Method and device for extracting and separating coal B tar through supercritical fluid

Abstract

The invention belongs to the technical field of coal pitch and ethylene tar processing, and relates to an extraction separation method for supercritical fluid extraction separation of a coal pitch and ethylene tar mixture (hereinafter referred to as coal tar B), and the method comprises the following steps: preparing coal tar B and a liquid medicine, and mixing the coal tar B and the liquid medicine to form a mixed liquid; providing a supercritical fluid, respectively inputting the mixed solution and the supercritical fluid into two ends of an extractor, enabling the mixed solution and the supercritical fluid to reversely flow, extracting to obtain a first extracting solution, a first extract and a residual fluid mixture, and discharging the first extracting solution from the upper part of the extractor, discharging the first extract and residual fluid mixture from the lower part of the extractor; and carrying out separation treatment on the first extraction liquid for at least five times to obtain five or more extracts. According to the technical scheme provided by the invention, each component of the coal B tar can be accurately extracted and separated, and the value of each extract is improved.

Description

Technical Field

[0001] This application relates to the field of coal tar pitch and ethylene tar processing technology, specifically to a supercritical fluid extraction method and apparatus for separating a mixture of coal tar pitch and ethylene tar (hereinafter referred to as coal ethylene tar). Background Technology

[0002] Coal tar pitch is a type of coal tar produced during the dry distillation of coal at 500–900℃. After the coal tar undergoes vacuum distillation to extract lighter components, the residue obtained at the bottom of the vacuum distillation tower is coal tar pitch. The density of coal tar pitch at 20℃ is 0.98 g / cm³. 3 ~1.30g / cm 3 The softening point is between 35℃ and 95℃, and the average molecular weight of coal tar pitch is between 1000 and 5000 g / mol. Coal tar pitch contains impurities such as metallic impurities, quinoline insolubles, sulfides, and nitrides.

[0003] Ethylene tar is a product of the high-temperature condensation of feedstock and products during the steam cracking process of ethylene pyrolysis. It is a byproduct of hydrocarbon cracking to produce ethylene, with a density of 1.02 g / cm³ at 20°C. 3 ~1.25g / cm 3 Ethylene tar has extremely low ash content and very few sulfides, making it a relatively ideal high-end carbon raw material. However, the average molecular weight of ethylene tar is only 200-1000 g / mol, which is significantly lower than that of coated pitch, which has a molecular weight of 1000-3000 g / mol.

[0004] Existing methods for producing lithium-ion battery and graphite electrode coated asphalt from ethylene tar are basically as follows: First, the ethylene tar is filtered to remove impurities. Then, the ethylene tar is fed into a coking furnace for pyrolysis and condensation reactions. This causes large saturated hydrocarbon molecules to break down into lighter components such as oil and gas, which are then discharged from the system. The small aromatic molecules condense into larger molecules, which are then extracted by distillation. Finally, modifiers are added, and the mixture is granulated and pulverized to become the raw material for coated asphalt. Although this method can produce coated asphalt with a high softening point, high sintering rate, and low ash content, basically meeting the three important technical requirements of coated asphalt (softening point above 250℃, sintering rate above 75%, and ash content below 0.1%w), the process is complex, requires large investments, and is costly.

[0005] To develop a simple and low-cost method for producing coated bitumen raw materials, this application discloses a method for producing high-end carbon raw materials such as coated bitumen using supercritical fluid extraction and separation of coal ethylene tar. The principle is as follows: the molecular weight of coated bitumen is 1000–3000 g / mol, while the average molecular weight of coal tar is 1000–5000 g / mol. Therefore, coal tar is more than sufficient as a raw material for coated bitumen in terms of molecular weight. Ethylene tar, with a molecular weight of only 200–1000 g / mol, is far lower than that of coated bitumen and obviously cannot be directly used as a raw material. However, by mixing coal tar and ethylene tar in a certain proportion, a mixture with a suitable molecular weight for producing coated bitumen raw materials can be created. After supercritical fluid extraction and separation, solid impurities such as metallic carbon particles are removed, and 5% of the carbon dioxide is removed. After removing lighter components such as ~8-cyclic aromatic hydrocarbons, anthracene oil, and saturated hydrocarbons, asphaltenes and gums remain. The asphalt produced by mixing these asphalts and gums in a specific ratio will obviously have a high softening point. This is because removing low-molecular-weight aromatic hydrocarbons and saturated hydrocarbons from the mixture, and then using the remaining asphalts and gums to make the coated asphalt, will inevitably result in a high softening point and a high sintering rate. Furthermore, after removing solid impurities such as metallic carbon particles from the mixture, the resulting coated asphalt will have a low ash content. Additionally, after removing harmful elements such as sulfur and nitrogen from the mixture, the high-quality coated asphalt will inevitably have low sulfur and nitrogen content. Therefore, the produced coated asphalt will undoubtedly be a high-quality product. In addition to being used as a coating material for asphalt, this raw material can also be further blended with extracts of aromatics, saturated hydrocarbons, etc., to synthesize high-end carbon raw materials such as needle coke, carbon black, and wall-protecting agents. Summary of the Invention

[0006] The technical problem to be solved by the embodiments of this application is to improve the existing method of producing coated asphalt using ethylene tar, which is too complicated, difficult to operate, has low yield, large investment and high production cost.

[0007] To address the aforementioned technical problems, this application provides a method for supercritical fluid extraction and separation of coal ethyl tar, employing the following technical solution: A method for separating coal ethyl tar by supercritical fluid extraction includes the following steps: Liquid coal ethyl tar and a pharmaceutical solution are provided, and the liquid coal ethyl tar and the pharmaceutical solution are mixed to form a mixture; A supercritical fluid is provided, and the mixture and the supercritical fluid are respectively input to both ends of the extractor. The mixture and the supercritical fluid flow counterclockwise to extract a first extract, a first extract, and a mixture of residual fluid. The first extract is discharged under reduced pressure from the upper outlet of the extractor, and the first extract and residual fluid mixture are discharged from the lower outlet of the extractor. The first extract includes compounds such as asphaltenes, gums, 5-8 ring aromatics, anthracene oil, saturated components, and supercritical fluid. The first extract consists of solid impurities such as metallic carbon particles. The first extract was subjected to at least five separation processes to obtain at least five different extracts. Asphalt and resin are blended in a specific ratio to synthesize high-end carbon raw materials such as coated asphalt.

[0008] Furthermore, the liquid coal ethyl tar is prepared through the following steps: The solid coal tar to be processed is placed in a melting tank, and ethylene tar is added in proportion. The material in the melting tank is heated using a first heating coil, causing the solid coal tar pitch to melt and then mix with ethylene tar to form liquid coal ethylene tar. The solid coal tar pitch is added in a proportion of 10%–90%, the ethylene tar is added in a proportion of 90%–10%, and the temperature of the liquid coal ethylene tar is 155℃–225℃. The density of the coal tar pitch at 20°C is 0.98 g / cm³. 3 ~1.30g / cm 3 The ethylene tar has a density of 1.02 g / cm³ at 20°C. 3 ~1.25g / cm 3 .

[0009] Furthermore, the fluid includes any one of fluorine, isopentane, isobutane, isopentane, n-butane, n-pentane, and propane. The purity of the fluid is 95% to 99.9%. The temperature of the fluid is 155℃~225℃.

[0010] Furthermore, prior to the step of introducing the mixture and supercritical fluid into the two ends of the extractor respectively, the following step is also included: The fluid is subjected to a first pressurization treatment to form the supercritical fluid, wherein the temperature of the fluid is 155℃~225℃, and the pressure of the supercritical fluid after the first pressurization treatment is 4MPa~16MPa; The mixture is subjected to a second pressurization treatment, wherein after the second pressurization treatment, the pressure of the mixture is 4 MPa to 16 MPa; and the temperature of the mixture is 155°C to 225°C. In the extractor, the ratio of the mixture to the supercritical fluid is 1:5 to 1:15, and the height-to-diameter ratio of the extractor is 5:1 to 30:1.

[0011] Furthermore, the liquid solution comprises a drug and diesel fuel, wherein the drug is selected from at least one of polyacrylic acid, fatty alcohol ether phosphate, sulfonic acid and sulfonates, sulfates, maleic anhydride sulfonate, alkyl sulfonates, methanol, and toluene; wherein the mass percentage concentration of the drug in the liquid solution is 1% to 50%. The amount of the added drug solution is 1.0% to 2.0% of the liquid coal ethyl tar.

[0012] Furthermore, the first extract output under reduced pressure at the upper outlet of the extractor is subjected to at least five separation processes to obtain at least five extracts, including the following steps: The first extract, which is depressurized and output from the upper outlet of the extractor, is fed into the first separator. Within the first separator, the first extract is separated to obtain a second extract, a second extract, and a mixture of residual fluid. The first separator has a pressure of 4 MPa to 14 MPa and a temperature of 150°C to 220°C. The second extract is depressurized and discharged from the upper outlet of the first separator and fed into the second separator. The mixture of the second extract and residual fluid is discharged from the bottom outlet of the first separator. This mixture is then transferred to an asphalt heating furnace or a thermal oil furnace for heating, and then enters an asphalt evaporation tower to evaporate and remove the remaining residual fluid. After evaporation, it is transferred from the bottom outlet to an asphalt stripping tower to strip away a small amount of residual fluid. The second extract is then discharged from the bottom of the asphalt stripping tower. All steps of removing the remaining residual fluid and removing a small amount of residual fluid are collected in a medium-pressure fluid recovery tank via pipelines and equipment for recycling. The second extract is asphaltenes; The second extract, which is depressurized and output from the upper outlet of the first separator, is fed into the second separator. Inside the second separator, the second extract is separated to obtain a third extract, a third extract, and a mixture of residual fluid. The pressure of the second separator is 4 MPa to 12 MPa, and the temperature is 145°C to 215°C. The third extract is depressurized and discharged from the upper outlet of the second separator and fed into the third separator. The mixture of the third extract and residual fluid is discharged from the bottom outlet of the second separator. The mixture of the third extract and residual fluid is regulated to the critical pressure using a colloidal regulating valve, and then transferred to a colloidal heat exchanger to be regulated to the critical temperature. After releasing a large amount of residual fluid in the colloidal critical column, it is discharged from the bottom outlet of the critical column and transferred to a colloidal evaporator to evaporate and remove the remaining residual fluid. After evaporation, it is discharged from the bottom outlet of the colloidal evaporator and transferred to a colloidal stripping column to strip and remove a small amount of residual fluid. Finally, the third extract is discharged from the bottom outlet of the colloidal stripping column. The release of a large amount of residual fluid, removal of the remaining residual fluid, and removal of a small amount of residual fluid are all collected in a medium-pressure fluid recovery tank through pipelines and equipment for recycling. The third extract is a gel; The third extract, which is depressurized and output from the upper outlet of the second separator, is fed into the third separator. Inside the third separator, the third extract is separated to obtain a fourth extract, a fourth extract, and a mixture of residual fluid. The pressure of the third separation process is 4 MPa to 9 MPa, and the temperature is 142°C to 210°C. The fourth extract is discharged under reduced pressure from the upper outlet of the three separators and fed into the fourth separator. The mixture of the fourth extract and residual fluid is discharged from the bottom outlet of the third separator. The mixture of the fourth extract and residual fluid is regulated to the critical pressure using a 5-8 ring aromatics regulating valve, then transferred to a 5-8 ring aromatics heat exchanger and regulated to the critical temperature. It is then transferred to a 5-8 ring aromatics critical tower to release a large amount of residual fluid, which is then discharged from the bottom outlet of the critical tower and transferred to a 5-8 ring aromatics evaporator to evaporate and remove the remaining residual fluid. The remaining residual fluid is then discharged from the bottom outlet of the 5-8 ring aromatics evaporator and transferred to a 5-8 ring aromatics stripping tower for stripping to remove a small amount of residual fluid. Finally, the fourth extract is discharged from the bottom outlet of the 5-8 ring aromatics stripping tower. All the processes described above—releasing a large amount of residual fluid, removing the remaining residual fluid, and removing a small amount of residual fluid—are collected in a medium-pressure fluid recovery tank via pipelines and equipment for recycling. The fourth extract is a 5- to 8-cyclic aromatic hydrocarbon. The fourth extract, which is depressurized and output from the upper outlet of the third separator, is fed into the fourth separator. Inside the fourth separator, the fourth extract is separated to obtain a fifth extract, a fifth extract, and a mixture of residual fluid. The pressure inside the fourth separator is 4MPa to 7MPa, and the temperature is 140℃ to 205℃. The fifth extract is depressurized and discharged from the upper outlet of the fourth separator and fed into the fifth separator. The mixture of the fifth extract and residual fluid is discharged from the bottom outlet of the fourth separator. The mixture of the fifth extract and residual fluid is regulated to the critical pressure using an anthracene oil regulating valve, then transferred to an anthracene oil heat exchanger to be regulated to the critical temperature, and then transferred to an anthracene oil critical tower to release a large amount of residual fluid. After being discharged from the bottom outlet of the critical tower, it is transferred to an anthracene oil evaporator to evaporate and remove the remaining residual fluid. After being discharged from the bottom outlet of the anthracene oil evaporator, it is transferred to an anthracene oil stripping tower to strip and remove a small amount of residual fluid. Finally, the fifth extract is discharged from the bottom outlet of the anthracene oil stripping tower. The above-mentioned processes of releasing a large amount of residual fluid, removing the remaining residual fluid, and removing a small amount of residual fluid are all collected in a medium-pressure fluid recovery tank through pipelines and equipment for recycling. The fifth extract is anthracene oil. The fifth extract, which is depressurized and output from the upper outlet of the fourth separator, is fed into the fifth separator. Within the fifth separator, the fifth extract is separated to obtain a mixture of a critical fluid, a sixth extract, and a residual fluid. Wherein, the pressure regulation of the fifth separator is the critical pressure of the fluid; the temperature regulation is the critical temperature of the fluid; The critical state fluid is discharged from the upper outlet of the fifth separator and fed into a medium-pressure fluid recovery tank. The sixth extract and residual fluid mixture is discharged from the bottom outlet of the fifth separator. This mixture is then transferred to a saturated hydrocarbon evaporator to evaporate and remove the remaining residual fluid. After evaporation, it is transferred to a saturated hydrocarbon stripping tower to strip away a small amount of residual fluid. Finally, the sixth extract is discharged from the bottom outlet of the saturated hydrocarbon stripping tower. All steps involving the removal of the remaining residual fluid and the removal of a small amount of residual fluid are collected in the medium-pressure fluid recovery tank via pipelines and equipment for recycling. The sixth extract is a saturated hydrocarbon.

[0013] Furthermore, the asphaltene and resin are blended in a certain proportion to form high-end carbon raw materials such as coated asphalt, wherein the asphaltene accounts for 30% to 70% of the coated asphalt raw material, and the resin accounts for 70% to 30% of the coated asphalt raw material.

[0014] To address the aforementioned technical problems, this application also provides a supercritical fluid extraction apparatus, employing the technical solution described below: A supercritical fluid extraction apparatus is provided for performing the supercritical fluid extraction method for separating coal ethyl tar as described above.

[0015] Compared with the prior art, the embodiments of this application have the following main advantages: This application provides a supercritical fluid extraction method for coal ethyl tar. By fully mixing liquid coal ethyl tar with a reagent solution, the reagent solution is used to demulsify, strongly disperse, and penetrate the coal ethyl tar, while also carrying out light components. This avoids severe emulsification caused by mixing supercritical fluid with coal ethyl tar, thereby improving the extraction effect and efficiency of supercritical fluid. By introducing supercritical fluid and combining it with countercurrent extraction, the useful substances in coal ethyl tar are fully dissolved in the supercritical fluid, thereby removing solid impurities such as metals and carbon particles from the coal ethyl tar. Then, through at least five separation processes, substances such as asphaltene, gum, 5-8 ring aromatics, anthracene oil, and saturated hydrocarbons are separated, thereby improving the purity of the extract and the quality of the product. Attached Figure Description

[0016] To more clearly illustrate the solution of this application, the accompanying drawings used in the description of the embodiments will be briefly introduced below. Obviously, the accompanying drawings described below are some embodiments of this application. For those skilled in the art, other drawings can be obtained based on these drawings without creative effort.

[0017] Figure 1 This is a flowchart of the supercritical fluid extraction method for separating coal ethyl tar according to an embodiment of this application; Figure 2 This is a flowchart illustrating the provision of coal tar and the provision of fluid in an embodiment of this application; Figure 3 This is a flowchart illustrating the separation process of the first extract at least five times according to an embodiment of this application.

[0018] Figure 4 This is a process flow diagram of a supercritical fluid extraction and separation device for coal ethyl tar according to an embodiment of this application.

[0019] Figure label: 100—Liquid coal ethyl tar output unit; 101—Melting tank; 102—Coal ethyl tar extraction pump; 103—First heating coil; 200—Drug supply unit; 201—Drug tank; 202—Dosing pump; 203—Mixer; 300—Extraction Unit; 301—Mixed Liquid Booster Pump; 302—Extractor; 304—Fluid Booster Pump; 303—Stripping Tower for Solid Impurities such as Metal Carbon Particles; 305—Second Heating Coil; 306—Mixed Liquid Feed Distributor; 400—Separation Unit: 401—First Pressure Reducing Valve, 402—First Heater, 403—First Separator, 403 / 1—Asphalt Heating Furnace, 403 / 2—Asphalt Evaporation Tower, 403 / 3—Asphalt Stripping Tower, 404—Second Pressure Reducing Valve, 405—Second Heater, 406—Second Separator, 406 / 1—Gelustic Pressure Reducing Valve, 406 / 2—Gelustic Heat Exchanger, 406 / 3—Gelustic Critical Tower, 406 / 4—Gelustic Evaporation Tower, 406 / 5—Gelustic Stripping Tower, 407—Third Pressure Reducing Valve, 408—Third Heater, 409—Third Separator, 409 / 1—5-8 Ring Aromatic Hydrocarbon Pressure Reducing Valve, 409 / 2—5-8 ring aromatics heat exchanger, 409 / 3—5-8 ring aromatics critical tower, 409 / 4—5-8 ring aromatics evaporator, 409 / 5—5-8 ring aromatics stripping tower, 410—Fourth pressure reducing valve, 411—Fourth heater, 412—Fourth separator, 412 / 1—Anthracene oil pressure reducing valve, 412 / 2—Anthracene oil heat exchanger, 412 / 3—Anthracene oil critical tower, 412 / 4—Anthracene oil evaporator, 412 / 5—Anthracene oil stripping tower, 413—Fifth pressure reducing valve, 414—Saturated hydrocarbon heat exchanger, 415—Fifth separator, 415 / 1—Saturated hydrocarbon evaporator, 415 / 2—Saturated hydrocarbon stripping tower, 416—Sixth pressure reducing valve. 500—Fluid supply unit; 501—Mixer cooler; 502—Medium-pressure fluid recovery tank; 503—Low-pressure fluid recovery tank; 504—Low-pressure fluid compressor; 505—Fluid heat exchanger; 600—Steam pipeline; 700—Solid coal tar pitch; 800—Liquid coal tar pitch. Detailed Implementation

[0020] Unless otherwise defined, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this application belongs; the terminology used herein in the specification of the application is for the purpose of describing particular embodiments only and is not intended to be limiting of the application; the terms "comprising" and "having," and any variations thereof, in the specification, claims, and foregoing drawings of this application are intended to cover non-exclusive inclusion. The terms "first," "second," etc., in the specification, claims, or foregoing drawings of this application are used to distinguish different objects, not to describe a particular order.

[0021] In this document, the term "embodiment" means that a particular feature, structure, or characteristic described in connection with an embodiment may be included in at least one embodiment of this application. The appearance of this phrase in various places throughout the specification does not necessarily refer to the same embodiment, nor is it a separate or alternative embodiment mutually exclusive with other embodiments. It will be explicitly and implicitly understood by those skilled in the art that the embodiments described herein can be combined with other embodiments.

[0022] Since matter is composed of particles and forces, and different substances have different particles and forces, their molecular structures also differ. Therefore, coal ethyl tar can actually be regarded as a colloidal substance composed of asphaltenes, gums, 5-8 ring aromatics, anthracene oil, saturated hydrocarbons, and gases arranged in rings from the inside out. Among them, asphaltenes have the largest molecular weight, the strongest force, and the strongest polarity, and are located at the center of various colloidal substances. Other types of substances are arranged in order of molecular weight from the inside out. In addition, solid impurities such as metals and carbon particles in coal ethyl tar are insoluble.

[0023] Therefore, this application employs supercritical fluid, utilizing its strong penetrating power and solubility, as well as the characteristic that these properties can change with pressure and temperature. This allows the supercritical fluid to penetrate between the particles of various colloidal substances. By adjusting to suitable pressure and temperature, the supercritical fluid gains the ability to dissolve these colloidal substances, achieving the desired extract from coal ethyl tar. Simultaneously, it removes solid impurities such as metals and carbon particles from the coal ethyl tar. Then, it separates asphaltene, gums, 5-8 ring aromatics, anthracene oil, saturated hydrocarbons, and other substances stepwise, facilitating the synthesis of various desired products or raw materials as needed.

[0024] Please see Figure 1 As shown, based on the above working principle, this application provides a method for supercritical fluid extraction and separation of coal ethyl tar, comprising the following steps: Step S100: Provide liquid coal ethyl tar and a pharmaceutical solution, and mix the liquid coal ethyl tar and the pharmaceutical solution to form a mixture; In step S200, supercritical fluid is provided, and the fluid released from the separation unit is recovered using equipment such as a mixing cooler 501, a medium-pressure fluid recovery tank 502, a low-pressure fluid recovery tank 503, and a low-pressure fluid compressor 504. After heat exchange in a fluid heat exchanger 505, the fluid is pressurized by a fluid booster pump 304 and then transported to the bottom inlet of the extractor 302. Step S300: Extraction operation. The mixture and the supercritical fluid are input to both ends of the extractor 302, respectively. The mixture and the supercritical fluid flow counterclockwise to extract a first extract, a first extract, and a mixture of residual fluid. The first extract is discharged under reduced pressure from the upper outlet of the extractor 302, and the first extract and the mixture of residual fluid are discharged from the lower outlet of the extractor 302. The first extract and the mixture of residual fluid are transferred to a stripping tower 303 for solid impurities such as metal carbon particles for stripping to remove residual fluid. The first extract is then discharged from the bottom outlet of the stripping tower 303. In this embodiment, the first extract comprises compounds such as asphaltenes, gums, 5-8 ring aromatics, anthracene oil, saturated hydrocarbons, and supercritical fluids, while the first extract consists of solid impurities such as metallic carbon particles. Specifically, the first extract is discharged intermittently from the bottom outlet of the stripping tower 303 for solid impurities such as metal carbon particles. Before discharging the first extract, water vapor must be blown into the stripping tower 303 for solid impurities such as metal carbon particles. The flow rate of the blown water vapor is 5 to 10% of the weight of the first extract, and the blowing time is not less than 120 minutes.

[0025] Step S400: The first extract is subjected to separation treatment at least five times to obtain at least five extracts.

[0026] In step S500, the asphalt and resin are blended in a certain proportion to form high-end carbon raw materials such as coated asphalt. The proportion of asphalt in the coated asphalt raw material is 30% to 70%, and the proportion of resin in the coated asphalt raw material is 70% to 30%.

[0027] Specifically, the proportion of asphalt in the coated asphalt raw material can be adjusted to any one of 40%, 50%, or 60%, or a range between any two of these values; the proportion of resin in the coated asphalt raw material can be adjusted to any one of 60%, 50%, or 40%, or a range between any two of these values. Step S600, fluid recovery and recycling: the water-insoluble fluid in the mixing cooler 501 is transferred to the low-pressure fluid recovery tank 503, then pressurized by the low-pressure fluid compressor 504 and transferred to the medium-pressure fluid recovery tank 502, and then heat-exchanged to 155℃~225℃ by the fluid heat exchanger 505 before being transferred to the inlet end of the fluid booster pump 304.

[0028] This application provides a method for supercritical fluid extraction and separation of coal ethyl tar. By fully mixing liquid coal ethyl tar with a reagent solution, the reagent solution is used to demulsify, strongly disperse, and penetrate the coal ethyl tar, while also carrying out light components. This avoids severe emulsification caused by mixing supercritical fluid with coal ethyl tar, thereby improving the extraction effect and efficiency of supercritical fluid. By introducing supercritical fluid and combining it with countercurrent extraction, the useful substances in coal ethyl tar are fully dissolved in the supercritical fluid, thereby removing solid impurities such as metal carbon particles. Then, through at least five separation processes, substances such as asphaltene, gum, 5-8 ring aromatics, anthracene oil, and saturated hydrocarbons are separated, thereby improving the purity of the extracted substances and the quality of the product.

[0029] Please see Figure 4 In some embodiments, the method and apparatus for supercritical fluid extraction and separation of coal ethyl tar include an extraction apparatus comprising a liquid coal ethyl tar output unit 100, a reagent supply unit 200, an extraction unit 300, a separation unit 400, a fluid supply unit 500, and a steam pipeline 600. The liquid coal ethyl tar output unit 100 includes a melting tank 101, a coal ethyl tar extraction pump 102, and a first heating coil 103. The outlet end of the melting tank 101 is connected to the inlet end of the coal ethyl tar extraction pump 102. The outlet end of the coal ethyl tar extraction pump 102 is connected in parallel to the liquid coal tar pitch 800 feed pipeline and then connected to the axial inlet end of the mixer 203. The inlet end of the first heating coil 103 is connected to the steam pipeline 600.

[0030] The liquid coal ethyl tar in step S100 is obtained through the following steps: S101 provides solid coal tar pitch 700 to be processed. In this embodiment, the density of the coal tar pitch is 0.98 g / cm³ under normal temperature conditions. 3 ~1.30g / cm 3 Its softening point is between 35℃ and 95℃; S102 provides ethylene tar to be processed, wherein the density of the ethylene tar is 1.01 g / cm³ at room temperature. 3 ~1.25g / cm 3 , S103 The solid coal tar pitch is placed in the melting tank 101 at a ratio of 10-90%, and the ethylene tar is placed in the melting tank 101 at a ratio of 90-10%. Specifically, the solid coal tar pitch can be adjusted to any one of 20%, 30%, 40%, 50%, 60%, 70%, 80% or any range between any two values ​​and placed in the melting tank 101, and the ethylene tar can be adjusted to any one of 80%, 70%, 60%, 50%, 40%, 30%, 20% or any range between any two values ​​and placed in the melting tank 101.

[0031] S104 uses the first heating coil 103 to heat the material in the melting tank 101, so that the solid coal tar pitch melts and is stirred and mixed with the ethylene tar to form liquid coal ethylene tar, wherein the temperature of the coal ethylene tar after heat treatment is 155℃~225℃.

[0032] In this embodiment, a first heating coil 103 is provided outside the melting tank 101. The first heating coil 103 is connected to the steam pipeline 600, and the steam pipeline 600 outputs low-pressure or medium-pressure steam to the first heating coil 103 to heat the melting tank 101. The solid coal tar in the melting tank 101 is melted and mixed with ethylene tar to form liquid coal ethylene tar, which is then extracted by the coal ethylene tar extraction pump 102 and transported to the extraction unit 300.

[0033] In other embodiments, the first heating coil 103 can also be connected to a thermal oil furnace, through which thermal oil is introduced into the first heating coil 103 to heat the melting tank 101, so that the solid coal tar pitch in the melting tank 101 melts and is stirred and mixed with ethylene tar to form liquid coal ethylene tar.

[0034] In other embodiments, liquid coal tar pitch 800 and ethylene tar can be directly transported from the outside to mix with the pharmaceutical solution to form a mixture.

[0035] This application embodiment provides a liquid coal ethyl tar output unit 100 and related preparation steps to provide molten coal ethyl tar in a liquid state for mixing with the pharmaceutical solution. This fully utilizes the pharmaceutical solution to demulsify, strongly disperse, and penetrate the coal ethyl tar, thereby improving the supercritical fluid extraction and separation rate to meet the needs of continuous large-scale industrial production.

[0036] Please see Figure 4 As shown, in some embodiments, the drug supply unit 200 includes a drug tank 201, a dosing pump 202, and a mixer 203. The drug tank 201 is connected to the input end of the dosing pump 202, the output end of the dosing pump 202 is connected to the radial inlet of the mixer 203, the axial inlet of the mixer 203 is connected to the output end of the coal ethyl tar extraction pump 102, and the axial outlet of the mixer 203 is connected to the extraction unit 300.

[0037] S105, in some embodiments, the liquid comprises a drug and diesel fuel, which are mixed under normal temperature and pressure conditions.

[0038] In some embodiments, the mass percentage concentration of the drug in the drug solution is 1% to 30%. Specifically, the mass percentage concentration of the drug can be set to any one of 1%, 2%, 5%, 10%, 15%, 20%, 25%, and 30%, or a range between any two of these values.

[0039] In some embodiments, the drug is selected from at least one of polyacrylic acid, fatty alcohol ether phosphate, sulfonic acid and sulfonate, sulfate, maleic anhydride sulfonate, alkyl sulfonate, methanol, and toluene; Please see Figure 4 As shown, step S100, which involves mixing the liquid coal ethyl tar with the pharmaceutical solution to form a first mixed solution, specifically includes the following steps: S106, the coal ethyl tar extraction pump 102 extracts liquid coal ethyl tar and inputs it into the mixer 203 from the axial inlet end; the dosing pump 202 extracts liquid chemicals and inputs them into the mixer 203 from the radial inlet end; the liquid coal ethyl tar and the liquid chemicals are fully mixed in the mixer 203 to form a mixture, which is then output from the axial outlet end of the mixer 203.

[0040] In some embodiments, the amount of the drug solution added to the mixture is 1.5% to 2% of the liquid coal ethyl tar. Specifically, the amount of the drug solution added is any one or any two values ​​of 1.5%, 1.6%, 1.7%, 1.8%, 1.9%, or 2% of the liquid coal ethyl tar.

[0041] In this embodiment, liquid coal ethyl tar and a chemical solution are thoroughly mixed in a mixer 203 to form a mixture. The chemical solution demulsifies, strongly disperses, and penetrates the coal ethyl tar, while simultaneously carrying out light components (such as asphaltenes, gums, 5-8 ring aromatics, anthracene oil, and saturated hydrocarbons). This facilitates the separation of solid impurities such as metals and carbon particles from the coal ethyl tar in a very short time. Then, through at least five separation processes, asphaltenes, gums, 5-8 ring aromatics, anthracene oil, and saturated hydrocarbons are separated, thereby improving the purity of the extracted substances and the quality of the product.

[0042] The extraction unit 300 includes a mixed liquid booster pump 301, an extractor 302, a mixed liquid feed distributor 306, a fluid booster pump 304, a stripping tower for solid impurities such as metal carbon particles 303, and a second heating coil 305. The outlet end of the mixed liquid booster pump 301 is connected to the top inlet end of the extractor 302 to inject the mixed liquid into the extractor. The outlet end of the fluid booster pump 304 is connected to the bottom inlet end of the extractor to inject supercritical fluid into the extractor. The inlet end of the stripping tower for solid impurities such as metal carbon particles 303 is connected to the bottom outlet end of the extractor to output a mixture of the first extract and the residual fluid. The second heating coil 305 is located outside the cylinder of the extractor 302 to heat the material at the bottom of the extractor 302.

[0043] Specifically, the height-to-diameter ratio of the extractor 302 is from 5:1 to 30:1. The height-to-diameter ratio of the extractor 302 can be adjusted to any one of 6:1, 7:1, 8:1, 9:1, 10:1, 15:1, 20:1, 25:1 or any range between any two values. The extractor 302 is equipped with a mixed liquid feed distributor 306, which is used to directly transfer the mixed liquid to the packing ring layer and disperse it into the packing ring layer. The extractor 302 is also equipped with a packing ring, which is used to allow the mixed liquid to fully contact the supercritical fluid in a countercurrent manner.

[0044] In some embodiments, before introducing the mixture and the supercritical fluid into the two ends of the extractor 302, step S300 further includes the following steps: The mixture is subjected to a second pressurization treatment.

[0045] In this embodiment, the mixture is output from the axial outlet end of the mixer 203 to the inlet end of the mixture booster pump 301. The mixture booster pump 301 performs a second pressurization process on the mixture. After the second pressurization process is completed, the pressure of the mixture is 4MPa to 16MPa.

[0046] In some embodiments, before introducing the mixture and the supercritical fluid into the two ends of the extractor 302, step S300 further includes the following steps: In this embodiment, the fluid is output from the bottom outlet of the medium-pressure fluid recovery tank 502, and after heat exchange in the fluid heat exchanger 505, it is sent to the inlet of the fluid booster pump 304. The fluid booster pump 304 performs a first pressurization process on the fluid. After the first pressurization process is completed, the fluid is converted into the supercritical fluid.

[0047] Specifically, the supercritical fluid can only be input into the extraction unit 300 when it forms a closed loop in the extraction unit 300, the separation unit 400, and the fluid supply unit 500 and is operating normally. Only in this way can the supercritical fluid continuously circulate into the mixture and extract the desired substances.

[0048] The supercritical fluid has a pressure of 4 MPa to 16 MPa, a temperature of 155°C to 225°C, and a concentration of 95% to 99.9%.

[0049] Please continue reading. Figure 1 As shown, in some embodiments, after the mixture and the supercritical fluid are introduced into both ends of the extractor in step S300, the ratio of the mixture to the supercritical fluid in the extractor is 1:5 to 1:15. Specifically, the ratio of the mixture to the supercritical fluid in the extractor can be set to any one of 1:5, 1:6, 1:8, 1:10, 1:12, 1:15 or a range formed between any two values.

[0050] In this embodiment, because the solid impurities such as metals and carbon particles in the coal ethyl tar have the largest molecular weight, the strongest force, and the strongest polarity, they are difficult to separate. The remaining impurities, such as asphaltenes, gums, 5-8 ring aromatics, anthracene oil, and saturated hydrocarbons, decrease in strength in that order. Therefore, by setting the ratio of the mixture to the supercritical fluid, solid impurities such as metals and carbon particles can be separated in a short time, followed by the separation of asphaltenes, gums, 5-8 ring aromatics, anthracene oil, and saturated hydrocarbons, thereby improving the extraction efficiency of the supercritical fluid. Please refer to [link to relevant documentation]. Figure 4 As shown, in some embodiments, the extraction unit 300 further includes a second heating coil 305, which is sleeved outside the extractor 302 and connected to a steam supply pipeline 600. The steam supply pipeline 600 transmits low-pressure or medium-pressure steam to the second heating coil 305, which heats the extractor 302 to maintain the temperature of the material inside the extractor 302 above 100°C, ensuring that the coal ethyl tar remains liquid and preventing condensation inside the extractor 302 that could cause blockage.

[0051] In some embodiments, the mixture is introduced from the top of the extractor 302, and the supercritical fluid is introduced from the bottom of the extractor 302. The mixture and the supercritical fluid are continuously countercurrently extracted in the extractor 302 to obtain a first extract and a first extract. The first extract is discharged from the upper end of the extractor 302, and the first extract and a mixture of residual fluid are discharged from the lower end of the extractor 302.

[0052] In this embodiment, the first extract includes solid impurities such as metallic carbon particles. The solid impurities are substances with the largest molecular weight, the greatest force, and the strongest polarity that cannot be dissolved. The first extract liquid includes asphaltenes, gums, 5-8 ring aromatics, anthracene oil, saturated hydrocarbons, and supercritical fluids.

[0053] This embodiment of the application adjusts the pressure of the mixture and the supercritical fluid, as well as the temperature within the extractor 302, to regulate the solubility of the supercritical fluid. This allows the light components of liquid coal ethyl tar (such as asphaltenes, gums, 5-8 ring aromatics, anthracene oil, and saturated hydrocarbons) to fully dissolve in the supercritical fluid, eliminating solid impurities such as metallic carbon particles from the coal ethyl tar. Then, through at least six separation processes, asphaltenes, gums, 5-8 ring aromatics, anthracene oil, and saturated hydrocarbons are separated, thereby improving the purity of the extract and the quality of the product.

[0054] For further details, please refer to Figure 4As shown, in some embodiments, the separation unit 400 includes, in sequence, the outlet end of a first pressure reducing valve 401, the tube-side inlet and outlet ends of a first heater 402, the top inlet and upper outlet ends of a first separator 403, the outlet end of a second pressure reducing valve 404, the tube-side inlet and outlet ends of a second heater 405, the top inlet and upper outlet ends of a second separator 406, the outlet end of a third pressure reducing valve 407, the tube-side inlet and outlet ends of a third heater 408, the top inlet and upper outlet ends of a third separator 409, the outlet end of a fourth pressure reducing valve 410, the tube-side inlet and outlet ends of a fourth heater 411, the top inlet and upper outlet ends of a fourth separator 412, the outlet end of a fifth pressure reducing valve 413, the tube-side inlet and outlet ends of a saturated hydrocarbon heat exchanger 414, the top inlet and upper outlet ends of a fifth separator 415, and the inlet end of a sixth pressure reducing valve 416. The inlet end of the first pressure reducing valve 401 is connected to the top outlet end of the extractor 302, and the outlet end of the seventh pressure reducing valve 419 is connected to the inlet end of the medium-pressure fluid recovery tank 502. The separation unit 400 further includes, in sequence, the inlet and outlet ends of the asphalt heating furnace 403 / 1, the inlet and bottom outlet ends of the asphalt evaporation tower 403 / 2, and the inlet and bottom outlet ends of the asphalt stripping tower 403 / 3 connected to the bottom outlet end of the first separator 403; the inlet and outlet ends of the colloidal pressure reducing valve 406 / 1, the shell-side inlet and outlet ends of the colloidal heat exchanger 406 / 2, the inlet and bottom outlet ends of the colloidal critical tower 406 / 3, the inlet and bottom outlet ends of the colloidal evaporation tower 406 / 4, and the inlet and bottom outlet ends of the colloidal stripping tower 406 / 5 connected to the bottom outlet end of the second separator 406; and the inlet and outlet ends of the 5-8 ring aromatics pressure reducing valve 409 / 1 and the shell-side outlet ends of the 5-8 ring aromatics heat exchanger 409 / 2 connected to the bottom outlet end of the third separator 409. The inlet and shell-side outlet ends of the anthracene oil pressure reducing valve 412 / 1, the shell-side inlet and shell-side outlet ends of the anthracene oil heat exchanger 412 / 2, the inlet and bottom outlet ends of the anthracene oil critical tower 412 / 3, the inlet and bottom outlet ends of the anthracene oil evaporator 412 / 4, and the inlet and bottom outlet ends of the anthracene oil stripping tower 412 / 5 are sequentially connected to the bottom outlet end of the fourth separator 412. The inlet and bottom outlet ends of the saturated hydrocarbon evaporator 415 / 1 and the inlet and bottom outlet ends of the saturated hydrocarbon stripping tower 415 / 2 are sequentially connected to the bottom outlet end of the fifth separator 415. The four outlets of the colloidal critical tower 406 / 3, the 5-8 ring aromatics critical tower 409 / 3, the anthracene oil critical tower 412 / 3, and the upper outlet of the fifth separator 415 are connected in parallel and then connected to the inlet of the medium-pressure fluid recovery tank 502. This connection is used to recover the medium-pressure fluid in a critical state released from the top of the four devices. The top outlets of the five evaporators—asphaltite evaporator 403 / 2, gum evaporator 406 / 4, 5-8 ring aromatic hydrocarbon evaporator 409 / 4, anthracene oil evaporator 412 / 4, and saturated hydrocarbon evaporator 415 / 1—are connected in parallel and then connected to the inlet of a low-pressure fluid recovery tank. This connection is used to recover the residual fluid released from the five evaporators. The residual fluid is pressurized by a low-pressure fluid compressor and then transferred to a medium-pressure fluid recovery tank for recycling by the extraction unit. The top outlets of the six stripping towers—303 (for solid impurities such as metal carbon particles), 403 / 3 (for asphalt), 406 / 5 (for gum), 409 / 5 (for 5-8 ring aromatics), 412 / 5 (for anthracene oil), and 415 / 2 (for saturated hydrocarbons)—are connected in parallel and then connected to the inlet of a mixing cooler. This is used to recover the fluid resulting from the mixture of residual fluid released from the six stripping towers and water vapor. After condensation and dehydration, the residual fluid is transferred via pipeline to a low-pressure fluid recovery tank. The wastewater separated from the mixed fluid is transferred to a wastewater treatment unit. Please see Figure 3 As shown, in this embodiment, step S400 performs at least five separation processes on the first extract to obtain at least five extracts, specifically including the following steps: S401, the first extract is passed into the first separator, and the first extract is separated in the first separator 403 to obtain a second extract, a second extract and a mixture of residual fluid. The second extract and the mixture of residual fluid are further separated to obtain a second extract, which is asphaltenes.

[0055] In this embodiment, the first extract is discharged from the extractor 302 to the first pressure reducing valve 401. The first pressure reducing valve 401 adjusts the pressure of the first extract to 4 MPa to 14 MPa. Specifically, the pressure of the first extract can be adjusted to any one of 4 MPa, 6 MPa, 8 MPa, 10 MPa, 12 MPa, and 14 MPa, or a range formed between any two of these values.

[0056] The first extract enters the first heater 402 after passing through the first pressure reducing valve 401. The first heater 402 adjusts the temperature of the first extract to 150℃~220℃. Specifically, the temperature of the first extract can be adjusted to any one of 150℃, 170℃, 190℃, and 210℃ or a range formed between any two of these values.

[0057] The second extract is discharged from the upper end of the first separator 403 and introduced into the second separator 406. The mixture of the second extract and residual fluid is discharged from the bottom outlet of the first separator 403. The mixture of the second extract and residual fluid is then transferred to the asphalt heating furnace 403 / 1 or the thermal oil furnace for heating, and then enters the asphalt evaporation tower 403 / 2 for evaporation to remove the remaining residual fluid. After evaporation, the mixture is transferred from the bottom outlet of the tower 403 / 2 to the asphalt stripping tower 403 / 3 for stripping to remove a small amount of residual fluid. The second extract is then discharged from the bottom of the asphalt stripping tower 403 / 3. The removal of the remaining residual fluid and the removal of a small amount of residual fluid are all collected in a medium-pressure fluid recovery tank through pipelines and equipment for recycling. In this embodiment, the second extract is asphaltenes.

[0058] Specifically, because the density and viscosity of the asphaltene are greater than those of the gums, 5-8 ring aromatics, anthracene oil, and other compounds, the residual fluid contained in the asphaltene is difficult to vaporize and remove. Therefore, a heating furnace must be installed at the bottom outlet of the first separator to provide heat to the mixture of the second extract and the residual fluid. Only after the temperature of the mixture of asphaltene and residual fluid reaches 210-285°C can it be transferred to the evaporation tower and stripping tower to continue releasing the contained residual fluid.

[0059] Specifically, stripping steam is blown into the asphalt stripping tower 403 / 3, and the amount of steam blown is 0 to 3% of the feed amount of the asphalt stripping tower 403 / 3.

[0060] The above description also applies to the four stripping towers: the colloidal stripping tower 406 / 5, the 5-8 ring aromatics stripping tower 409 / 5, the anthracene oil stripping tower 412 / 5, and the saturated hydrocarbon stripping tower 415 / 2, wherein the temperature of the stripping towers is 155-250℃.

[0061] Specifically, the upper part of the asphalt evaporation tower 403 / 2 is equipped with a foam separation net to prevent the extract from being carried out by the residual fluid, which would affect the separation effect and the fluid quality. The temperature of the evaporation tower is 160-285℃.

[0062] The above description also applies to the four evaporation towers: colloidal evaporation tower 406 / 4, 5-8 ring aromatic evaporation tower 409 / 4, anthracene oil evaporation tower 412 / 4, and saturated hydrocarbon evaporation tower 415 / 1.

[0063] S402, the second extract is passed into the second separator, and the second extract is separated in the second separator 406 to obtain a third extract and a mixture of the third extract and residual fluid. The mixture of the third extract and residual fluid is further separated to obtain a third extract, which is a colloid.

[0064] In this embodiment, the second extract is discharged from the first separator 403 to the second pressure reducing valve 404. The second pressure reducing valve 404 adjusts the pressure of the second extract to 4 MPa to 12 MPa. Specifically, the pressure of the second extract can be adjusted to any one of 4 MPa, 6 MPa, 8 MPa, and 10 MPa or a range formed between any two of these values.

[0065] The second extract enters the second heater 405 after passing through the second pressure reducing valve 404. The second heater 405 adjusts the temperature of the second extract to 145℃~215℃. Specifically, the temperature of the second extract can be adjusted to any one of 155℃, 180℃, 195℃, and 200℃, or a range formed between any two of these values.

[0066] The third extract is discharged from the upper end of the second separator 406 and introduced into the third separator 409. The mixture of the third extract and residual fluid is discharged from the lower end of the second separator 406. The mixture of the third extract and residual fluid is regulated to the critical pressure by the colloidal regulating valve 406 / 1, then transferred to the colloidal heat exchanger 406 / 2 to be regulated to the critical temperature, and then transferred to the colloidal critical tower 406 / 3 to release a large amount of residual fluid. After being discharged from the bottom outlet of the critical tower 406 / 3, it is transferred to the colloidal evaporation tower 406 / 4 to evaporate and remove the remaining residual fluid. After being discharged from the bottom outlet of the colloidal evaporation tower 406 / 4, it is transferred to the colloidal stripping tower 406 / 5 to strip and remove a small amount of residual fluid. Finally, the third extract is discharged from the bottom outlet of the colloidal stripping tower 406 / 5. The above-mentioned processes of releasing a large amount of residual fluid, removing the remaining residual fluid, and removing a small amount of residual fluid are all collected by pipelines and equipment into a medium-pressure fluid recovery tank for recycling. The third extract is a gel; Specifically, because the fluid selected in this application has very low solubility in hydrocarbons under critical conditions, and coal ethyl tar is also a hydrocarbon, this characteristic is utilized to control the pressure and temperature of the mixture of the third extract and the residual fluid to the critical conditions of the fluid. When the mixture of the third extract and the residual fluid enters the critical column 406 / 3, a large amount of residual fluid will automatically be released from the mixture and discharged from the top outlet of the critical column 406 / 3, and transferred to the medium-pressure fluid recovery tank 502. The above description also applies to the three devices operating in a critical state: the 5-8 ring aromatic hydrocarbon critical tower 409 / 3, the anthracene oil critical tower 412 / 3, and the fifth separator 415.

[0067] In this embodiment, the third extract is a gel.

[0068] S403, the third extract is passed into the third separator, and the third extract is separated in the third separator 409 to obtain a fourth extract, a fourth extract and a mixture of residual fluid. The fourth extract and the mixture of residual fluid are further separated to obtain a fourth extract, which is a 5-8 ring aromatic hydrocarbon.

[0069] In this embodiment, the third extract is discharged from the second separator 406 to the third pressure reducing valve 410. The third pressure reducing valve 410 adjusts the pressure of the third extract to 4 MPa to 9 MPa. Specifically, the pressure of the third extract can be adjusted to any one of 4 MPa, 6 MPa, and 8 MPa, or a range formed between any two of these values.

[0070] The third extract enters the third heater 408 after passing through the third pressure reducing valve 407. The third heater 408 adjusts the temperature of the third extract to 142℃~210℃. Specifically, the temperature of the third extract can be adjusted to any one of 146℃, 170℃, 190℃, and 200℃, or a range formed between any two of these values.

[0071] The fourth extract is discharged under reduced pressure from the upper outlet of the third separator 409 and fed into the fourth separator 412. The mixture of the fourth extract and residual fluid is discharged from the bottom outlet of the third separator 409. The mixture of the fourth extract and residual fluid is regulated to the critical pressure using a 5-8 ring aromatics regulating valve 409 / 1, regulated to the critical temperature using a 5-8 ring aromatics heat exchanger 409 / 2, and then transferred to a 5-8 ring aromatics critical tower 409 / 3 to release a large amount of residual fluid before being discharged from the bottom outlet of the critical tower 409 / 3 and transferred to a 5-8 ring aromatics evaporator 409. After the remaining residual fluid is removed by evaporation in column 409 / 4, it is discharged from the bottom outlet of column 409 / 4 and transferred to column 409 / 5 for stripping to remove a small amount of residual fluid. Then, the fourth extract is discharged from the bottom outlet of column 409 / 5. The above-mentioned release of a large amount of residual fluid, removal of the remaining residual fluid, and removal of a small amount of residual fluid are all collected by pipelines and equipment into a medium-pressure fluid recovery tank for recycling. The fourth extract is 5-8 ring aromatics. In this embodiment, the fourth extract is 5-8 ring aromatics.

[0072] S404, the fourth extract is passed into the fourth separator, and the fourth extract is separated in the fourth separator 412 to obtain a fifth extract, a fifth extract and a mixture of residual fluid. The fifth extract and the mixture of residual fluid are further separated to obtain a fifth extract, which is anthracene oil.

[0073] In this embodiment, the fourth extract is discharged from the fourth separator 412 to the fifth pressure reducing valve 413. The fifth pressure reducing valve 413 adjusts the pressure of the fourth extract to 4 MPa to 7 MPa. Specifically, the pressure of the fourth extract can be adjusted to any one of 4 MPa and 6 MPa or a range between any two values.

[0074] The fourth extract enters the fourth heater 411 after passing through the fourth pressure reducing valve 410. The fourth heater 411 adjusts the temperature of the fourth extract to 140℃~205℃. Specifically, the temperature of the fourth extract can be adjusted to any one of 143℃, 160℃, 180℃, and 190℃, or a range formed between any two of these values.

[0075] The fifth extract is discharged under reduced pressure from the upper outlet of the fourth separator 412 and fed into the fifth separator 415. The mixture of the fifth extract and residual fluid is discharged from the bottom outlet of the fourth separator 412. The mixture of the fifth extract and residual fluid is regulated to the critical pressure by the anthracene oil regulating valve 412 / 1, and to the critical temperature by the anthracene oil heat exchanger 412 / 2. It is then transferred to the anthracene oil critical tower 412 / 3 to release a large amount of residual fluid. After that, it is discharged from the bottom outlet of the critical tower 412 / 3 and transferred to the anthracene oil evaporator 412 / 4 to evaporate and remove the remaining residual fluid. After that, it is discharged from the bottom outlet of the anthracene oil evaporator 412 / 4 and transferred to the anthracene oil stripping tower 412 / 5 to strip and remove a small amount of residual fluid. Finally, the fifth extract is discharged from the bottom outlet of the anthracene oil stripping tower 412 / 5. All the above-mentioned processes of releasing a large amount of residual fluid, removing the remaining residual fluid, and removing a small amount of residual fluid are collected in a medium-pressure fluid recovery tank through pipelines and equipment for recycling. In this embodiment, the fifth extract is anthracene oil.

[0076] S405, the fifth extract is passed into the fifth separator, and the fifth extract is separated in the fifth separator 415 to obtain a mixture of fluid in the critical state, a sixth extract and a residual fluid. The mixture of the sixth extract and the residual fluid is further separated to obtain a sixth extract, which is a saturated hydrocarbon.

[0077] In this embodiment, the pressure of the sixth separator 415 is controlled at the critical pressure of the fluid, and the temperature is controlled at the critical temperature of the fluid. The seventh extract is already a fluid in a critical state. The critical state fluid is discharged from the upper outlet of the sixth separator 415 and fed into the medium-pressure fluid recovery tank 502. The mixture of the sixth extract and residual fluid is discharged from the bottom outlet of the sixth separator 415. The mixture of the sixth extract and residual fluid is fed into the saturated evaporation tower 415 / 1 to evaporate the remaining residual fluid. After evaporation, the mixture is discharged from the bottom outlet of the tower 415 / 1 and transferred to the saturated hydrocarbon stripping tower 415 / 2 for stripping to remove a small amount of residual fluid. The sixth extract is discharged from the bottom outlet of the saturated hydrocarbon stripping tower 415 / 2. The removal of the remaining residual fluid and the removal of a small amount of residual fluid are all collected in the medium-pressure fluid recovery tank by pipelines and equipment for recycling. The sixth extract is saturated hydrocarbon.

[0078] The fluid supply unit 500 includes a mixing cooler 501, a medium-pressure fluid recovery tank 502, a low-pressure fluid recovery tank 503, a low-pressure fluid compressor 504, and a fluid heat exchanger 505. The top outlet of the mixing cooler 501 is connected to the inlet of the low-pressure fluid recovery tank 503. The top outlet of the low-pressure fluid recovery tank 503 is connected to the inlet of the low-pressure fluid compressor 504. The outlet of the low-pressure fluid compressor 504 is connected to the inlet of the medium-pressure fluid recovery tank 502. The other inlet of the medium-pressure fluid recovery tank 502 is connected to the outside. If the medium-pressure fluid is consumed or its concentration decreases, fluid can be replenished from a fluid storage tank outside the device. The bottom outlet of the medium-pressure fluid recovery tank 502 is connected to the inlet of the fluid heat exchanger 505 shell. The outlet of the fluid heat exchanger 505 shell is connected to the inlet of the fluid booster pump 304.

[0079] Specifically, the fluid temperature at the top outlet of the mixing cooler 501 is ≤60℃, the fluid temperature at the shell outlet of the heat exchanger 505 is ≥155℃~225℃, and the concentration of the fluid is 95%~99.9%.

[0080] Furthermore, the steam pipeline 600 is connected to the steam inlet ends of 19 pieces of equipment, including the first heater, second heater, third heater, fourth heater, fluid heat exchanger, asphalt evaporation tower, colloidal evaporation tower, 5-8 ring aromatic hydrocarbon evaporation tower, anthracene oil evaporation tower, saturated hydrocarbon evaporation tower, first heating coil, second heating coil, asphalt stripping tower, colloidal stripping tower, 5-8 ring aromatic hydrocarbon stripping tower, anthracene oil stripping tower, saturated hydrocarbon stripping tower, and solid impurity stripping tower 303 (such as metal carbon particle stripping tower), for heating the materials in the equipment. The steam condensate after heat exchange with the materials in the equipment is connected to the condensate recovery pipeline. If the steam condensate is contaminated by the materials, it is connected to the sewage system.

[0081] This application provides a supercritical fluid extraction device, which, in conjunction with a supercritical fluid extraction method for separating coal ethyl tar, can improve the extraction and separation effect and efficiency of supercritical fluid, thereby increasing the purity and product quality of the extracted substances. Simultaneously, through at least six separation processes, useful substances in coal ethyl tar are separated. The operation is simple, does not require the addition of large amounts of solvent, and further improves the product quality of the extracted substances.

[0082] Obviously, the embodiments described above are only some embodiments of this application, not all embodiments. The accompanying drawings show preferred embodiments of this application, but do not limit the patent scope of this application. This application can be implemented in many different forms; rather, the purpose of providing these embodiments is to provide a more thorough and comprehensive understanding of the disclosure of this application. Although this application has been described in detail with reference to the foregoing embodiments, those skilled in the art can still modify the technical solutions described in the foregoing specific embodiments, or make equivalent substitutions for some of the technical features. Any equivalent structures made using the content of this application's specification and drawings, directly or indirectly applied to other related technical fields, are similarly within the scope of patent protection of this application.

Claims

1. A method for supercritical fluid extraction and separation of coal ethyl tar, characterized in that, Includes the following steps: Liquid coal ethyl tar and a pharmaceutical solution are provided, and the liquid coal ethyl tar and the pharmaceutical solution are mixed to form a mixture; A supercritical fluid is provided, and the mixture and the supercritical fluid are respectively input to both ends of the extractor. The mixture and the supercritical fluid flow counterclockwise to extract a first extract, a first extract, and a mixture of residual fluid. The first extract is discharged under reduced pressure from the upper outlet of the extractor, and the first extract and residual fluid mixture are discharged from the lower outlet of the extractor. The first extract includes compounds such as asphaltenes, gums, 5-8 ring aromatics, anthracene oil, saturated components, and supercritical fluid. The first extract consists of solid impurities such as metals and carbon particles. The first extract was subjected to at least five separation processes to obtain at least five extracts. Asphalt and resin are blended in a specific ratio to synthesize high-end carbon raw materials such as coated asphalt.

2. The method for supercritical fluid extraction and separation of coal ethyl tar according to claim 1, characterized in that, The liquid coal ethyl tar is prepared through the following steps: The solid coal tar to be processed is placed in a melting tank, and ethylene tar is added in proportion. The material in the melting tank is heated using a first heating coil, causing the solid coal tar pitch to melt and then mix with ethylene tar to form liquid coal ethylene tar. The solid coal tar pitch is added in a proportion of 10%–90%, the ethylene tar is added in a proportion of 90%–10%, and the temperature of the liquid coal ethylene tar is 155℃–225℃. The density of the coal tar pitch at 20°C is 0.98 g / cm³. 3 ~1.30g / cm 3 The ethylene tar has a density of 1.02 g / cm³ at 20°C. 3 ~1.25g / cm 3 .

3. The method for supercritical fluid extraction and separation of coal ethyl tar according to claim 1, characterized in that, The fluid includes any one of fluorine, isopentane, isobutane, isopentane, n-butane, n-pentane, and propane. The purity of the fluid is 95% to 99.9%. The temperature of the fluid is 155℃~225℃.

4. The method for supercritical fluid extraction and separation of coal ethyl tar according to claim 1, characterized in that, Before the step of introducing the mixture and supercritical fluid into both ends of the extractor respectively, the following steps are also included: The fluid is subjected to a first pressurization treatment to form the supercritical fluid, wherein the temperature of the fluid is 155℃~225℃, and the pressure of the supercritical fluid after the first pressurization treatment is 4MPa~16MPa; The mixture is subjected to a second pressurization treatment, wherein after the second pressurization treatment, the pressure of the mixture is 4 MPa to 16 MPa; and the temperature of the mixture is 155°C to 225°C. In the extractor, the ratio of the mixture to the supercritical fluid is 1:5 to 1:15, and the height-to-diameter ratio of the extractor is 5:1 to 30:

1.

5. The method for supercritical fluid extraction and separation of coal ethyl tar according to claim 1, characterized in that, The solution comprises a drug and diesel fuel, wherein the drug is selected from at least one of polyacrylic acid, fatty alcohol ether phosphate, sulfonic acid and sulfonates, sulfate esters, maleic anhydride sulfonate, alkyl sulfonates, methanol, and toluene; wherein the mass percentage concentration of the drug in the solution is 1% to 50%. The amount of the added drug solution is 1.0% to 2.0% of the liquid coal ethyl tar.

6. The method for supercritical fluid extraction and separation of coal ethyl tar according to claim 1, characterized in that, The first extract output under reduced pressure from the upper outlet of the extractor is subjected to at least five separation processes to obtain at least five extracts, including the following steps: The first extract, which is depressurized and output from the upper outlet of the extractor, is fed into the first separator. Within the first separator, the first extract is separated to obtain a second extract, a second extract, and a mixture of residual fluid. The first separator has a pressure of 4 MPa to 14 MPa and a temperature of 150°C to 220°C. The second extract is depressurized and discharged from the upper outlet of the first separator and fed into the second separator. The mixture of the second extract and residual fluid is discharged from the bottom outlet of the first separator. This mixture is then transferred to an asphalt heating furnace or a thermal oil furnace for heating, and then enters an asphalt evaporation tower to evaporate and remove the remaining residual fluid. After evaporation, it is transferred from the bottom outlet to an asphalt stripping tower to strip away a small amount of residual fluid. The second extract is then discharged from the bottom of the asphalt stripping tower. All steps of removing the remaining residual fluid and removing a small amount of residual fluid are collected in a medium-pressure fluid recovery tank via pipelines and equipment for recycling. The second extract is asphaltenes; The second extract, which is depressurized and output from the upper outlet of the first separator, is fed into the second separator. Inside the second separator, the second extract is separated to obtain a third extract, a third extract, and a mixture of residual fluid. The pressure of the second separator is 4 MPa to 12 MPa, and the temperature is 145°C to 215°C. The third extract is depressurized and discharged from the upper outlet of the second separator and fed into the third separator. The mixture of the third extract and residual fluid is discharged from the bottom outlet of the second separator. The mixture of the third extract and residual fluid is regulated to the critical pressure using a colloidal regulating valve, and then transferred to a colloidal heat exchanger to be regulated to the critical temperature. After releasing a large amount of residual fluid in the colloidal critical column, it is discharged from the bottom outlet of the critical column and transferred to a colloidal evaporator to evaporate and remove the remaining residual fluid. After evaporation, it is discharged from the bottom outlet of the colloidal evaporator and transferred to a colloidal stripping column to strip and remove a small amount of residual fluid. Finally, the third extract is discharged from the bottom outlet of the colloidal stripping column. The release of a large amount of residual fluid, removal of the remaining residual fluid, and removal of a small amount of residual fluid are all collected in a medium-pressure fluid recovery tank through pipelines and equipment for recycling. The third extract is a gel; The third extract, which is depressurized and output from the upper outlet of the second separator, is fed into the third separator. Inside the third separator, the third extract is separated to obtain a fourth extract, a fourth extract, and a mixture of residual fluid. The pressure of the third separation process is 4 MPa to 9 MPa, and the temperature is 142°C to 210°C. The fourth extract is discharged under reduced pressure from the upper outlet of the three separators and fed into the fourth separator. The mixture of the fourth extract and residual fluid is discharged from the bottom outlet of the third separator. The mixture of the fourth extract and residual fluid is regulated to the critical pressure using a 5-8 ring aromatics regulating valve, then transferred to a 5-8 ring aromatics heat exchanger and regulated to the critical temperature. It is then transferred to a 5-8 ring aromatics critical tower to release a large amount of residual fluid, which is then discharged from the bottom outlet of the critical tower and transferred to a 5-8 ring aromatics evaporator to evaporate and remove the remaining residual fluid. The remaining residual fluid is then discharged from the bottom outlet of the 5-8 ring aromatics evaporator and transferred to a 5-8 ring aromatics stripping tower for stripping to remove a small amount of residual fluid. Finally, the fourth extract is discharged from the bottom outlet of the 5-8 ring aromatics stripping tower. All the processes described above—releasing a large amount of residual fluid, removing the remaining residual fluid, and removing a small amount of residual fluid—are collected in a medium-pressure fluid recovery tank via pipelines and equipment for recycling. The fourth extract is a 5- to 8-cyclic aromatic hydrocarbon. The fourth extract, which is depressurized and output from the upper outlet of the third separator, is fed into the fourth separator. Inside the fourth separator, the fourth extract is separated to obtain a fifth extract, a fifth extract, and a mixture of residual fluid. The pressure inside the fourth separator is 4MPa to 7MPa, and the temperature is 140℃ to 205℃. The fifth extract is depressurized and discharged from the upper outlet of the fourth separator and fed into the fifth separator. The mixture of the fifth extract and residual fluid is discharged from the bottom outlet of the fourth separator. The mixture of the fifth extract and residual fluid is regulated to the critical pressure using an anthracene oil regulating valve, and then transferred to an anthracene oil heat exchanger to be regulated to the critical temperature. After releasing a large amount of residual fluid in the anthracene oil critical tower, it is discharged from the bottom outlet of the critical tower and transferred to an anthracene oil evaporator to evaporate and remove the remaining residual fluid. After evaporation, it is discharged from the bottom outlet of the anthracene oil evaporator and transferred to an anthracene oil stripping tower to strip and remove a small amount of residual fluid. Finally, the fifth extract is discharged from the bottom outlet of the anthracene oil stripping tower. The release of a large amount of residual fluid, removal of the remaining residual fluid, and removal of a small amount of residual fluid are all collected in a medium-pressure fluid recovery tank through pipelines and equipment for recycling. The fifth extract is anthracene oil. The fifth extract, which is depressurized and output from the upper outlet of the fourth separator, is fed into the fifth separator. Within the fifth separator, the fifth extract is separated to obtain a mixture of a critical fluid, a sixth extract, and a residual fluid. Wherein, the pressure regulation of the fifth separator is the critical pressure of the fluid; the temperature regulation is the critical temperature of the fluid; The critical state fluid is discharged from the upper outlet of the fifth separator and fed into a medium-pressure fluid recovery tank. The sixth extract and residual fluid mixture is discharged from the bottom outlet of the fifth separator. This mixture is then transferred to a saturated hydrocarbon evaporator to evaporate and remove the remaining residual fluid. After evaporation, it is transferred to a saturated hydrocarbon stripping tower to strip away a small amount of residual fluid. The sixth extract is then discharged from the bottom outlet of the saturated hydrocarbon stripping tower. All steps involving the removal of the remaining residual fluid and the removal of a small amount of residual fluid are collected in the medium-pressure fluid recovery tank via pipelines and equipment for recycling. The sixth extract is a saturated hydrocarbon.

7. The method for supercritical fluid extraction and separation of coal ethyl tar according to claim 1, characterized in that, The process involves blending asphalt and resin in a specific ratio to synthesize high-end carbon raw materials such as coated asphalt. The asphalt content in the coated asphalt raw material is 30% to 70%, and the resin content is 70% to 30%.

8. An apparatus for supercritical fluid extraction of coal ethyl tar, characterized in that, This is used to perform the supercritical fluid extraction method for separating coal ethyl tar as described in any one of claims 1 to 7.

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