Asphaltene separation apparatus and separation method

Abstract

The application discloses an asphaltene separation device and an asphaltene separation method. The asphaltene separation device comprises a separation cabin, the separation cabin is in a cylindrical structure, electric heating wires are filled between the inner wall and the outer wall of the separation cabin, the electric heating wires are connected with temperature sensors, a stirring shaft is penetrated through the center of the end face of the bottom end of the separation cabin, stirring blades are sleeved with the end part of the stirring shaft, the stirring blades are in the separation cabin, the end part of the stirring shaft is connected with a stirring motor, and the stirring motor is outside the separation cabin. The asphaltene separation device and the separation method solve the problem that a long time is consumed in the asphaltene separation process, and meet the demand of people for rapid asphaltene separation. The asphaltene separation device is provided with a stirring device composed of a stirring shaft and stirring blades, the dissolution and separation time is reduced through the stirring mode, and the temperature sensors and the electric heating wires are provided, so that the temperature in the separation cabin can be accurately controlled, and the dissolution speed of solutes is accelerated.

Description

TECHNICAL FIELD

[0001] The present application belongs to the technical field of material component separation equipment, and relates to an asphaltene separation device. BACKGROUND

[0002] Asphaltene is a complex mixture composed of high molecular weight hydrocarbons and non-metallic derivatives, without specific molecular formula, which can be dissolved in hot benzene but not in C5-C7 normal alkane. The proportion of asphaltene and other heavy components in the oil determines the viscosity and flowability of the crude oil. The higher the asphaltene content, the worse the flowability of the crude oil, and the more difficult the development of the corresponding crude oil.

[0003] At present, the separation and content determination of asphaltene are mostly combined with four-component analysis and gravimetric method. Through Soxhlet extraction, asphaltene, saturates, aromatics and resin are eluted by using the different solubilities of different components in each extractant. After each component is dried to constant weight, the corresponding mass percentage is calculated by gravimetric method. The existing technology has the problem of long time consumption in asphaltene separation. SUMMARY

[0004] The purpose of the present application is to provide an asphaltene separation device, and another purpose of the present application is to provide an asphaltene separation method, which solves the problem of long time consumption in asphaltene separation in the prior art.

[0005] The technical scheme adopted by the present application is that the asphaltene separation device comprises a cylindrical separation cabin, electric heating wires are filled between the inner and outer walls of the separation cabin, a stirring shaft is penetrated through the center of the end face of the bottom end of the separation cabin, stirring blades are sleeved with the end of the stirring shaft extending into the separation cabin, a stirring motor is connected with the end of the stirring shaft outside the separation cabin, and two sample flow outlets are symmetrically arranged around the stirring shaft below the end face of the bottom end of the separation cabin.

[0006] The present application also has the following characteristics:

[0007] A cabin cover is arranged above the separation cabin, a fixed support is arranged below the separation cabin, the fixed support is fixedly connected with the end face of the bottom end of the separation cabin above, and a shock pad is connected with the fixed support below.

[0008] The structure of the sample flow outlet is hollow tubular, a rotating insert baffle is arranged on one side of the bottom end of the sample flow outlet, the structure of the rotating insert baffle is circular plate-shaped, a plurality of small holes are uniformly opened along one side of the diameter on the plate face of the rotating insert baffle, and a solvent collection bottle is arranged below the lower end of each sample flow outlet.

[0009] The structure of the cabin cover is circular plate-shaped, a cylindrical recess is opened on one side of the cabin cover, the inner diameter of the recess in the cabin cover is matched with the outer diameter of the top end of the separation cabin, a temperature sensor is connected with the electric heating wire, and a power supply is connected with the electric heating wire.

[0010] Another technical solution adopted by the present application is an asphaltene separation method, which is implemented according to the following steps: after adding a crude oil sample and a n-heptane solvent into a separation cabin, the power is turned on; after heating and stirring, the power is turned off, and after standing for 3-5 minutes, the one-side rotating insert baffle is rotated to make the solvent flow into a solvent collection bottle; after the solvent collection is completed, the rotating insert baffle is rotated to block the sample flow outlet; the n-heptane solvent is added again, and the operation is repeated until the newly collected n-heptane solvent is clear; the remaining sample in the cabin is weighed, the cabin is poured into a toluene solvent, and the power is turned on; after heating and stirring, the power is turned off, and after standing for 3-5 minutes, the other-side rotating insert baffle is rotated to make the solvent enter the solvent collection bottle; after the solvent collection is completed, the rotating insert baffle is rotated to block the sample flow outlet; the toluene solvent is added again, and the operation is repeated until the newly collected toluene solvent is clear; after the clear toluene solution is evaporated and dried, a black solid material is obtained.

[0011] The feature of another technical solution of the present application is also that:

[0012] The heating and stirring are completed by the power control of the heating wire, the stirring motor and the stirring blade; the n-heptane solvent collected by the solvent collection bottle contains the alkane components and aromatic components in the crude oil sample, and the toluene solution collected by the solvent collection bottle contains the asphaltene components in the crude oil sample.

[0013] The mass of the first added crude oil sample in the separation cabin is the same as the mass of the n-heptane solvent added each time; in the asphaltene separation method, the mass of the toluene solvent added each time is the same as the mass of the crude oil sample that is not dissolved in the n-heptane solvent obtained by weighing the remaining sample in the cabin.

[0014] The specific content of the heating and stirring is that when the temperature in the separation cabin is heated to 55-60 DEG C, the stirring motor is operated at a speed of 80 r / min for 15-20 min.

[0015] The clear n-heptane solvent collected by the solvent collection bottle does not contain the alkane components and aromatic components in the crude oil sample, and the clear toluene solution collected by the solvent collection bottle does not contain the asphaltene components in the crude oil sample; the black solid material obtained after the toluene solution is evaporated and dried is asphaltene.

[0016] The present application has the beneficial effect of solving the problem of long time consumption in the asphaltene separation process, and meeting the demand of people for rapid asphaltene separation. The asphaltene separation device provided by the present application is provided with a stirring device composed of a stirring shaft and stirring blades, which reduces the dissolution and separation time through stirring; a temperature sensor and a heating wire are provided, which can accurately control the temperature in the separation cabin and accelerate the dissolution speed of solute. BRIEF DESCRIPTION OF DRAWINGS

[0017] Figure 1This is a schematic diagram of the asphalt separation device provided by the present invention;

[0018] Figure 2 This is a schematic diagram of the rotating insert baffle structure in this invention;

[0019] Figure 3 This is a full-wavelength scan of asphaltene obtained in the asphaltene separation method of the present invention;

[0020] Figure 4 This is the asphalt standard curve obtained in the asphalt separation method of the present invention.

[0021] In the diagram, 1. Separation chamber; 2. Chamber cover; 3. Fixing bracket; 4. Shock-absorbing pad; 5. Temperature sensor; 6. Power supply; 7. Stirring motor; 8. Sample outlet; 9. Heating wire; 10. Rotating baffle; 11. Stirring shaft; 12. Stirring blades; 13. Solvent collection bottle. Detailed Implementation

[0022] The present invention will now be described in detail with reference to the accompanying drawings and specific embodiments.

[0023] The purpose of this invention is to provide an asphalt separation device, such as... Figure 1 As shown, it includes a separation chamber 1, a cover 2 on the top of the separation chamber, a fixed bracket 3 and a shock-absorbing pad 4 at the bottom, a temperature sensor 5, a power supply 6, a stirring motor 7 and two sample outlets 8 on the outside, a stirring device and a heating wire 9 inside, and a rotating insert baffle 10 inside the sample outlet 8.

[0024] The stirring device includes a stirring shaft 11 and stirring blades 12, and solvent collection bottles 13 are placed under the two sample outlets 8 respectively; the temperature sensor 5 can display the real-time temperature inside the sample chamber and is connected to the heating wire 9 to control the temperature of the sample chamber to reach the set temperature.

[0025] like Figure 2 As shown, half of the rotating baffle 10 is a non-porous stainless steel plug and the other half is a small-pore stainless steel leak, which helps to implement the outflow of the extractant while retaining the remaining insoluble components. The rotating baffle 10 can be manually rotated to control the closure and flow of the sample outlet 8. One end of the stirring shaft 11 is connected to the stirring blade 12, and the other end is connected to the stirring motor 7. The stirring is started by the power supply 6 control device.

[0026] Another technical solution adopted in this invention is an asphaltene separation method, which is implemented according to the following steps:

[0027] Step 1: Add an appropriate amount of crude oil sample and n-heptane solvent to separation chamber 1, then turn on power supply 6;

[0028] Step 2: The solution in the separation chamber 1 is heated by heating wire 9 and stirred by stirring blade 12, so that the alkane and aromatic components in the crude oil sample are dissolved in n-heptane solvent.

[0029] Step 3: After the saturated and aromatic components in the crude oil sample have dissolved in the n-heptane solvent, turn off the power supply 6, let it stand for 3-5 minutes, then rotate the rotating insert baffle 10 on one side so that the n-heptane solvent passes through the rotating insert baffle 10 and enters the solvent collection bottle 13 on that side through the sample outlet 8.

[0030] Step 4: After the n-heptane solvent in the separation chamber 1 has been collected, rotate the rotating insert baffle 10 from step 3 back to its original position so that the rotating insert baffle 10 blocks the sample outlet 8.

[0031] Step 5: After adding an appropriate amount of n-heptane solvent, turn on power 6 and repeat steps 2 to 4 until the newly collected n-heptane solvent in step 4 is clear, that is, the newly collected n-heptane solvent in step 4 does not contain the saturated components and aromatic components of the crude oil sample, then proceed to step 6.

[0032] Step 6: Add toluene solvent into separation chamber 1 and turn on power 6;

[0033] Step 7: The solution in the separation chamber 1 is heated by heating wire 9 and stirred by stirring blade 12, and the asphaltene component in the remaining crude oil sample is dissolved in toluene solvent;

[0034] Step 8: Turn off the power and let it stand for 3-5 minutes. Then, rotate the rotating insert baffle 10 on the other side to allow the toluene solvent to pass through the rotating insert baffle 10 on that side and enter the solvent collection bottle 13 on that side through the sample outlet 8 on that side.

[0035] Step 9: After the toluene solvent in the separation chamber 1 has been collected, rotate the rotating insert baffle 10 back to its original position so that the rotating insert baffle 10 blocks the sample outlet 8.

[0036] Step 10: Turn the power back on 6 and repeat steps 7 to 9 until the newly collected toluene solvent in step 9 is clear, that is, the newly collected toluene solvent in step 9 does not contain the asphaltenes component in the remaining crude oil sample, then proceed to step 11.

[0037] Step 11: The toluene solution containing asphaltene obtained in Step 10 is evaporated and dried using a rotary evaporator. The resulting black solid substance is asphaltene.

[0038] Example 1

[0039] like Figure 1As shown, the asphalt separation device includes a cylindrical separation chamber 1. Heating wires 9 are filled between the inner and outer walls of the separation chamber 1. A stirring shaft 11 passes through the center of the bottom end face of the separation chamber 1. A stirring blade 12 is sleeved at one end of the stirring shaft 11 extending into the separation chamber 1. A stirring motor 7 is connected to the other end of the stirring shaft 11 outside the separation chamber 1. Two sample outlets 8 are symmetrically arranged around the stirring shaft below the bottom end face of the separation chamber 1. A chamber cover 2 is provided above the separation chamber 1, and a fixed support 3 is provided below the separation chamber 1. The fixed support 3 is fixed to the bottom end face of the separation chamber 1 at the top, and a shock-absorbing pad 4 is connected below the fixed support 3. The sample outlets 8 are hollow tubular in structure. A rotating baffle 10 is provided inside the sample outlet 8 near the bottom of the separation chamber 1. The rotating baffle 10 is circular in structure, and several small holes are evenly opened along one side of its diameter on the surface of the rotating baffle 10. Solvent collection bottles 13 are respectively installed below the lower ends of the two sample outlets 8. The hatch cover 2 has a circular plate structure. A cylindrical groove is opened on one side of the hatch cover 2. The inner diameter of the groove on the hatch cover 2 is matched with the outer diameter of the top end face of the separation chamber 1. The heating wire 9 is connected to the temperature sensor 5 and the heating wire 9 is connected to the power supply 6.

[0040] Example 2

[0041] The asphaltene separation method provided in this embodiment is implemented according to the following steps: Crude oil sample and n-heptane solvent are added to separation chamber 1, and power supply 6 is turned on; after heating and stirring; power supply 6 is turned off, and after standing for 3 minutes, one side of the rotating baffle 10 is rotated to allow the solvent to flow into solvent collection bottle 13; after solvent collection is completed, the rotating baffle 10 is rotated to block the sample outlet 8; n-heptane solvent is added back and the operation is repeated until the newly collected n-heptane solvent is clear; the remaining sample in the chamber is weighed, toluene solvent is added to separation chamber 1, and power is turned on; after heating and stirring; power supply 6 is turned off, and after standing for 3 minutes, the other side of the rotating baffle 10 is rotated to allow the solvent to enter solvent collection bottle 13; after solvent collection is completed, the rotating baffle 10 is rotated to block the sample outlet 8; toluene solvent is added back and the operation is repeated until the newly collected toluene solvent is clear; the clear toluene solution is evaporated and dried to obtain a black solid substance.

[0042] Example 3

[0043] The asphaltene separation method provided in this embodiment is implemented according to the following steps: Crude oil sample and n-heptane solvent are added to separation chamber 1, and power supply 6 is turned on; after heating and stirring; power supply 6 is turned off, and after standing for 4 minutes, one side of the rotating baffle 10 is rotated to allow the solvent to flow into solvent collection bottle 13; after solvent collection is completed, the rotating baffle 10 is rotated to block the sample outlet 8; n-heptane solvent is added back and the operation is repeated until the newly collected n-heptane solvent is clear; the remaining sample in the chamber is weighed, toluene solvent is added to separation chamber 1, and power is turned on; after heating and stirring; power supply 6 is turned off, and after standing for 4 minutes, the other side of the rotating baffle 10 is rotated to allow the solvent to enter solvent collection bottle 13; after solvent collection is completed, the rotating baffle 10 is rotated to block the sample outlet 8; toluene solvent is added back and the operation is repeated until the newly collected toluene solvent is clear; the clear toluene solution is evaporated and dried to obtain a black solid substance.

[0044] Heating and stirring are controlled by power supply 6 via heating wire 9, stirring motor 7, and stirring blades 12. The n-heptane solvent collected in solvent collection bottle 13 contains alkane and aromatic components from the crude oil sample, while the toluene solution collected in solvent collection bottle 13 contains asphaltenes from the crude oil sample. The mass of the crude oil sample added to separation chamber 1 for the first time is the same as the mass of the n-heptane solvent added each time. In the asphaltenes separation method, the mass of the toluene solvent added each time is the same as the mass of the crude oil sample insoluble in n-heptane solvent obtained by weighing the remaining sample in the chamber.

[0045] Example 4

[0046] The asphaltene separation method provided in this embodiment is implemented according to the following steps: Crude oil sample and n-heptane solvent are added to separation chamber 1, and power supply 6 is turned on; after heating and stirring; power supply 6 is turned off, and after standing for 5 minutes, one side of the rotating baffle 10 is rotated to allow the solvent to flow into solvent collection bottle 13; after solvent collection, the rotating baffle 10 is rotated to block the sample outlet 8; n-heptane solvent is added back and the operation is repeated until the newly collected n-heptane solvent is clear; the remaining sample in the chamber is weighed, toluene solvent is added to separation chamber 1, and power is turned on; after heating and stirring; power supply 6 is turned off, and after standing for 5 minutes, the other side of the rotating baffle 10 is rotated to allow the solvent to enter solvent collection bottle 13; after solvent collection, the rotating baffle 10 is rotated to block the sample outlet 8; toluene solvent is added back and the operation is repeated until the newly collected toluene solvent is clear; the clear toluene solution is evaporated and dried to obtain a black solid substance.

[0047] Heating and stirring are controlled by power supply 6 via heating wire 9, stirring motor 7, and stirring blades 12. The n-heptane solvent collected in solvent collection bottle 13 contains alkane and aromatic components from the crude oil sample, while the toluene solution collected in solvent collection bottle 13 contains asphaltenes from the crude oil sample. The mass of the crude oil sample added to separation chamber 1 for the first time is the same as the mass of the n-heptane solvent added each time. In the asphaltenes separation method, the mass of the toluene solvent added each time is the same as the mass of the crude oil sample insoluble in n-heptane solvent obtained by weighing the remaining sample in the chamber. The specific heating and stirring process involves heating the temperature inside separation chamber 1 to 55℃-60℃ while simultaneously running stirring motor 7 at 80 r / min for 15-20 minutes. The clear n-heptane solvent collected in solvent collection bottle 13 does not contain alkane and aromatic components from the crude oil sample, and the clear toluene solution collected in solvent collection bottle 13 does not contain asphaltenes from the crude oil sample. The black solid substance obtained after evaporating and drying the toluene solution is asphaltenes.

[0048] The asphaltene content obtained according to the above embodiments was determined and a standard curve was plotted. The determination steps are as follows:

[0049] 1. Preparation of asphaltene mother liquor: Weigh 25 mg of the prepared asphaltene using a precision electronic balance and completely dissolve it in 100 mL of toluene to prepare an asphaltene toluene solution mother liquor with a final concentration of 250 mg / L.

[0050] 2. Take six 5mL centrifuge tubes and prepare asphaltene toluene test solutions with a volume of 4mL and final concentrations of 0mg / L, 2.5mg / L, 5mg / L, 7.5mg / L, 10mg / L, and 12.5mg / L, respectively.

[0051] 3. Transfer all the above-mentioned test solutions in batches into quartz cuvettes, and perform a full wavelength scan of 200nm-320nm using a UV spectrophotometer to obtain the results as shown below. Figure 3 The image shown is a full-wavelength scan of asphalt.

[0052] 4. Table 1 shows a regular absorption variation at 300 nm that depends on the asphaltenes concentration. A standard curve is plotted with the asphaltenes concentration in the solution on the x-axis and the absorbance at 300 nm on the y-axis. Figure 4 As shown.

[0053]

[0054] Table 1. Regular absorption peaks of the asphalt-based test liquids at 300 nm

[0055] Experimental test results show that the formula for the standard curve of asphaltene solubility is: y = 0.288x + 0.0003, R 2=1 indicates that there is a good linear relationship between the absorbance value at 300nm and the asphaltene content. Therefore, the asphaltene content obtained in the above embodiment meets the requirements.

[0056] Based on the difference in solubility of asphaltenes in different solvents, this invention employs hot solvents and mechanical stirring to reduce crude oil viscosity and promote the sequential dissolution and separation of hydrocarbon and asphaltenes components. The asphaltenes separation device proposed in this invention includes a temperature sensor 5 and a heating wire 9, which can precisely control the temperature within the separation chamber 1, facilitating crude oil viscosity reduction and accelerating solute dissolution. A stirring device consisting of a stirring shaft 11 and stirring blades 12 is also included, which helps reduce the dissolution and separation time of asphaltenes. This device enables rapid dissolution and separation of asphaltenes in crude oil, featuring simple operation, fast separation speed, good repeatability, and high precision. It solves the problems of time-consuming and complex asphaltenes elution processes, meeting the needs of rapid asphaltenes separation in industrial and educational settings.

Claims

1. An asphalt separation device, characterized in that: The separation chamber includes a cylindrical separation chamber (1), with heating wires (9) filling the space between the inner and outer walls of the separation chamber (1). A stirring shaft (11) is inserted through the center of the bottom end face of the separation chamber (1). A stirring blade (12) is sleeved on one end of the stirring shaft (11) that extends into the separation chamber (1). A stirring motor (7) is connected to the other end of the stirring shaft (11) outside the separation chamber (1). Two sample outlets (8) are symmetrically arranged around the stirring shaft below the bottom end face of the separation chamber (1). The sample outlet (8) has a hollow tube structure. A rotating insert baffle (10) is provided on the side of the sample outlet (8) near the bottom of the separation chamber (1). The rotating insert baffle (10) has a circular plate structure. Several small holes are evenly opened on the plate surface of the rotating insert baffle (10) along the diameter side. Solvent collection bottles (13) are respectively provided below the lower ports of the two sample outlets (8). The separation chamber (1) is provided with a cover (2) above it. The cover (2) is in the shape of a circular plate. A cylindrical groove is opened on one side of the cover (2). The inner diameter of the groove on the cover (2) is matched with the outer diameter of the top end face of the separation chamber (1). The heating wire (9) is connected to a temperature sensor (5) and a power source (6).

2. The asphalt separation device according to claim 1, characterized in that: A fixed bracket (3) is provided below the separation chamber (1). The fixed bracket (3) is fixedly connected to the bottom end face of the separation chamber (1) above, and a shock-absorbing pad (4) is connected below the fixed bracket (3).

3. A method for separating asphaltene, characterized in that, The asphaltene separation device as described in claim 1 is implemented according to the following steps: After adding crude oil sample and n-heptane solvent to the separation chamber (1), the power supply (6) is turned on; after heating and stirring; the power supply (6) is turned off, and after standing for 3-5 minutes, the rotating insert baffle (10) on one side is rotated to allow the solvent to flow into the corresponding solvent collection bottle (13); after the solvent collection is completed, the rotating insert baffle (10) is rotated to block the sample outlet (8); n-heptane solvent is added back and the operation is repeated until the newly collected n-heptane solvent is clear; the remaining sample in the chamber is weighed, toluene solvent is added to the separation chamber (1) and the power supply is turned on; after heating and stirring; the power supply (6) is turned off, and after standing for 3-5 minutes, the rotating insert baffle (10) on the other side is rotated to allow the solvent to enter another solvent collection bottle (13); after the solvent collection is completed, the rotating insert baffle (10) is rotated to block the sample outlet (8); toluene solvent is added back and the operation is repeated until the newly collected toluene solvent is clear; The heating and stirring are controlled by the power supply (6) to control the heating wire (9), stirring motor (7) and stirring blade (12); the n-heptane solvent collected in the solvent collection bottle (13) contains alkane components and aromatic components from the crude oil sample, and the toluene solution collected in the solvent collection bottle (13) contains asphaltenes from the crude oil sample. The mass of the crude oil sample added to the separation chamber (1) for the first time is the same as the mass of the n-heptane solvent added each time; the mass of the toluene solvent added each time in the asphaltene separation method is the same as the mass of the crude oil sample that is insoluble in n-heptane solvent obtained by weighing the remaining sample in the chamber. The specific content of the heating and stirring is that when the temperature inside the separation chamber (1) is heated to 55℃-60℃, the stirring motor (7) runs at a speed of 80 r / min for 15min-20min. The clear n-heptane solvent newly collected in the solvent collection bottle (13) does not contain alkane components and aromatic components from the crude oil sample, and the clear toluene solution newly collected in the solvent collection bottle (13) does not contain asphaltenes components from the crude oil sample; after evaporating and drying the toluene solution containing asphaltenes, a black solid substance is obtained; the black solid substance obtained after evaporating and drying the toluene solution is asphaltenes.

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