Hydroprocessing apparatus for waste lubricating oil and method of using same
By using adsorbent packing material in a waste lubricating oil hydrotreating pretreatment unit for atmospheric pressure adsorption distillation and regeneration, the problem of removing water, light hydrocarbons and polar additives from waste lubricating oil is solved, catalyst clogging is avoided, and the adsorbent can be recycled and the unit can be operated for a long period of time.
Patent Information
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- CHINA ENERGY INVESTMENT CORP LTD
- Filing Date
- 2025-01-03
- Publication Date
- 2026-07-03
AI Technical Summary
Existing hydrogenation pretreatment methods for waste lubricating oil suffer from problems such as scaling and blockage of distillation unit pipelines and pore blockage of hydrogenation catalyst channels. In particular, they have a weak ability to remove polar additive components, which affects the long-term operation of the unit.
A hydrogenation pretreatment device is adopted, including a distillation column, a condenser and a gas supply unit. Adsorption distillation is carried out using adsorbent packing material under normal pressure to remove water and light hydrocarbons from waste lubricating oil. The adsorbent packing material is regenerated through the gas supply unit, and polar additives are desorbed to realize the recycling of adsorbent.
It effectively removes water, light hydrocarbons, and polar additives from waste lubricating oil, avoids catalyst pore blockage, realizes the recycling of adsorbent, reduces production costs, and ensures long-term operation of the unit.
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Figure CN122326320A_ABST
Abstract
Description
Technical Field
[0001] This disclosure relates to the field of waste lubricating oil hydrotreating technology, specifically to a hydrotreating device for waste lubricating oil and its application method. Background Technology
[0002] Long-term use of fan lubricating oil can lead to deterioration, and discarding or incinerating waste lubricating oil will cause serious environmental pollution. Lubricating oil is composed of base oil and additives. Although the properties of waste fan lubricating oil change somewhat, its main components are still base oil and additives. Compared with processes such as acid earth refining, solvent refining, hydrorefining, and thin-film regeneration, hydrorefining has advantages such as no pollution, high product yield, good quality, good operational flexibility, and adaptability to large-scale production. It is an important and advanced process for waste lubricating oil regeneration.
[0003] Among related technologies, the Kleen and KTI processes are widely used and relatively mature pretreatment methods, such as atmospheric and vacuum distillation. However, for contaminants from fan oil additives, direct distillation can lead to scaling and blockage of the distillation unit's pipelines, affecting the long-term operation of the unit. While processes such as Hylude, BERC, and domestic patents use mild hydrogenation or light solvent extraction methods to remove some contaminants, they have a weak ability to remove polar additive components, which can still cause blockage of the hydrogenation catalyst pores and even blockage of the entire bed. Summary of the Invention
[0004] The purpose of this disclosure is to provide a hydrogenation pretreatment device for waste lubricating oil and its application method, so as to solve the technical problems existing in the related art.
[0005] To achieve the above objectives, a first aspect of this disclosure provides a hydrotreating pretreatment apparatus for waste lubricating oil, comprising: The processing module includes a distillation column, a condenser, and a gas supply unit. The distillation column has an internal cavity filled with adsorbent packing material. The distillation column is equipped with a first outlet pipe, a second outlet pipe, a third outlet pipe, a first inlet pipe, and a second inlet pipe that are connected to the cavity. The first outlet pipe is connected to the condenser and is used to discharge water and light hydrocarbons from the waste lubricating oil. The second outlet pipe is used to discharge polar additives from the waste lubricating oil. The third outlet pipe is used to discharge the pretreated waste lubricating oil. The first inlet pipe is used to allow waste lubricating oil from the waste oil supply unit to flow into the cavity. The second inlet pipe is connected to the gas supply unit and is used to supply regeneration gas to the cavity.
[0006] Optionally, a first switching valve is provided on the first inlet pipe, and a second switching valve is provided on the second inlet pipe, wherein the switching states of the first switching valve and the second switching valve are different.
[0007] Optionally, the processing module further includes a reboiler and a fourth outlet pipe, wherein the reboiler is connected to the cavity and the third outlet pipe respectively through the fourth outlet pipe.
[0008] Optionally, the processing module further includes a desorbate storage tank, which is connected to the end of the second outlet pipe away from the distillation column.
[0009] Optionally, the hydrogenation pretreatment device for waste lubricating oil includes multiple processing modules, each of which is connected in parallel to the waste oil supply unit via a first inlet pipe, and each of which is connected in parallel to the gas supply unit via a second inlet pipe. In addition, at least one of the processing modules has a distillation column in an atmospheric pressure adsorption distillation state, and at least one of the processing modules has an adsorbent packing in a regeneration state.
[0010] A second aspect of this disclosure provides a method for use in a hydrotreating pretreatment apparatus for waste lubricating oil as described above, comprising: The cavity of the distillation column is filled with adsorbent packing material; The waste lubricating oil before entering the distillation column is pretreated to remove solid particles from the waste lubricating oil, and the treated waste lubricating oil flows into the cavity through the first inlet pipe; A normal pressure adsorption distillation operation is performed so that water and light hydrocarbons are discharged through the first outlet pipe and the condenser. The pretreated waste lubricating oil is discharged from the third outlet pipe; The gas supply unit supplies gas to the cavity through the second inlet pipe to regenerate the adsorbent packing in the distillation column, and discharges the desorbed polar additives through the second outlet pipe.
[0011] Optionally, the atmospheric pressure adsorption distillation operation of the waste lubricating oil in the distillation column includes: The distillation is carried out at a pressure of 0.1 MPa to 0.2 MPa in the distillation column, with 20 to 60 trays of adsorbent packing and a reflux ratio of 0.1 to 4; the temperature of the bottom of the distillation column is 250°C to 300°C, and the temperature of the top of the distillation column is 150°C to 200°C; the waste blower lubricating oil is discharged at a rate of 2 hours... -1 ~20h -1 The space velocity is used for adsorption distillation.
[0012] Optionally, regenerating the adsorbent packing in the distillation column includes: The process is carried out at a pressure of -0.08MPa to -0.02MPa inside the distillation column, the heating temperature of the distillation column is 250℃ to 300℃, and the gas flow rate of the gas supply unit is 200ml / min to 800ml / min.
[0013] Optionally, the first inlet pipe is switched on and off by setting a first switching valve on the first inlet pipe, and the second inlet pipe is switched on and off by setting a second switching valve on the second inlet pipe, so that the first inlet pipe and the second inlet pipe are in different on / off states.
[0014] Optionally, multiple processing modules are provided, and the multiple processing modules are respectively connected in parallel to the waste oil supply unit through the first inlet pipe, and the multiple processing modules are respectively connected in parallel to the gas supply unit through the second inlet pipe; Furthermore, in at least one of the processing modules, the distillation column of at least one processing module is in an atmospheric pressure adsorption distillation state, and the adsorbent packing material in at least one processing module is in a regeneration state.
[0015] Through the above technical solution, in the process of treating the waste lubricating oil, adsorbent packing is filled into the cavity, waste lubricating oil is added into the cavity, and water and light hydrocarbons in the waste lubricating oil are discharged through the first outlet pipe through a distillation operation. The condenser condenses the vapor flowing out from the first outlet pipe. At the same time, the adsorbent packing filled in the cavity can adsorb polar additives in the waste lubricating oil. After adsorption is completed, the treated waste lubricating oil in the cavity is discharged from the third outlet pipe. Then, regeneration gas is supplied to the cavity through the second inlet pipe via the gas supply unit, thereby desorbing the polar additives adsorbed in the adsorbent packing and discharging them through the second outlet pipe. In the above process, while removing water, light hydrocarbons, and polar additives, the adsorbent packing is also regenerated in the cavity, thereby realizing the recycling of the adsorbent packing. This avoids frequent disassembly of the distillation column to replace the adsorbent packing, saves raw materials and production costs, and avoids the problem of catalyst pore blockage and entire bed blockage caused by the presence of polar additives in the waste lubricating oil treated by the distillation column during subsequent hydrogenation processes.
[0016] Other features and advantages of this disclosure will be described in detail in the following detailed description section. Attached Figure Description
[0017] The accompanying drawings are provided to further illustrate the present disclosure and form part of the specification. They are used together with the following detailed description to explain the present disclosure, but do not constitute a limitation thereof. In the drawings: Figure 1 This is a schematic diagram of the structure of a hydrogenation pretreatment device for waste lubricating oil provided in an exemplary embodiment of this disclosure; Figure 2 This is a flowchart of a method for a hydrogenation pretreatment apparatus for waste lubricating oil provided in an exemplary embodiment of this disclosure; Figure 3 This is a flowchart of a method for a hydrogenation pretreatment apparatus for waste lubricating oil provided in another exemplary embodiment of this disclosure.
[0018] Explanation of reference numerals in the attached figures 10 - Processing module; 11 - Distillation column; 110 - Chamber; 111 - First outlet pipe; 112 - Second outlet pipe; 113 - Third outlet pipe; 114 - First inlet pipe; 1140 - First switching valve; 115 - Second inlet pipe; 1150 - Second switching valve; 116 - First distillation column; 117 - Second distillation column; 118 - Third distillation column; 12 - Condenser; 13 - Gas supply unit; 14 - Reboiler; 15 - Fourth outlet pipe; 16 - Desorbent storage tank; 17 - Reflux tank; 20 - Waste oil supply unit. Detailed Implementation
[0019] The specific embodiments of this disclosure will be described in detail below with reference to the accompanying drawings. It should be understood that the specific embodiments described herein are for illustration and explanation only and are not intended to limit this disclosure.
[0020] In this disclosure, unless otherwise stated, directional terms such as "up," "down," "left," and "right" are used to indicate orientation or positional relationships only for the convenience of describing this disclosure and simplifying the description, and are not intended to indicate or imply that the device or element referred to must have a specific orientation, or a specific orientation structure and operation, and therefore should not be construed as a limitation of this disclosure. The terms "inner" and "outer" refer to the inner and outer contours of the corresponding structures.
[0021] Additionally, it should be noted that the terms used, such as "first" and "second," are used to distinguish one element from another and do not indicate sequence or importance. Furthermore, in the description referring to the accompanying drawings, the same reference numerals in different drawings denote the same element.
[0022] In the description of this disclosure, it should also be noted that, unless otherwise expressly specified and limited, the terms "set up," "connect," "link," and "install" should be interpreted broadly. For example, they can refer to a fixed connection, a detachable connection, or an integral connection; they can refer to a direct connection or an indirect connection through an intermediate medium. Those skilled in the art can understand the specific meaning of the above terms in this disclosure according to the specific circumstances.
[0023] refer to Figure 1 As shown, the first aspect of this disclosure provides a hydrogenation pretreatment device for waste lubricating oil, including a treatment module 10. The treatment module 10 includes a distillation column 11, a condenser 12, and a gas supply unit 13. The distillation column 11 has a cavity 110 inside, which is filled with adsorbent packing. The distillation column 11 is provided with a first outlet pipe 111, a second outlet pipe 112, a third outlet pipe 113, a first inlet pipe 114, and a second inlet pipe 115 communicating with the cavity 110. The first outlet pipe 111 is connected to the condenser 12 and is used to discharge water and light hydrocarbons in the waste lubricating oil. The second outlet pipe 112 is used to discharge polar additives in the waste lubricating oil. The third outlet pipe 113 is used to discharge the pretreated waste lubricating oil. The first inlet pipe 114 is used to allow waste lubricating oil from the waste oil supply unit 20 to flow into the cavity 110. The second inlet pipe 115 is connected to the gas supply unit 13 and is used to supply regenerated gas to the cavity 110.
[0024] Through the above technical solution, in the process of treating the waste lubricating oil, the adsorbent packing is filled into the cavity 110, the waste lubricating oil is added into the cavity 110, and the water and light hydrocarbons in the waste lubricating oil are discharged through the first outlet pipe 111 by distillation. The condenser 12 condenses the steam flowing out from the first outlet pipe 111. At the same time, the adsorbent packing filled in the cavity 110 can adsorb the polar additives in the waste lubricating oil. After the adsorption is completed, the treated waste lubricating oil in the cavity 110 is discharged from the third outlet pipe 113. Then, regeneration gas is supplied to the cavity 110 through the second inlet pipe 115 by the gas supply unit 13, thereby desorbing the polar additives adsorbed in the adsorbent packing and discharging them through the second outlet pipe 112. In the above process, while removing water, light hydrocarbons and polar additives, the adsorbent packing is also regenerated in the cavity 110, thereby realizing the recycling of the adsorbent packing. This avoids the frequent disassembly of the distillation column 11 to replace the adsorbent packing, saves raw materials and production costs, and prevents the waste lubricating oil treated by the distillation column 11 from clogging the catalyst channels in the subsequent hydrogenation process due to the presence of polar additives, thus preventing the entire bed from becoming blocked.
[0025] In one exemplary embodiment provided in this disclosure, the regeneration gas supplied by the gas supply unit 13 to the cavity 110 may be nitrogen or air, and in this disclosure, the gas flow rate of the gas supply unit 13 is 200 ml / min to 800 ml / min.
[0026] Optionally, such as Figure 1As shown, a first switching valve 1140 is installed on the first inlet pipe 114, and a second switching valve 1150 is installed on the second inlet pipe 115. The switching states of the first switching valve 1140 and the second switching valve 1150 are different. Since the first inlet pipe 114 is used to supply waste lubricating oil into the cavity 110, and the second inlet pipe 115 is used to supply regeneration gas into the cavity, the on / off states of the first switching valve 1140 and the second switching valve 1150 can be adjusted to adapt to the specific operating state of the distillation column 11.
[0027] Specifically, during the removal of water and light hydrocarbons from waste lubricating oil, the first switch valve 1140 is adjusted to the open state to allow the first inlet pipe 114 to be open. At this time, the waste lubricating oil to be treated can enter the cavity 110 through the first inlet pipe 114, and the distillation column 11 performs atmospheric pressure adsorption distillation to remove water and light hydrocarbons from the waste lubricating oil. During the above process, the second switch valve 1150 is in a different switching state than the first switch valve 1140, that is, the second switch valve 1150 is in the closed state. At this time, the regeneration gas cannot enter the cavity 110 through the second inlet pipe 115, thereby avoiding the regeneration gas from affecting the atmospheric pressure adsorption distillation operation of the distillation column 11.
[0028] Similarly, during the regeneration of the adsorbent packing, the second switch valve 1150 can be adjusted to the open state, the distillation column 11 can perform depressurization heating treatment on the adsorbent, and then the regeneration gas can be introduced into the cavity 110 through the second inlet pipe 115 to realize the regeneration operation of the adsorbent packing; while the first switch valve 1140 is adjusted to the closed state to stop the waste lubricating oil from entering the cavity 110, so as to avoid the waste lubricating oil entering the cavity 110 and affecting the regeneration of the adsorbent packing.
[0029] Optionally, such as Figure 1 As shown, the processing module 10 may further include a reboiler 14 and a fourth outlet pipe 15. The reboiler 14 is connected to the cavity 110 and the third outlet pipe 113 via the fourth outlet pipe 15. By providing the reboiler 14, the waste lubricating oil in the distillation column 11 can be heated. The light components (components with lower boiling points) in the waste lubricating oil will evaporate preferentially, forming steam that rises to the upper part of the column, thereby facilitating the precipitation of water and light hydrocarbons. The heavy components remain at the bottom of the column and flow out through the third outlet pipe 113.
[0030] In this disclosure, the reboiler 14, the third outlet pipe 113, and the fourth outlet pipe 15 are all located at the bottom of the distillation column 11.
[0031] Optionally, such as Figure 1As shown, the processing module 10 may further include a desorbate storage tank 16, which is connected to the end of the second outlet pipe 112 away from the distillation column 11. In this way, the polar additives removed from the waste lubricating oil can enter the desorbate storage tank 16 through the second outlet pipe 112 to realize the recovery and utilization of the polar additives.
[0032] In addition, a desorption tail gas outlet is formed on the desorbed material storage tank 16 for discharging the desorption tail gas.
[0033] The distillation column 11 also includes a reboiler 14, which is connected to the first outlet pipe 111 and is located downstream of the condenser 12.
[0034] In summary, since the removal of water and light hydrocarbons from waste lubricating oil and the regeneration of the adsorbent packing are two independent processes, in order to improve the removal efficiency of water and light hydrocarbons and the regeneration efficiency of the adsorbent packing, in an exemplary embodiment provided in this disclosure, the hydrogenation pretreatment device for waste lubricating oil may include multiple processing modules 10. The multiple processing modules 10 are respectively connected in parallel to the waste oil supply unit 20 through a first inlet pipe 114, and the multiple processing modules 10 are respectively connected in parallel to the gas supply unit 13 through a second inlet pipe 115. Among the multiple processing modules 10, the distillation column 11 of at least one processing module 10 is in an atmospheric pressure adsorption distillation state, and the adsorbent packing in at least one processing module 10 is in a regeneration state. In the process of treating the waste lubricating oil, the hydrogenation pretreatment device of multiple treatment modules 10 can have different operating states for the distillation columns 11 of different treatment modules 10. Specifically, while one distillation column 11 of a treatment module 10 is performing atmospheric pressure adsorption distillation to remove water and light hydrocarbons from the waste lubricating oil, another distillation column 11 of a treatment module 10 can perform adsorbent packing regeneration, thereby reducing the waiting time in the operation process, ensuring continuous treatment of waste lubricating oil, and improving the treatment efficiency of waste lubricating oil.
[0035] Since the regeneration time of the adsorbent packing is longer than the time required to remove moisture and light hydrocarbons from the waste lubricating oil during the treatment of the waste lubricating oil (the ratio of the regeneration time of the adsorbent packing to the time required to remove moisture and light hydrocarbons from the waste lubricating oil is 1.2 to 2.0), in an exemplary embodiment provided in this disclosure, the number of the above-mentioned processing modules 10 can be three. In this way, when one of the three processing modules 10 is regenerating the adsorbent packing, at least one of the other two processing modules 10 has completed the regeneration of the adsorbent packing. That is, at this time, the waste lubricating oil can be dehydrated and light hydrocarbons through the processing module 10, thereby realizing continuous operation of the waste lubricating oil.
[0036] A second aspect of this disclosure provides a method for use in the above-described hydrotreating apparatus for waste lubricating oil, such as... Figure 2 The above includes: S101. Fill the cavity 110 of the distillation column 11 with adsorbent packing material; S102. The waste lubricating oil before entering the distillation column 11 is pretreated to remove solid particles from the waste lubricating oil, and the treated waste lubricating oil flows into the cavity 110 through the first inlet pipe 114. S103. Perform atmospheric pressure adsorption distillation to discharge water and light hydrocarbons through the first outlet pipe 111 and condenser 12. S104. Discharge the pretreated waste lubricating oil from the third outlet pipe 113; S105, the gas supply unit 13 supplies gas to the cavity 110 through the second inlet pipe 115 to regenerate the adsorbent packing in the distillation column 11, and discharges the desorbed polar additive through the second outlet pipe 112.
[0037] Through the above technical solution, in the process of treating the waste lubricating oil, the adsorbent packing is filled into the cavity 110, the waste lubricating oil is added into the cavity 110, and the water and light hydrocarbons in the waste lubricating oil are discharged through the first outlet pipe 111 by distillation. The condenser 12 condenses the steam flowing out from the first outlet pipe 111. At the same time, the adsorbent packing filled in the cavity 110 can adsorb the polar additives in the waste lubricating oil. After the adsorption is completed, the treated waste lubricating oil in the cavity 110 is discharged from the third outlet pipe 113. Then, regeneration gas is supplied to the cavity 110 through the second inlet pipe 115 by the gas supply unit 13, thereby desorbing the polar additives adsorbed in the adsorbent packing and discharging them through the second outlet pipe 112. In the above process, while removing water, light hydrocarbons and polar additives, the adsorbent packing is also regenerated in the cavity 110, thereby realizing the recycling of the adsorbent packing. This avoids the frequent disassembly of the distillation column 11 to replace the adsorbent packing, saves raw materials and production costs, and prevents the waste lubricating oil treated by the distillation column 11 from causing catalyst pore blockage in the subsequent hydrogenation process due to the presence of polar additives, thus preventing the entire bed from becoming blocked.
[0038] refer to Figure 3 As shown, according to an embodiment of this disclosure, another method for a hydrotreating apparatus for waste lubricating oil is also provided, comprising: S201. Fill the cavity 110 of the distillation column 11 with adsorbent packing material; S202. The waste lubricating oil before entering the distillation column 11 is pretreated to remove solid particles from the waste lubricating oil, and the treated waste lubricating oil flows into the cavity 110 through the first inlet pipe 114. S203. Perform atmospheric pressure adsorption distillation operation at a pressure of 0.1MPa~0.2MPa inside distillation column 11. The number of trays for the adsorbent packing is 20~60, and the reflux ratio is 0.1~4. The temperature of the bottom of distillation column 11 is 250℃~300℃, and the temperature of the top of distillation column 11 is 150℃~200℃. The waste fan lubricating oil is discharged at a rate of 2 hours... -1 ~20h -1 The space velocity is used for adsorption distillation so that water and light hydrocarbons are discharged through the first outlet pipe 111 and condenser 12. S204. Discharge the pretreated waste lubricating oil from the third outlet pipe 113; S205, the gas supply unit 13 supplies gas to the cavity 110 through the second inlet pipe 115, and the operation is carried out at a pressure of -0.08MPa to -0.02MPa in the distillation column 11. The heating temperature of the distillation column 11 is 250℃ to 300℃, and the gas flow rate of the gas supply unit 13 is 200ml / min to 800ml / min, so as to regenerate the adsorbent packing in the distillation column 11 and discharge the desorbed polar additive through the second outlet pipe 112.
[0039] S206. By setting a first switching valve 1140 on the first inlet pipe 114, the on / off state of the first inlet pipe 114 is controlled. By setting a second switching valve 1150 on the second inlet pipe 115, the on / off state of the second inlet pipe 115 is controlled, thereby allowing the first inlet pipe 114 and the second inlet pipe 115 to be in different on / off states. By adjusting the on / off states of the first switching valve 1140 and the second switching valve 1150, the system can be adapted to the specific operating state of the distillation column 11. Specifically, during the removal of water and light hydrocarbons from waste lubricating oil, the first switch valve 1140 is adjusted to the open state to allow the first inlet pipe 114 to be open. At this time, the waste lubricating oil to be treated can enter the cavity 110 through the first inlet pipe 114, and the distillation column 11 performs atmospheric pressure adsorption distillation to remove water and light hydrocarbons from the waste lubricating oil. During the above process, the second switch valve 1150 is in a different switching state than the first switch valve 1140, that is, the second switch valve 1150 is in the closed state. At this time, the regeneration gas cannot enter the cavity 110 through the second inlet pipe 115, thereby avoiding the regeneration gas from affecting the atmospheric pressure adsorption distillation operation of the distillation column 11.
[0040] S207. Multiple processing modules 10 are set up, and the multiple processing modules 10 are connected in parallel to the waste oil supply unit 20 through the first inlet pipe 114, and the multiple processing modules 10 are connected in parallel to the gas supply unit 13 through the second inlet pipe 115; and among the multiple processing modules 10, at least one of the processing modules 10 has its distillation column 11 in atmospheric pressure adsorption distillation state, and at least one of the processing modules 10 has its adsorbent packing in a regeneration state. In the process of treating the waste lubricating oil, the hydrogenation pretreatment device of the multiple processing modules 10 can have different working states for the distillation columns 11 of different processing modules 10. Specifically, while the distillation column 11 of one processing module 10 is performing atmospheric pressure adsorption distillation to remove water and light hydrocarbons from the waste lubricating oil, the distillation column 11 of another processing module 10 can perform adsorbent packing regeneration, thereby reducing the waiting time in the operation process, ensuring continuous processing of waste lubricating oil, and improving the processing efficiency of waste lubricating oil.
[0041] This disclosure does not limit the specific types of adsorbent fillers. For example, in the embodiments provided in this disclosure, the adsorbent filler can be one or both of modified alumina and modified silica.
[0042] In the process of modifying the above-mentioned alumina and silica, the modified alumina and silica can be impregnated with equal volumes of nitric acid solution, sodium hydroxide solution and hydrogen peroxide, then washed with deionized water and dried.
[0043] To improve the adsorption effect on polar additives, the particle size of the above adsorbent filler is 0.5 mm to 2.0 mm.
[0044] In the embodiments provided in this disclosure, the ratio of the regeneration time of the adsorbent packing to the operation time of adsorption distillation (the time for removing water and light hydrocarbons from waste lubricating oil) is 1.2 to 2.0.
[0045] Regarding the above-mentioned hydrogenation pretreatment apparatus for waste lubricating oil, which includes multiple processing modules 10 (the multiple processing modules 10 may include a first distillation column 116, a second distillation column 117, and a third distillation column 118), the following are comparative examples and several exemplary embodiments provided in this disclosure: Example 1 The waste lubricating oil used in Example 1 contains 2 wt% water, 8 wt% light hydrocarbons, 450 ppm phosphorus, and 2350 ppm sulfur. The adsorbent filler is modified alumina treated with 10 mol / L sodium hydroxide solution, with a particle size of 1.5 mm.
[0046] (1) The operating pressure of the first distillation column 116 is 0.15 MPa, the theoretical number of plates of the adsorbent packing is 40, the feed flow rate of the waste blower lubricating oil is 30 kg / h, and the space velocity is 5 h⁻¹. -1 The reflux ratio at the top of the first distillation column 116 is 2.0, and the flow rate of the effluent from the top of the first distillation column 116 is 2.8 kg / h. The effluent from the bottom of the first distillation column 116, 26.9 kg / h, is treated waste blower lubricating oil, which enters the hydrorefining section. The bottom temperature of the first distillation column 116 is 270℃, and the top temperature of the first distillation column 116 is 170℃.
[0047] (2) The adsorbent packing of the first distillation column 116 is regenerated, and at the same time the second distillation column 117 begins to adsorb and distill the waste fan lubricating oil according to the parameters in step (1) above. The regeneration operation pressure of the first distillation column 116 is -0.05MPa, the column bottom heating temperature is 270℃, the nitrogen flow rate is 500ml / min, and the desorbed products are polar additives and a small amount of waste oil, which are discharged from the top of the column into the desorbed product storage tank 16. (3) After the adsorption distillation operation is completed in the second distillation column 117, the adsorbent packing regeneration stage is entered. The time ratio of adsorbent packing regeneration to adsorption distillation is 1.5. The third distillation column 118 starts to perform adsorption distillation and adsorbent packing regeneration according to the parameters in steps (1) and (2). During this process, the first distillation column 116 completes the adsorbent packing regeneration and performs adsorption distillation again. Each distillation column 11 is carried out alternately according to the operation sequence.
[0048] (3) The waste fan lubricating oil obtained from the bottom of distillation column 11 was tested and found to have a water content of <1ppm, a light hydrocarbon content of <1ppm, a phosphorus content of 22ppm, and a sulfur content of 48ppm.
[0049] Example 2 The difference between this embodiment and Embodiment 1 is that the water content in the waste blower lubricating oil is 3wt%, the light hydrocarbon content is 6wt%, the phosphorus content is 251ppm, and the sulfur content is 4870ppm; the adsorbent filler is modified alumina treated with 9mol / L hydrogen peroxide solution, with a particle size of 1.0mm.
[0050] (1) The operating pressure of the first distillation column 116 is 0.18 MPa, the theoretical number of plates of the adsorbent packing is 55, the feed flow rate of the waste blower lubricating oil is 30 kg / h, and the space velocity is 8 h⁻¹. -1 The reflux ratio at the top of the column is 1.5, and the flow rate of the effluent from the top of the column is 2.6 kg / h. The effluent from the bottom of the column, 27.2 kg / h, is the treated waste blower lubricating oil, which enters the hydrorefining section. The temperature of the bottom of the column is 300℃, and the temperature of the top of the column is 200℃.
[0051] (2) The adsorbent packing of the first distillation column 116 is regenerated, and at the same time, the second distillation column 117 begins to adsorb and distill the waste fan lubricating oil according to the parameters in step (1). The regeneration operation pressure of the first distillation column 116 is -0.03MPa, the column bottom heating temperature is 300℃, the nitrogen flow rate is 600ml / min, and the desorbed products are polar additives and a small amount of waste oil, which are discharged from the top of the column into the desorbed product storage tank 16; (3) After the adsorption distillation operation is completed in the second distillation column 117, the adsorbent packing regeneration stage is entered. The time ratio of adsorbent packing regeneration to adsorption distillation is 1.8. The third distillation column 118 starts to perform adsorption distillation and adsorbent packing regeneration according to the parameters in steps (1) and (2). During this process, the first distillation column 116 completes the adsorbent packing regeneration and performs adsorption distillation again. Each distillation column 11 is carried out alternately according to the operation sequence.
[0052] The waste fan lubricating oil obtained from the bottom of distillation column 11 was tested and found that the treated waste fan lubricating oil had a water content of <1ppm, a light hydrocarbon content of <1ppm, a phosphorus content of 9ppm, and a sulfur content of 95ppm.
[0053] Example 3 The difference between this embodiment and Embodiment 1 is that the water content in the waste blower lubricating oil is 4wt%, the light hydrocarbon content is 4wt%, the phosphorus content is 403ppm, and the sulfur content is 3780ppm; the adsorbent filler is modified silica treated with 10mol / L nitric acid solution, with a particle size of 0.5mm.
[0054] (1) The operating pressure of the first distillation column 116 is 0.12 MPa, the theoretical number of plates of the adsorbent packing is 60, the feed flow rate of the waste blower lubricating oil is 20 kg / h, and the space velocity is 3. h-1 The reflux ratio at the top of the column is 3.0, and the flow rate of the effluent from the top of the column is 1.5 kg / h. The effluent from the bottom of the column, 18.3 kg / h, is the treated waste blower lubricating oil, which enters the hydrorefining section. The temperature of the bottom of the column is 250℃, and the temperature of the top of the column is 150℃.
[0055] (2) The adsorbent packing of the first distillation column 116 is regenerated, and at the same time, the second distillation column 117 begins to adsorb and distill the waste fan lubricating oil according to the parameters in step (1). The regeneration operation pressure of the first distillation column 116 is -0.07MPa, the column bottom heating temperature is 250℃, the nitrogen flow rate is 300ml / min, and the desorbed products are polar additives and a small amount of waste oil, which are discharged from the top of the column into the desorbed product storage tank 16; (3) After the adsorption distillation operation is completed in the second distillation column 117, the adsorbent packing regeneration stage is entered. The time ratio of adsorbent packing regeneration to adsorption distillation is 1.9. The third distillation column 118 starts to perform adsorption distillation and adsorbent packing regeneration according to the parameters in steps (1) and (2). During this process, the first distillation column 116 completes the adsorbent packing regeneration and performs adsorption distillation again. Each distillation column 11 is carried out alternately according to the operation sequence.
[0056] The waste fan lubricating oil obtained from the bottom of distillation column 11 was tested and found that the treated waste fan lubricating oil had a water content of <1ppm, a light hydrocarbon content of <1ppm, a phosphorus content of 14ppm, and a sulfur content of 88ppm.
[0057] Comparative Example 1 The method in Comparative Example 1 is the same as in Example 1, except that the adsorbent used in this comparative example is unmodified silica. The waste fan lubricating oil obtained from the bottom of distillation column 11 was tested, and the treated waste fan lubricating oil showed a water content of <1 ppm, a light hydrocarbon content of <1 ppm, a phosphorus content of 225 ppm, and a sulfur content of 1220 ppm. This demonstrates that modified silica can achieve a better removal effect on polar additives containing phosphorus and sulfur.
[0058] The preferred embodiments of this disclosure have been described in detail above with reference to the accompanying drawings. However, this disclosure is not limited to the specific details of the above embodiments. Within the scope of the technical concept of this disclosure, various simple modifications can be made to the technical solutions of this disclosure, and these simple modifications all fall within the protection scope of this disclosure.
[0059] It should also be noted that the various specific technical features described in the above specific embodiments can be combined in any suitable manner without contradiction. In order to avoid unnecessary repetition, this disclosure will not describe the various possible combinations separately.
[0060] Furthermore, various different embodiments of this disclosure can be combined in any way, as long as they do not violate the spirit of this disclosure, they should also be regarded as the content disclosed in this disclosure.
Claims
1. A hydrotreating pretreatment device for waste lubricating oil, characterized in that, include: The processing module includes a distillation column, a condenser, and a gas supply unit. The distillation column has an internal cavity filled with adsorbent packing material. The distillation column is equipped with a first outlet pipe, a second outlet pipe, a third outlet pipe, a first inlet pipe, and a second inlet pipe that are connected to the cavity. The first outlet pipe is connected to the condenser and is used to discharge water and light hydrocarbons from the waste lubricating oil. The second outlet pipe is used to discharge polar additives from the waste lubricating oil. The third outlet pipe is used to discharge the pretreated waste lubricating oil. The first inlet pipe is used to allow waste lubricating oil from the waste oil supply unit to flow into the cavity. The second inlet pipe is connected to the gas supply unit and is used to supply regeneration gas to the cavity.
2. The hydrotreating pretreatment apparatus for waste lubricating oil according to claim 1, characterized in that, A first switching valve is provided on the first inlet pipe, and a second switching valve is provided on the second inlet pipe. The switching states of the first switching valve and the second switching valve are different.
3. The hydrotreating pretreatment apparatus for waste lubricating oil according to claim 1, characterized in that, The processing module also includes a reboiler and a fourth outlet pipe, wherein the reboiler is connected to the cavity and the third outlet pipe respectively through the fourth outlet pipe.
4. The hydrotreating pretreatment apparatus for waste lubricating oil according to claim 1, characterized in that, The processing module also includes a desorbate storage tank, which is connected to the end of the second outlet pipe away from the distillation column.
5. The hydrotreating pretreatment apparatus for waste lubricating oil according to any one of claims 1-4, characterized in that, The hydrogenation pretreatment device for waste lubricating oil includes multiple processing modules. The multiple processing modules are connected in parallel to the waste oil supply unit through the first inlet pipe, and the multiple processing modules are connected in parallel to the gas supply unit through the second inlet pipe. Among the multiple processing modules, the distillation column of at least one processing module is in atmospheric pressure adsorption distillation state, and the adsorbent packing in at least one processing module is in regeneration state.
6. A method for hydrotreating waste lubricating oil applied to any one of claims 1-5, characterized in that, include: The cavity of the distillation column is filled with adsorbent packing material; The waste lubricating oil before entering the distillation column is pretreated to remove solid particles from the waste lubricating oil, and the treated waste lubricating oil flows into the cavity through the first inlet pipe; A normal pressure adsorption distillation operation is performed so that water and light hydrocarbons are discharged through the first outlet pipe and the condenser. The pretreated waste lubricating oil is discharged from the third outlet pipe; The gas supply unit supplies gas to the cavity through the second inlet pipe to regenerate the adsorbent packing in the distillation column, and discharges the desorbed polar additives through the second outlet pipe.
7. The method for hydrotreating waste lubricating oil according to claim 6, characterized in that, The atmospheric pressure adsorption distillation operation of waste lubricating oil in the distillation column includes: The distillation is carried out at a pressure of 0.1 MPa to 0.2 MPa in the distillation column, with 20 to 60 trays of adsorbent packing and a reflux ratio of 0.1 to 4; the temperature of the bottom of the distillation column is 250°C to 300°C, and the temperature of the top of the distillation column is 150°C to 200°C; the waste blower lubricating oil is discharged at a rate of 2 hours... -1 ~20h -1 The space velocity is used for adsorption distillation.
8. The method for hydrotreating waste lubricating oil according to claim 6, characterized in that, Regenerating the adsorbent packing in the distillation column includes: The process is carried out at a pressure of -0.08MPa to -0.02MPa inside the distillation column, the heating temperature of the distillation column is 250℃ to 300℃, and the gas flow rate of the gas supply unit is 200ml / min to 800ml / min.
9. The method for a hydrotreating pretreatment apparatus for waste lubricating oil according to any one of claims 6-8, characterized in that, By setting a first switching valve on the first inlet pipe to control the on / off state of the first inlet pipe, and by setting a second switching valve on the second inlet pipe to control the on / off state of the second inlet pipe, the first inlet pipe and the second inlet pipe are in different on / off states.
10. The method for a hydrotreating pretreatment apparatus for waste lubricating oil according to any one of claims 6-8, characterized in that, Multiple processing modules are provided, and the multiple processing modules are respectively connected in parallel to the waste oil supply unit through the first inlet pipe, and the multiple processing modules are respectively connected in parallel to the gas supply unit through the second inlet pipe; Furthermore, in at least one of the processing modules, the distillation column of at least one processing module is in an atmospheric pressure adsorption distillation state, and the adsorbent packing material in at least one processing module is in a regeneration state.