Extraction separation equipment for high-viscosity organic residues and extraction separation method thereof
By using blended solvents and subcritical extraction technology in the treatment of high viscosity organic residues, the problems of large solvent usage and high energy consumption in the prior art are solved, efficient and low-energy-consuming organic matter recovery is achieved, and the resource utilization of organic residues is promoted.
Patent Information
- Application Number
- CN202411772110.X
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2024-12-04
- Publication Date
- 2025-03-07
- Estimated Expiration
- Not applicable · inactive patent
AI Technical Summary
The existing solvent extraction method has problems such as excessive solvent usage, high energy consumption, and complex extraction equipment when treating high viscosity organic residues.
Blended solvents are used as extraction agents, and the organic matter in the high viscosity organic residue is separated from the inorganic components under subcritical conditions. Heating the extractant into a subcritical state, enhancing the solubility to high viscosity organic matter, and reducing the viscosity of organic matter at high temperature energy, providing conditions for subsequent sedimentation and filtration.
The reduction of the amount of extractant, the reduction of energy consumption and the simplification of the extraction device are achieved, the recovery efficiency of organic matter in high viscosity organic residues is improved, and the resource utilization of organic residues is promoted.
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Figure CN119566046A_ABST
Abstract
Description
Technical Field
[0001] The invention belongs to the technical field of high-viscosity organic residue recovery, and in particular relates to an extraction and separation device for high-viscosity organic residue and an extraction and separation method thereof. Background Art
[0002] High-viscosity organic residues, including oil-containing silt and chemical organic kettle residues, are organic solid wastes with high pollution properties generated in the production process of oil extraction, petrochemicals, and organic chemical industries. These hazardous wastes are mixtures of high-viscosity organic matter and inorganic catalysts or clays. High-viscosity organic residues have a serious impact on the environment and production. Among them, in the process of shale oil extraction and refining, the shale oil has too much silt content, and the asphaltene and colloid content is high, which is difficult to completely separate by conventional demulsification methods.
[0003] Solvent extraction is one of the common treatment methods for the harmlessness and resource utilization of highly viscous organic residues. However, the existing solvent extraction methods have problems such as excessive solvent usage, high energy consumption in the extraction process, and complex extraction equipment.
[0004] The information disclosed in this background technology section is only intended to enhance the understanding of the overall background of the invention and should not be regarded as an acknowledgment or any form of suggestion that the information constitutes the prior art already known to a person skilled in the art. Summary of the invention
[0005] The object of the present invention is to provide an extraction and separation device for highly viscous organic residues and an extraction and separation method thereof, which have the advantages of low amount of extractant, low energy consumption and simple extraction device.
[0006] In order to achieve the above object, a technical solution provided by a specific embodiment of the present invention is as follows: an extraction and separation device for highly viscous organic residues, comprising:
[0007] An extraction device, comprising an extraction tank and a heater connected to each other, wherein the extraction tank is used to contain a mixture of highly viscous organic residue and an extractant, and the heater is used to heat the mixture in the extraction tank and increase the gas pressure in the extraction tank so that the extractant is converted to a subcritical state;
[0008] Flash tank;
[0009] The filtering device comprises a filtering pipeline connected between the extraction tank and the flash tank, and a plurality of filtering mechanisms arranged on the filtering pipeline;
[0010] The mixture in the extraction tank is filtered through a filtering device and transferred to a flash tank, the extractant in the mixture in the flash tank is vaporized, and the organic matter in the highly viscous organic residue is obtained in the flash tank.
[0011] In one or more embodiments of the present invention, the extraction separation equipment further includes a condenser and a recovery tank, the recovery tank is connected to the flash tank, and the condenser is disposed between the recovery tank and the flash tank.
[0012] In one or more embodiments of the present invention, the recovery tank is connected to the extraction tank for conveying the recovered extractant into the extraction tank.
[0013] In one or more embodiments of the present invention, the condenser has a refrigerant cavity for accommodating refrigerant, and the heater has a heat medium cavity for accommodating heat medium. The outlet of the refrigerant cavity is connected to the inlet of the heat medium cavity, so that the refrigerant in the refrigerant cavity that is liquefied and heated by the gaseous extractant can be used as the heat medium of the heater.
[0014] In one or more embodiments of the present invention, the outlet of the heat medium cavity is communicated with the inlet of the coolant cavity, and a heat sink is connected between the outlet of the heat medium cavity and the inlet of the coolant cavity.
[0015] In one or more embodiments of the present invention, a gas outlet is provided on the extraction tank, the gas outlet is connected to a condenser, and a vacuum pump is connected between the gas outlet and the condenser.
[0016] In one or more embodiments of the present invention, the filtering mechanism comprises:
[0017] The housing is installed on the filter pipe and has a filter cavity therein. The filter cavity has a feed inlet and a discharge port connected to the filter pipe;
[0018] A filter screen is arranged at or near the discharge port;
[0019] A scraper assembly includes a driving machine installed on the housing and a filter cake scraper connected to the output end of the driving machine, wherein the driving machine can drive the filter cake scraper to move so as to separate the filter cake on the filter screen from the filter screen; and / or,
[0020] A plurality of filtering mechanisms are arranged at intervals on the filtering pipeline, and the mesh sizes of the filtering nets in the plurality of filtering mechanisms increase sequentially along the direction of material flow.
[0021] In one or more embodiments of the present invention, a filter cake outlet communicating with the filter chamber is provided at the bottom of the housing, and a filter cake collector is connected to the filter cake outlet.
[0022] A specific embodiment of the present invention also provides a method for extracting and separating highly viscous organic residues, comprising the following steps:
[0023] Heating a mixed system of highly viscous organic residue and an extractant to make the extractant reach a subcritical state and perform extraction treatment, wherein the extractant comprises at least two organic solvents having a boiling point of 20 to 80° C.;
[0024] Separating the mixed system of the highly viscous organic residue and the extractant to obtain an extract containing the extractant and organic matter;
[0025] The extractant in the extract is vaporized to obtain organic matter.
[0026] In one or more embodiments of the present invention, the extractant is at least two of pentane, hexane, petroleum ether, methanol, ethanol, ether, acetone, benzene, dichloromethane, and chloroform.
[0027] Compared with the prior art, the extraction and separation equipment and extraction and separation method of high-viscosity organic residue of the present invention are a device and method that uses a co-mixed solvent as an extractant and separates organic matter and inorganic components in high-viscosity organic residue under subcritical conditions; the present invention uses the synergistic effect of multiple mixed solvents to dissolve high-viscosity organic matter in high-viscosity organic residue; the extractant is heated and pressurized to enter a subcritical state, further enhancing the solubility of the system for high-viscosity organic matter, and at the same time, high temperature within a certain range can further reduce the viscosity of high-viscosity organic matter, providing operating conditions for subsequent sedimentation and filtration. Finally, the present invention provides an energy thermal coupling process to further save energy and reduce consumption for the system. Finally, the recovery of organic matter in high-viscosity organic residue is achieved, and the resource utilization of organic residue is realized. BRIEF DESCRIPTION OF THE DRAWINGS
[0028] In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings required for use in the embodiments or the description of the prior art will be briefly introduced below. Obviously, the drawings described below are only some embodiments recorded in the present invention. For ordinary technicians in this field, other drawings can be obtained based on these drawings without paying creative work.
[0029] Figure 1 A schematic diagram of an extraction and separation device for highly viscous organic residues according to an embodiment of the present invention;
[0030] Figure 2 It is a partial schematic diagram of a filtering device in one embodiment of the present invention.
[0031] Description of main reference numerals:
[0032] 1. Extraction device; 11. Extraction tank; 12. Heater; 13. Stirring mechanism; 2. Filtering device; 21. Filtering pipe; 22. Filtering mechanism; 221. Shell; 2211. Feed inlet; 2212. Discharge outlet; 2213. Filter cake outlet; 2214. Filter chamber; 222. Filter screen; 223. Scraper assembly; 2231. Driving machine; 2232. Filter cake scraper; 224. Filter cake collector; 3. Flash tank; 4. Condenser; 5. Recovery tank; 6. Vacuum pump; 7. Radiator. DETAILED DESCRIPTION
[0033] In order to enable those skilled in the art to better understand the technical solutions in the present invention, the technical solutions in the embodiments of the present invention will be clearly and completely described below in conjunction with the drawings in the embodiments of the present invention. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work should fall within the scope of protection of the present invention.
[0034] like Figure 1 As shown, an extraction and separation device for high-viscosity organic residue in an embodiment of the present invention comprises an extraction device 1, a flash tank 3 and a filtering device 2; the extraction device 1 comprises an extraction tank 11 and a heater 12 connected to each other, the extraction tank 11 is used to contain a mixture of high-viscosity organic residue and an extractant, the heater 12 is used to heat the mixture in the extraction tank 11 and increase the gas pressure in the extraction tank 11 so that the extractant is converted to a subcritical state; the filtering device 2 comprises a filtering pipe 21 connected between the extraction tank 11 and the flash tank 3, and a plurality of filtering mechanisms 22 arranged on the filtering pipe 21; wherein, the mixture in the extraction tank 11 is filtered by the filtering device 2 and transferred to the flash tank 3, the extractant in the mixture in the flash tank 3 is vaporized, and the organic matter in the high-viscosity organic residue is obtained in the flash tank 3.
[0035] It can be understood that the extraction and separation equipment heats the extractant to a subcritical state so that it can better dissolve the organic matter in the highly viscous organic residue and reduce the amount of extractant used; through the cooperation of the extraction device 1, the flash tank 3, and the filtering device 2, only one heating is required in the entire extraction process, and at the same time, the pressure of the gas in the flash tank 3 can be lower than the pressure of the gas in the extraction tank 11. Therefore, after the extractant in the subcritical state flashes out of the tank 3, the extractant can be vaporized to achieve separation of the extractant and the organic matter, thereby reducing the energy consumption required for the extraction and separation equipment, and the entire extraction and separation equipment has the advantage of a simple structure.
[0036] When the extractant is heated to enter the subcritical state, a high pressure is generated in the extraction tank 11. The pressure in the flash tank 3 is lower than the other pressures in the extraction tank 11 because the pressure difference between the two tanks is between 0.3 and 2.8 MPa, that is, the pressure difference can drive the material from the extraction tank 11 to the flash tank 3.
[0037] It should be noted that the communication between the various components and the outlets, inlets, etc. in the present invention can be through pipelines or directly connected. For details, please refer to Figure 1 A valve may be provided on the pipeline to control the opening and closing of the pipeline.
[0038] The high-viscosity organic residue treated by the present invention is a high-viscosity organic hazardous waste with a viscosity range of 0.1-120 Pa·S and a solid content of 2%-90% under room temperature conditions. The volume ratio of the extractant to the high-viscosity organic residue is 0.8-1.5, thereby achieving the effect of saving the extractant.
[0039] Pressurizing and heating the extractant to bring it into a subcritical state can not only improve the solubility of the extractant in organic matter in the high-viscosity organic residue, but also, high temperature within a certain range can further reduce the viscosity of the high-viscosity organic matter in the high-viscosity organic residue, thereby providing operating conditions for subsequent sedimentation and filtration.
[0040] The extraction tank 11 may be provided with a stirring mechanism 13 for stirring the mixture of the high-viscosity organic residue and the extractant so that the high-viscosity organic residue and the extractant are fully mixed. The extraction tank 11 may be considered to be a relatively closed space, so when the heater 12 heats the extraction tank 11, the temperature and pressure in the extraction tank 11 will increase, thereby converting the extraction therein into a subcritical state.
[0041] The stirring mechanism 13 includes a connected stirring paddle, a rotating shaft, a magnetic coupler and a motor, which can achieve the function of stirring the materials in the extraction tank 11. The stirring rate is 30 to 180 rad / min, and the extraction stirring time is 0.5 to 2 hours. After stirring, it can be left to stand for a period of time for full extraction. The standing sedimentation time is 0.5 to 2 hours.
[0042] The extraction tank 11 can be provided with a plurality of drainage ports at different heights between the lower end and the bottom. The liquid level of the fluid leading to the filter device 2 can be adjusted according to the solid component content in the high-viscosity organic residue to avoid the formation of a large filter cake that causes resistance to the passage of fluid in the filter device 2.
[0043] The extractant includes at least two organic solvents with a boiling point of 20 to 80° C.; for example, the extractant is at least two of pentane, hexane, petroleum ether, methanol, ethanol, ether, acetone, benzene, dichloromethane, and chloroform. The purpose of selecting multiple organic solvents is to better dissolve the organic matter in the high-viscosity organic residue, that is, different organic solvents can be selected for the main components of the high-viscosity organic residue to improve the solubility of the organic solvent.
[0044] A material outlet is provided at the bottom of the flash tank 3. A screw pump or a gear pump may be provided at the material outlet of the flash tank 3 or near the material outlet. Since the material at the bottom of the flash tank 3 is mainly oily organic matter with a high viscosity, a screw pump or a gear pump helps the material discharge process.
[0045] Among them, since the temperature of the mixture entering the flash tank 3 is still relatively high, the extractant and water therein will vaporize under the condition of reduced pressure, and the temperature of the remaining substances in the flash tank 3 is still relatively high. At this time, the material should be discharged as soon as possible, because when the temperature is high, the viscosity of the remaining substances in the flash tank 3 is relatively low, which is convenient for discharging.
[0046] Preferably, the flash tank 3 may also be provided with an additional heating mechanism (not shown in the figure), which, in addition to heating the remaining material in the flash tank 3 to further reduce its viscosity, can also vaporize part of the remaining extractant in the remaining material in the flash tank 3, which is beneficial to the recycling of the extractant.
[0047] like Figure 1 As shown, the extraction and separation equipment further includes a condenser 4 and a recovery tank 5, the recovery tank 5 is connected to the flash tank 3, and the condenser 4 is arranged between the recovery tank 5 and the flash tank 3. That is, the condenser 4 can be arranged on the pipeline between the recovery tank 5 and the flash tank 3, and the extractant in the flash tank 3 is vaporized and condensed and liquefied by the condenser 4 through the pipeline to become liquid and flow into the recovery tank 5, and the liquid in the recovery tank 5.
[0048] Furthermore, the recovery tank 5 is connected to the extraction tank 11, and is used to transport the recovered extractant to the extraction tank 11. Figure 1 As shown, the recovery tank 5 is connected to the extraction tank 11 through a pipeline, and a valve and a driving pump (not shown in the figure) can be provided on the pipeline. In addition to the extractant, the liquid in the recovery tank 5 also contains some water. Therefore, a phase separator or a phase separation mechanism (not shown in the figure) can be installed in the recovery tank 5 to separate the extractant and water in time, and the separated extractant is transported to the extraction tank 11 through the driving pump to realize the recycling of the extractant.
[0049] In a specific embodiment, the condenser 4 has a refrigerant cavity (not shown) for accommodating refrigerant, and the heater 12 has a heat medium cavity for accommodating heat medium, and the outlet of the refrigerant cavity is connected to the inlet of the heat medium cavity, so that the refrigerant in the refrigerant cavity, which is liquefied and heated by the gaseous extractant, is used as the heat medium of the heater 12. Such a setting can play a role in energy recycling. Of course, if the heated refrigerant is used as the heat medium of the heater 12, the temperature is not enough, and the heater 12 can heat the heat medium to the required temperature.
[0050] Furthermore, the outlet of the heat medium cavity is connected to the inlet of the cold medium cavity, and a radiator 7 is connected between the outlet of the heat medium cavity and the inlet of the cold medium cavity. After the heat medium in the heat medium cavity is cooled by the radiator 7, it can be used as the cold medium in the cold medium cavity, which plays an energy-saving role and realizes the recycling of the heat medium and the cold medium, that is, the heat medium and the cold medium can be the same substance, such as commonly used cooling oil, heat transfer oil, etc. Specifically, the radiator 7 can be a commonly used air-cooled radiator 7 on the market.
[0051] like Figure 1 As shown, in this embodiment, two sets of extraction and separation equipment can be provided, wherein the refrigerant cavity of the condenser 4 in the first set of equipment is communicated with the heat medium cavity of the heater 12 in the second set of equipment, and the refrigerant cavity containing the refrigerant of the condenser 4 in the second set of equipment is communicated with the heat medium cavity of the heater 12 in the first set of equipment; that is, the refrigerant in the refrigerant cavity of the condenser 4 in the first set of equipment is liquefied and heated by the gaseous extractant and is used as the heat medium of the heater 12 in the second set of equipment, thereby achieving the effect of energy recovery.
[0052] like Figure 2 As shown, the filtering mechanism 22 includes a housing 221, a filter screen 222 and a scraper assembly 223; the housing 221 is mounted on the filtering pipe 21, and a filtering chamber 2214 is arranged therein, and the filtering chamber 2214 has an inlet 2211 and an outlet 2212 connected to the filtering pipe 21; the filter screen 222 is arranged at or near the outlet 2212; the scraper assembly 223 includes a driving machine 2231 mounted on the housing 221, and a filter cake scraper 2232 connected to the output end of the driving machine 2231, and the driving machine 2231 can drive the filter cake scraper 2232 to move so that the filter cake on the filter screen 222 is separated from the filter screen 222. The filter screen 222 plays the role of filtering the material, that is, filtering the material in the filtering device 2, so that the liquid part enters the subsequent flash tank 3.
[0053] Specifically, the driving motor 2231 can be a rotating motor, and a flow meter (not shown in the figure) can be provided on the filter pipe 21. When the flow in the filter pipe 21 decreases, the rotating motor can drive the filter cake scraper 2232 to rotate, so that the filter cake scraper 2232 contacts the filter screen 222, thereby causing the filter cake (solid residue) on the filter screen 222 to fall off and maintain the filtering efficiency.
[0054] Furthermore, a plurality of filter mechanisms 22 may be provided at intervals on the filter pipe 21, so as to realize multi-stage filtering of the material, thereby improving the filtering efficiency and filtering effect. Along the direction of material movement, the mesh numbers of the filter nets 222 in the plurality of filter mechanisms 22 may be increased successively, the upstream filter mechanism 22 may filter larger solids, and the downstream filter mechanism 22 may filter smaller solids, thereby reducing the filtering resistance and improving the filtering efficiency, wherein the mesh number of the filter net 222 in the most downstream filter mechanism 22 may be a maximum of 2800 meshes, realizing filtering of particulate matter above 3 μm. In other embodiments, the mesh numbers of the filter nets 222 in the plurality of filter mechanisms 22 are all the same or partially the same.
[0055] Specifically, the flow rate of the fluid (material) in the filter mechanism 22 can be controlled between 5 and 60 m3 / h; the mesh size of the filter screen 222 of the filter pipe 21 can be selected according to actual needs.
[0056] Furthermore, the bottom of the housing 221 is provided with a filter cake outlet 2213 connected to the filter chamber 2214, and the filter cake outlet 2213 is connected to a filter cake collector 224. The filter cake collector 224 can be connected to the bottom of the housing 221 through a flange to facilitate the cleaning of the filter cake.
[0057] like Figure 1 As shown, the extraction tank 11 is provided with a gas outlet. In one or more embodiments of the present invention, the extraction tank 11 is provided with a gas outlet. The extraction tank 11 is provided with a gas outlet, and the gas outlet is connected to the condenser 4. A vacuum pump 6 is connected between the gas outlet and the condenser 4. The gas outlet, the condenser 4 and the vacuum pump 6 are connected by pipelines, and valves can be provided on the pipelines between them. After the extraction and separation is completed, some extractant may still remain in the material in the extraction tank 11. At this time, the valve can be opened to vaporize the extractant in the extraction tank 11 under the action of the vacuum pump 6 and enter the recovery tank 5 after passing through the condenser 4.
[0058] Furthermore, the vacuum pump 6 and the flash tank 3 may also be connected through a pipeline, and a valve may also be provided on the pipeline. When there is residual extractant in the flash tank 3 and the temperature and pressure are not sufficient to vaporize the extractant, the valve on the pipeline between the vacuum pump 6 and the flash tank 3 may be opened, and the vacuum pump 6 performs vacuum treatment on the flash tank 3 to reduce the pressure in the flash tank 3. At this time, the extractant in the flash tank 3 may be vaporized in turn due to the reduced pressure (close to a vacuum state) and enter the recovery tank 5 after passing through the condenser 4.
[0059] A specific embodiment of the present invention further provides a method for extracting and separating highly viscous organic residues, which can be based on the above-mentioned extraction and separation equipment for highly viscous organic residues. The extraction and separation method comprises the following steps:
[0060] S1, heating a mixed system of highly viscous organic residue and an extractant to make the extractant reach a subcritical state, and performing an extraction process, wherein the extractant comprises at least two organic solvents having a boiling point of 20 to 80° C.;
[0061] S2, separating the mixed system of the highly viscous organic residue and the extractant to obtain an extract containing the extractant and organic matter;
[0062] S3, vaporizing the extractant in the extract to obtain organic matter.
[0063] Preferably, the extractant is at least two of pentane, hexane, petroleum ether, methanol, ethanol, ether, acetone, benzene, dichloromethane and chloroform.
[0064] like Figure 1 The specific process of the extraction and separation device of the highly viscous organic residue and the extraction and separation method thereof of the present invention can be as follows:
[0065] Put the highly viscous organic residue into the extraction tank, mix it with the extractant (including at least two organic solvents) under the action of mixing and stirring, close the valves V1 to V5 and heat the extraction tank to 80 to 240° C., wherein the extractant is converted to a subcritical state, and the pressure of the extraction operation is 2 to 8 MPa;
[0066] When the extractant is in a high-temperature subcritical state, a stirring paddle is used to fully extract and mix the materials therein, the stirring rate is 30 to 180 rad / min, the extraction stirring time is 0.5 to 2 hours, and the static precipitation time after stirring is 0.5 to 2 hours.
[0067] Open valve V2, and slowly open valve V1. At this time, there is a pressure difference between the extraction tank and the flash tank, which pushes the material (the extractant containing organic matter and some solid slag) into the filtration device. When the pressure of the extraction tank and the flash tank are consistent, the material stops flowing from the extraction tank to the flash tank. At this time, open valve V7 and valve V6 in sequence, and then slowly open valve V5. At this time, adjust valve V5 to make the pressure difference between the extraction tank and the flash tank between 0.3 and 2.8 MPa. The material continues to flow from the extraction tank to the flash tank, and the fluid (material) flow rate can be controlled at 5 to 60 m 3 / h. When the filter device runs for a period of time and the resistance drop increases significantly, the driver of the filter device is started, and the driver drives the filter cake scraper to scrape the filter cake from the filter net and drop it into the filter cake collector.
[0068] After the liquid filtered by the multi-stage filtering mechanism enters the flash tank, when there is no obvious fluid in the filtering device, valves V1 and V2 are closed, and valve V5 is further opened to achieve the purpose of pressure relief. After the pressure relief, the liquid in the flash tank is vaporized, and the vaporized steam is liquefied through the condenser. The liquefied liquid enters the recovery tank, and the phase separator in the recovery tank can separate the water phase until the pressure in the flash tank is normal pressure;
[0069] Among them, the high-temperature cooling oil (refrigerant) heated in the condenser is transferred to the heater in another set of equipment to be used as heat medium. The heat medium heated in the heater in another set of equipment is further cooled by the air-cooled radiator and then returned to the condenser of this set of equipment to be used as cooling oil.
[0070] If there is still residual mixed solvent in the extraction tank and the flash tank, turn on the vacuum pump, perform vacuum operation on the extraction tank and the flash tank, and use the residual heat of the materials to vaporize the remaining extractant and water. If the residual heat is insufficient, the extraction tank and the flash tank can be heated, and then the gas enters the condenser and condenses into the recovery tank;
[0071] Finally, the materials in the flash tank are discharged from the flash tank using the residual heat and the screw pump, and the solid residue in the extraction tank is cleaned using the manhole on the extraction tank;
[0072] Among them, two or more sets of extraction and separation devices can be used alternately to complete the continuous operation of high-viscosity organic residues. According to the properties of high-viscosity organic residues, the same batch of high-viscosity organic residues can be subjected to two repeated extraction and separation methods to further reduce the organic matter content in the high-viscosity organic residues.
[0073] The extraction and separation device for high-viscosity organic residue and the extraction and separation method thereof of the present invention are described in detail below with reference to specific examples.
[0074] Example 1
[0075] Canadian oil sand (high-viscosity organic residue) is treated. The asphalt oil content in the Canadian oil sand is 16.7wt%, the moisture content is 4.8wt%, and the remaining sand and clay content is 78.5wt%. The extraction and separation device of the high-viscosity organic residue and the extraction and separation method thereof are used for extraction and separation. The extraction agent is methanol and pentane (the volume ratio of methanol to pentane is 3:7), the volume ratio of the extraction agent to the Canadian oil sand is 1.2:1, during extraction, the heating temperature in the extraction tank is 160°C, the extraction pressure is 2.93MPa, the extraction stirring speed is 50rad / min, the stirring time is 40 minutes, the precipitation time is 1h, and after filtering by a filtering device, the final recovered oil (recovered organic matter) in the flash tube accounts for 78% of the oil component in the original Canadian oil sand, and the oil content in the solid residue remaining in the extraction tank is 4.2%.
[0076] Example 2
[0077] The invention discloses a method for treating phenol-based distillation still residue (high-viscosity organic residue), wherein the heavy component content of phenol-based distillation still residue is 69.3wt%, the water content is 8wt%, and the remaining sand and clay content is 22.7wt%. The extraction and separation device of the high-viscosity organic residue and the extraction and separation method thereof are used for extraction and separation treatment. The extraction agent is methanol and ether (the volume ratio of methanol to ether is 7:3), the volume ratio of the extraction agent to the oil sand is 1.3:1, during extraction, the heating temperature in the extraction tank is 120°C, the extraction pressure is 3.4MPa, the extraction stirring speed is 40rad / min, the stirring time is 40 minutes, the precipitation time is 1h, after filtering by a filtering device, the final recovered oil (recovered organic matter) in the flash tube accounts for 96% of the oil component in the original Canadian oil sand, and the oil content in the remaining solid residue in the extraction tank is 10.2%.
[0078] In summary, the extraction and separation device for high-viscosity organic residues and the extraction and separation method thereof of the present invention have the following beneficial effects:
[0079] The present invention adopts a blended solvent (two or more organic solvents as extractants) and a subcritical environment to extract organic matter (organic matter) in a high-viscosity residue material. This extraction method can minimize the amount of extraction solvent used, reduce the viscosity of the system, and reduce the energy loss caused by solvent recovery in the back end.
[0080] The present invention adopts the method of heating the low-boiling point extractant to make the system reach a subcritical state. This process reduces the use of a pressure pump, reduces the viscosity of the material, and uses the air pressure difference to drive the fluid to flow to complete the filtering operation. This process reduces the energy consumption of a screw pump or a gear pump.
[0081] The present invention utilizes the residual temperature of the superheated material to flash evaporate the low-boiling point extractant under reduced pressure, thereby reducing the energy consumed in the solvent separation process.
[0082] The filtering mechanism used in the present invention has a filter cake scraper structure and a filter cake collector, which can effectively reduce the resistance generated by the formation of the filter cake and reduce the risk of material blockage, which is a necessary condition for achieving low-energy consumption and high-efficiency multi-stage filtration.
[0083] It will be apparent to those skilled in the art that the invention is not limited to the details of the exemplary embodiments described above and that the invention can be implemented in other specific forms without departing from the spirit or essential features of the invention. Therefore, the embodiments should be considered exemplary and non-limiting in all respects, and the scope of the invention is defined by the appended claims rather than the foregoing description, and it is intended that all variations falling within the meaning and scope of the equivalent elements of the claims be included in the invention. Any reference numeral in a claim should not be considered as limiting the claim to which it relates.
[0084] In addition, it should be understood that although the present specification is described according to implementation modes, not every implementation mode contains only one independent technical solution. This description of the specification is only for the sake of clarity. Those skilled in the art should regard the specification as a whole. The technical solutions in each embodiment may also be appropriately combined to form other implementation modes that can be understood by those skilled in the art.
Claims
1. An extraction and separation device for highly viscous organic residues, characterized in that: include: An extraction device, comprising an extraction tank and a heater connected to each other, wherein the extraction tank is used to contain a mixture of highly viscous organic residue and an extractant, and the heater is used to heat the mixture in the extraction tank and increase the gas pressure in the extraction tank so that the extractant is converted to a subcritical state; Flash tank; The filtering device comprises a filtering pipeline connected between the extraction tank and the flash tank, and a plurality of filtering mechanisms arranged on the filtering pipeline; The mixture in the extraction tank is filtered through a filtering device and transferred to a flash tank, the extractant in the mixture in the flash tank is vaporized, and organic matter in the highly viscous organic residue is obtained in the flash tank.
2. The extraction and separation equipment for highly viscous organic residues according to claim 1, characterized in that: The extraction and separation equipment also includes a condenser and a recovery tank. The recovery tank is connected to the flash tank, and the condenser is arranged between the recovery tank and the flash tank.
3. The extraction and separation equipment for highly viscous organic residues according to claim 2, characterized in that: The recovery tank is connected to the extraction tank and is used to transport the recovered extractant into the extraction tank.
4. The extraction and separation equipment for highly viscous organic residues according to claim 2, characterized in that: The condenser has a refrigerant cavity for accommodating refrigerant, and the heater has a heat medium cavity for accommodating heat medium. The outlet of the refrigerant cavity is connected to the inlet of the heat medium cavity, so that the refrigerant in the refrigerant cavity that is liquefied and heated by the gaseous extractant is used as the heat medium of the heater.
5. The extraction and separation equipment for highly viscous organic residues according to claim 4, characterized in that: The outlet of the heat medium cavity is communicated with the inlet of the cold medium cavity, and a radiator is connected between the outlet of the heat medium cavity and the inlet of the cold medium cavity.
6. The extraction and separation equipment for highly viscous organic residues according to claim 2, characterized in that: The extraction tank is provided with a gas outlet, the gas outlet is communicated with a condenser, and a vacuum pump is connected between the gas outlet and the condenser.
7. The extraction and separation equipment for highly viscous organic residues according to claim 1, characterized in that: The filtering mechanism comprises: The housing is installed on the filter pipe and has a filter cavity therein. The filter cavity has a feed inlet and a discharge port connected to the filter pipe; A filter screen is arranged at or near the discharge port; The scraper assembly comprises a driving machine installed on a shell and a filter cake scraper connected to the output end of the driving machine. The driving machine can drive the filter cake scraper to move so as to separate the filter cake on the filter screen from the filter screen.
8. The extraction and separation equipment for highly viscous organic residues according to claim 7, characterized in that: The bottom of the housing is provided with a filter cake outlet communicating with the filter cavity, and the filter cake outlet is connected to a filter cake collector; and / or, A plurality of filtering mechanisms are arranged at intervals on the filtering pipeline, and the mesh sizes of the filtering nets in the plurality of filtering mechanisms increase sequentially along the direction of material flow.
9. A method for extracting and separating highly viscous organic residues, characterized in that: The following steps are involved: Heating a mixed system of highly viscous organic residue and an extractant to make the extractant reach a subcritical state and perform extraction treatment, wherein the extractant comprises at least two organic solvents having a boiling point of 20 to 80° C.; Separating the mixed system of the highly viscous organic residue and the extractant to obtain an extract containing the extractant and organic matter; The extractant in the extract is vaporized to obtain organic matter.
10. The extraction and separation method of highly viscous organic residue according to claim 9, characterized in that: The extractant is at least two of pentane, hexane, petroleum ether, methanol, ethanol, ether, acetone, benzene, dichloromethane and chloroform.
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