Process and system for processing high solids coal-based oil residue

Abstract

Processing method and processing system for high solid content coal-based oil residue. The processing method comprises: (1) extracting and first-stage centrifugal separation of high solid content coal-based oil residue; storing, heating and first-stage sedimentation separation of the obtained first-stage centrifugal clear liquid; (2) second-stage separation of the obtained first-stage high solid content bottom liquid; mixing the obtained second-stage separation clear liquid with a trapping agent; performing catalyst trapping on the obtained trapping agent mixture and then performing second-stage sedimentation separation; (3) mixing and blending the obtained first-stage dry phase and second-stage dry phase with washing oil; heating and oil extraction of the obtained dry phase mixture, and outputting solid powder; (4) membrane separation filtration of the obtained second-stage low solid content clear liquid, and then producing needle coke to obtain needle coke products; flash evaporation and molding of the obtained second-stage medium solid content clear liquid to obtain coal-based pitch products. The processing system comprises a first-stage processing separation unit, a second-stage processing separation unit, a dry phase processing unit and a second-stage sedimentation separation liquid processing unit.

Description

Technical Field

[0001] This invention belongs to the field of oil residue processing, specifically relating to a processing method and system for high-solids coal-based oil residue. Background Technology

[0002] Existing processing methods for coal-based oil residue involve dissolving the solid residue using extraction technology, then separating the asphalt, solids, and ash. This is typically a single processing step, producing primary, intermediate, and high-grade asphalt based on ash and solids content. Currently, there is no processing method for high-solids-content coal-based oil residue. If high-solids-content coal-based oil residue (50-65 wt% solids content) is processed using existing methods to produce asphalt with different ash and solids content grades, the ash and catalyst in the high-solids-content residue cannot be completely removed. The resulting asphalt will not meet the premium grade requirements, let alone the ash content requirements of needle coke feedstock. Summary of the Invention

[0003] The first objective of this invention is to provide a processing method for high-solids coal-based oil residue. This processing method can remove ash and catalyst, two solids, in two steps to obtain coal-based pitch products and needle coke products, thus realizing a circular economy and being environmentally friendly.

[0004] The second objective of this invention is to provide a processing system for high-solids coal-based oil residue. This system is capable of performing the aforementioned processing method to remove ash and catalyst, two solids, in two steps, to obtain coal-based pitch products, needle coke products, and solid powder, thereby achieving a circular economy and environmental protection.

[0005] To achieve the first objective of this invention, the following technical solution is adopted:

[0006] A processing method for high-solids coal-based oil residue includes the following steps:

[0007] (1) Extract the high-solids coal-based oil residue raw material with solvent oil and output the extraction mixture; then perform the first-stage centrifugation separation on the obtained extraction mixture and output the first-stage centrifugation clear liquid and the first-stage dry phase; then store, heat and perform the first-stage sedimentation separation on the obtained first-stage centrifugation clear liquid in sequence and output the first-stage low-solids clear liquid and the first-stage high-solids bottom liquid.

[0008] (2) Perform a second-stage separation on the first-stage high-solid-content bottom liquid obtained in step (1) to output a second-stage separated clear liquid and a second-stage dry phase; then add a capture agent to the obtained second-stage separated clear liquid and mix to output a capture agent mixture; then use the obtained capture agent mixture to capture the catalyst and then perform a second-stage sedimentation separation to output a second-stage low-solid-content clear liquid, a second-stage medium-solid-content clear liquid and a second-stage high-solid-content bottom liquid respectively.

[0009] (3) Use washing oil to blend and mix the primary dry phase obtained in step (1) and the secondary dry phase obtained in step (2) to output the dry phase mixture; then heat and remove oil from the obtained dry phase mixture to output solid powder.

[0010] (4) The secondary low solid content liquid obtained in step (2) is subjected to membrane separation and filtration and then needle coke production to obtain needle coke product;

[0011] The secondary solid-containing liquid obtained in step (2) is subjected to flash evaporation and molding in sequence to obtain coal-based pitch products.

[0012] The present invention relates to a processing method for high-solids coal-based oil residue. Preferably, the feeding method for the first-stage sedimentation separation is to feed the material from top to bottom in sequence by a spiral feed under bottom aeration; preferably, intermittent aeration; preferably, the spiral angle is 5-10° with the horizontal direction.

[0013] The present invention provides a processing method for high-solids coal-based oil residue. Preferably, step (2) further includes the following step: the secondary high-solids bottom liquid obtained in step (2) is returned from the front end to the second-stage separation device for recycling processing.

[0014] The present invention provides a processing method for high-solids coal-based oil residue. Preferably, the processing method further includes step (5), in which the secondary separation liquid obtained in step (2) is returned from the front end to the extraction device for recycling under abnormal operating conditions.

[0015] The present invention provides a processing method for high-solids coal-based oil residue. Preferably, step (2) further includes the following step: the secondary separation liquid obtained in step (2) is returned from the front end to the second-stage separation device for recycling.

[0016] The present invention relates to a processing method for high-solids coal-based oil residue. Preferably, the circulation method of the secondary separation liquid obtained in step (2) is to circulate and concentrate it according to the separation concentration concentration formula. When the solid content of the obtained secondary separation liquid has not dropped to 1.8wt%, the reflux ratio is automatically adjusted by interlocking, and it is returned from the front end to the second-stage separation device for circulation processing. Until the solid content concentration of the obtained secondary separation liquid drops to 1.8wt%, it is mixed with the capture agent and sent to the second-stage sedimentation separation device for processing.

[0017] The present invention provides a processing method for high-solids coal-based oil residue. Preferably, step (1) further includes the following step: the primary separation liquid obtained in step (1) is returned from the front end to the first-stage separation device for recycling processing.

[0018] The present invention relates to a processing method for high-solids coal-based oil residue. Preferably, the circulation method of the primary separation liquid obtained in step (1) is to circulate and concentrate it according to the separation concentration concentration formula. When the solid content of the primary centrifugal liquid obtained has not dropped to 5.7-7wt%, the reflux ratio is automatically adjusted by interlocking, and it is returned from the front end to the first-stage separation device for circulation processing. Until the solid content of the primary separation liquid obtained drops to 5.7-7wt%, it is heated and sent to the first-stage sedimentation separation device for processing.

[0019] The present invention relates to a processing method for high-solids coal-based oil residue. Preferably, in step (1) and / or step (2), the separation concentration concentration formula is as follows:

[0020]

[0021] f1 = a × (1 - c)

[0022] Where, f1: solids concentration of the separated supernatant in the first cycle; n: number of cycles; f n f represents the solids concentration of the separated supernatant from the nth cycle. n <8f1; a: Initial feed solids concentration of the first-stage separation unit, a constant; b: Clear liquid recovery rate, a constant of 0-100%; c: Dry phase concentration rate, a constant of 0-100%; d: Reflux ratio, reflux ratio = outlet clear liquid return amount / inlet feed amount, a constant of 0-100%.

[0023] This invention relates to a processing method for high-solids coal-based oil residue. Preferably, the processing method further includes: introducing wash oil to flush the secondary separator and the primary centrifuge during system start-up and shutdown; and / or

[0024] The processing method further includes: introducing wash oil under abnormal operating conditions to adjust the concentration of the feed to the secondary separator and the primary centrifuge; preferably, the adjustment limit is related to f. n <8f1 coordinated allocation.

[0025] To achieve the second objective of this invention, a processing system for high-solids coal-based oil residue is provided. The processing system includes a primary processing and separation unit, a secondary processing and separation unit, a dry phase processing unit, and a secondary settling and separation liquid processing unit, which are sequentially connected by pipelines.

[0026] The primary processing and separation unit includes, in sequence via pipelines, an extraction tank, a primary centrifuge, a primary centrifugal clarified liquid tank, a primary heating furnace, and a primary sedimentation separation tank; wherein...

[0027] The extraction tank is equipped with a feed inlet and is connected to a high solids oil residue feed pipeline. The high solids oil residue feed pipeline is also connected to a solvent oil pipeline for feeding high solids oil residue and solvent oil separately to extract the high solids oil residue and output an extraction mixture.

[0028] The feed inlet of the first-stage centrifuge is connected to the outlet of the extraction tank, and is used to receive the extraction mixture from the extraction tank and perform first-stage centrifugation separation on it, outputting a first-stage centrifugal clear liquid and a first-stage dry phase, thereby separating out some of the solids contained therein.

[0029] The inlet of the primary centrifugal clear liquid tank is connected to the primary centrifugal clear liquid outlet of the primary centrifuge, and the primary centrifugal clear liquid tank, the primary heating furnace and the primary sedimentation separation tank are connected in sequence through pipelines to store, heat and perform first-stage sedimentation separation of the primary centrifugal clear liquid from the primary centrifuge in sequence, and output primary low solid content clear liquid and primary high solid content bottom liquid.

[0030] The secondary processing and separation unit includes a secondary separator, a pipeline mixer, and a secondary settling tank, which are connected sequentially by pipelines; wherein...

[0031] The inlet of the secondary separator is connected to the outlet of the primary high-solids-content liquid of the primary processing and separation unit. It is used to receive the primary high-solids-content liquid from the primary processing and separation unit and perform a second-stage separation on it, outputting a secondary separation clear liquid and a secondary dry phase, thereby separating out the ash and catalyst.

[0032] The pipeline mixer is provided with a feed inlet and a reagent addition inlet. Its feed inlet is connected to the secondary separation clear liquid outlet of the secondary separator, and its reagent addition inlet is located at its bottom and connected to a reagent addition pipeline for inputting a capture agent to mix the received secondary separation clear liquid from the secondary separator and outputting a capture agent mixture.

[0033] The inlet of the secondary sedimentation tank is connected to the outlet of the pipeline mixer. It is used to receive and use the scavenger mixture from the pipeline mixer to capture the catalyst before performing a second-stage sedimentation separation. This completes the capture and separation of the catalyst. The secondary low-solids clear liquid is output from the upper outlet, the secondary medium-solids clear liquid is output from the middle outlet, and the secondary high-solids bottom liquid is output from the lower outlet, thereby separating out the residual catalyst.

[0034] The dry phase processing unit includes a dry phase buffer tank and a drying and forming device connected sequentially by pipelines; wherein...

[0035] The dry phase buffer tank is provided with a dry phase inlet and an oil phase inlet. Its dry phase inlet is connected to the primary dry phase outlet of the primary processing and separation unit and the secondary dry phase outlet of the secondary processing and separation unit, respectively. Its oil phase inlet is connected to a wash oil pipeline for introducing wash oil to blend and mix the primary dry phase from the primary processing and separation unit and the secondary dry phase from the secondary processing and separation unit, and output dry phase mixture.

[0036] The inlet of the drying and forming device is connected to the outlet of the dry phase buffer tank, and is used to receive the dry phase mixture from the dry phase buffer tank, heat it and remove oil, and output solid powder.

[0037] The secondary sedimentation separation liquid processing unit includes a secondary low-solids-content needle-shaped coke sub-unit and a secondary medium-solids-content flash evaporation forming sub-unit; wherein...

[0038] The secondary low-solids-content liquid needle coke subunit includes a membrane separation device and a needle coke device connected in sequence by pipelines. The inlet of the membrane separation device is connected to the secondary low-solids-content liquid outlet of the secondary processing and separation unit, and is used to sequentially perform membrane separation and filtration on the secondary low-solids-content liquid from the secondary processing and separation unit to produce needle coke product. The inlet of the secondary medium-solids-content liquid flash evaporation and forming subunit is connected to the secondary medium-solids-content liquid outlet of the secondary processing and separation unit, and is used to sequentially flash evaporate and form the secondary medium-solids-content liquid from the secondary processing and separation unit to obtain coal-based pitch product.

[0039] Preferably, in the processing system of the present invention, the primary sedimentation separation tank is a cylindrical tank; a feed pipe is provided at the top of the tank along the tangent of the tank for feeding; a vertical empty pipe is provided along the center of its vertical axis for introducing nitrogen gas from top to bottom to aerate the bottom of the tank; a spiral structure is provided around the periphery of the vertical empty pipe for the feed from the feed pipe to settle downwards in a swirling flow along its spiral guide according to the feed push flow speed; the downward inclination angle of the feed pipe is consistent with the downward inclination angle of the spiral blades in the spiral structure, and the downward inclination angle is 5-10°, forming a swirling downward flow channel.

[0040] In the processing system of the present invention, preferably, the length of the feed pipe entering the primary sedimentation separation tank is 1 / 4 to 1 / 6 of the tank diameter.

[0041] Preferably, the processing system of the present invention includes a first material conveying pipeline from the lower outlet of the secondary settling separator to the feed inlet of the secondary separator, for conveying the secondary high-solids bottom liquid from the secondary settling separator back to the secondary separator for separation.

[0042] Preferably, the processing system of the present invention includes a second material conveying pipeline from the outlet of the secondary separated liquid of the secondary separator to the inlet of the extraction tank, for returning the secondary separated liquid from the secondary separator to the extraction tank for cyclic processing.

[0043] Preferably, in the processing system of the present invention, a second reflux pipeline is provided from the outlet of the secondary separated clarified liquid of the secondary separator to its inlet, for recirculating the secondary separated clarified liquid output from the secondary separator back to the secondary separator for further processing; preferably, a secondary solids content meter is provided on the third material conveying pipeline from the secondary separator to the pipeline mixer, and a secondary regulating valve is provided on the second reflux pipeline, wherein the secondary solids content meter and the secondary regulating valve are interlocked according to the separation concentration concentration formula.

[0044] Preferably, the processing system of the present invention includes a first reflux pipeline from the outlet of the primary centrifugal clear liquid tank to the inlet of the primary centrifuge, for circulating the primary separated clear liquid output from the primary centrifugal clear liquid tank back to the primary separator for further processing.

[0045] Preferably, in the processing system of the present invention, a primary solid content meter is installed on the fourth material conveying pipeline from the primary centrifugal clear liquid tank to the primary heating furnace, and a primary regulating valve is installed on the first reflux pipeline. The primary solid content meter and the primary regulating valve are interlocked according to the separation concentration concentration formula.

[0046] Preferably, in the processing system of the present invention, a fifth material conveying pipeline is provided from the outlet of the primary low-solids liquid in the primary settling separator to the inlet of the secondary low-solids liquid needle coke unit, for conveying the primary low-solids liquid from the primary settling separator to the secondary low-solids liquid needle coke unit when the operating conditions are good.

[0047] Preferably, the processing system of the present invention includes a sixth material conveying pipeline from the outlet of the primary low-solids liquid in the primary settling separator to the inlet of the secondary medium-solids liquid flash evaporation molding subunit, for conveying the primary low-solids liquid from the primary settling separator to the secondary medium-solids liquid flash evaporation molding subunit under normal operating conditions.

[0048] Preferably, the processing system of the present invention includes a seventh material conveying pipeline from the outlet of the primary low-solids liquid of the primary sedimentation separator to the inlet of the pipeline mixer, for conveying the primary low-solids liquid from the primary sedimentation separator to the pipeline mixer under abnormal operating conditions.

[0049] Preferably, in the processing system of the present invention, the washing oil pipeline further branches into washing oil branch pipes, which are connected to the feed inlet of the secondary separator. These branch pipes are used to introduce washing oil to flush the secondary separator and the primary centrifuge when the system is started or stopped, and to introduce washing oil to adjust the concentration of the feed to the secondary separator and the primary centrifuge under abnormal operating conditions.

[0050] The present invention also provides a processing method for processing high-solids coal-based oil residue using the aforementioned processing system.

[0051] The beneficial effects of this invention are as follows:

[0052] The processing method and system for high-solids coal-based oil residue of the present invention can remove ash and catalyst, two solids, in two steps, extract asphaltene from the high-solids coal-based oil residue for processing into high-end raw materials to obtain high-grade coal-based asphalt products, and obtain needle coke products, thus realizing a circular economy and green environmental protection. Attached Figure Description

[0053] Figure 1 This is a schematic diagram of the structure of the processing system for high-solids coal-based oil residue of the present invention in one embodiment;

[0054] Figure 2 This is a schematic diagram of the structure of a primary settling separator in one embodiment of the processing system for high-solids coal-based oil residue of the present invention. Detailed Implementation

[0055] The technical solution and its effects of the present invention will be further described below with reference to specific embodiments / examples. The following embodiments / examples are only for illustrating the content of the present invention, and the invention is not limited to the following embodiments or examples. Any foresightful modifications made to the present invention based on the concept of the present invention are within the scope of protection claimed by the present invention.

[0056] like Figure 1-2 As shown, a processing method for high-solids coal-based oil residue includes the following steps:

[0057] (1) Extract the high-solids coal-based oil residue raw material with solvent oil and output the extraction mixture; then perform the first-stage centrifugation separation on the obtained extraction mixture to output the first-stage centrifuged clear liquid and the first-stage dry phase (thereby separating some of the solids); then store, heat and perform the first-stage sedimentation separation on the obtained first-stage centrifuged clear liquid in sequence to output the first-stage low-solids clear liquid and the first-stage high-solids bottom liquid.

[0058] (2) Perform a second-stage separation on the primary high-solids bottom liquid obtained in step (1) to output a secondary clear liquid and a secondary dry phase; then add a scavenging agent to the obtained secondary clear liquid and mix to output a scavenging agent mixture; then use the obtained scavenging agent mixture to capture the catalyst and then perform a second-stage sedimentation separation to complete the capture and separation of the catalyst, and output a secondary low-solids clear liquid, a secondary medium-solids clear liquid and a secondary high-solids bottom liquid respectively (thereby separating the residual catalyst).

[0059] (3) Use washing oil to blend and mix the primary dry phase obtained in step (1) and the secondary dry phase obtained in step (2) to output the dry phase mixture; then heat and remove oil from the obtained dry phase mixture to output solid powder.

[0060] (4) The secondary low solid content liquid obtained in step (2) is subjected to membrane separation and filtration and then needle coke production to obtain needle coke product;

[0061] The secondary solid-containing liquid obtained in step (2) is subjected to flash evaporation and molding in sequence to obtain coal-based pitch products.

[0062] Those skilled in the art understand that there are currently technologies for producing asphalt from coal-based oil residue with 40-50 wt% solids content. However, these technologies cannot completely remove the two solid components (ash and catalyst) in high-solids coal-based oil residue. Instead, they remove them simultaneously. This inevitably results in some asphalt being separated along with the high-solids bottom liquid, affecting the processing and production of premium-grade asphalt and reducing the yield and quality of coal-based asphalt products.

[0063] The present invention relates to a processing method and system for high-solids coal-based oil residue, which can remove ash and catalyst in two steps, extracting asphaltene from the high-solids coal-based oil residue for processing into high-end raw materials to obtain coal-based pitch products and needle coke products, thus achieving a circular economy and environmental protection. First, a first-stage centrifugal separation is used to reduce the total solids content, i.e., ash and catalyst substances. Then, a first-stage sedimentation separation is used, so that the clarified liquid is used as raw material for producing coal-based pitch products. The concentrated first-stage high-solids bottom liquid undergoes a second-stage separation, mainly separating more than 95 wt% of ash and more than 92 wt% of catalyst from the solids. The second-stage sedimentation separation mainly uses a scavenging agent to capture and remove the catalyst from the solids through sedimentation. In this way, both ash and catalyst substances, two inorganic substances, are completely removed, yielding the raw material for producing needle coke products.

[0064] Those skilled in the art will understand that the high-solids coal-based oil residue described in this invention refers to high-solids coal-based oil residue with a solids content of 50-65 wt%.

[0065] In one embodiment, the high-solids coal-based oil residue comprises:

[0066] Light oil: 5-15 wt%, for example, 7 wt%;

[0067] Wash oil: 6-15wt%, for example, 7wt%;

[0068] Asphalt: 20-35 wt%, for example, 25.5 wt%;

[0069] Ash content: 28-32 wt%, for example, 29 wt%;

[0070] Catalyst: 15-35 wt%, for example, 31 wt%.

[0071] Moisture content: 0.2-0.5 wt%, for example, 0.3 wt%.

[0072] Other components are 0-0.3 wt%, for example, 0.2 wt%.

[0073] In one embodiment, the high-solids coal-based oil residue has a water content of <0.3wt%, such as 0.25wt% and 0.2wt%; and a softening point of ≥180℃, such as 185℃.

[0074] Those skilled in the art will understand that solvent oil used as an extractant can be wash oil and / or heavy oil. In one embodiment, in step (1), the solvent oil includes wash oil and heavy oil, and the mass ratio of wash oil to heavy oil is (2-3):1, for example, 2.5:1; preferably, the wash oil is selected from wash oil with a distillation range of 230-300°C, and the heavy oil is selected from heavy oil with a distillation range of 210-380°C.

[0075] To improve the extraction effect, in one embodiment, in step (1), the mass ratio of the solvent oil to the high solids coal-based oil residue is (2.5-4):1, for example, 3:1 and 3.5:1.

[0076] To improve the extraction effect, in one embodiment, in step (1), the extraction temperature is 110-120°C, such as 112°C, 114°C, 116°C and 118°C; and / or the residence time is 4-8h, such as 6h.

[0077] In one embodiment, in step (1), the wash oil is selected from wash oil with an extraction distillation range of 230-300℃, a water content of ≤1wt%, and a standard density of 1.07-1.11 g / cm³. 3 The normal operating temperature is 30-70℃, the chlorine content is ≤18mg / l, the acid value is ≤0.4mg / g, and the ash content is ≤0.1wt%.

[0078] In one embodiment, in step (1), the heavy oil is selected from heavy oil with an extraction distillation range of 210-380℃, a water content of ≤1wt%, and a standard density of 0.97-1.04 g / cm³. 3 The normal operating temperature is 70-130℃, the chlorine content is ≤17mg / l, the acid value is ≤0.4mg / g, and the ash content is ≤0.3wt%.

[0079] Those skilled in the art will understand that normal temperature refers to the transport and storage temperature of oil.

[0080] In this invention, the extraction is continuous extraction.

[0081] To improve the effect of the first-stage centrifugal separation and remove the total solids (ash and catalyst), in one embodiment, the conditions for the first-stage centrifugal separation in step (1) include: a differential speed of 1-28 rpm, such as 5 rpm, 10 rpm, 15 rpm, 20 rpm and 25 rpm; and / or a rotational speed of 2000-3500 rpm, such as 2500 rpm and 3000 rpm; and / or a feed temperature of 90-120°C, such as 100°C and 110°C.

[0082] In order to improve the effect of the first-stage sedimentation separation and further remove the total solids (ash and catalyst), in one embodiment, the conditions for the first-stage sedimentation separation in step (1) include: a pressure of 3-5 kPa, such as 4 kPa; and / or a temperature of 190-230°C, such as 200°C, 210°C and 220°C; and / or a residence time of 70-90 h, such as 75 h, 80 h and 85 h.

[0083] In one embodiment, the feeding method for the first-stage sedimentation separation is to feed the material from top to bottom in a spiral manner with bottom aeration; preferably, the spiral angle is 5-10° with the horizontal direction, such as 7°.

[0084] In one embodiment, the feeding method for the second-stage sedimentation separation is to feed from top to bottom with bottom aeration; intermittent aeration is preferred.

[0085] To improve the effect of the second-stage separation and remove residual ash, in one embodiment, the conditions for the second-stage separation in step (2) include: a differential speed of 20-60 rpm, such as 25 rpm, 30 rpm, 35 rpm, 40 rpm, 45 rpm, 50 rpm and 55 rpm; and / or a rotational speed of 6000-6600 rpm, such as 6200 rpm, 6300 rpm and 6400 rpm; and / or a feed temperature of 90-140℃, such as 100℃, 110℃, 120℃ and 130℃.

[0086] To improve the effect of the second-stage sedimentation separation and remove residual catalyst, in one embodiment, the conditions for the second-stage sedimentation separation in step (2) include: a pressure of 4-8 kPa, such as 5 kPa, 6 kPa and 7 kPa; and / or a temperature of 145-180°C, such as 150°C, 160°C and 170°C; and / or a residence time of 45-55 h, such as 50 h.

[0087] In one embodiment, in step (2), the capturing agent includes an oil slurry powder settling agent, such as SSA-1.

[0088] In order to improve the separation effect of the catalyst, in one embodiment, in step (2), the amount of the capturing agent is ≥300ppm, so that the catalyst removal rate in the secondary separation liquid can reach more than 90.9wt%.

[0089] To harmonize the solids concentration of the primary and secondary dry phases, wash oil can be used to homogenize their solids concentration before removing the wash oil. In one embodiment, in step (3), the amount of wash oil used is such that it harmonizes and mixes the primary dry phase obtained in step (1) and the secondary dry phase obtained in step (2) until the dry phase concentration in the resulting dry phase mixture is 50-55 wt%, such as 51 wt%, 52 wt%, 53 wt%, and 54 wt%, thereby making its solids concentration more uniform.

[0090] In one embodiment, in step (3), the wash oil is selected from wash oils with a distillation range of 230-300℃, such as wash oil products produced by Xinjiang Coal Chemical Group.

[0091] In order to improve the separation effect, in one embodiment, step (1) further includes the following step: returning the primary separation liquid obtained in step (1) from the front end to the first-stage separation device for circulation processing, thereby further separating the solids contained therein.

[0092] In one embodiment, the primary separation liquid obtained in step (1) is circulated and concentrated according to the separation concentration concentration formula. When the solid content of the primary centrifugal liquid has not dropped to 5.7-7wt%, the reflux ratio is automatically adjusted by interlocking, and it is returned from the front end to the first-stage separation device for circulation processing. When the solid content of the primary separation liquid drops to 5.7-7wt% (e.g., 5.8wt%, 6wt%, 6.2wt%, 6.4wt%, 6.6wt%, and 6.8wt%), it is heated and sent to the first-stage sedimentation separation device for processing.

[0093] In order to avoid increasing the loss of asphalt and needle coke raw materials and increase the output of coal-based pitch products and needle coke products, in one embodiment, step (2) further includes the following step: the secondary high solid content bottom liquid obtained in step (2) is returned from the front end to the second-stage separation device for recycling processing, thereby reusing the asphalt raw materials in the obtained secondary high solid content bottom liquid.

[0094] To further separate solids or when the secondary separation liquid output from the second stage separation is in abnormal condition, it needs to be recycled. In one embodiment, the processing method further includes step (5), in which the secondary separation liquid obtained in step (2) is returned from the front end to the extraction device for recycling under abnormal conditions, thereby further separating the total solids (including ash and catalyst) therein and reducing the total solids concentration of the secondary separation liquid obtained after recycling.

[0095] In order to further separate the ash, in one embodiment, step (2) further includes the following steps: returning the secondary separation liquid obtained in step (2) from the front end to the second-stage separation device for recycling, thereby further separating the solids therein and reducing the solids concentration of the secondary separation liquid obtained after recycling.

[0096] In one embodiment, the secondary separation liquid obtained in step (2) is circulated and concentrated according to the separation concentration concentration formula. When the solid content of the obtained secondary separation liquid has not dropped to 1.8 wt%, the reflux ratio is automatically adjusted by interlocking and the liquid is returned from the front end to the second-stage separation device for circulation processing. When the solid content of the obtained secondary separation liquid drops to 1.8 wt%, it is mixed with the capture agent and sent to the second-stage sedimentation separation device for further processing to further reduce the solid content.

[0097] In one embodiment, in step (1) and / or step (2), the separation concentration concentration formula is as follows:

[0098]

[0099] f1 = a × (1 - c);

[0100] Where, f1: solids concentration of the separated supernatant in the first cycle; n: number of cycles; f n f represents the solids concentration of the separated supernatant from the nth cycle. n <8f1; a: Initial feed solids concentration of the first-stage separation unit, a constant; b: Clear liquid recovery rate, a constant of 0-100%; c: Dry phase concentration rate, a constant of 0-100%; d: Reflux ratio, reflux ratio = outlet clear liquid return amount / inlet feed amount, a constant of 0-100%.

[0101] In one embodiment, the processing method further includes: introducing wash oil to flush the secondary separator and the primary centrifuge during system start-up and shutdown; and / or

[0102] The processing method further includes: introducing wash oil under abnormal operating conditions to adjust the concentration of the feed to the secondary separator and the primary centrifuge; preferably, the adjustment limit is related to f. n <8f1 coordinated allocation.

[0103] In one embodiment, in step (1), the composition of the obtained primary centrifuged liquid includes: ash content ≤ 3 wt%; solid content ≤ 5.7 wt%.

[0104] In one embodiment, in step (1), the composition of the obtained primary low-solids clear liquid includes: ash content ≤ 0.1 wt%; solids content ≤ 0.2 wt%.

[0105] In one embodiment, in step (1), the composition of the obtained primary high-solids liquid includes: ash content ≤ 12 wt%; solids content 28 wt%.

[0106] In one embodiment, in step (2), the composition of the obtained secondary separation liquid includes: ash content ≤ 0.6 wt%; solid content ≤ 1.8 wt%.

[0107] In one embodiment, in step (2), the composition of the obtained secondary low-solids clear liquid includes: ash content ≤ 0.05 wt%; solids content ≤ 0.1 wt%.

[0108] In one embodiment, in step (2), the composition of the resulting secondary solid-containing liquid includes: ash content ≤ 0.1 wt%; solid content ≤ 0.16 wt%.

[0109] In one embodiment, in step (2), the composition of the obtained secondary high-solids bottom liquid includes: ash content ≤ 1.1 wt%; solids content ≤ 3.26 wt%.

[0110] In one embodiment, in step (4), the components of the obtained secondary low-solids clear liquid after membrane separation and filtration include: ash content ≤ 0.02 wt%; solids content ≤ 0.03 wt%.

[0111] In one embodiment, in step (4), the resulting needle coke product conforms to the GB / T 32158-2015 standard.

[0112] In one embodiment, in step (4), the obtained coal-based tar pitch product conforms to the GB / T 38772-2020 standard.

[0113] Those skilled in the art will understand that the equipment used in each step of this invention is commonly used in the field.

[0114] In step (4), the flash evaporation and molding processes in the needle coke production process and the coal-based pitch product generation process are commonly used processes in this field, and will not be described in detail here.

[0115] The present invention also provides a processing system for high-solids coal-based oil residue.

[0116] like Figure 1-2 As shown, in one embodiment, the processing system includes a primary processing and separation unit, a secondary processing and separation unit, a dry phase processing unit, and a secondary sedimentation separation liquid processing unit, which are sequentially connected by pipelines; wherein,

[0117] The primary processing and separation unit includes an extraction tank 101, a primary centrifuge 102, a primary centrifugal clear liquid tank 103, a primary heating furnace 104, and a primary sedimentation separation tank 105, which are connected in sequence by pipelines.

[0118] in,

[0119] The extraction tank 101 is provided with a feed inlet and is connected to a high solids oil residue feed pipeline. The high solids oil residue feed pipeline is also connected to a solvent oil pipeline for feeding high solids oil residue and solvent oil separately to extract the high solids oil residue and output the extraction mixture.

[0120] The feed inlet of the first-stage centrifuge 102 is connected to the outlet of the extraction tank 101, and is used to receive the extraction mixture from the extraction tank 101 and perform first-stage centrifugation separation on it, outputting first-stage centrifugal clear liquid and first-stage dry phase, thereby separating out some of the solids contained therein.

[0121] The inlet of the primary centrifugal clear liquid tank 103 is connected to the primary centrifugal clear liquid outlet of the primary centrifuge 102, and the primary centrifugal clear liquid tank 103, the primary heating furnace 104 and the primary sedimentation separation tank 105 are connected in sequence through pipelines to store, heat and perform first-stage sedimentation separation of the primary centrifugal clear liquid from the primary centrifuge 102 in sequence, and output primary low solid content clear liquid and primary high solid content bottom liquid.

[0122] The secondary processing and separation unit includes a secondary separator 201, a pipeline mixer 202, and a secondary settling tank 203, which are connected sequentially by pipelines; wherein...

[0123] The inlet of the secondary separator 201 is connected to the outlet of the primary high solid content liquid of the primary processing and separation unit. It is used to receive the primary high solid content liquid from the primary processing and separation unit and perform a second-stage separation on it, outputting a secondary separation clear liquid and a secondary dry phase, thereby separating out the ash and catalyst therein.

[0124] The pipeline mixer 202 is provided with a feed inlet and a reagent addition inlet. Its feed inlet is connected to the secondary separation clear liquid outlet of the secondary separator 201, and its reagent addition inlet is located at its bottom and connected to a reagent addition pipeline for inputting a capture agent to mix the received secondary separation clear liquid from the secondary separator 201 and outputting a capture agent mixture.

[0125] The inlet of the secondary sedimentation separator 203 is connected to the outlet of the pipeline mixer 202. It is used to receive and utilize the scavenger mixture (catalyst carried in the feed) from the pipeline mixer 202 to capture the catalyst before performing a second-stage sedimentation separation. This completes the capture and separation of the catalyst. The secondary low-solids clear liquid is output from the upper outlet, the secondary medium-solids clear liquid is output from the middle outlet, and the secondary high-solids bottom liquid is output from the lower outlet, thereby separating out the residual catalyst.

[0126] The dry phase processing unit includes a dry phase buffer tank 301 and a drying and forming device 302 connected in sequence by pipelines; wherein...

[0127] The dry phase buffer tank 301 is provided with a dry phase inlet and an oil phase inlet. Its dry phase inlet is connected to the primary dry phase outlet of the primary processing and separation unit and the secondary dry phase outlet of the secondary processing and separation unit, respectively. Its oil phase inlet is connected to a wash oil pipeline for introducing wash oil to blend and mix the primary dry phase from the primary processing and separation unit and the secondary dry phase from the secondary processing and separation unit, and output dry phase mixture.

[0128] The inlet of the drying and forming device 302 is connected to the outlet of the dry phase buffer tank 301, and is used to receive the dry phase mixture from the dry phase buffer tank 301 and heat and remove oil from it.

[0129] Output solid powder;

[0130] The secondary sedimentation separation liquid processing unit includes a secondary low-solids-content needle-shaped coke sub-unit and a secondary medium-solids-content flash evaporation forming sub-unit 403; wherein...

[0131] The secondary low-solids-content liquid needle coke subunit includes a membrane separation device 401 and a needle coke device 402 connected in sequence by pipelines. The inlet of the membrane separation device 401 is connected to the secondary low-solids-content liquid outlet of the secondary processing and separation unit, and is used to sequentially perform membrane separation and filtration on the secondary low-solids-content liquid from the secondary processing and separation unit to produce needle coke and obtain needle coke product.

[0132] The inlet of the secondary solid-containing liquid flash evaporation and molding subunit 403 is connected to the secondary solid-containing liquid outlet of the secondary processing and separation unit, and is used to flash evaporate and mold the secondary solid-containing liquid from the secondary processing and separation unit in sequence to obtain coal-based pitch products.

[0133] The processing system for high-solids coal-based oil residue of the present invention can be used in the aforementioned method.

[0134] Those skilled in the art will understand that the extraction tank 101 is a commonly used extraction device in the art. In one embodiment, the extraction tank 101 employs a combination of frame and paddle stirring for extraction and mixing.

[0135] In one embodiment, a first material conveying pipeline 5 is provided from the lower outlet of the secondary settling separator 203 to the feed inlet of the secondary separator 201, for returning the secondary high-solids bottom liquid from the secondary settling separator 203 to the secondary separator 201 for separation, thereby avoiding the loss of asphalt raw materials and increasing the yield of coal-based pitch products.

[0136] In one embodiment, the discharge end of the high solids oil residue feed pipeline is also equipped with an extraction evaporator, which is used to cool the high solids oil residue and solvent oil before feeding them into the extraction tank 101.

[0137] Those skilled in the art will understand that the needle coke apparatus 402 is a commonly used needle coke apparatus in the art. In one embodiment, the needle coke apparatus 402 includes a coking tower, an extraction tower, an atmospheric distillation tower, and a vacuum distillation tower connected by pipelines, for sequentially coking, extracting, atmospheric distillation, and vacuum distillation of the liquid after membrane separation and filtration to obtain needle coke product. Further details are omitted here.

[0138] Those skilled in the art will understand that the secondary solid-containing liquid flash evaporation forming subunit 403 is a commonly used flash evaporation forming system in the art. In one embodiment, the secondary solid-containing liquid flash evaporation forming subunit 403 includes a flash evaporation device and a forming device connected by pipelines; the flash evaporation device includes a flash heat exchanger, an atmospheric pressure tower, a heating furnace, a vacuum tower, and a heat exchanger connected by pipelines, used to sequentially perform heat exchange and heating, atmospheric pressure distillation, heating, vacuum distillation, and heat exchange on the secondary solid-containing liquid from the secondary processing and separation unit; the forming device includes a liquid asphalt lift pump, a liquid asphalt silo, and a liquid asphalt circulation pump connected by pipelines, used to sequentially lift, store, and load the material obtained after processing by the flash evaporation device. Further details are omitted here.

[0139] In one embodiment of this invention, in the secondary solid-containing liquid flash evaporation forming subunit 403 of the secondary sedimentation separation liquid processing unit, the secondary solid-containing liquid is pumped to 0.65 MPa by a booster pump and then sent to a flash heat exchanger to be heated to 370-385°C. It is then sent to an atmospheric distillation tower for atmospheric distillation, with the bottom temperature of the tower being 350-380°C and the top pressure being 8-15 kPa. Next, it is sent to a heating furnace to be heated to 390-420°C. Then, it is sent to a vacuum distillation tower for vacuum distillation, with the bottom temperature of the tower being 360-388°C and the top pressure being 8-15 kPa. Finally, the wash oil and heavy oil are extracted, and the resulting coal-based pitch product is pumped to a liquid product pitch tank for storage.

[0140] Those skilled in the art will understand that the drying and forming apparatus 302 is a commonly used device in the art. In one embodiment, the drying and forming apparatus 302 includes a drying tower, a dry phase heating furnace, a washing tower, and a vacuum pump connected by pipelines, used to extract wash oil from the dry phase mixture from the dry phase buffer tank 301 and output solid powder. Further details will not be provided here.

[0141] In one embodiment of the present invention, the drying and forming device 302 in the dry phase processing unit includes a dry phase preheater, a dry phase heater, a dry phase heating furnace, a dry phase drying tower, a dry vapor phase scrubbing tower, a dry material cooler, and a wash oil cooler, all connected by pipelines. The wash oil is high-temperature wash oil. The dry phase mixture in the dry phase buffer tank 301 is sent to the dry phase preheater to exchange heat with the wash oil from the dry vapor phase scrubbing tower to 238°C, then sent to the dry phase heater to be heated to 300°C, then sent to the dry phase heating furnace to be heated to 365°C, and finally sent to the dry phase drying tower for rapid flash drying. The material is then separated from the top of the tower. The gas phase wash oil exits, and solid powder at 285°C is output from the bottom of the tower. After being cooled to 60°C by the dry material cooler, the solid powder is sent to the powder storage silo of the powder forming unit for storage. The gas phase wash oil at the top of the dry phase drying tower is sent to the dry gas phase washing tower for washing. The gas phase wash oil is output from the top of the tower and sent to the dry phase preheater to exchange heat with the dry phase mixture sent there for cooling. The cooled wash oil is collected and stored in the wash oil tank. After the dry gas phase washing tower is saturated, part of the dust-containing wash oil is cooled with circulating water by the wash oil cooler (preferably cooled to ≤60°C) and sent to the dry phase buffer tank 301 as supplementary wash oil.

[0142] Those skilled in the art will understand that, in the corresponding conveying process, booster pumps are installed to pump the materials to the corresponding equipment. For example, booster pumps are installed on the extraction mixture outlet pipeline of extraction tank 101, the primary centrifugal clarified liquid outlet pipeline of primary centrifugal clarified liquid tank 103, the primary high solids content bottom liquid output pipeline of primary sedimentation separation tank 105, the primary low solids content clarified liquid output pipeline of primary sedimentation separation tank 105, the secondary low solids content clarified liquid output pipeline of secondary sedimentation separation tank 203, the secondary medium solids content clarified liquid output pipeline of secondary sedimentation separation tank 203, the secondary high solids content bottom liquid output pipeline of secondary sedimentation separation tank 203, and the dry phase mixture output pipeline of dry phase buffer tank 301, to pump the corresponding materials to the corresponding equipment.

[0143] In one embodiment, the primary sedimentation separator 105 is a cylindrical tank. A feed pipe 1053, tangentially arranged along the top of the tank, is provided for feeding material. A vertical empty pipe 1051 is provided along its vertical axis center for introducing nitrogen gas from top to bottom to aerate the tank bottom. Preferably, nitrogen gas is introduced intermittently to aerate the tank bottom. A spiral structure 1052 is provided around the periphery of the vertical empty pipe 1051, allowing the material from the feed pipe 1053 to settle downwards in a swirling flow along its spiral guide at the feed flow velocity. The downward inclination angle of the feed pipe 1053 is consistent with the downward inclination angle of the spiral blades in the spiral structure 1052, and the downward inclination angle is 5-10° (e.g., 7°), forming a swirling downward flow channel.

[0144] In one embodiment, the length of the feed pipe 1053 entering the primary sedimentation separator 105 is 1 / 4 to 1 / 6 of the diameter of the separator, for example, 1 / 5.

[0145] In one embodiment, the pressure inside the primary settling separator 105 is 3-5 kPa, such as 3.5 kPa, 4 kPa and 4.5 kPa; and / or the temperature is 190-230°C, such as 200°C, 210°C and 220°C; and / or the material residence time is 70-90 h, such as 75 h, 80 h and 85 h; and the solids settling velocity is 0.024-0.044 m / h, such as 0.034 m / h.

[0146] Those skilled in the art will understand that the secondary sedimentation separator 203 is a commonly used sedimentation separation device in the art. In one embodiment, the secondary sedimentation separator 203 is a cylindrical tank; a feed inlet is provided at the top of the tank for top-feeding; a nitrogen aeration pipe is provided at the bottom of the tank for periodic aeration of the bottom. In one embodiment, the pressure inside the secondary sedimentation separator 203 is 4-8 kPa, such as 5 kPa, 6 kPa, and 7 kPa; and / or the temperature is 145-180°C, such as 150°C, 160°C, and 170°C; and / or the residence time is 45-55 h, such as 50 h; and the solids settling velocity is 0.11-0.31 m / h, such as 0.21 m / h.

[0147] Those skilled in the art will understand that the primary centrifuge 102 is a commonly used centrifugal device in the art. In one embodiment, the primary centrifuge 102 is a horizontal screw centrifuge LW520×2184-NB, manufactured by Chongqing Jiangbei Machinery Co., Ltd. In one embodiment, the differential speed of the primary centrifuge 102 is 1-28 rpm, such as 5 rpm, 10 rpm, 15 rpm, 20 rpm, and 25 rpm; the rotational speed is 2000-3500 rpm, such as 2500 rpm and 3000 rpm; and the feed temperature is 90-120℃, such as 100℃ and 110℃. It is mainly used to reduce the solid content in the extract, and the ash content is correspondingly reduced.

[0148] Those skilled in the art will understand that the secondary separator 201 is a commonly used separation device in the art. In one embodiment, the secondary separator 201 is a KYDH211SD-23 separator manufactured by Nanjing Oasis Machinery Factory. In one embodiment, the differential speed of the secondary separator 201 is 20-60 rpm, such as 30 rpm, 40 rpm, and 50 rpm; the rotational speed is 6000-6600 rpm, such as 6200 rpm and 6400 rpm; the feed temperature is 90-140℃, such as 100℃, 110℃, 120℃, and 130℃; the feed load is 10 tons / h; the discharge pressure is 0.8 MPa; and the separator dimensions are 1800×1200×1750 mm.

[0149] In one embodiment, a second material conveying pipeline 6 is provided from the outlet of the secondary separated liquid of the secondary separator 201 to the inlet of the extraction tank 101, for returning the secondary separated liquid from the secondary separator 201 to the extraction tank 101 for recycling, thereby further separating out the total solids (ash and catalyst) and reducing the total solids content.

[0150] In one embodiment, a second reflux pipeline 7 is provided from the outlet of the secondary separated clear liquid of the secondary separator 201 to its inlet, for recirculating the secondary separated clear liquid output from the secondary separator 201 back to the secondary separator 201 for further separation of ash and catalyst and other solids. Preferably, a secondary solids content meter 204 is provided on the third material conveying pipeline 8 from the secondary separator 201 to the pipeline mixer 202, and a secondary regulating valve 205 is provided on the second reflux pipeline 7. The secondary solids content meter 204 and the secondary regulating valve 205 are interlocked according to the separation concentration concentration formula, for interlocking and adjusting the opening and closing and the opening degree of the secondary regulating valve 205 according to the solids content of the material (the same as the secondary separated clear liquid output from the secondary separator 201) in the third material conveying pipeline 8 detected by the secondary solids content meter 204, thereby adjusting its reflux flow and its destination.

[0151] In one embodiment, a first reflux pipeline 9 is provided from the outlet of the primary centrifugal clear liquid tank 103 to the inlet of the primary centrifuge 102. This pipeline is used to reflux the primary separated clear liquid output from the primary centrifugal clear liquid tank 103 back to the primary separator 102 for further separation and removal of ash, catalyst, and other solids. Preferably, a primary solids content meter 106 is provided on the fourth material conveying pipeline 10 from the primary centrifugal clear liquid tank 103 to the primary heating furnace 104. A primary regulating valve 107 is provided on the first reflux pipeline 9. The primary solids content meter 106 and the primary regulating valve 107 are interlocked according to the separation concentration concentration formula. Based on the solids content of the material (which is the same as the primary separated clear liquid output from the primary centrifugal clear liquid tank 103) detected by the primary solids content meter 106, the opening and closing and the degree of opening of the primary regulating valve 107 are interlocked to regulate its reflux flow rate and its destination.

[0152] In one embodiment, a fifth material conveying pipeline 11 is provided from the primary low-solids liquid outlet of the primary settling separator 105 to the feed inlet of the secondary low-solids needle coke subunit. This pipeline is used to convey a portion of the primary low-solids liquid from the primary settling separator 105 to the secondary low-solids needle coke subunit for the production of needle coke products when operating conditions are favorable.

[0153] In one embodiment, a sixth material conveying pipeline 12 is provided from the primary low-solids liquid outlet of the primary settling separator 105 to the feed inlet of the secondary medium-solids liquid flash evaporation molding subunit 403. This pipeline is used to convey the primary low-solids liquid from the primary settling separator 105 to the secondary medium-solids liquid flash evaporation molding subunit 403 for flash evaporation molding under normal operating conditions.

[0154] To improve the catalyst separation effect, under abnormal operating conditions, the primary low-solids liquid output from the primary settling separator 105 needs to be mixed again with a scavenging agent for a second-stage settling separation. In one embodiment, a seventh material conveying pipeline 13 is provided from the primary low-solids liquid outlet of the primary settling separator 105 to the feed inlet of the pipeline mixer 202. This pipeline is used to partially convey the primary low-solids liquid from the primary settling separator 105 to the pipeline mixer 202 under abnormal operating conditions, mix it with the scavenging agent, and then send it to the secondary settling separator for further settling separation to further separate the catalyst.

[0155] In one embodiment, the washing oil pipeline is further branched into a washing oil branch pipe, which is connected to the feed inlet of the secondary separator 201. The washing oil branch pipe is used to introduce washing oil to flush the secondary separator 201 and the primary centrifuge 102 when the system is started or stopped, and to introduce washing oil to adjust the concentration of the feed to the secondary separator 201 and the primary centrifuge 102 under abnormal operating conditions.

[0156] The present invention relates to a processing system and method for high-solids coal-based oil residue. This processing method can remove ash and catalyst in two steps, extract asphaltene from the high-solids coal-based oil residue for processing into high-end raw materials to obtain high-grade coal-based asphalt products and needle coke products, thus realizing a circular economy and green environmental protection.

[0157] The processing system and method of the present invention for high-solids coal-based oil residue are also applicable to high-solids oil-based oil residue.

[0158] The present invention will be further illustrated below through specific embodiments.

[0159] Example 1 (S1)

[0160] A certain high-solids coal-based oil residue 1, its composition includes:

[0161] Light oil: 7 wt%; Wash oil: 7 wt%; Asphaltenes: 25.5 wt%; Ash: 29 wt%; Catalyst: 31 wt%; Moisture: 0.3 wt%; Other components <0.2 wt%;

[0162] For the aforementioned high-solids coal-based oil residue 1, the processing method of the present invention is adopted and the following is utilized: Figure 1-2 The processing system shown performs the processing, specifically including the following steps:

[0163] (1) Solvent oil is introduced into the extraction tank 101 to extract the high-solids coal-based oil residue 1 from the feed, and the extracted mixture is output; then the obtained extracted mixture is sent to a primary centrifuge 102 for first-stage centrifugal separation, and a primary centrifugal clear liquid and a primary dry phase are output; then the obtained primary centrifugal clear liquid is sequentially sent to a primary centrifugal clear liquid tank 103, a primary heating furnace 104 and a primary sedimentation separation tank 105 for storage, heating and first-stage sedimentation separation, and a primary low-solids clear liquid and a primary high-solids bottom liquid are output; wherein...

[0164] The solvent oil is obtained by mixing wash oil and heavy oil at a mass ratio of 2.5:1; and the wash oil is wash oil with an extraction distillation range of 230-300℃, water content ≤1wt%, and standard density of 1.07-1.11g / cm³. 3 The normal operating temperature is 30-70℃, chlorine content ≤18mg / l, acid value ≤0.4mg / g, and ash content ≤0.1wt%. The heavy oil is a heavy oil with an extraction distillation range of 210-380℃, moisture ≤1wt%, and standard density of 0.97-1.04g / cm³. 3 The normal operating temperature is 70-130℃, the chlorine content is ≤17mg / l, the acid value is ≤0.4mg / g, and the ash content is ≤0.3wt%.

[0165] The mass ratio of the solvent oil to the high-solids coal-based oil residue is 3:1;

[0166] Continuous extraction is performed, with the feed temperature and extraction temperature of the extraction tank 101 being 115°C and the residence time being 6 hours.

[0167] The conditions for the first stage of centrifugal separation include: a feed temperature of 115℃;

[0168] The conditions for the first-stage sedimentation separation include: a pressure of 4 kPa; a temperature of 210 °C; and a residence time of 80 h.

[0169] The first-stage sedimentation separation adopts, as follows: Figure 2 The primary sedimentation separation tank 105 shown is used for feeding, and the feeding method is to feed from top to bottom in a spiral manner with intermittent aeration at the bottom, with the spiral angle being 7° with the horizontal direction; the intermittent interval is 20 hours.

[0170] The resulting primary separated liquid is heated to 200°C in a primary heating furnace 104;

[0171] (2) The primary high-solids bottom liquid obtained in step (1) is sent to the secondary separator 201 for secondary separation, outputting secondary clear liquid and secondary dry phase; then it is mixed with the capture agent in the pipeline mixer 202, outputting the capture agent mixture; then the obtained capture agent mixture is sent to the secondary settling tank 203 for catalyst capture and then for secondary settling separation, outputting secondary low-solids clear liquid, secondary medium-solids clear liquid and secondary high-solids bottom liquid respectively; wherein

[0172] The conditions for the second-stage separation include: a feed temperature of 115℃;

[0173] The conditions for the second-stage sedimentation separation include: a pressure of 5 kPa, a temperature of 160°C, and a residence time of 48 h.

[0174] The capturing agent is SSA-1;

[0175] The amount of the capturing agent used is 300 ppm;

[0176] (3) The wash oil, the primary dry phase obtained in step (1), and the secondary dry phase obtained in step (2) are respectively sent to the dry phase buffer tank 301, and the primary dry phase and the secondary dry phase are mixed by the introduced wash oil until the dry phase concentration in the resulting dry phase mixture is 52wt%, and the dry phase mixture is output; then the resulting dry phase mixture is sent to the drying and forming device 302 for drying and oil removal, and solid powder is output; wherein,

[0177] The wash oil is the wash oil used in step (1);

[0178] (4) The secondary low solid content liquid obtained in step (2) is sent to the membrane separation device 401 for membrane separation and filtration, and then sent to the needle coke device 402 for needle coke production to obtain needle coke product.

[0179] The secondary solid-containing liquid obtained in step (2) is sent to the secondary solid-containing liquid flash evaporation molding subunit 403 for flash evaporation and molding in sequence to obtain coal-based pitch product.

[0180] Example 2 (S2)

[0181] The high-solids coal-based oil residue 1 was processed according to the processing method of Example 1; the only difference between it and Example 1 is the following:

[0182] In step (1), the first-stage sedimentation separation uses a conventional sedimentation tank (carbon steel storage tank, manufactured by Sichuan Xinfu Petrochemical Equipment Manufacturing Co., Ltd.) for conventional feeding.

[0183] Example 3 (S3)

[0184] The high-solids coal-based oil residue 1 was processed according to the processing method of Example 1; the only difference between it and Example 1 is the following:

[0185] In step (1), the first-stage centrifugal slurry output from the first-stage centrifuge 102 is first returned from the front end to the first-stage centrifuge 102 for recycling. The recycling method is to concentrate the slurry according to the concentration formula. When the solid content of the obtained first-stage centrifugal slurry has not dropped to 5.7wt%, the reflux ratio is automatically adjusted by interlocking to return it from the front end to the first-stage centrifuge 102 for recycling. Until the solid content of the obtained first-stage centrifugal slurry drops to 5.7wt%, it is then sent to the first-stage centrifugal slurry tank 103, the first-stage heating furnace 104 and the first-stage sedimentation separation tank 105 in sequence.

[0186] Example 4 (S4)

[0187] The high-solids coal-based oil residue 1 was processed according to the processing method of Example 1; the only difference between it and Example 1 is the following:

[0188] In step (2), the secondary separated liquid output from the secondary separator 201 is first returned from the front end to the secondary separator 201 for recycling. The recycling method is to recycle and concentrate according to the separation concentration concentration formula. When the solid content of the obtained secondary separated liquid has not dropped to 1.8wt%, the reflux ratio is automatically adjusted by interlocking and it is sent back to the extraction device for recycling. When the solid content of the obtained secondary separated liquid drops to 1.8wt%, it is then sent to the pipeline mixer 202 along with the capture agent.

[0189] Example 5 (S5)

[0190] The high-solids coal-based oil residue 1 was processed according to the processing method of Example 1; the only difference between it and Example 1 is the following:

[0191] In step (1), the first-stage centrifugal filtrate output from the first-stage centrifuge 102 is first returned from the front end to the first-stage centrifuge 102 for recycling. The recycling method is to concentrate the filtrate according to the concentration formula. When the solid content of the obtained first-stage centrifugal filtrate has not dropped to 5.7wt%, the reflux ratio is automatically adjusted by interlocking to return it from the front end to the first-stage centrifuge 102 for recycling. Until the solid content of the obtained first-stage centrifugal filtrate drops to 5.7wt%, it is then sent to the first-stage centrifugal filtrate tank 103, the first-stage heating furnace 104 and the first-stage sedimentation separation tank 105 in sequence.

[0192] In step (2), the secondary separated liquid output from the secondary separator 201 is first returned from the front end to the secondary separator 201 for recycling. The recycling method is to recycle and concentrate according to the separation concentration concentration formula. When the solid content of the obtained secondary separated liquid has not dropped to 1.8wt%, the reflux ratio is automatically adjusted by interlocking and it is sent back to the extraction device for recycling. When the solid content of the obtained secondary separated liquid drops to 1.8wt%, it is then sent to the pipeline mixer 202 along with the capture agent.

[0193] Example 6 (S6)

[0194] The high-solids coal-based oil residue 1 was processed according to the processing method of Example 1; the only difference between it and Example 1 is the following:

[0195] In step (1), the solvent oil is obtained by mixing wash oil and heavy oil at a mass ratio of 2:1; in step (1), the mass ratio of the solvent oil to the high solid content coal-based oil residue is 2.5:1.

[0196] In step (1), the feed temperature and extraction temperature of the extraction tank 101 are 110°C, and the residence time is 8h;

[0197] In step (1), the conditions for the first-stage centrifugal separation include: the feed temperature is 90℃;

[0198] In step (1), the conditions for the first-stage sedimentation separation include: a pressure of 3 kPa and a temperature of 190 °C;

[0199] In step (1), the obtained primary separated liquid is heated to 180°C in primary heating furnace 104;

[0200] In step (2), the conditions for the second-stage separation include: the feed temperature is 90°C;

[0201] In step (2), the conditions for the second-stage sedimentation separation include: a pressure of 4 kPa and a temperature of 145 °C.

[0202] Example 7 (S7)

[0203] The high-solids coal-based oil residue 1 was processed according to the processing method of Example 1; the only difference between it and Example 1 is the following:

[0204] In step (1), the solvent oil is obtained by mixing wash oil and heavy oil in a mass ratio of 3:1;

[0205] In step (1), the mass ratio of the solvent oil to the high-solids coal-based oil residue is 4:1;

[0206] In step (1), the feed temperature and extraction temperature of the extraction tank 101 are 120°C, and the residence time is 8 hours;

[0207] In step (1), the conditions for the first-stage centrifugal separation include: the feed temperature is 120℃;

[0208] In step (1), the conditions for the first-stage sedimentation separation include: a pressure of 5 kPa and a temperature of 230 °C.

[0209] In step (1), the obtained primary separated liquid is heated to 230°C in primary heating furnace 104;

[0210] In step (2), the conditions for the second-stage separation include: the feed temperature is 140℃;

[0211] In step (2), the conditions for the second-stage sedimentation separation include: a pressure of 8 kPa and a temperature of 180 °C.

[0212] Comparative Example 1 (D1)

[0213] The high-solids coal-based oil residue 1 was processed according to the processing method of Example 1; the only difference between it and Example 1 is the following:

[0214] The second-stage separation and second-stage sedimentation separation in step (2) were not performed;

[0215] In step (3), the wash oil and the primary dry phase obtained in step (1) are respectively sent to the dry phase buffer tank 301.

[0216] Comparative Example 2 (D2)

[0217] The high-solids coal-based oil residue 1 was processed according to the processing method of Example 1; the only difference between it and Example 1 is the following:

[0218] In step (1), the extraction mixture was not subjected to the first stage of centrifugation; instead, the first stage of sedimentation was performed directly.

[0219] In step (2), the first-stage high-solids bottom liquid was not subjected to a second-stage separation. Instead, a capture agent was directly added to it and mixed before the second-stage sedimentation separation was carried out.

[0220] No step (3).

[0221] Comparative Example 3 (D3)

[0222] The high-solids coal-based oil residue 1 is processed according to the method in Example 1 of the Specific Embodiments section of CN 110229690 A.

[0223] result:

[0224] The materials obtained in each step of Examples 1-8 (S1-8) and Comparative Examples 1-3 (D1-3) were sampled, analyzed and tested, and the results are shown in Figure 1.

[0225] Table 1 shows the analysis and test results of the materials obtained in each step of S1-8 and D1-3.

[0226]

[0227]

[0228]

[0229] Note: " / " indicates that there is no corresponding step or material, no relevant data, or no change can be detected; "outside grade" and "extra grade" indicate unqualified products or products outside the relevant standards.

[0230] The grading standard for needle coke products is based on the technical specifications for coal-based needle coke (GB / T 32158-2015).

[0231] The grading standards for coal-based pitch products are based on the technical indicators and test methods for coal liquefaction pitch (GB / T38772-2020).

[0232] According to the comparison between Example 1 and Comparative Example 1 and the data in Table 1, compared with Comparative Example 1, Example 1 of the present invention further reduced the solid content through the second-stage separation and second-stage sedimentation separation in step (2), and obtained Grade 1 needle coke product and Grade 1 coal-based pitch product. The grades of needle coke product and coal-based pitch product have been greatly improved, from sub-grade and extra-grade to Grade 1.

[0233] Based on the comparison between Example 1 and Comparative Example 2 and the data in Table 1, it can be seen that, compared with Comparative Example 1 which only performed the first-stage sedimentation separation and added a scavenging agent for the second-stage sedimentation separation, Example 1 of the present invention further reduced the solids content by performing the first-stage centrifugation separation before the first-stage sedimentation separation and the second-stage separation before adding a scavenging agent for the second-stage sedimentation separation. This resulted in the acquisition of Grade 1 needle coke products and Grade 1 coal-based tar pitch products. The grades of both needle coke products and coal-based tar pitch products were significantly improved, from substandard and extra-grade products to Grade 1 products.

[0234] According to the comparison between Example 1 and Comparative Example 3 and the data in Table 1, compared with Comparative Example 3 which uses the method of CN 110229690 A, the processing method of Example 1 of the present invention can better remove ash and catalyst from the high solid content coal-based oil residue 1, and obtain Grade 1 needle coke product and Grade 1 coal-based pitch product. The grades of needle coke product and coal-based pitch product have been greatly improved, from substandard and extra-grade products to Grade 1 products.

[0235] According to the comparison between Example 1 and Example 2 and the data in Table 1, compared with Example 2, Example 1 of the present invention, by setting the feeding method of the first-stage sedimentation separation in step (1) to "feeding from top to bottom in sequence with intermittent aeration at the bottom, with the spiral angle being 7° with the horizontal direction", further improves the effect of the first-stage sedimentation separation, reduces the solid content in the first-stage low-solid-content clear liquid obtained by the first-stage sedimentation separation, and obtains first-grade needle coke product and first-grade coal-based pitch product. The grades of needle coke product and coal-based pitch product are greatly improved, from grade 2 to grade 1.

[0236] According to the comparison between Example 1 and Example 3 and the data in Table 1, compared with Example 1, Example 3 of the present invention further reduces the solid content of the primary separation liquid entering the primary sedimentation separation tank by using the circulation method of the present invention in step (1), and obtains Grade 1 needle coke product and Grade 1 coal-based pitch product.

[0237] According to the comparison between Example 1 and Example 4 and the data in Table 1, compared with Example 1, Example 4 of the present invention further reduces the solid content of the secondary separation liquid entering the secondary settling tank by using the circulation method of the present invention in step (2), and obtains superior needle coke product and superior coal-based pitch product. The grades of needle coke product and coal-based pitch product are greatly improved, from Grade 1 product to superior product.

[0238] According to the comparison between Example 1 and Example 5 and the data in Table 1, compared with Example 1, Example 5 of the present invention further reduces the solid content of the first-stage separation liquid entering the first-stage settling tank and the solid content of the second-stage separation liquid entering the second-stage settling tank by simultaneously using the circulation method of the present invention in steps (1) and (2), thereby obtaining superior needle coke products and superior coal-based pitch products. The grades of both needle coke products and coal-based pitch products have been greatly improved, from Grade 1 to superior grade.

[0239] Based on the comparison between Example 1 and Examples 6 and 7 and the data in Table 1, it can be seen that, compared with Examples 6 and 7, Example 1 of the present invention obtained Grade 1 needle coke product and Grade 1 coal-based pitch product. The grades of both needle coke product and coal-based pitch product have been greatly improved, from Grade 2 to Grade 1.

Claims

1. A processing method for high-solids coal-based oil residue, characterized in that, The processing method includes the following steps: (1) Extract the high-solids coal-based oil residue raw material using solvent oil and output the extraction mixture; then perform the first-stage centrifugation separation on the obtained extraction mixture and output the first-stage centrifugation clear liquid and the first-stage dry phase; then store, heat and perform the first-stage sedimentation separation on the obtained first-stage centrifugation clear liquid and output the first-stage low-solids clear liquid and the first-stage high-solids bottom liquid. (2) Perform a second-stage separation on the first-stage high-solids bottom liquid obtained in step (1) to output the second-stage separated clear liquid and the second-stage dry phase; then add a capture agent to the obtained second-stage separated clear liquid and mix to output the capture agent mixture; then use the obtained capture agent mixture to capture the catalyst and then perform a second-stage sedimentation separation to output the second-stage low-solids clear liquid, the second-stage medium-solids clear liquid and the second-stage high-solids bottom liquid respectively. (3) Use washing oil to blend and mix the primary dry phase obtained in step (1) and the secondary dry phase obtained in step (2) to output the dry phase mixture; then heat and remove oil from the obtained dry phase mixture to output solid powder. (4) The secondary low solid content liquid obtained in step (2) is subjected to membrane separation and filtration and then needle coke production to obtain needle coke product; The secondary solid-containing liquid obtained in step (2) is subjected to flash evaporation and molding in sequence to obtain coal-based pitch products.

2. The processing method according to claim 1, characterized in that, The feeding method for the first stage sedimentation separation is to feed the material from top to bottom in a spiral manner under bottom aeration.

3. The processing method according to claim 2, characterized in that, Bottom aeration is intermittent.

4. The processing method according to claim 2, characterized in that, The helix angle is 5-10° with the horizontal direction.

5. The processing method according to claim 2, characterized in that, Step (2) further includes the following steps: returning the secondary high-solids-content bottom liquid obtained in step (2) from the front end to the second-stage separation for recycling; and / or, The processing method further includes step (5), in which, under abnormal operating conditions, the secondary separation liquid obtained in step (2) is returned from the front end to the extraction in step (1) for recycling; and / or, Step (2) also includes the following steps: the secondary separation liquid obtained in step (2) is returned from the front end to the second stage separation for recycling.

6. The processing method according to any one of claims 1-5, characterized in that, Step (1) also includes the following steps: the first-stage centrifugal clear liquid obtained in step (1) is returned from the front end to the first-stage centrifugal separation for recycling.

7. A processing system for high-solids coal-based oil residue, characterized in that, The processing system includes a primary processing and separation unit, a secondary processing and separation unit, a dry phase processing unit, and a secondary sedimentation separation liquid processing unit, which are connected sequentially by pipelines; wherein... The primary processing and separation unit includes an extraction tank (101), a primary centrifuge (102), a primary centrifugal clarified liquid tank (103), a primary heating furnace (104), and a primary sedimentation separation tank (105), which are connected sequentially by pipelines; wherein, The extraction tank (101) is provided with a feed inlet and is connected to a high solids oil residue feed pipeline. The high solids oil residue feed pipeline is also connected to a solvent oil pipeline for feeding high solids oil residue and solvent oil separately to extract the high solids oil residue and output the extraction mixture. The feed inlet of the first-stage centrifuge (102) is connected to the outlet of the extraction tank (101) to receive the extraction mixture from the extraction tank (101) and perform first-stage centrifugal separation on it, outputting first-stage centrifugal clear liquid and first-stage dry phase, thereby separating out some of the solids contained therein; The inlet of the primary centrifugal clear liquid tank (103) is connected to the primary centrifugal clear liquid outlet of the primary centrifuge (102), and the primary centrifugal clear liquid tank (103), the primary heating furnace (104) and the primary sedimentation separation tank (105) are connected in sequence through pipelines to store, heat and perform first-stage sedimentation separation of the primary centrifugal clear liquid from the primary centrifuge (102) in sequence, and output primary low solid content clear liquid and primary high solid content bottom liquid; The secondary processing and separation unit includes a secondary separator (201), a pipeline mixer (202), and a secondary settling tank (203) connected sequentially by pipelines; wherein, The inlet of the secondary separator (201) is connected to the outlet of the primary high solid content liquid of the primary processing and separation unit, and is used to receive the primary high solid content liquid from the primary processing and separation unit and perform a second-stage separation on it, outputting a secondary separation clear liquid and a secondary dry phase, thereby separating out the ash and catalyst therein; The pipeline mixer (202) is provided with a feed inlet and a reagent addition inlet. Its feed inlet is connected to the secondary separation clear liquid outlet of the secondary separator (201). Its reagent addition inlet is located at its bottom and is connected to a reagent addition pipeline for inputting a capture agent to mix the secondary separation clear liquid received from the secondary separator (201) and outputting a capture agent mixture. The inlet of the secondary settling separator (203) is connected to the outlet of the pipeline mixer (202) to receive and utilize the scavenger mixture from the pipeline mixer (202) for catalyst capture and then perform secondary settling separation, thereby completing the capture and separation of the catalyst. The secondary low-solids clear liquid is output from the upper outlet, the secondary medium-solids clear liquid is output from the middle outlet, and the secondary high-solids bottom liquid is output from the lower outlet, thereby separating the residual catalyst therein. The dry phase processing unit includes a dry phase buffer tank (301) and a drying and forming device (302) connected in sequence by pipelines; wherein, The dry phase buffer tank (301) is provided with a dry phase inlet and an oil phase inlet. Its dry phase inlet is connected to the primary dry phase outlet of the primary processing and separation unit and the secondary dry phase outlet of the secondary processing and separation unit, respectively. Its oil phase inlet is connected to a washing oil pipeline for introducing washing oil to blend and mix the primary dry phase from the primary processing and separation unit and the secondary dry phase from the secondary processing and separation unit, and output dry phase mixture. The inlet of the drying and forming device (302) is connected to the outlet of the dry phase buffer tank (301) for receiving the dry phase mixture from the dry phase buffer tank (301) and heating and removing oil from it to output solid powder. The secondary sedimentation separation liquid processing unit includes a secondary low-solids-content needle-shaped coke sub-unit and a secondary medium-solids-content flash evaporation forming sub-unit (403); wherein... The secondary low-solids-content liquid needle coke subunit includes a membrane separation device (401) and a needle coke device (402) connected in sequence by pipelines. The inlet of the membrane separation device (401) is connected to the secondary low-solids-content liquid outlet of the secondary processing and separation unit, and is used to sequentially perform membrane separation and filtration on the secondary low-solids-content liquid from the secondary processing and separation unit to produce needle coke and obtain needle coke product. The inlet of the secondary solid-containing liquid flash evaporation and molding subunit (403) is connected to the secondary solid-containing liquid outlet of the secondary processing and separation unit, and is used to flash evaporate and mold the secondary solid-containing liquid from the secondary processing and separation unit in sequence to obtain coal-based pitch products.

8. The processing system according to claim 7, characterized in that, The primary settling separator (105) is a cylindrical tank. A feed pipe (1053) is provided at the top of the tank along the tangent of the tank body for feeding. A vertical empty pipe (1051) is provided along the center of its vertical axis for introducing nitrogen from top to bottom to aerate the bottom of the tank. A spiral structure (1052) is provided around the periphery of the vertical empty pipe (1051) for the feed from the feed pipe (1053) to settle downwards in a swirling manner along its spiral guide according to the feed push flow speed. The downward inclination angle of the feed pipe (1053) is consistent with the downward inclination angle of the spiral blades in the spiral structure (1052), and the downward inclination angle is 5-10°, forming a swirling downward flow channel.

9. The processing system according to claim 8, characterized in that, The length of the feed pipe (1053) entering the primary sedimentation separator (105) is 1 / 4 to 1 / 6 of the diameter of the separator.

10. The processing system according to any one of claims 7-9, characterized in that, A first material conveying pipeline (5) is provided from the lower outlet of the secondary settling tank (203) to the inlet of the secondary separator (201) for returning the secondary high-solids bottom liquid from the secondary settling tank (203) to the secondary separator (201) for separation; and / or, A second material conveying pipeline (6) is provided from the outlet of the secondary separated clarified liquid of the secondary separator (201) to the inlet of the extraction tank (101) for recycling the secondary separated clarified liquid from the secondary separator (201) back to the extraction tank (101); and / or, A second reflux line (7) is provided from the outlet of the secondary separated clear liquid of the secondary separator (201) to its inlet, for recycling the secondary separated clear liquid output from the secondary separator (201) back to the secondary separator (201) for further processing.

11. The processing system according to claim 10, characterized in that, A secondary solids content meter (204) is installed on the third material conveying pipeline (8) from the secondary separator (201) to the pipeline mixer (202), and a secondary regulating valve (205) is installed on the second return pipeline (7). The secondary solids content meter (204) and the secondary regulating valve (205) are interlocked according to the separation concentration concentration formula.

12. The processing system according to any one of claims 7-9 and 11, characterized in that, A first reflux pipeline (9) is provided from the outlet of the primary centrifugal clear liquid tank (103) to the inlet of the primary centrifuge (102) for circulating the primary centrifugal clear liquid output from the primary centrifugal clear liquid tank (103) back to the primary centrifuge (102) for processing.

13. The processing system according to claim 12, characterized in that, A primary solids content meter (106) is installed on the fourth material conveying pipeline (10) from the primary centrifugal clear liquid tank (103) to the primary heating furnace (104), and a primary regulating valve (107) is installed on the first reflux pipeline (9). The primary solids content meter (106) and the primary regulating valve (107) are interlocked according to the separation concentration concentration formula.

14. The processing system according to any one of claims 7-9, 11 and 13, characterized in that, A fifth material conveying pipeline (11) is provided from the primary low-solids-content liquid outlet of the primary settling separator (105) to the feed inlet of the secondary low-solids-content needle coke subunit, for conveying the primary low-solids-content liquid from the primary settling separator (105) to the secondary low-solids-content needle coke subunit when operating conditions are optimal; and / or, A sixth material conveying pipeline (12) is provided from the primary low-solids liquid outlet of the primary settling separator (105) to the inlet of the secondary medium-solids liquid flash evaporation forming subunit (403) for conveying the primary low-solids liquid from the primary settling separator (105) to the secondary medium-solids liquid flash evaporation forming subunit (403) under normal operating conditions; and / or, A seventh material conveying pipeline (13) is provided from the outlet of the primary low solid content liquid of the primary sedimentation separator (105) to the inlet of the pipeline mixer (202) for conveying the primary low solid content liquid from the primary sedimentation separator (105) to the pipeline mixer (202) under abnormal operating conditions.

15. The processing system according to claim 14, characterized in that, The washing oil pipeline also branches into washing oil branch pipes, which are connected to the feed inlet of the secondary separator (201) and are used to introduce washing oil to flush the secondary separator (201) and the primary centrifuge (102) when the system is started or stopped, and to introduce washing oil to adjust the concentration of the feed to the secondary separator (201) and the primary centrifuge (102) under abnormal operating conditions.

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