connecting conduit, 10-vacuum pump) is used to provide a filter power unit. The 0.1μm nylon filter membrane is placed between the filter cup 1 and the sand core filter head 2, and then fixed with clamp 3. After the toluene insolubles of the coal-based modified asphalt sample are filtered, the nylon filter membrane with toluene insolubles is taken out, dried and constant weight is obtained, and the toluene insoluble content of the coal-based modified asphalt is calculated.

[0081] like Figure 2As shown in the figure, the schematic diagram of the four-component separation device of coal-based modified asphalt consists of three parts: the first part is constant temperature (constant temperature water bath with water circulation b and glass adsorption column a); the temperature of the glass adsorption column is maintained constant during the adsorption process; the second part is filtration (c vacuum pump and e sand core filter layer); the third part is to collect the solutions of each component (ground-mouth triangular bottle d). By replacing the ground-mouth triangular bottles with labels, corresponding to different solvent flushing agents, the asphaltene, saturated fraction, aromatic fraction and colloid of the corresponding coal-based modified asphalt are collected. Then the ground-mouth triangular bottles of different component solutions are concentrated and dried to constant weight, and the asphaltene, saturated fraction, aromatic fraction and colloid content of the coal-based modified asphalt are calculated.

Claims

1. An experimental analysis method for determining five components of coal-based modified asphalt, characterized in that: The steps include: Step 1: pretreat the coal-based modified asphalt sample, add n-heptane to the pretreated coal-based modified asphalt sample, and obtain a colorless and transparent n-heptane solution after ultrasonic dispersion, dissolution and centrifugation. The n-heptane solution is a mixture of saturated fraction, aromatic fraction and colloid, and then concentrate for standby use; Toluene solvent is added to the residue in the centrifuge tube, and then filtered after ultrasonic dispersion and centrifugation to obtain a toluene insoluble solution and an asphaltene solution; Step 2: Prepare the aluminum oxide adsorbent before analysis by activating it and then filling it, soaking the aluminum oxide with n-heptane and setting it aside; Step 3: Separating the concentrated solution of the n-heptane solution in step 1 to obtain a saturated fraction to obtain a colorless saturated fraction solution; Step 4: separating the aromatic components from the concentrated solution of the n-heptane solution in step 1 to obtain a yellow to dark brown aromatic component solution; Step 5: separating the colloid from the concentrated solution of the n-heptane solution in step 1 to obtain a dark brown-black colloid solution; Step 6: Desolventize and weigh the asphaltene solution in step 1, the colorless saturated fraction solution in step 3, the yellow-dark brown aromatic fraction solution in step 4, and the dark brown-black colloid solution in step 5; Step 7: Calculate the toluene insoluble matter, asphaltenes, saturated fractions, aromatic fractions, and colloids of the coal-based modified asphalt sample.

2. The test analysis method for determining five components of coal-based modified asphalt according to claim 1, characterized in that: The step 1 is specifically as follows: 1) Heat the coal-based modified asphalt sample in an oven at 135°C-150°C to a fluid state and stir it thoroughly; 2) Prepare n-heptane, toluene, dichloromethane, and anhydrous ethanol reagents (all reagents used are analytical grade) for use; 3) Weighing samples: Weigh 0.9g-1.0g of the uniform coal-based modified asphalt sample treated in step 1) and mark it as m1, and 0.1μm nylon filter membrane and mark it as M0, place the weighed sample in a clean centrifuge tube, add 40ml-50ml of n-heptane at a temperature of 65℃-70℃, tighten the bottle cap and place it in an ultrasonic instrument for ultrasonic dispersion and dissolution for 5min-10min; then put it in a high-speed centrifuge, centrifuge it at a speed of 8000 rpm-10000 rpm for 5min-10min, take it out and let it stand for 5min-10min; collect the upper layer solution in an ordinary conical flask, repeat this step 3-5 times until the final n-heptane solution collected is colorless and transparent. At this time, the mixed n-heptane solution collected is a mixture of saturated fraction, aromatic fraction and colloid, marked as m2, and evaporate and concentrate it to 10ml-15ml in a constant temperature water bath (b) with water circulation in a four-component separation device for use; 4) Add 40ml-50ml of analytical pure toluene at a temperature of 60℃-70℃ to the residue in the centrifuge tube, then ultrasonically oscillate for 5min-10min to disperse and dissolve it, then put it into a high-speed centrifuge, centrifuge it at a speed of 8000 rpm-10000 rpm for 5min-10min, take it out and let it stand for 5min-10min; collect the upper toluene solution and transfer it to a constant weight ground-mouth conical flask d; repeat this step until the collected toluene solution is colorless and transparent, pour the residue in the centrifuge tube into a funnel equipped with quantitative filter paper, place a constant weight ground-mouth conical flask d under the funnel, and after filtering, collect the toluene insoluble matter on the quantitative filter paper for standby use; 5) Filtration: Take the toluene insoluble matter collected by the quantitative filter paper in step 1 (4) and rinse it with hot toluene solvent at a temperature of 60°C-70°C in a glass filtration device (using a 0.1 μm nylon filter membrane) until the toluene solvent in the ground-mouth filtration bottle is colorless and clear after rinsing, and mark it as m7. Collect the toluene soluble solution in the centrifuge tube and the glass filtration device. This solution is the asphaltene solution and is marked as m3; 6) Remove the solvent: Place the filter membrane with toluene insoluble matter in a vacuum drying oven at a temperature of 105°C-110°C and a pressure of -0.1Mpa for 30 minutes. Weigh the filter membrane with toluene insoluble matter and mark it as M7. Calculate the toluene insoluble matter content of the coal-based modified asphalt.

3. The test analysis method for determining five components of coal-based modified asphalt according to claim 1, characterized in that: The step 2 is specifically as follows: 1) Activation of aluminum oxide: 100g-150g of neutral 100-200 mesh aluminum oxide for chromatography is activated in a muffle furnace at 450°C-500°C for 5.5h-6.5h, and after cooling, it is placed in a glass container, and 0.5%-1% of the mass of aluminum oxide is added in distilled water, shaken well, and allowed to stand for 24h-36h for use; 2) Take 40g-45g of activated aluminum oxide and put it into the glass adsorption column a in the four-component separation device, use the sand core filter e as the aluminum oxide support, and gently tap the column with a leather hammer to make the aluminum oxide compact and uniform; 3) Add 40ml-50ml of n-heptane to moisten the aluminum oxide in the glass adsorption column a, and then the aluminum oxide is soaked in n-heptane for use.

4. The test analysis method for determining five components of coal-based modified asphalt according to claim 3, characterized in that: The step three is specifically as follows: Transfer 10ml-15ml of the n-heptane concentrated solution obtained in step 13) to the glass adsorption column a, and then add 80ml-100ml of analytical grade n-heptane to rinse the glass adsorption column a for 3-5 times, collect the concentrated solution after rinsing into the ground-mouth triangle flask d, connect the constant weight ground-mouth triangle flask d with a frosted mouth to the lower part of the frosted glass adsorption column, and then slowly pour the concentrated liquid after rinsing into the glass adsorption column a; turn on the filtration device after 15min-30min, adjust the filtration speed to 1ml / min-2ml / min, stop filtration when the n-heptane in the glass adsorption column a is filtered until no liquid drips, and the constant weight ground-mouth triangle flask d contains a colorless saturated solution, marked as m4.

5. The test analysis method for determining five components of coal-based modified asphalt according to claim 4, characterized in that: The step 4 is specifically as follows: Replace the constant weight ground-mouth conical flask d at the lower end of the glass adsorption column a, add 80ml-100ml of n-heptane-dichloromethane (1:1) into the glass adsorption column a, wait for 10min-20min, start the vacuum pump c with a pressure regulator for filtration, adjust the filtration speed to 2ml / min-3ml / min, and stop filtration when the toluene in the glass adsorption column a is filtered until no liquid drips. The constant weight ground-mouth conical flask d contains a yellow to dark brown aromatic solution, marked as m5.

6. The test analysis method for determining five components of coal-based modified asphalt according to claim 5, characterized in that: The step five is specifically as follows: Replace the constant weight ground-mouth conical flask d at the lower end of the glass adsorption column a, add 80ml-100ml of anhydrous ethanol-dichloromethane (1:1) into the glass adsorption column a, wait for 10min-20min, start the vacuum pump c with a pressure regulator for filtration, adjust the filtration speed to 2ml / min-3ml / min, and stop filtration when the toluene-ethanol in the glass adsorption column a is filtered until no liquid drips. The constant weight ground-mouth conical flask d contains a dark brown-black colloidal solution, marked as m6.

7. The test analysis method for determining five components of coal-based modified asphalt according to claim 6, characterized in that: The step six is ​​specifically as follows: Take the components of the solution in the ground-mouth conical flasks d marked as m3, m4, m5, and m6, and evaporate the solvent in a constant temperature water bath until the remaining solvent is 0.3ml-0.5ml. Put them into a vacuum drying oven at 105℃-110℃ and keep them at a negative pressure of 90Kpa-100Kpa for 1h-2h. After cooling in a desiccator for 20min-40min, weigh their masses respectively: M 3、 M 4、 M 5、 M6; then place it in a dryer and dry it for 20min-40min for constant weight check, until the difference between two consecutive weighings does not exceed 0.0005g, and the weighing accuracy is 0.0001g. The saturated content, aromatic content, gum and asphaltene are calculated by weighing.

8. The test analysis method for determining five components of coal-based modified asphalt according to claim 7, characterized in that: The step seven is specifically as follows: Calculate the specific content of each component based on the weighed sample mass: Toluene insoluble matter: (M7-M0) / m1×100%; Asphaltene: M3 / m1×100%; Saturated fraction: M4 / m1×100%; Aromatic fraction: M5 / m1×100%; Colloid:M6 / m1×100%.

Images